AU2013206605B2 - High load triallate emulsifiable concentrate formulations - Google Patents

High load triallate emulsifiable concentrate formulations Download PDF

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AU2013206605B2
AU2013206605B2 AU2013206605A AU2013206605A AU2013206605B2 AU 2013206605 B2 AU2013206605 B2 AU 2013206605B2 AU 2013206605 A AU2013206605 A AU 2013206605A AU 2013206605 A AU2013206605 A AU 2013206605A AU 2013206605 B2 AU2013206605 B2 AU 2013206605B2
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triallate
formulation
surfactant
emulsifiable concentrate
concentrate formulation
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Ross Rainbird
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Imtrade Australia Pty Ltd
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Imtrade Australia Pty Ltd
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Abstract

28/08/13,jb20105 amended cap specification.docx,269 -269 An emulsifiable concentrate formulation of triallate including: triallate wherein the triallate comprises at least 600 g/L of the emulsifiable concentrate formulation, at least one solid, liquid-containing, or liquid agriculturally acceptable surfactant, and, optionally, at least one agriculturally acceptable solvent; wherein the liquid components of the emulsifiable concentrate formulation from a solubilizing moiety for triallate.

Description

28/08/13,jb20105 amended cap specification.docx, 1 HIGH LOAD TRIALLATE EMULSIFIABLE CONCENTRATE FORMULATIONS FIELD OF THE INVENTION [0001] This invention relates to liquid formulations of the selective herbicide triallate (trichloroallyl N,N diisopropylthiocarbamate). In particular the invention relates to emulsifiable concentrate formulations of triallate that contain a high level of triallate as active agent and to methods of preparing said formulations. [0002] This specification incorporates by reference the entire contents of the specification filed under Australian Provisional Patent Application No. 2012902790 including any and all Appendices thereto, which Appendices form part of that specification. BACKGROUND OF THE INVENTION [0003] Triallate is widely used as a selective pre-emergence herbicide, e.g. for the control of wild oats in cereal crops. Triallate was developed by Monsanto and has been on the market for four decades with no recorded development of weed resistance. The phytotoxic action of triallate in soil is attributed to vapour absorption by shoots of susceptible seedlings. The chemical structure and synthesis of triallate has been described in US 3167571, US 3330821, US 3330643. The use of antidotes/safeners for triallate has been described in US 4303439. Some synergistic herbicidal combinations that include triallate have been described in US 4276079 and WO 2003/047343, while amphiphilic graft copolymer formulations of triallate have been disclosed in US 5753248. Micro-encapsulated formulations of triallate formed by interfacial polycondensation were disclosed in US 4417916.
28/08/13jb20105 amended cap specification.docx,2 -2 [0004] Emulsifiable concentrates of triallate have been sold in Australia and elsewhere under trade names such as Avadex, Avadex BW, Avadex Xtra and Far-GO. Avadex BW has been sold as an emulsifiable concentrate with 400 g/L of triallate. Avadex Xtra has been sold as an emulsifiable concentrate with 500 g/L triallate. Far-GO has been sold as an emulsifiable concentrate with 4 pounds per (US) gallon of triallate (which is equivalent to approx 480 g/L). Granular formulations of triallate have been sold under the trade names Fortress and Buckle, for example, and an aerial granule has been sold under the trade name Avadex Excel 15G. [0005] Many general characteristics of emulsifiable concentrate formulations have been described in US 2003/0072776 (Sun et al., filed July 2001). The Sun specification provides the following teachings about emulsifiers, solvents and optional ingredients. Emulsifiers [00061 The emulsifiers of the emulsifiable concentrates comprise at least one emulsifier, which may be a non-ionic surfactant, an ionic surfactant, or a blend of both types of surfactants. It is also possible that an emulsifier in an emulsifiable concentrate may be a cationic surfactant. Useful non-ionic surfactants are said to include alkoxylated block polymers, alkoxylated alcohols, alkoxylated alkylphenols, alkoxylated amines, alkoxylated amides, alkoxylated fatty esters, alkoxylated oils, fatty esters, alkoxylated fatty acids, sorbitan derivatives, and the like. [0007] Typical ionic surfactants found in emulsifiers include alkylaryl sulfonates; alkylarylsulfonic acids; carboxylated alcohol ethoxylates and alkylphenol ethoxylates; carboxylic acids/fatty acids; diphenyl sulfonate derivatives; olefin sulfonates; phosphate esters; phosphorus organic derivatives; quaternary surfactants; sulfates and sulfonates of oils and fatty acids; sulfates and sulfonates of ethoxylated alkylphenols; sulfates of 28/08/13,jb20105 amended cap specification.docx,3 -3 ethoxylated alcohols; sulfates of fatty esters; sulfonates of dodecyl and tridecylbenzenes; sulfonates of naphthalene and alkyl naphthalene; sulfonates of petroleum; sulfosuccinamates; alkanolamides; alkoxylated amines (with low EO values); sarcosine derived surfactants such as, ammonium lauroyl sarcosinate, and the like. [0008] Preferred emulsifiers may be alkoxylated alcohols and alkyphenols, preferably of from about 4 to about 50 ethylene oxide units and a hydrophobe of from about 4 to about 16 carbon atoms. Other preferred surfactants may be alkylphenol EO/PO block copolymers, e.g., that sold under the trade name WITCONOL NS 108 LQ, and alkoxylated amine salts of ethoxylated alkylphenol sulfates, e.g., that supplied under the trade name WITCOLATE 1335 by Crompton Corporation, Witco Group. [0009] Developing an effective emulsifier package (blend of emulsifiers) requires careful screening of potential emulsifiers (surfactants), conducting emulsion tests according to prescribed methods or established laboratory protocols, and optimizing the performance of the most promising emulsifier(s). The screening of potential emulsifier packages is dependent upon pesticide active type, and solvents. Those skilled in the art of EC technology understand the importance of hydrophilic-lipophilic balance and surfactant choice for such formulations. The emulsifier (surfactant) is preferably present at from about 1 to about 50 weight percent of the emulsifiable concentrate, more preferably from about 3 to about 10 weight percent. Solvents [0010] The selection of a suitable solvent system is made by taking into consideration the solubility of the active(s) and the chemical and toxicological profiles of the solvent(s). The solvents include all EPA approved solvents, and the list of suitable solvents may include aliphatic paraffinic oils, such as kerosene or refined paraffins; aromatic solvents, such as xylenes; C 9
-CI
2 28/08/13,jb20105 amended cap specification.docx,4 -4 aromatic solvents, such as supplied under the trade names AROMATIC 100, 150, and 200 (as sold by Exxon Chemical), ISOPAR L, SOLVESSO 100, 150, and 200; chlorinated hydrocarbons, such as chlorobenzene; alcohols, such as butanol and benzyl alcohol; ketones, such as cyclohexanone and N-methyl pyrollidone; and ethers, such as diethylene glycol and diethoxol. In addition, the solvent may include vegetable oils, methylated vegetable oils, petrol-oils, sugar esters of fatty acids, e.g., sucrose esters, and the like. [0011] Preferred solvents may be C 9
-C
12 hydrocarbon solvents because of their low cost and their ability to solubilize many pesticide toxicants. [0012] Sun teaches that the solvent may be present at from 0 to about 95 weight percent of the emulsifiable concentrate, preferably from about 20 to about 50 weight percent. Optional Ingredients [0013] Other additives may be included in emulsifiable concentrate formulations of triallate at levels less than about 5 weight percent. Such additives can include, for example, an antifreeze, a pH buffer or a finely divided hydrophobic filler. [0014] Sun also teaches that emulsifiable concentrates according to the invention disclosed therein can be diluted with water to a desired level of active ingredients and applied to the targets using suitable means. Typically, according to Sun, the amount of active component in the formulations as applied to targets is from about 1 to about 95 weight percent. [0015] There are a significant number of commercially available formulations of triallate in Australia. They are usually in the form of emulsifiable concentres (EC). Each of the above commercially available triallate EC formulations contains at most 500g/L of triallate active ingredient, 28/08/13,jb20105 amended cap specification.docx,5 -5 which suggests that 500g/L represents an upper practical limit in the amount of triallate that can be packaged in EC form using methods known to the art. [0016] In this specification, the term "solubilising moiety for triallate" is to be taken to refer to any liquid system in which triallate is miscible, including liquid systems that include conventional agriculturally acceptable solvents and also liquid systems that include conventional agriculturally acceptable liquid, or liquid-containing surfactants, provided that triallate dissolves in said liquid system. A solubilising moiety for triallate may contain one, two, or even more liquid components. The weight of a solubilising moiety for triallate is taken to be the sum of weights of liquid components, being the components that are liquid at 20'C, that constitute the solubilising moiety system for triallate. For the avoidance of doubt, if a solubilising moiety for triallate happens to include one or more solubilised solids (e.g., a solid dissolved surfactant), the weight of the solubilising moiety for triallate is taken to be the sum of the weights of the liquid components of the solvent system for triallate, but does not include the weights of non-triallate solid components that may be dissolved. The term "agriculturally acceptable solvent for triallate" is to be taken to refer to solvents for triallate wherein each component of the solvent has been approved for inclusion in an agricultural formulation in at least one country. The term "agriculturally acceptable" means registered or otherwise approved for use in agriculture in at least one country. [0017] The "triallate/solubilising moiety ratio" in a triallate EC, which may be calculated by dividing the weight of triallate active ingredient in a given weight of a triallate EC formulation by the weight of the solubilising moiety for triallate (as defined hereinbefore) in the same weight of the triallate EC formulation, is an important ratio as it affects: 1. The quantity of solvent released to the environment as a consequence of applying a given amount of triallate formulation to a cultivation zone; 28/08/13jb20105 amended cap specification.docx,6 -6 2. The amount of high-quality packaging material that is utilised in carrying a given amount of triallate active ingredient to a cultivation zone; 3. The amount of used packaging material that needs to be recycled or otherwise disposed of after applying a given amount of triallate active ingredient to a cultivation zone; 4. The contact toxicity of triallate EC formulation to a farm worker; 5. The flammability of triallate EC formulation; 6. The vapour pressure of solvent (frequently aromatic hydrocarbon) that is released to air in a given time after a spill has occurred; 7. The weight of goods that must be carried by a farm worker in applying a given amount of triallate active ingredient to a cultivation zone; 8. The cost of freight (volume and weight basis) in transporting the triallate formulation from factory to field; 9. The capacity to demonstrate superior formulation expertise to farmers. [0018] All of the issues mentioned above should be affected advantageously when a given amount of triallate in an EC formulation is associated with a lesser amount of solubilising moiety, i.e., when the triallate/solubilising moiety ratio is greater.
28/08/13,jb20105 amended cap specification.docx,7 -7 [0019] As an illustration of prior art, one may consider a conventional commercial triallate EC formulation consisting of the following ingredients. component parts by weight g/L Triallate 95% technical 526 Aromatic solvent 470 Anionic surfactant (60% solid in 40% 2- 38 ethylhexanol) Non-ionic surfactant (solvent-free solid) 25 [0020] In the above formulation triallate is present at 0.95x526 = 500 parts by weight and solubilising moiety for triallate is present at 470 + 0.4x38 = 485 parts by weight. The triallate/solubilising moiety ratio is 500/485 = 1.03. SUMMARY OF THE INVENTION [0021] According to aspects of the present invention there are provided emulsifiable concentrate formulations of triallate having significantly increased triallate/solubilising moiety ratios which demonstrate significant advantages over previously known and used emulsifiable concentrate formulations of triallate and methods for preparing such emulsifiable concentrate formulations. DESCRIPTION OF INVENTION [0022] According to one aspect of the invention there is provided an emulsifiable concentrate formulation of triallate including: triallate wherein the triallate comprises at least 600 g/L of the emulsifiable concentrate formulation, at least one solid, liquid-containing, or liquid agriculturally acceptable surfactant, and, optionally, at least one agriculturally acceptable solvent; 28/08/13,jb20 105 amended cap specification.docx,8 -8 wherein the liquid components of the emulsifiable concentrate formulation form a solubilizing moiety for triallate. [0023] The triallate may comprise at least 700 g/L of the emulsifiable concentrate formulation. [0024] The triallate may comprise at least 800 g/L of the emulsifiable concentrate formulation. [0025] The triallate may comprise at least 850 g/L of the emulsifiable concentrate formulation. [0026] The triallate may comprise at least 900 g/L of the emulsifiable concentrate formulation. [0027] According to another aspect of the invention there is provided an emulsifiable concentrate formulation of triallate including: triallate, wherein the triallate comprises at least 600 g/L of the emulsifiable concentrate formulation; at least one solid, liquid-containing, or liquid, agriculturally acceptable surfactant; optionally, at least one agriculturally acceptable solvent; wherein the liquid components of the emulsifiable concentrate formulation form a solubilising moiety for triallate, and wherein the triallate/solubilising moiety weight ratio is greater than 2. [0028] According to another aspect of the invention there is provided an emulsifiable concentrate formulation of triallate wherein the triallate/solubilising moiety weight ratio is greater than 4. [0029] According to another aspect of the invention there is provided an emulsifiable concentrate formulation of triallate wherein the triallate/solubilising moiety weight ratio is greater than 6.
28/08/13,jb20105 amended cap specification.docx,9 -9 [0030] According to another aspect of the invention there is provided an emulsifiable concentrate formulation of triallate as discussed above wherein said at least one optional agriculturally acceptable solvent for triallate comprises at least one member of the set consisting of petroleum-based aromatic hydrocarbons, diethyleneglycol monoethyl ether, dimethyl adipate, dimethyl succinate, n-methyl pyrrolidone, and xylene. [0031] An emulsifiable concentrate formulation of triallate as claimed in claim 9 wherein said at least one optional agriculturally acceptable solvent is present in the range of from 0 to 400 g/L of the formulation. [0032] The said at least one optional agriculturally acceptable solvent may be present in the range of from 80 to 200 g/L of the formulation. [0033] The said at least one optional agriculturally acceptable solvent may be present in the range of from 80 to 120 g/L of the formulation. [0034] According to another aspect of the invention there is provided an emulsifiable concentrate formulation of triallate wherein the at least one solid, liquid-containing, or liquid agriculturally acceptable surfactant is at least one of a first surfactant chosen from the set consisting of alkylphenol alkoxylates, fatty acid alkoxylates, alkoxylated triglycerides and EO/PO diblock materials, wherein alkoxylate includes ethoxylate, propoxylate, and mixed ethoxylate-propoxylate, including multi-block ethoxylate/propoxylate materials. [0035] The at least one of a first surfactant may be chosen from the set consisting of nonylphenol EO-PO diblock materials with one block having 7 11 EO (on an average basis) and the other block having 8-12 PO (on an average basis).
28/08/13,jb20105 amended cap specification.doex,10 - 10 [0036] The at least one of a first surfactant may be chosen from the set consisting of alkoxylated triglycerides being alkoxylated castor oils (including castor oil 36 EO (on an average basis) and castor oil 54 EO (on an average basis)), and alkoxylated coconut oils. [0037] The at least one of a first surfactant may be chosen from EO/PO diblock materials having EO block lengths in the range 12-35 and HLB values in the range 5-20. [0038] The at least one of a first surfactant may be present in the range of from 30 to 450 g/L of the formulation. [0039] Alternatively, the at least one of a first surfactant may be present in the range of 30 to 100 g/L of the formulation. [0040] According to another aspect of the invention there is provided an emulsifiable concentrate formulation as disclosed above, wherein the at least one solid, liquid-containing or liquid agriculturally acceptable surfactant includes at least one of a second surfactant chosen from the set consisting of calcium alkylbenzene sulfonic acid in liquid concentrate form, alkylphenol ether sulphate/alkylamine ethoxylate salt, and alcohol ether sulphate/alkylamine ethoxylate salt. [0041] The at least one of a second surfactant may be chosen from the set consisting of calcium alkylbenzene sulfonic acid salt in liquid form wherein the alkyl moiety, which may be straight or branched, is C 8
-C
1 4 alkyl. The alkyl moiety, which may be straight or branched, may be Cio-C 12 alkyl. [0042] The at least one of a second surfactant may be chosen from the set consisting of alkylphenol ether sulphate/alkylamine ethoxylate salt and alcohol ether sulphate/alkylamine ethoxylate salt, wherein the alkylamine moiety is C 14
-C
1 6 alkyl, including tallowamine.
28/08/13,jb20105 amended cap specification.docx,I1 - 11 [0043] The at least one of a second surfactant may be present in the range of from 0 to 120 g/L of the formulation. [0044] The at least one of a second surfactant may be present in the range of from 30 to 100 g/L of the formulation. [0045] The at least one of a second surfactant may be calcium alkylbenzene sulfonic acid, net of solvent, in the range from 15 to 60 g/L of the formulation. [0046] According to another aspect of the present invention there is provided an emulsifiable concentrate formulation of triallate including: triallate, wherein the triallate comprises at least 600 g/L of the emulsifiable concentrate formulation; at least one solid, liquid-containing, or liquid, agriculturally acceptable surfactant; optionally, at least one agriculturally acceptable solvent; wherein the liquid components of the emulsifiable concentrate formulation form a solubilising moiety for triallate, and wherein the triallate/solubilising moiety weight ratio is greater than 2. [0047] The agriculturally acceptable solvent may comprise at least one member of the set consisting of alkane compounds, aromatic compounds, alkylaryl compounds, alcohol-containing compounds, aldehyde-containing compounds, ether-containing compounds, ester-containing compounds, ketone containing compounds, lactam-containing compounds, amide-containing compounds, chlorinated compounds. [0048] The agriculturally acceptable solvent may comprise at least one member of the set consisting of solvent naphtha (petroleum), heavy aromatic fraction, xylene, toluene, pyrrolidones including N-alkylated pryrrolidones such as N-methyl pyrrolidone, cyclohexanone, acetone, glycol ethers such as diethyleneglycol monomethyl ether (including the material sold under the trade name Carbitol), ethyleneglycolmonobutylethers (including the material sold 28/08/13,jb20105 amended cap specification.doex, 12 - 12 under the trade name Butyl Glysolv), propylene glycol monomethyl ether (including the material sold under the trade name Glysolv PM), methanol, ethanol, isopropanol, decanol, paraffins, hexane, acetic acid C 6
-C
8 branched alkyl ester ((including the material sold under the trade name Exxate 700). [0049] An emulsifiable concentrate formulation according to the invention may include at least one agriculturally acceptable surfactant, wherein the cumulative amount (net of carrier solvent) of the at least one agriculturally acceptable surfactants is in the range from 40 to 200 g/L and preferably in the range from 60 to 150 g/L, more preferably, in the range from 80 to 110 g/L. [0050] The at least one agriculturally acceptable surfactant may comprise a non-ionic surfactant. [0051] The at least one agriculturally acceptable non-ionic surfactant may be chosen from the categories in the set consisting of alkoxylated block polymers, alkoxylated alcohols, alkoxylated alkylphenols, alkoxylated amines, alkoxylated amides, alkoxylated fatty esters, alkoxylated oils, fatty esters, alkoxylated fatty acids, sorbitan derivatives. [0052] The at least one agriculturally acceptable non-ionic surfactant may be chosen from the set consisting of nonylphenol ethoxylate (including materials sold under the trade name Teric N9, Teric N15, Teric N30), octylphenol ethoxylate (including materials sold under the trade name Teric X5, Terix X8, Teric X10), alkoxylated alkylphenol (including materials sold under the trade name Termul 200, Orisurf 200), vegetable oil ethoxylate (including materials sold under the trade name Termul 1284, Termul 1285), tristyryl phenol ethoxylates (including material sold under the trade name Termul 3150), alcohol ethoxylates such as tridecyl alcohol -9EO (including material sold under the trade name Teric 13A9), Ci-C 1 4 alcohols reacted with 2 moles EO (including material sold under the trade name Teric 12A2N), block copolymers such as polyoxyethylene/polyoxypropylene block copolymer 28/08/13,jb20105 amended cap specification.docx, 13 - 13 (including materials sold under the trade names Teric PE62, Teric PE64, Teric PE 68), and fatty amine higher-mole ethoxylates (such as tallowamine ethoxylates and oleyl amine ethoxylate) which have non-ionic characteristics such as cloud point and compatibility with anionic surfactants (including materials sold under the trade name Terwet 3780). [0053] Alternatively the at least one agriculturally acceptable surfactant comprises an anionic surfactant. [0054] The at least one agriculturally acceptable anionic surfactant may be chosen from the categories in the set consisting of alkylaryl sulfonates; alkylarylsulfonic acids; carboxylated alcohol ethoxylates and alkylphenol ethoxylates; carboxylic acids/fatty acids; diphenyl sulfonate derivatives; olefin sulfonates; phosphate esters; phosphorus organic derivatives; sulfates and sulfonates of oils and fatty acids; sulfates and sulfonates of ethoxylated alkylphenols; sulfates of ethoxylated alcohols; sulfates of fatty esters; sulfonates of dodecyl and tridecylbenzenes; sulfonates of naphthalene and alkyl naphthalene; sulfonates of petroleum; sulfosuccinamates; alkoxylated amines; sarcosine derived surfactants such as, ammonium lauroyl sarcosinate; alkoxylates as above other than ethoxylates (such a propoxylates, butoxylates). [0055] The at least one agriculturally acceptable anionic surfactant may be chosen from the set consisting of linear and branched alkylbenzenesulphonates and salts thereof which may be provided as a non aqueous solution, (such as calcium Cio-CI 4 alkylbenzenesulfonate) (including materials sold under the trade name NANSA EVM70/2E which is carried in 2 ethylhexanol), alkyl sulphates such as sodium lauryl sulphate (including material sold under the trade name Empicol LX/N), alkyl ether sulfates such as sodium lauryl ether (2EO) sulphate (including material sold under the trade name Emipmin KESX70/AU), alkyl phosphates (including material sold under the trade names Alkanate PA100, Alkanate PG30, and Alkanate PL50), alkyl ether phosphates (including material sold under the trade name Alkanate 28 /08/13jb20105 amended cap specification.docx, 14 - 14 PK100), alkylphenol ether sulfate/tallowamine ethoxylate salts (including materials sold under the trade names Toximul TANS-5, Toximaul TANS-6, Toximul TANS-8, Toximul TANS- 15), and alcohol ether sulphate/tallowamine ethoxylate salts (including materials sold under the trade names Toximul TAABS-5, Toximul TAABS-8). [0056] Alternatively, the at least one agriculturally acceptable surfactant is at least one cationic surfactant such as fatty amine lower-mole ethoxylates (which may be incompatible with anionic surfactants). [0057] Alternatively, the at least one agriculturally acceptable surfactant may be at least one zwitterionic surfactant (i.e., a surfactant which simultaneously carries anionic and cationic charge). Examples of zwitterioninc surfactants include betaine surfactants. [0058] Alternatively, the at least one agriculturally acceptable surfactant may be at least one cationic surfactant and at least one zwitterionic surfactant. [0059] An emulsifiable concentrate formulation of triallate according to the present invention may also contain a perfume, an antifoam, a stenching agent, an embittering agent (the latter two agents to discourage ingestion). [0060] Further, it has been discovered that in some circumstances the amount of agriculturally acceptable solvent can be minimised and even eliminated and that acceptably stable emulsifiable concentrate formulations can still be prepared. Thus, according to another aspect of the present invention there is provided an emulsifiable concentrate formulation of triallate including triallate and a solubilising moiety for triallate, wherein the solubilising moiety for triallate comprises at least one agriculturally acceptable surfactant but not agriculturally acceptable solvent, wherein the loading of triallate in the emulsifiable concentrate formulation is greater than 600 g/L.
28/08/13jb20105 amended cap specification.docx,15 - 15 [0061] The utilizable ranges of agriculturally acceptable solvents and agriculturally acceptable surfactants will vary according to the desired triallate/solvent ratio. The higher the triallate/solvent ratio, the more restricted are the ranges of utilizable agriculturally acceptable solvents and agriculturally acceptable surfactants. [0062] The density of the emulsifiable concentrate is at least 1.05 g/ml, preferably 1.1 g/ml, and more preferably at least 1.15 g/ml. [0063] According to another aspect of the present invention there is provided a method of preparing an emulsifiable concentrate formulation of triallate, including the steps of: adding an agriculturally acceptable solvent for triallate to a clean empty formulation vessel; adding triallate which has been heated above its melting point to the formulation vessel in a series of addition steps each of which addition steps is followed by agitation of the contents of the formulation vessel; adding at least one agriculturally acceptable surfactant and additional agriculturally acceptable solvent, with the latter being used to clear residual surfactant from pumps or process lines used for the addition of the at least one agriculturally acceptable surfactant; agitating the resulting contents of the formulation vessel for at least 30 minutes; abstracting and testing a representative sample of the product according to a testing regime for specific gravity, pH 1% aqueous, emulsion characteristics, foam persistence, and active constituent content. [0064] Formulations incorporating diluted emulsifiable concentrates according to the present invention can be used for selectively killing or suppressing weeds such as wild oats, annual ryegrass, wireweed, phalaris spp, fumitory, cereal oats, sand fescue, silvergrass, wintergrass, paradoxa grass, corn gromwell, rough poppy, bromegrass, barleygrass, Three-cornered Jack, caltrop, yellow burr weed, deadnettle, or speedwell in the presence of crop plants such as wheat, barley, triticale, chickpeas, faba beans, lupins, peas, linseed, canola, and safflower.
28/08/13,jb20105 amended cap specification.docx,16 - 16 [0065] Emulsifiable concentrate formulations according to aspects of the present invention are physically compatible with a range of other agricultural chemical formulations including those supplied under the trade names ChemAg Chlorsulfuron 750, Imtrade Mandate 750 WG Selective Herbicide, Imtrade Trifluralin 480 EC Herbicide, Eradicator 450 MIPA based, Glyphosate 888 WG, MONZA, Roundup Max, Eradicator 540, Eradicator 510, and Glyphosate 360. [0066] The current industry standard at 500 g/L was established by the initial market entrants and maintained for good commercial reasons. Pesticide/herbicide formulations typically enter the market with high profit margins, and often at lower loadings than those which later became industry standards. The profit margins dwarf the savings to be made by raising the active loading. Accordingly, the benefit to cost balance does not exist early in the commercial life of a formulation. Also, typically, subsequent market entrants seek to replicate existing products and therefore introduce formulation variants at the same concentration, because the proposed introduction of formulations at higher concentrations of active ingredient often trigger demands by pesticide/herbicide regulators for more data and/or submissions or arguments for approval, i.e., the regulatory barrier is higher. [0067] One of the advantages of a higher loading product formulation according to the present invention is that lesser quantities of the formulation are required to achieve the same application rate when diluted for application to the crop to be treated. A 900 g/L emulsifiable concentrate is applied at 5/9 of the rate of application of a standard 500 g/L emulsifiable concentrate if the end user applies active ingredient in the same absolute amount per unit of area. Consequently, such a 900 g/L emulsifiable concentrate will pro rata use appreciably less packaging/labelling/storage/transport. There will also be less environmental impact through reduced solvent use.
28/08/13,jb20105 amended cap specification.docx, 17 -17 [0068] Mastering a stable formulation at a loading higher than 500 g/L is difficult. Significant investments in time and materials are required to develop reproducible stable high loading emulsifiable concentrate formulations. DESCRIPTION OF PREFERRED EMBODIMENTS AND EXAMPLES [0069] In order that the present invention may be more readily comprehended, reference is made to the following examples, some of which are preferred embodiments of the present invention. In the examples when a surfactant is presented in the form of a solution (e.g., Ninate 60E, as manufactured by Stefan, comprising calcium alkybenzene sulphonate 60% in solvent, being 2ethylhexanol, 40%), the weight of the surfactant is given as the weight of the surfactant solution. To determine the weight of the surfactant (as distinct from the weight of the surfactant solution) it is necessary to deduct the weight of the solvent from the weight of the surfactant solution. An instance of this can be seen in the first table below, in relation to the anionic solvent. Example 1 [0070] The following triallate emulsifiable concentrate according to the invention was made by mixing the following components. Component Source Parts by Weight (g/L) Triallate 95% technical 947.4 Aromatic solvent 150 Recochem of Perth 106.3 (e.g., Recosol 150) Australia Anionic surfactant e.g., calcium Manufactured by Stepan 76.2
CIO--C
14 alkylbenzenesulfonate (Corresponds to (60% solid in 40% 2-ethylhexanol) 45.7 g solid (e.g., Ninate 60E) surfactant) 28/08/13,jb20105 amended cap specification.docx, 18 - 18 Non-ionic surfactant; e.g., Manufactured by 50.1 alkoxylated alyklyphenol e.g., Huntsman Termul 200. (solvent-free solid) [0071] In the above formulation triallate is present at 0.95x947.4 = 900 parts by weight and solubilising moiety is present at 106.3 + 0.4x76.2 = 136.8 parts by weight. The triallate/solvent ratio is thus 900/136.8 = 6.6 . [0072] In Example 1, the formulation procedure for a 1 0,000L batch, inclusive of quality control measures, was as follows, with the steps being identified numerically as 1.1, 1.2, 1.3 and so on. [0073] 1.1 Ensure formulation vessel is empty and clean. [0074] 1.2 Charge the formulation vessel with solvent as follows with agitator off: 1. Aromatic solvent 150 (e.g., Recosol 150) 800 kg [0075] 1.3 Charge the formulation vessel with active ingredient as follows, with intermittent agitation following the addition of every 1000 kg or so. As triallate 95% technical material has a nominal melting point of the order of 30 0 C, depending on its form, gentle heating may be required to establish a liquid form prior to processing: 2. Triallate 95% Tech 9474 kg [0076] 1.4 Charge the formulation vessel with the surfactants as follows, clearing residual surfactant from any pumps or process lines used with the remaining complement of solvent: 28/08/13,jb20105 amended cap specification.docx,19 - 19 3. Alkylbenzenesulfonic acid, calcium salt in 2-ethylhexanol (e.g., Ninate 60E) 4. Alkoxylated alkylphenol (e.g., Termul 200) 501 kg 5. Aromatic solvent 150 (e.g., Recosol 150) 263 kg [0077] 1.5 Continue agitating for a minimum of 30 minutes following the addition of the last ingredient. [0078] 1.6 Sample approximately IL of product, ensuring it is representative. [0079] 1.7 Sub-sample 250mL from the original 1 L sample, and subject it to the following testing regime. [0080] 1.7.1 Specific gravity (CIPAC MT3. 1) 1.7.2 pH 1% aqueous (CIPAC MT75.3) 1.7.3 Emulsion characteristics (CIPAC MT36.1) 1.7.4 Persistent foam (CIPAC MT47.2) 1.7.5 Active constituent (Triallate) content (using a validated method as disclosed in Appendix 11 hereto, which Appendix forms part of the specification). [0081] 1.8 If the specific gravity is within the bounds of the acceptable range listed in the specification, record the value and proceed to the next test. If the specific gravity is outside of the bounds of the acceptable range listed in the specification, agitate the formulation charge until specific gravity 28/08/13,jb20105 amended cap specification.docx,20 - 20 is constant. If still outside of the bounds of the acceptable range, quarantine the batch for further investigations and possible rework. [0082] 1.9 If the pH 1% aqueous test result is satisfactory, record results and proceed to the next test. If pH 1% aqueous test result is outside the bounds of the acceptable range listed in the specification, quarantine the batch for further investigations and possible rework. [0083] 1.10 If emulsion stability in standard hard water is satisfactory, record results and proceed to the next test. If emulsion stability is outside the bounds of the acceptable range listed in the specification, adjust the contents of surfactants (Alkylbenzenesulfonic acid, calcium salt in 2 ethylhexanol (Ninate 60E) and Alkoxylated alkylphenol (Termul 200)). After suitable agitation time to ensure homogeneity, resample and retest. Repeat adjustment process until emulsion stability is within the bounds of the acceptable range. [0084] 1.11 If persistent foaming characteristics are satisfactory, record results and proceed to the next test. If persistent foaming characteristics are outside the bounds of the acceptable range quarantine the batch for further investigations and possible rework. [0085] 1.12 If the active constituent level is satifactory, record results. If the active constituent level is outside the bounds of the acceptable range listed in the specification, adjust the level accordingly by adding additional aromatic solvent 150 (where the active content is high) or additional triallate active constituent (where the active content is low). After suitable agitation time to ensure homogeneity, resample and retest. Repeat adjustment process until active constituent levels are within the bounds of the acceptable range.
28/08/13,jb20105 amended cap specification.docx,21 -21 [0086] 1.13 Catalogue and store a retention sample of approximately 200g. Tests to Confirm the Suitability of the Formulation of Example 1 [0087] For the test methods identified by the prefix CIPAC, refer to International Pesticides Analytical Council (CIPAC) published methodology. The Brookfield viscometer used for measuring viscosity of this formulation and the other formulations identified in the other Examples and Trials identified in this specification (including in Appendices 1 to 10 to the specification of Australian Provisional Patent Application No. 2012902790) was Brookfield Viscometer Model LVT Serial No. 102809, and the spindle used was Spindle No. 2. The spindle rotation rate was 60 rpm. parameter test method Required outcome Observed outcome appearance visual homogeneous liquid homogeneous liquid assay validated chromatographic 875 - 925 g/L complies method, 98-102% accuracy, linearity R > 0.99 pH (1%) CIPAC MT 75.3 4-10 7.7 Spec Gravity CIPAC MT 3.1 1.00-3.00 1.185 (SG) Emulsion CIPAC MT 47.2 <2 ml cream and < complies characteristics trace oil after 30 min, complete resuspension after 24 hrs Persistent CIPAC MT 47.2 < 60 ml after 1 min 12ml (1 min) foaming cold stability visual no phase separation complies 28/08/13jb20105 amended cap specification.docx,22 - 22 viscosity Brookfield viscometer 0 - 2000 cPs 35 cPs 20 0 C viscosity 5'C Brookfield viscometer 0 - 2000 cPs 80 cPs long term As above, after storage at complies performance 54 0 C for 2 weeks CIPAC MT 46.1 Example 2 [0088] The following triallate emulsifiable concentrate formulation according to the invention was made by mixing the following components. Component Source Parts by Weight (g/L) Triallate 95% technical 806.0 Block co-polymer Manufactured by 170.0 (e.g., Teric PE62) Huntsman Block co-polymer Manufactured by 170.0 (e.g., Teric PE64) Huntsman [0089] In the above formulation triallate is present at 0.95x806.0 = 766 parts by weight. [0090] In Example 2, the formulation of a nominally 1 0,OOOL batch of product, inclusive of quality control measures, is as follows, with the steps being identified numerically as 1.1, 1.2, 1.3, and so on. [0091] 1.1 Ensure formulation vessel is empty and clean. [0092] 1.2 Charge the formulation vessel with surfactant as follows with agitator off (while published melting points for these surfactants have not been provided by the manufacturer, claimed pour points, i.e., the 28/08/13,jb20105 amended cap specification.docx,23 - 23 temperatures at which the material can be poured, are said to be <0 for Teric PE 62 and 9'C for Teric PE64): 1. Block co-polymer (e.g., Teric PE62) 1700 kg 2. Block co-polymer (e.g., Teric PE64) 1700 kg [0093] 1.3 Charge the formulation vessel with active ingredient as follows, with intermittent agitation following the addition of every 1000 kg or so. As triallate 95% technical material has a nominal melting point of the order of 30 0 C, depending on its form, gentle heating may be required to establish a liquid form prior to processing: 3. Triallate 95% Tech 8060 kg [0094] 1.4 Continue agitating for a minimum of 30 minutes following the addition of the last ingredient. [0095] 1.5 Sample approximately IL of product, ensuring it is representative. [0096] 1.6 Sub-sample 250mL from the original IL sample, and subject it to the following testing regime. [0097] 1.6.1 Specific gravity (CIPAC MT3. 1) 1.6.2 pH 1% aqueous (CIPAC MT75.3) 1.6.3 Emulsion characteristics (CIPAC MT36.1) 1.6.4 Persistent foam (CIPAC MT47.2) 28/08/13,jb20105 amended cap specification.docx,24 - 24 1.6.5 Active constituent (Triallate) content (using a validated method as disclosed in Appendix 11 to the specification of Australian Provisional Patent Application No. 2012902790). [0098] 1.7 If the specific gravity is within the bounds of the acceptable range listed in the specification, record the value and proceed to the next test. If the specific gravity is outside of the bounds of the acceptable range listed in the specification, agitate the formulation charge until specific gravity is constant. If still outside of the bounds of the acceptable range, quarantine the batch for further investigations and possible rework. [0099] 1.8 If the pH 1% aqueous test result is satisfactory, record results and proceed to the next test. If pH 1% aqueous test result is outside the bounds of the acceptable range listed in the specification, quarantine the batch for further investigations and possible rework. [0100] 1.9 If emulsion stability in standard hard water is satisfactory, record results and proceed to the next test. If emulsion stability is outside the bounds of the acceptable range listed in the specification, quarantine the batch for further investigations and possible rework. [0101] 1.10 If persistent foaming characteristics are satisfactory, record results and proceed to the next test. If persistent foaming characteristics are outside the bounds of the acceptable range quarantine the batch for further investigations and possible rework. [0102] 1.11 If the active constituent level is satifactory, record results. If the active constituent level is outside the bounds of the acceptable range listed in the specification, adjust the level accordingly by adding additional surfactant (where the active content is high) or additional triallate active constituent (where the active content is low). After suitable agitation 28/08/13,jb20105 amended cap specification.docx,25 - 25 time to ensure homogeneity, resample and retest. Repeat adjustment process until active constituent levels are within the bounds of the acceptable range. [0103] 1.12 Catalogue and store a retention sample of approximately 200g. [0104] 1.13 Generate a certificate of analysis noting results of testing. [0105] The tests to confirm the suitability of the formulation are the same as those identified in the discussion of Example 1. Drawings [0106] Drawings relating to the validation method for the active constituent and illustrating a trial are identified as follows: [0107] Fig. 1 is a chromatogram of a sample identified as Triallate A standard. [0108] Fig. 2 is a chromatogram of a sample identified as Triallate 900EC Validation Blank 1. [0109] Fig. 3 is a chromatogram of a sample identified as Triallate Validation Spike Blank 1. [0110] Fig. 4 is a chromatogram of a sample identified as Triallate 900EC Validation Spike Blank 2. [0111] Fig. 5 is a chromatogram of a sample identified as Triallate 900EC Validation Spike Blank 3.
28/08/13,jb20105 amended cap specification.docx,26 - 26 [0112] Fig. 6 is a chromatogram of a sample identified as Triallate 900EC Validation Linearity 1. [0113] Fig. 7 is a chromatogram of a sample identified as Triallate 900EC Validation Linearity 2. [0114] Fig. 8 is a chromatogram of a sample identified as Triallate 900EC Validation Linearity 3. [0115] Fig. 9 is a chromatogram of a sample identified as Triallate 900EC Validation Linearity 4. [0116] Fig. 10 is a chromatogram of a sample identified as Triallate 900EC Validation Linearity 5. [0117] Fig. 11 is a chromatogram of a sample identified as Triallate 900EC Validation Linearity 6. [0118] Fig. 12 is a chromatogram of a sample identified as Triallate 900EC Validation Precision 1. [0119] Fig. 13 is a chromatogram of a sample identified as Triallate 900EC Validation Precision 2. [0120] Fig. 14 is a chromatogram of a sample identified as Triallate 900EC Validation Precision 3. [0121] Fig. 15 is a chromatogram of a sample identified as Triallate 900EC Validation Precision 4. [0122] Fig. 16 is a chromatogram of a sample identified as Triallate 900EC Validation Precision 5.
28/08/13,jb20105 amended cap specification.docx,27 - 27 [0123] Fig. 17 is a graph of Gas Chromatogram response versus Triallate concentration. [0124] Fig. 18 is a bar graph of herbicide control. Trials [0125] Series of trials were conducted to ascertain suitable solvent surfactant combinations. The triallate used in all trials was triallate 95% technical. Solvents and Surfactants [0126] Table A identifies the solvents used in the trials and contains comments and identifying acronyms (where such were used). TABLE A Name Description Comments Recosol 150 Petroleum-based Equivalent to Solvesso aromatic hydrocarbon 150, also designated distillate fraction R 150, distillation range approx 180 - 210 deg C, flash point approx 66 deg C Recosol 100 Petroleum-based Equivalent to Solvesso aromatic hydrocarbon 100, also designated distillate fraction R100, distillation range approx 160 - 180 deg C, flash point approx 50 deg C 28/08/13,jb20105 amended cap specification.doex,28 -28 Recosol 200 Petroleum-based Equivalent to Solvesso aromatic hydrocarbon 200, also designated distillate fraction R200, distillation range approx 220 plus deg C, flash point approx 100 deg C Butyl Glysolv Ethylene glycol monobutyl ether Ethylene glycol EGMBE, EGME monobutyl ether Diethylene glycol DGME, DGMEE monoethyl ether Dimethyl Succinate Dimethyl Adipate N methyl pyrrolidone NMP Exxate 700 C6-C8 acetate, acetic acid C6-C8 branched alkyl ester toluene xylene acetone Propylene glycol PGME, PGMME monomethyl ether Propylene glycol Diethylene glycol Dipropylene glycol [0127] Table B identifies in general terms the surfactants used in the trials and Table C contains more details on the surfactants, including sources.
28/08/13jb20105 amended cap specification.docx,29 - 29 TABLE B Name General Description Category (A,N,C) A=anionic N=non-ionic C=cationic Termul 200 Nonylphenol alkoxylate N Termul 203 Polypropyleneglycol alkoxylate N Toximul 8320 Butanol alkoxylate N Toximul TANS 5 Low-solvent alkylphenol ether A,N,C sulphate/tallowamine ethoxylated salt Toximul TANS 6 Low-solvent alkylphenol ether A,N,C sulphate/tallowamine ethoxylated salt Toximul TANS 8 Low-solvent alkylphenol ether A,N,C sulphate/tallowamine ethoxylated salt Toximul TANS 15 Low-solvent alkylphenol ether A,N,C sulphate/tallowamine ethoxylated salt Toximul TAABS Low-solvent branched alcohol ether A,N,C 5 sulphate/tallowamine ethoxylated salt Toximul TAABS Low-solvent branched alcohol ether A,N,C 8 sulphate/tallowamine ethoxylated salt NANSA EVM 70 Calcium alkylbenzenesulfonate in 2 A ethylhexyl alcohol Ninate 60E Calcium alkylbenzenesulfonate in 2 A ethylhexyl alcohol Rhodacal 60/BE-C Calcium alkylbenzenesulfonate in 2 A ethylhexyl alcohol 28/08/13,jb20105 amended cap specification.doex,30 - 30 Rhodacal 70 Calcium alkylbenzenesulfonate in 2 A ethylhexyl alcohol Rhodacal 70B Calcium alkylbenzenesulfonate in 2 A ethylhexyl alcohol Kemmat HF60 Calcium dodecyl lbenzenesulfonate A Teric N2 Nonylphenol-2-EO N Teric N8 Nonylphenol-8-EO N Teric N9 Nonylphenol-9-EO N Teric N10 Nonylphenol-10-EO N Teric N13 Nonylphenol-13-EO N Teric N15 Nonylphenol-15-EO N Teric N20 Nonylphenol-20-EO N Teric N30 Nonylphenol-30-EO N Termul 1284 Castor oil-36-EO N Termul 1285 Castor oil-54-EO N Teric PE62 EO/PO block copolymer N Teric PE64 EO/PO block copolymer N Teric PE68 EO/PO block copolymer N Makon TSP 16 Tristyryl- 1 6-EO N Pluronic PE 6400 PE/PO/PE block copol N Pluronic PE 6800 PE/PO/PE block copol
N
28/08/13,jb20105 amended cap specification.docx,31 -31 TABLE C Name Termul 200 Nonylphenol 9 EO/i OPO, HLB 16.1, solid Orisurf 200 Equivalent to Termul 200 Termul 203 Alcohol alkoxylate, HLB 17.5 PO-EO-PO triblock, 35PO-25EO-30PO Toximul 8320 Stepan, Butyl EO/PO block, HLB 12 Toximul TANS 5 Stepan, HLB 8. Ether sulphate component is anionic, tallowamine ethoxylate can be non-ionic or cationic depending on pH and chemical environment Toximul TANS 6 Stepan, HLB. 10 Ether sulphate component is anionic, tallowamine ethoxylate can be non-ionic or cationic depending on pH and chemical environment Toximul TANS 8 Stepan, HLB 12. Ether sulphate component is anionic, tallowamine ethoxylate can be non-ionic or cationic depending on pH and chemical environment Toximul TANS 15 Stepan, HLB 14. Ether sulphate component is anionic, tallowamine ethoxylate can be non-ionic or cationic depending on pH and chemical environment Toximul TAABS 5 Stepan, class of anionic detergent blend. Ether sulphate component is anionic, tallowamine ethoxylate can be non-ionic or cationic depending on pH and chemical environment Toximul TAABS 8 Stepan, class of anionic detergent blend. Ether sulphate component is anionic, tallowamine ethoxylate can be non-ionic or cationic depending on pH and chemical environment. NANSA EVM 70 Linear alkylate 70% active may be in various solvents such as isobutanol or 2-ethyl hexanol Ninate 60E Stepan, 60% active linear calcium alkylbenzenesulfonate in 2-ethylhexanol, 60% active 28/08/13,jb20105 amended cap specification.docx,32 -32 Rhodacal 60/BE-C Rhodia, mixture of linear dodecylbenzene sulfonate calcium salt, 60% active Rhodacal 70 Rhodia, branched dodecylbenzene sulfonate calcium salt, 70% active Rhodacal 70B Rhodia, mixture of linear dodecylbenzene sulfonate calcium salt, 70% active Kemmat HF60 Handan Xindiya, calcium dodecylbenzene sulfonate 60% active Teric N2 Huntsman nonylphenolethoxlate Teric N8 Huntsman nonylphenolethoxlate Teric N9 Huntsman nonylphenolethoxlate Teric N 10 Huntsman nonylphenolethoxlate Teric N 13 Huntsman nonylphenolethoxlate Teric N15 Huntsman nonylphenolethoxlate Teric N20 Huntsman nonylphenolethoxlate Teric N30 Huntsman nonylphenolethoxlate Termul 1284 Huntsman, paste, HLB 12.6 Termul 1285 Huntsman, paste, HLB 14.4 Teric PE62 Huntsman PE/PO diblock copol 17 moles EO, HLB 7 Teric PE64 Huntsman PE/PO diblock copol, 25 moles EO, HLB 15 Teric PE68 Huntsman PE/PO diblock copol, 150 moles EO, HLB 29 Makon TSP 16 Stepan, HLB 13 Pluronic PE 6400 BASF, triblock copol PE/PO/PE, 1750 g/mol polypropylene glycol block, 40% polyethyleneglycol in molecule Pluronic PE 6800 BASF, triblock copol PE/PO/PE,1750 g/mol polypropylene glycol block, 80% polyethyleneglycol in molecule 28/08/13,jb20105 amended cap specification.docx,33 - 33 Varying Non-Ionic Surfactant and Surfactant Ratio [0128] In this set of trials all triallate formulations contained triallate at a loading of 900 g/L. In each formulation as trialled, a single anionic surfactant was used, namely that supplied under the trade name Ninate 60E (calcium C10
C
16 alkylbenzenesulfonate, linear, CAS# 68584-23-6, as 60% in 2-ethyl hexanol, supplied by Stepan). In each formulation of these trials, a single solvent was used, namely, Recosol 150 (solvent naphtha, heavy aromatic, CAS #64742-94-5, supplied by Recochem, Perth, Australia). [0129] A range of non-ionic surfactants was used in this set of trials as follows, with the surfactant being identified initially by the trade name under which it was supplied: Termul 200 (alkylphenol poly-ether EO/PO (ethyleneoxide/propylene oxide) block copolymer, 9 mol EO, 10 mol PO, CAS #37251-69-7 CHECK, HLB=16.1, manufactured by Huntsman), Teric N2 (nonylphenol 2-EO, HLB=5.7, manufactured by Huntsman), Teric N8 (nonylphenol 8-EO, HLB=12.3, manufactured by Huntsman), Teric N13 (nonylphenol 13-EO, HLB=14.4, manufactured by Huntsman), Teric N20 (nonylphenol 20-EO, HLB=16, manufactured by Huntsman), Termul 1284 (castor oil PEG 36 CAS #61791-12-6, HLB=12.6, manufactured by Huntsman), Termul 1285 (castor oil PEG 54 (polyethylene glycol) CAS #61791-12-6, HLB=14.4, manufactured by Huntsman), Teric PE62 (EO/PO block copolymer, 17 moles EO, HLB = 7, CAS # 9003-11-6, manufactured by Huntsman), Teric PE64 (EO/PO block copolymer, 25 Moles EO, HLB = 15, CAS # 9003-11-6, manufactured by Huntsman), 28/08/13,jb20105 amended cap specification.docx,34 -34 Teric PE 68 (EO/PO block copolymer, 150 Moles EO, HLB = 29, CAS # 9003-11-6, manufactured by Huntsman), TSP 16 (tristyrylphenol ethoxylate, HLB = 13, CAS #99734-09-5, manufactured by Stepan company), Pluronic PE 6400 (PE/PO/PE block copol, PO block mol wt 1750, 40% PE in molecule, contains CAS # 9003-11-6, HLB=15, manufactured by BASF), Pluronic PE 6800 (PE/PO/PE block copol, PO block mol wt 1750, 80% PE in molecule, contains CAS # 9003-11-6, HLB=29, manufactured by BASF), and Termul 203 (alcohol alkoxylate, HLB 17.5, manufactured by Huntsman). [0130] Three ratios of anionic to non-ionic surfactants were investigated for each different non-ionic surfactant. These ratios were 90:10, 60:40 and 30:70 respectively. More details of these trials are set out in Appendix 1 to the specification of Australian Provisional Patent Application No. 2012902790. [0131] All formulations failed in terms of emulsion stability or cold temperature stability except for the following formulations: Triallate 900 g/L, Recosol 150 106 g/L, Ninate 60E 76 g/L, Termul 200 50 g/L. [0132] In the following Tables, which summarise the results of the trials, the following indicators apply: E - Emulsion characteristics ascertained at 5% aq. CTS - Cold temp stability assessed at 2'C HLB - Hydrophilic Lipophilic Balance P- Pass F- Fail 28/08/13,jb20105 amended cap specification.docx,35 - 35 TABLE 1 Trial using different non-ionic surfactants at varying surfactant ratio (Control: Termul 200 as non-ionic surfactant Loading of Triallate: 900 g/L (approx.) Anionic Surfactant: Ninate 60E Solvent: R150) Summary 30:70 60:40 90:10 A. Alkoxylated alkyl phenol of Results (a) (b) (c) Code Trade Name E CTS E CTS E CTS Al Termul 200 PASS F P P P F P B. Nonyl Phenol ethoxylates Code Trade Name E CTS E CTS E CTS B3 Teric N2 FAIL F P F P F P B4 Teric N8 FAIL F P F P F P B5 Teric N13 FAIL F F F P F P B6 Teric N20 FAIL F P F P F P C. Castor Oil Ethoxylates Code Trade Name E CTS E CTS E CTS C7 Termul 1284 FAIL P F P F F P C8 Termul 1285 FAIL P F P F F P 28/08/13,jb20105 amended cap specification.docx,36 - 36 D. Block Co-polymer Code Trade Name E CTS E CTS E CTS D9 PE62 FAIL F P F F F P DI0 PE64 FAIL F P F P F P Dl PE68 FAIL F F F F D12 TSP16 FAIL F F P F D13 PE6400 FAIL F F F D14 PE6800 FAIL F F F D15 Termul 203 FAIL F F F P F P Varying Anionic Surfactant [0133] Formulations using a non-ionic surfactant (such as that supplied under the trade name Termul 200) and differing anionic surfactant, being ether calcium alkyl benzyl sulphonate, alkyl phenol ether sulphonate, or branched alcohol ether sulphate, were prepared. The anionic surfactants used have the following HLB values: Nansa EVM 70/2E, HLB=9, Rhodacal 70, HLB=8.6; Rhodacal 70B, HLB=8.6; Toximul TAABS 5, HLB=9, Toximul TAABS 8, HLB=10. More details of these trials are set out in Appendix 2 to the specification of Australian Provisional Patent Application No. 2012902790. At a loading of 900 g/L of triallate most of the formulations gave satisfactory results for emulsion characteristics but unsatisfactory results for cold temperature stability.
28/08/13,jb20105 amended cap specification.docx,37 -37 TABLE 2 Trial using different anionic surfactants at constant surfactant ratio (Control: Ninate 60E as anionic surfactant Termul 200 as Non-ionic Surfactant R150 as solvent) Loading of Triallate: 900 g/L A. Calcium Alkylbenzene Summary 60:40 Sulphonate of Results (b) Code Trade Name E CTS IEI Nansa EVM 70/2E Pass P P IF1 Rhodacal 70 Pass P P IGI Rhodacal 70B Pass P P B. Alkyl phenol ether sulphate / Summary 60:40 tallowamine ethoxylated salts of Results (b) Code Trade Name E CTS IH 1 Toximul TANS 5 Fail P F III Toximul TANS 6 Fail P F MI. I Toximul TANS 8 Fail P F C. Branched alcohol ether sulphate/tallowamine ethoxylated salts Code Trade Name E CTS IKI Toximul TAABS 5 Fail P F ILI Toximul TAABS 8 Fail P F 28/08/13,jb20105 amended cap specification.docx,38 -38 Varying Loading Only [0134] In each formulation of this set of trials, the anionic surfactant was Ninate 60E, and the non-ionic surfactant was Termul 200, and the ratio of these surfactants was 60:40. The solvent was Recosol 150. More details of these trials are set out in Appendix 3 to the specification of Australian Provisional Patent Application No. 2012902790. [0135] The formulations contained loadings of 1050 g/L, 1000 g/L, and 950 g/L triallate respectively, and none were found to be stable. This may indicate that 900 g/L may be an upper triallate limit for the invention. TABLE3 Trial using Termul 200 and Ninate 60E surfactants at varying Triallate concentration (Control: Termul 200 as non-ionic surfactant Anionic Surfactant: Ninate 60E Solvent: R150) Summary 60:40 A. Alkoxylated alkyl phenol of Results Code Trade Name E CTS Eta Termul 200 (Triallate 1050) FAIL F 1ib Termul 200 (Triallate 1000) FAIL F Termul 200 (Triallate 950) FAIL
F
28/08/13,jb20105 amended cap specification.docx,39 -39 Varying Solvent [0136] In this set of trials all triallate formulations contained triallate at a loading of 900 g/L. Throughout this set of the trials, the anionic surfactant was Ninate 60E, and the non-ionic surfactant was Termul 200. The surfactant ratio was 60:40. The solvents used in these trials were, as identified by their trade names (where applicable): Recosol 150, Recosol 200, Xylene, toluene, dimethyl adipate, NMP (Nmethylpryrrolidone), and DGME (diethyleneglycolmonoethylether). Recosol solvents are graded and identified according to their minimum flashpoints in Fahrenheit. More details of these trials are set out in Appendix 4 to the specification of Australian Provisional Patent Application No. 2012902790. [0137] Satisfactory formulations were obtained with the solvents Recosol 150, xylene, dimethyl adipate, NMP and DGME. It therefore appears that high loading triallate formulations according to the present invention can be made with a range of common agricultural solvents. TABLE 4 Trials using different solvents at constant surfactant ratio (Control: Termul 200 as non-ionic surfactant; Ninate 60E as Anionic Surfactant; Solvent as R150) Loading of Triallate: 900 g/L Summary 60:40 A. solvents used of Results Code Trade Name E CTS IAl Recosol 150 PASS P P IIAl Recosol 200 FAIL P F 28/08/13,jb20105 amended cap specification.docx,40 -40 IIIA1 Xylene PASS P P IVAl Toluene FAIL P F VAl Dimethyl adipate PASS P P VIAl NMP PASS P P VIIAl DGME PASS P P Varying Loading and Non-Ionic Surfactant [0138] Triallate loadings were set at 850 g/L and 800 g/L. The anionic surfactant was that identified as Ninate 60E and the solvent was Recosol 150 solvent. Termul 1284 and Termul 1285 are castor oil ethoxylates. More details of these trials are set out in Appendix 5 to the specification of Australian Provisional Patent Application No. 2012902790. [0139] Termul 1285 provided satisfactory 800 g/L and 850 g/L triallate loading formulations at both 30:70 and 60:40 ratios. However, Termul 1284 provided satisfactory 800 g/L and 850 g/L triallate loading formulations at 60:40 ratio only. Termul 1284 and Termul 1285 differ in the degree of ethoxylation of the castor oil parent material on which they are based, with Termul 1285 being more highly ethoxylated than Termul 1284.
28/08/13,jb20105 amended cap specification.docx,41 -41 TABLE 5 Trial using Termul 1284 and Termul 1285 against Ninate 60E surfactants at varying Triallate concentration (Control: Termul 200 as non-ionic surfactant Anionic Surfactant: Ninate 60E Solvent: R150) Target surfactant systems HLB: 11 - 14 Summary 30:70 60:40 A. Castor Oil Ethoxylates of Results (a) (b) Trade Name of Surfactant and E CTS E CTS Code Triallate Loading E4i Termul 1284 (Triallate 850) PASS F P P P E4ii Termul 1284 (Triallate 800) PASS F P P P E4iii Termul 1285 (Triallate 850) PASS P P P P E4iv ITermul 1285 (Triallate 800) PASS P P P P Varying Anionic Surfactant and Loading [0140] In this set of trials all triallate formulations contained triallate at a loading of 900 g/L. In each formulation of the trials, a single non-ionic surfactant was used: Termul 200 (alkylphenol poly-ether EO/PO block copolymer, 9 mol EO, 10 mol PO, CAS #37251-69-7 CHECK, manufactured by Huntsman and distributed by ISM, Perth). In each formulation in this set of trials, a single solvent was used, namely, Recosol 150. The reference anionic surfactant was that supplied under the trade name Ninate 60E. More details of these trials are set out in Appendix 6 to the specification of Australian Provisional Patent Application No. 2012902790.
28/08/13,jb20105 amended cap specification.docx,42 - 42 [0141] The alternative anionic surfactants used were those identified by the trade names as follows: Nansa EVM 70/2E (calcium Cio-C 1 4 linear alkyl benzene sulphonate, 70% in 2-ethylhexanol, CAS # 90194-26-6, supplied by Huntsman), Rhodacal 70 (calcium alkylbenzene sulphonate, branched, 70% in solvent, supplied by Rhodia), Rhodacal 70B (calcium alkylbenzene sulphonate, linear, 70% in solvent, supplied by Rhodia), Toximul TANS 5 (alkylphenol ether sulphate/tallowamine ethoxylate, HLB 8, supplied by Stepan), Toximul TANS 6 (alkylphenol ether sulphate/tallowamine ethoxylate, HLB 10, supplied by Stepan), Toximul TANS 8 (alkylphenol ether sulphate/tallowamine ethoxylate, HLB 12, supplied by Stepan), Toximul TAABS 5 (branched alcohol ether sulphate/tallowamine ethoxylated salts, supplied by Stepan), and Toximul TAABS 8 (branched alcohol ether sulphate/tallowamine ethoxylated salts, supplied by Stepan). [0142] Throughout this set of trials, the ratio of anionic to non-ionic surfactants was fixed at 60:40. [0143] All formulations in this set of trials failed in terms of emulsion stability or cold temperature stability aside from the calcium alkylbenzene sulphonate type. This suggests that a formulation of 900 g/L triallate can only be achieved with a relatively narrow selection of surfactant combinations. Based on the results of the trials, a 900 g/L triallate formulation could only be obtained when the anionic surfactant was calcium alkylbenzene sulphonate type, and the non-ionic surfactant was Termul 200, and the ratio of surfactants was 60:40.
28/08/13jb20105 amended cap specification.docx,43 - 43 [0144] Triallate loadings were set at 800 g/L and 700 g/L. The non-ionic surfactant was that identified as Termul 200, and the ratio of anionic to non ionic surfactants was set at 60:40. [0145] The calcium alkylbenzenesulfonate family (Kemmat, Nansa, Rhodacal) were all effective at triallate loadings of 800 g/L and 700 g/L. Toximal TANS 5 and Toximal TANS 6 were effective at triallate loadings of 800 g/L and 700 g/L, as was Toximul TAABS 5. Other anionic surfactants were effective at one triallate loading but not the other. TABLE 6 Trial using different anionic surfactants at constant surfactant ratio (Control: Ninate 60E as anionic surfactant Termul 200 as Non-ionic Surfactant R150 as solvent) A. Calcium Alkylbenzene Summary 800 g/L 700 g/L Sulphonate of Results Code Trade Name E CTS E CTS 9A Kemmat HF60 Pass P P P P 9B Nansa EVM 70/2E Pass P P P P 9C Rhodacal 70 Pass P P P P 91) Rhodacal 70B Pass P P P P 28/08/13,jb20105 amended cap specification.docx,44 - 44 B. Alkyl phenol ether sulphate / Summary tallowamine ethoxylated salts of Results Code Trade Name E CTS E CTS 9E Toximul TANS 5 Pass P P P P 9F Toximul TANS 6 Pass P P P P 9G Toximul TANS 8 Pass P P F P C. Branched alcohol ether sulphate/tallowamine ethoxylated salts Code Trade Name E CTS E CTS 911 Toximul TAABS 5 Pass P P P P 91 Toximul TAABS 8 Fail F P F P Varying Non-Ionic Surfactants within Desired Hydrophilic-Lipophilic Balance Values [0146] Formulations using anionic surfactant, being calcium alkyl benzyl sulphonate (as supplied under the trade mark Ninate 60E) and non-ionic surfactant (such as those supplied under the trade name PE62, PE64, PE68, or TSP 16), combinations to achieve desired hydrophilic lipophilic balance (HLB) values, and a solvent, were prepared with varying loadings of triallate. For preferred formulations the system HLB is in the range 11-14, built up from components with HLBs identified previously. The ratio of anionic (Ninate) to total non-ionic (sum of 2 components) was 60:40. More details of these trials are set out in Appendix 7 to the specification of Australian Provisional Patent Application No. 2012902790. All formulations with mixed non-ionic components failed. All gave unsatisfactory results in terms of cold temperature stability characteristics and emulsion characteristics.
28/08/13,jb20105 amended cap specification.docx,45 -45 TABLE 7 Trial using non-ionic surfactant - Block Co-polymer combo - (Teric PE62 and Teric PE64) with varying Triallate concentration (Control: Termul 200 as non-ionic surfactant Ninate 60E as anionic surfactant Recosol 150 as Solvent) Target surfactant system HLB: 11 - 14 A. Castor Oil Ethoxylates Summary and/or Block-Copolymers of Results Loading of Triallate and E CTS Code Trade Names of Surfactants E6a Triallate 900 (PE62 : PE64) FAIL F F E6b Triallate 900 (PE62 : PE68) FAIL F F E6c Triallate 900 (PE62 : TSP16) FAIL F F E6d Triallate 850 (PE62 : PE64) FAIL F F E6e Triallate 800 (PE 62 : PE64) FAIL F F E6f Triallate 800 (PE 62 : PE68) FAIL F F E6g Triallate 800 (PE62 : TSP16) FAIL F F Combinations of Varying Non-Ionic Surfactant at Different Fixed Surfactant Ratios [0147] At loadings of about 900 g/L of triallate, and using varying combinations of anionic surfactant, being calcium alkyl benzyl sulphonate (supplied under the trade name Ninate 60E) and a blend of non-ionic surfactants, being nonyl phenol ethoxylates in varying combinations, unsatisfactory outcomes in terms of cold temperature stability resulted. One non-ionic surfactant was that identified by the trade name Teric N2, while the other was chosen from the group consisting of higher Teric N surfactants.
28/08/13,jb20105 amended cap specification.docx,46 - 46 More details of these trials are set out in Appendix 8 to the specification of Australian Provisional Patent Application No. 2012902790. TABLE8 Trial using different non-ionic surfactants of Teric N series at varying surfactant ratio against Ninate 60E (Control: Termul 200 as non-ionic surfactant Loading of Triallate: 900 g/L Anionic Surfactant: Ninate 60E Solvent: R150: 105 g/L) A. Nonyl Phenol ethoxylates Ninate:Teric combo Summary (surfactant ratio at 30:70) of Results Code Trade Name E CTS N60E (38 g/L): Teric N2 (25 g/L): FAIL P F Ea Teric N8 (64 g/L) FI N60E (38 g/L): Teric N2 (35 g/L): FAIL P F E3b Teric N8 (54 g/L) N60E (37 g/L): Teric N2 (36 g/L): FAIL F F E3c Teric N13 (53 g/L) N60E (39 g/L): Teric N2 (53 g/L): FAIL F F E3d Teric N20 (37 g/L) B. Nonyl Phenol ethoxylates Ninate: Teric combo (surfactant ratio at 60:40) N60E (75 g/L): Teric N2 (38 g/L): FAIL F F E3e Teric N8 (14 g/L) N60E (77 g/L): Teric N2 (41 g/L): FAIL F F E3f Teric N8 (12 g/L) N60E (77 g/L): Teric N2 (43 g/L): FAIL F F E3g Teric N13 (11 g/L) 28/08/13,jb20105 amended cap specification.doex,47 - 47 N60E (77 g/L): Teric N2 (44 g/L): FAIL F F E3h Teric N13 (8 g/L) N60E (76 g/L): Teric N2 (45 g/L): FAIL F F E3i Teric N20 (9 g/L) N60E (76 g/L): Teric N2 (46 g/L): FAIL F F E3j Teric N20 (5 g/L) Varying Non-Ionic Surfactants in Absence of Conventional Agriculturally Acceptable Solvent [0148] Trials using anionic surfactant, being calcium alkyl benzyl sulphonate (supplied under the trade name Ninate 60E), and non-ionic surfactant, being Block Co-polymer (such as that supplied under the trade names PE62 or PE63), without using any agriculturally acceptable solvents and varying the triallate loading from 700 g/L to 900 g/L, gave unsatisfactory results in terms of cold temperature stability for a 900 g/L loading but satisfactory results for 700 g/L and 800 g/L triallate loading. More details of these trials are set out in Appendix 9 to the specification of Australian Provisional Patent Application No. 2012902790. TABLE 9 Trial using Teric PE62 and Teric PE64 surfactants at varying Triallate concentrations, with no solvent and no anionic surfactant (Control: Termul 200 as non-ionic surfactant Ninate 60E as anionic surfactant Recosol 150 as Solvent) Summary A. Block Co-polymer of Results Loading of Triallate and E CTS Code Surfactant 28/08/13,jb20105 amended cap specification.docx,48 -48 Triallate 900 g/L E5a Teric PE62 at 256 g/L FAIL F F Triallate 900 g/L E5b Teric PE64 at 256 g/L FAIL F F Triallate 800 g/L E5c Teric PE62 at 339 g/L Pass P P Triallate 800 g/L E5d Teric PE64 at 344 g/L Pass P P Triallate 700 g/L E5e Teric PE62 at 428 g/L Pass P P Triallate 700 g/L E5f. Teric PE64 at 433 g/L Pass P P Minimal-Solvent Formulations [0149] Formulations containing minimal quantities of solvents derived from the anionic surfactant compound, being calcium alkyl benzyl sulphonate (as supplied under the trade name Ninate 60E) and non-ionic surfactants, being block co-polymers (as supplied under the trade names Teric PE62, Teric PE64 and Termul 203) and varying the loading of triallate from 700 g/L to 850 g/L. Only solvents included as part of the anionic surfactant were included. Triallate loadings of 850, 800 and 700 g/L were explored. The solvent-free surfactants used as components were those identified by the trade names: PE62, PE64 and Termul 203. Binary and tertiary combinations of these components were explored. More details of these trials are set out in Appendix 10 to the specification of Australian Provisional Patent Application No. 2012902790. [0150] At a loading of 850 g/L triallate, satisfactory results were achieved in terms of cold temperature stability but not in terms of emulsion characteristics for some block co-polymer combinations. At a loading of 800 g/L triallate, satisfactory results were achieved in terms of cold temperature 28/08/13,jb20105 amended cap specification.docx,49 -49 stability and emulsion characteristics for some block co-polymers and block co-polymer combinations, but not for another block co-polymer, and the block co-polymer-non-ionic surfactant combinations used. [0151] At a loading of 700 g/L triallate, satisfactory results in terms of cold temperature stability and emulsion characteristics were achieved using some block co-polymers, and a block co-polymer combination, but not for combinations of the anionic surfactant-block-copolymer combination. At 800 and 700 g/L triallate loading, formulations were obtained where the PE surfactant series (EO/PO block copolymer), and blends thereof, acted as solvent as well as surfactant. TABLE 10 Trials of minimal-solvent formulation using block co-polymer - Termul 203, Teric PE62 and Teric PE64 surfactants at varying Triallate concentration (Control: Termul 200 as non-ionic surfactant Ninate 60E as anionic surfactant Recosol 150 as Solvent) Target surfactant system HLB: 11 - 14 Trial 850 g/L Triallate loading 800 g/L Triallate loading 700 g/L Triallate loading (Surfactants Summary of Results Summary of Results Summary of Results identified by Trade Names) Code E CTS Code E CTS Code E CTS PE 62 E6a FAIL F P E7a FAIL F P E8a PASS P P PE 64 E6b FAIL n/a F E7b PASS P P E8b PASS P P PE 62:PE 64 F P (50:50) E6c FAIL P PASS P PB 62:PE 64 FP ( 2: E FAIL P PASS P E PASS P P Termul 203 Eoe FAIL n/a F E7e FAIL n/a F EMe FAIL n/a F Termul 203:E FAIL n/a F F 62:PE 64 (10:27:63) E6 f IL F E9 F I P FAI P 28/08/13,jb20105 amended cap specification.doex,50 - 50 Termul 203:5 E FAIL n/a F FAIL n/a F FAIL n/a F 6F64(043) I61 FAIL na F FAIL na F FAIL na F 62:PE 64 (20:30:50) E6i E7g E8g Termul 203:PE n/a n/a Ln/a 62:PE 64 (30:34:36) E6h FAIL F FAIL F FAIL F Termul 203a:PE to n/a n/a commrcia/all 62:PE 64 (40:37:23) E6i E7i s Termul 203 :PE FALn/a FALn/a F ALn/a F 62:PE 64 (50:40:10) IE6j E7j E8j Compatibility Trials [0152] Compatibility trials using a triallate emulsifiable concentrate formulation according to Example I of the present invention, a commercially available agricultural chemical formulation (identified by the trade name under which it is supplied) and water were carried out. The results are set out in Table 11. TABLE 11 Trial Sample Amounts Observation Compatibility (based on result mid-range recommende d rates) Water 95 g Milky emulsion, no separation, no 1 Triallate 900EC 0.90 g solids formation, Compatible no cream or oil Chlorsulfuron 750WG 0.07 g formation Water 99 g Milky emulsion, no separation, no 2 Triallate 900EC 0.91 g solids formation, Compatible no cream or oil Mandate 750 0.05 g formation 28/08/13,jb20105 amended cap specification.docx,51 -51 Water 98.4 g Milky emulsion, no separation, no 3 Triallate 900EC 0.91 g solids formation, Compatible no cream or oil Trifluralin 480EC 0.65 g formation Water 91.9 g Milky emulsion, no separation, no 4 Triallate 900EC 0.91 g solids formation, Compatible no cream or oil Eradicator 450 8.01 g formation Water 95.8 g Milky emulsion, no separation, no 5 Triallate 900EC 0.90 g solids formation, Compatible no cream or oil Glyphosate NH 4 3.30 g formation 888WDG Water 99 g Milky emulsion, no separation, no 6 Triallate 900EC 0.90 g solids formation, Compatible no cream or oil Monza 0.12 g formation Water 93.4 g Milky emulsion, no separation, no 7 Triallate 900EC 0.92 g solids formation, Compatible no cream or oil Round up Power Max 5.69 g formation Water 91.8 g Milky emulsion, no separation, no 8 Triallate 900EC 0.89 g solids formation, Compatible no cream or oil Eradicator 510 7.31 g formation Water 97.4 g Milky emulsion, no separation, no 9 Triallate 900EC 0.90 g solids formation, Compatible no cream or oil Eradicator 540 6.47 g formation 28/08/13,jb20105 amended cap specification.docx,52 - 52 Water 93.8 g Milky emulsion, no separation, no 10 Triallate 900EC .091 g solids formation, Compatible no cream or oil Glyphosate 360 5.31 g formation Examples of Formulations Exhibiting Satisfactory Characteristics [0153] Examples of triallate formulations prepared according to the present invention which exhibit satisfactory characteristics (as demonstrated by the trials discussed above are set out in Table 12 for ease of reference. TABLE 12 Trial Appendix Triallate Solvent and Anionic Non-ionic number g/L loading g/L surfactant surfactant (+ and loading and loading impurity g t . g/L portion) A1.b Campaign 900 Recosol 150 Ninate 60E Termul 200 1 (+47) 106 76 50 IA. 1 Campaign 900 Recosol 150 Ninate 60E Termul 200 (+47) 106 76 50 IIIA1 Campaign 899 Xylene Ninate 60E Termul 200 (+47) 105 77 51 VIAl Campaign 900 n-methyl-2- Ninate 60E Termul 200 4 (+47) pyrrolidone 76 50 106 28/08/13,jb20105 amended cap specification.doex,53 - 53 VIIAl Campaign 898 Diethyleneglyc Ninate 60E Termul 200 4 (+47) ol monoethyl 77 52 ether DGME 106 E4ib Campaign 848 Recosol 150 Ninate 60E Termul 1284 5 (+45) 167 78 50 E4iib Campaign 801 Recosol 150 Ninate 60E Termul 1284 5 (+42) 218 76 51 E4iiia Campaign 850 Recosol 150 Ninate 60E Termul 1285 5 (+45) 167 38 90 E4iiib Campaign 849 Recosol 150 Ninate 60E Termul 1285 5 (+45) 165 78 51 E4iva Campaign 798 Recosol 150 Ninate 60E Termul 1285 5 (+42) 218 39 91 E4ivb Campaign 800 Recosol 150 Ninate 60E Termul 1285 5 (+42) 217 77 52 9A1 Campaign 799 Recosol 150 Kemmat Termul 200 6 (+42) 219 HF60 50 77 9B1 Campaign 800 Recosol 150 Nansa EVM Termul 200 6 (+42) 218 70/2E 51 76 9C1 Campaign 801 Recosol 150 Rhodacal 70 Termul 200 28/08/13,jb20105 amended cap specification.docx,54 -54 6 (+42) 218 77 50 9D1 Campaign 800 Recosol 150 Rhodacal Termul 200 6 (+42) 219 70B 51 76 9E1 Campaign 801 Recosol 150 Toximul Termul 200 6 (+42) 218 TANS 5 50 77 9F1 Campaign 800 Recosol 150 Toximul Termul 200 6 (+42) 219 TANS 6 51 77 9G1 Campaign 801 Recosol 150 Toximul Termul 200 6 (+42) 218 TANS 8 50 76 9H1 Campaign 800 Recosol 150 Toximul Termul 200 6 (+42) 218 TAABS 5 51 77 911 Campaign 799 Recosol 150 Toximul Termul 200 6 (+42) 219 TAABS 8 51 77 9A2 Campaign 699 Recosol 150 Kemmat Termul 200 6 (+37) 324 HF60 51 77 9B2 Campaign 699 Recosol 150 Nansa EVM Termul 200 6 (+37) 325 70/2E 51 77 9C2 Campaign 700 Recosol 150 Rhodacal 70 Termul 200 6 (+37) 324 77 51 9D2 Campaign- 700 Recosol 150 Rhodacal Termul 200 6 (+37) 324 70B 50 77 28/08/13jb20105 amended cap specification.docx,55 - 55 9E2 Campaign 701 Recosol 150 Toximul Termul 200 6 (+37) 324 TANS 5 50 76 9F2 Campaign 699 Recosol 150 Toximul Termul 200 6 (+37) 324 TANS 6 50 77 9H2 Campaign 699 Recosol 150 Toximul Termul 200 6 (+37) 324 TAABS 5 51 77 912 Campaign 700 Recosol 150 Toximul Termul 200 6 (+37) 324 TAABS 8 50 77 E7b Campaign 805 zero PE64 zero 9 (+42) 340 E7c Campaign 806 zero- PE62 zero 9 (+42) 170 PE64 170 E7d Campaign 805 zero PE62 zero 9 (+42) 85 PE64 255 E8a Campaign 705 zero PE62 zero 9 (+37) 446 E8b Campaign 705 zero PE64 zero 9 (+37) 446 E8c Campaign 704 zero PE62 zero 9 (+37) 223 PE64 28/08/13,jb20105 amended cap specification.doex,56 -56 223 E8d Campaign 705 zero PE62 zero 9 (+37) 112 PE64 334 Note 1: Ninate 60E given weight incudes carrier solvent Note 2: Rhodacal 60/BE-C given weight includes carrier solvent Note 3: Kemmat HF60 given weight includes carrier solvent Note 4: Nansa EVM 70/2E given weight includes carrier solvent Note 5: Rhodacal 70 given weight includes carrier solvent Note 6: Other anionic surfactants, weight includes carrier solvent Note 7: Butyl glysolv = ethyleneglycolmonobutyl ether = EDME Source of Technical Grade Active (Triallate (CAS# 2303-17-5)): Manufactured by China Petrochemical Lanhua Hongda Co Agrichemical Factory, 31 Fuli East Road, Xigu Sect., Lanzhou Gansu, CHINA Purchased from China Jiangsu International Economic Technical Cooperation Corporation, 24F, No. 8 Zhongshan Nanlu, Nanjing, 210005, P.R. China Safety Trial [0154] A trial was conducted to ascertain the safety of an emulsifiable concentrate formulation prepared according to the present invention when applied in a spray at the rate of 500 g active ingredient/hectare to shallow sown Kaspa Peas. The results indicated that the emulsifiable concentrate formulation according to the present invention is as safe to use as a conventional emulsifiable concentrate formulation.
28/08/13,jb20105 amended cap specification.docx,57 - 57 Efficiency [0155] A trial indicated that an emulsifiable concentrate formulation prepared according to the present invention offered equivalent efficacy on a target species as a conventional emulsifiable concentrate formulation, when each were applied to the target species at equal active equivalent application rates to the target species. EXAMPLE BEl [0156] The formulation of example 1 (900 g/L triallate) was designated FEl and was compared with a commercially available 500g/L triallate emulsifiable concentrate designated CA500. [0157] Pots containing potting mix were sown to wheat (Derrimut variety) and wild oats (Avena sterilis). Wheat was sown at 4cm depth and wild oats was sown at 2cm depth in 0.55L pots. Five replicate pots were established for each herbicide treatment. Spraying was conducted in a cabinet sprayer with an output of 100 L/ha using twin T-Jet 001 nozzles with the boom moving at 3.6 km/hr. Each herbicide was sprayed onto the soil surface and then incorporated immediately after spraying to simulate an incorporated by sowing (IBS) system. The pots were kept outdoors in a shade-house and watered as required. FEl and CA500 were applied at the rates of (i) 400g ai/ha, (ii) 800 g ai/ha and (iii) 1600 g ai/ha. Assessment was at 4 weeks after application, based on individual pot assessment of percentage control of each herbicide on wild oats and wheat measured as a visual estimation of plant biomass reduction (% control) compared to untreated pots. [0158] Both FEl and CA500 were effective and had similar efficacy on wild oats.
28/08/13,jb20105 amended cap specification.docx,58 - 58 Wheat data (% biomass reduction relative to control) FE1 RepI Rep2 Rep3 Rep4 Rep5 CA500 RepI Rep2 Rep3 Rep4 Rep5 Rate Rate g 8 ai/ha ai/ha 400 0 0 10 10 15 400 10 10 15 20 20 800 10 15 15 20 30 800 5 10 10 20 20 1600 0 15 15 20 30 1600 10 15 20 30 40 Wild Oats data (% biomass reduction relative to control) FE1 RepI Rep2 Rep3 Rep4 Rep5 CA500 RepI Rep2 Rep3 Rep4 Rep5 Rate Rate g g ai/ha ai/ha 400 100 100 90 90 100 99 98 100 100 100 800 100 100 100 100 100 100 100 100 100 100 1600 100 100 100 100 100 100 100 100 100 100 [0159] A further trial indicated that an emulsifiable concentrate formulation prepared according to the present invention when applied in a spray at the rate of 500 g active ingredient/hectare in combination with trifluralin was as effective as a spraying combination formed from a conventional emulsifiable formulation of triallate and trifluralin. EXAMPLE BE2 [0160] Formulations FEI (see above) and CA500 were applied to pots containing herbicide susceptible ryegrass biotype SLR4 buried at 1cm depth. FEi and CA500 were applied as described in the table below, either in isolation or in conjunction with 1.75 L/ha trifluralin 480 g/L commercial herbicide.
28/08/13,jb20105 amended cap specification.docx,59 - 59 Herbicide and rate Results (percent control) 1.6 L/ha CA500 85 +/- 2.2 1.6 L/ha CA500 plus 1.75 L/ha trifluralin 100+/-0 480 EC 890 ml/ha FEl 85+/-1.8 890 ml/ha FE plus 1.75 L/ha trifluralin 98 +/- 1.6 480 EC untreated 0 [0161] Seed was sown at 1cm depth in 10cm x 10cm pots and sprayed. The seed was then covered by 0.5cm soil to simulate incorporation which is the most common practice of applying pre-emergence herbicides in no-til agriculture. Herbicide application was performed using a laboratory boom sprayer with twin T-jet fan nozzles at a speed of 1 metre per second. Output from the sorayer was calibrated at 110 L/ha at a pressure of 250 kPa. Using this testing procedure, volatilisation losses were minimised by the immediate and even incorporation of herbicide. The experiment was conducted outdoors in a shade house in March-April 2012 (in South Australia) as a randomised complete design with five replications. [0162] Herbicide effects were measured 3 weeks after spraying. Seedlings were considered emerged if they had reached the 2-leaf stage at this time. Survival % was recorded by comparing the surviving number of 2 leaved seedlings in the sprayed treatments to the number present before spraying. Percentage control was calculated by subtracting % survival from 100. [0163] More details of the trials are set out in Appendix 12 to the specification of Australian Provisional Patent Application No. 2012902790, which Appendix forms part of that specification.
28/08/13,jb20105 amended cap specification.docx,60 - 60 [0164] The complete disclosures of any patents, patent documents, and publications cited herein are incorporated by reference in their entirety as if each were individually incorporated. Various modifications and alterations to this invention will become apparent to those skilled in the art without departing from the scope and spirit of this invention. It should be understood that this invention is not intended to be unduly limited by the illustrative embodiments and examples set forth herein and that such examples and embodiments are presented by way of example only with the scope of the invention intended to be limited only by the claims set forth herein as follows. [0165] Throughout this specification and the claims which follow, unless the context requires otherwise, the word "comprise", and variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated integer or step or group of integers or steps but not the exclusion of any other integer or step or group of integers or steps. [0166] The reference in this specification to any prior publication (or information derived from it), or to any matter which is known, is not, and should not be taken as an acknowledgment or admission or any form of suggestion that that prior publication (or information derived from it) or known matter forms part of the common general knowledge in the field of endeavour to which this specification relates.
28/08/13,jb20105 amended cap specification.docx,61 - 61 APPENDIX 1 Trial # Ala TRIALLATE 900 TRIALS Triallate active present at 900gIL Trial details: Trial using Termul 200 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E: Termul 200 (30:70) Anionic/Non-ionic surfactant Solvent used: Ninate 60E: Termul 200: Recosol 150 FORMULATION Component CAS # Function Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 2303-17-5 Active ingredient 4737.2 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 64742-94-5 Solvent 531.4 106 used: Recosol 150 Calcium Cl 0-16 alkyl benzenesulfonic acid CABS in 2-ethyl hexanol 68584-23-6) & Surfactant 189.6 38 2-ethyl used: Ninate 60E (anionic surfactant) hexanol (104-76-7) Alkoxylated alkyl phenol 37251-69-7 Surfactant 445.6 89 used: Termul 200 (non-ionic surfactant) Total 5903.8 RESULTS OF FORMULATION Remark Parameter Method Required Results s Appearance Visual Dark yellow to brown liquid, Brown liquid Passed homogeneous Validated chromatographic method Assay (Accuracy: 98-102%) 875 to 925g/L Triallate n/a (Linearity: R > 0.99) (Precision: s/average < 2%) pH at 1% aq. Solution MT 75.3 4 to 10 Specific gravity (temperature at 20C) CIPAC MT 3.1 1.00 to 1.30 n/a 28/08/13,jb20105 amended cap specification.docx,62 - 62 <2mL cream after 30 min, Etrace Emulsion characteristics CIPAC MT 36.1 of oil after 30 min and complete milky emulsion, 3.5mL Failed re-emulsion after 24h cream@bottom Persistent Foaming CIPAC MT 47.2 <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, brown liquid, Test paamte maitanedwihi (Accelerated Ageing) MT75.3 r equir s, ranm phase omogeneouslere m Passed separation in any format phase separation in any GeneralRemark Viscosity
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fora (temperature at 5C) M190to20csn/a ViscosityMT120t 0cs emperature at 20C) M190to20csn/a Test parameter maintained within Long Term Performance 'Various as per above required range after accelerated n/a General Remarks aging to approximate 2 years. PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # Alb TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 200 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E: Termui 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Termul 200 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name)
S-
2 ,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4737.3 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 381.1 76 used: Ninate 60E (anionic surfactant) 28/08/13,jb20105 amended cap specification.docx,63 - 63 Alkoxylated alkyl phenol 252.4 50 used: Termul 200 (non-ionic surfactant) Total 5902.2 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate 912g/L Passed pH at 4 to 10 7.16 Passed 1% aq. Solution4to1 Specific gravity 1.00 to 1.30 1.183 Passed (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, no Passed Emulsion characteristics of oil after 30 min and complete separation, no re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min 12ml in 1 min Passed Cold temp. stability Dark yellow to brown liquid, brown liquid, (Accelerated Ageing) homogeneous, free from phase haseseon in any Passed separation in any format phase separation in any format nature at 5C) 0 to 2000cPs 72cps Passed nature at 20) 0 to 2000cPs 34cps Passed Test parameter maintained within Long Term Performance required range after accelerated aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA Trial# Alc TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 200 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Termul 200 (90:10) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Termul 200 : Recosol 150 28/08/13,jb20105 amended cap specification.docx,64 -64 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4736.9 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 568.6 114 used: Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 65 13 used: Termul 200 (non-ionic surfactant) Total 5901.9 RESULTS OF FORMULATION Remark Parameter Required Results S Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4to1n Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete milky emulsion, 5mL Failed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, brown liquid, Cod ep.stbliy homogeneous, free from phase hooeeu,.refo Passed (Accelerated Ageing) homogeneous, free from pae paesprto nay Pse separation in any format phase separation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL?
FAIL
28/08/13,jb20105 amended cap specification.docx,65 - 65 Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # B3a TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric N2 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N2 (30:70) AnioniclNon-ionic surfactant Solvent used: Ninate 60E :Teric N2 : Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4736.3 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.3 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 442.9 89 used: Teric N2 (non-ionic surfactant) Total 5900 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity (temperature at 20C) 1.00 to 1.30 n/a 28/08/13,jb20105 amended cap specification.docx,66 - 66 <2mL cream after 30 min, trace clear emulsion, 5mi Emulsion characteristics of oil after 30 min and complete ol&cre bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, brown liquid, Cod em. tailty homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) homogen fre frmas phase separation in any separation in any format format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial# B3b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric N2 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N2 (60:40) AnioniclNon-ionic surfactant Solvent used: Ninate 60E :Teric N2 : Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4737.0 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 381.1 76 used: Ninate 60E (anionic surfactant) 28/08/13,jb20105 amended cap specification.docx,67 - 67 Nonyl Phenol ethoxylates used: Teric N2 (non-ionic surfactant) 252.1 50 Total 5901.6 RESULTS OF FORMULATION ParaeterRemark Parameter Required Results R Appearance Dark yellow to brown liquid, homogeneous Brown liquid Passed Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity tem erature at 20C) 1.00 to 1.30n/a <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete clear emulsion, SmI Failed re-emulsion after 24h oil&cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, brown liquid, (Accelerated Ageing) homogeneous, free from phase homogeneous, free from Passed separation in any format phase separation in any Viscosity format temperature at 5o 2000cPsn/a Viscosity temperature at 200 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # B3c TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric N2 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N2 (90:10) Anionic/Non-ionic surfactant Solvent used: Ninate 60E :Teric N2: Recosol 150 28/08/13,jb20105 amended cap specification.docx,68 -68 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4737.6 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 568.7 114 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 62.7 13 used: Teric N2 (non-ionic surfactant) Total 5900.4 RESULTS OF FORMULATION Remark Parameter Required Results S Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace clear emulsion, 5mI Emulsion characteristics of oil after 30 min and complete oi l&cream @bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, brown liquid, Cod ep.stbliy homogeneous, free from phase hooeeu refo Passed (Accelerated Ageing) homogeneous, free from pae paesprto nay Pse separation in any format phase separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL?
FAIL
28/08/13,jb20105 amended cap specification.docx,69 - 69 Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # B4a TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric N8 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N8 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Teric N8 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4737.1 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 445.1 89 used: Teric N8 (non-ionic surfactant) Total 5903.1 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity 100 to 1.30 n/a (temperature at 20C) 28/08/13,jb20105 amended cap specification.docx,70 - 70 <2mL cream after 30 min, trace . Emulsion characteristics of oil after 30 min and complete milky emulsion, 2ml of Failed re-emulsion after 24h cream & oil@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, brown liquid, (Accelerated Ageing) homogeneous, free from phase homogeneous, free from Passed separation in any format phase separation in any Viscosity format (temperature at 5C) 0 o20csn/a Viscosity 0t 0~~ (temperature at 20C) 1 Eo200~ n/a Test parameter maintained within Long Term Performance required range after accelerated n/a _ aing to aproimte2 eas General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # B4b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric N8 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N8 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Teric N8 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4736.3 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.3 106 used: Recosol 150 51 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 381.1 76 used: Ninate 60E (anionic surfactant) 28/08/13jb20105 amended cap specification.docx,71 - 71 Nonyl Phenol ethoxylates 252.5 50 used: Teric N8 (non-ionic surfactant) Total 5901.2 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4t10n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, 2ml of Emulsion characteristics of oil after 30 min and complete cream & oil@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability homogenous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # B4c TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric N8 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N8 (90:10) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Teric N8 : Recosol 150 28/08/13,jb20105 amended cap specification.docx,72 - 72 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4737.1 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 568.6 114 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 63.1 13 used: Teric N8 (non-ionic surfactant) Total 5900.2 RESULTS OF FORMULATION Remark Parameter Required Results S Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 100 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion 5mi of Emulsion characteristics of oil after 30 min and complete m emliottm Failed re-emulsion after 24h cream & oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Ctemp. stability homogeneous, free from phase homogeneous, free from Passed eing separation in any format phase separation in any format Viscosity Vsoiy0 to 2000cPs n/a (temperature at 5C) Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL?
FAIL
28/08/13jb20105 amended cap specification.docx,73 - 73 Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # B5a TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric N13 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N13 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Teric N13 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4736.9 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 443.6 89 used: Teric N13 (non-ionic surfactant) Total 5901.4 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) 28/08/13,jb20105 amended cap specification.docx,74 - 74 <2mL cream after 30 min, trace milky emulsion, 4.5ml of Emulsion characteristics of oil after 30 min and complete cream & oil@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Forms crystal Failed separation in any format Viscosity 0 o20csn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS AND COLD STAB FAILED Trial # B5b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric N13 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N13 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Teric N13 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4736.7 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 381.1 76 used: Ninate 60E (anionic surfactant) 28/08/13,jb20105 amended cap specification.docx,75 - 75 Nonyl Phenol ethoxylates 251.2 50 used: Teric N13 (non-ionic surfactant) Total 5900.4 RESULTS OF FORMULATION Rema Parameter Required Results rks Appearance Dark yellow to brown liquid, Brown liquid Passe homogeneous d Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace milky emulsion 2.1ml of Emulsion characteristics of oil after 30 min and complete Failed re-emulsion after 24h cream & oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability hoDarkeo to bro liqid homogeneous, free from Passe (Accelerated Ageing) homogeneous, fre from phase phase separation in any d separation in any format format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0t 0~~ / (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # B5c TRIALLATE 900 TRIALS Triallate active present at 900giL Trial details: Trial using Teric N13 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N13 (90:10) Anionic/Non-ionic surfactant Solvent used: Ninate 60E :Teric N13: Recosol 150 28/08/13,jb20105 amended cap specification.docx,76 - 76 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4736.3 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.3 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 568.5 114 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 64.2 13 used: Teric N13 (non-ionic surfactant) Total 5900.3 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity temperaturee at 20C) 1.00 to 1.30 n/a <2mL cream after 30 min, trace . Emulsion characteristics of oil after 30 min and complete milky emulsion, 4.5ml of Failed re-emulsion after 24h cream & oil@bottom Persistent Foaming <60mL after 1 min n/a Cold temp stability Dark yellow to brown liquid, brown liquid, (Accelerated Ageing) homogeneous, free from phase homogeneous, free from Passed separation in any format phase separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years.
28/08/13,jb20105 amended cap specification.docx,77 - 77 General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # B6a TRIALLATE 900 TRIALS Triallate active present at 900gIL Trial details: Trial using Teric N20 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N20 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Teric N20 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4737.1 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 448.6 90 used: Teric N20 (non-ionic surfactant) Total 5906.6 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4tol1 n/a 28/08/13,jb20105 amended cap specification.docx,78 - 78 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, 5ml of Emulsion characteristics of oil after 30 min and complete cream & oil@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity 0t 0~~ / (temperature at 5C) 0 to 2000cPs n/a Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # B6b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric N20 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Teric N20 (60:40) AnioniclNon-ionic surfactant/ Solvent used: Ninate 60E :Teric N20 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4738.1 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.5 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid 381.2 76 in 2-ethyl hexanol 28/08/13jb20105 amended cap specification.docx,79 - 79 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 252.3 50 used: Teric N20 (non-ionic surfactant) Total 5903.1 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4to1n Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace milky emulsion, 3m of Emulsion characteristics of oil after 30 min and complete cream & oil@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) homogen fre frmas phase separation in any separation in any format format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # B6c TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric N20 as non-ionic surfactants at varying concentration against Ninate 60E 28/08/13,jb20105 amended cap specification.docx,80 - 80 Ratio of N60E : Teric N20 (90:10) Anionic/Non-ionic surfactant Solvent used: Ninate 60E :Teric N20 : Recosol 150 FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4738.3 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.5 106 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 568.8 114 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 64.0 13 used: Teric N20 (non-ionic surfactant) Total 5902.6 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace milky emulsion, 5ml of Emulsion characteristics of oil after 30 min and complete cream & oil@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 to 200cPs n/a (temperature at 20C) 0t 00~ 28/08/13,jb20105 amended cap specification.docx,81 - 81 Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # Ca TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 1284 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Termul 1284 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Termul 1284: Recosol 150 Trial # IA11-ti FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 47380 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.5 106 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.6 38 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 444.0 89 used: Termul 1284 (non-ionic surfactant) Total 5903.1 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous 28/08/13,jb20105 amended cap specification.doex,82 - 82 Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, 1.7m of Emulsion characteristics of oil after 30 min and complete mlk emliom Passed re-emulsion after 24h cream & oil@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STABILITY FAILED Trial # C7b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 1284 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Termul 1284 (60:40) Anionic/Non-ionic surfactant Solvent used: Ninate 60E :Termul 1284: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4739.1 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 534.9 107 used: Recosol 150 380.1 76 28/08/13,jb20105 amended cap specification.docx,83 - 83 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 255.6 51 used: Termul 1284 (non-ionic surfactant) Total 5909.7 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4 to 10 Specific gravity 1 00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace off white milky emulsion, Emulsion characteristics of oil after 30 min and complete no separation, no cream Passed re-emulsion after 24h @ bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Cold temp. stability homogeneous, free from phase unstable, forms crystal @ Failed (Accelerated Ageing) hooeeufe rmpaebottom Fie separation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a G aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB
FAILED
28/08/13,jb20105 amended cap specification.docx,84 - 84 Trial# C7c TRIALLATE 900 TRIALS Triallate active present at 900gIL Trial details: Trial using Termul 1284 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Termul 1284 (90:10) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Termul 1284: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.9 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 569.9 114 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 67.2 13 used: Termul 1284 (non-ionic surfactant) Total 5906.7 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 100 to 1.30 n/a (temperature at 20C) 1.00_to_1.30_n/a <2mL cream after 30 min, trace . Emulsion characteristics of oil after 30 min and complete milky emulsion, 4.5ml of Failed re-emulsion after 24h cream & oil@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, brown liquid, hoogneus free. fromlit phasenous fre Passe (Accelerated Ageing) homogeneous, free from phase phase separation in any Passed separation in any format format 28/08/13,jb20105 amended cap specification.docx,85 - 85 Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # C8a TRIALLATE 900 TRIALS Triallate active present at 900giL Trial details: Trial using Termul 1285 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Termul 1285 (30:70) Anionic/Non-ionic surfactant Solvent used: Ninate 60E :Termul 1285 : Recosol 150 FORMULATION (Cheomponname) Amount, g Loading, gIL S-2,3,3-tricholoroallyl 4736.5 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.3 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 442.5 89 used: Termul 1285 (non-ionic surfactant) Total 5899.8 28/08/13,jb20105 amended cap specification.docx,86 - 86 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace . Emulsion characteristics of oil after 30 min and complete milky emulsion, 0.25m of Passed re-emulsion after 24h cream & oil@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, forms tiny crystals on the (Accelerated Ageing) homogeneous, free from phase sides of the container Failed separation in any format Viscosity n/a (temperature at 50) 0t 00~ Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # C8b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 1285 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Termul 1285 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Termul 1285 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4738 896 eg. Triallate Tech (95% purity) 28/08/13jb20105 amended cap specification.docx,87 - 87 Solvent naphtha (petroleum), heavy aromatic 548.5 109 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 387.2 77 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 251.5 50 used: Termul 1285 (non-ionic surfactant) Total 5925.2 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4to10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace off white milky emulsion, Emulsion characteristics of oil after 30 min and complete no separation, no cream Passed re-emulsion after 24h @ bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Crystalized at the bottom Failed separation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB
FAILED
28/08/13,jb20105 amended cap specification.docx,88 - 88 Trial # C8c TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 1285 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Termul 1285 (90:10) Anionic/Non-ionic surfactant Solvent used: Ninate 60E :Termul 1285: Recosol 150 FORMULATION Component Amount, g Loading, g/IL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4737.1 898 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 541.0 108 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 570.8 114 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 66.0 13 used: Termul 1285 (non-ionic surfactant) Total 5914.9 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 100 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, mI of Emulsion characteristics of oil after 30 min and complete cream & oil@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.docx,89 - 89 C Dark yellow to brown liquid brown liquid, homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity Vsoiy0 to 2000cPs n/a (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # D9a TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 62 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 62 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :PE 62: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4737.1 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) Block Co-polymer 444.6 89 used: PE 62 (non-ionic surfactant) 28/08/13,jb20105 amended cap specification.docx,90 -90 Total 5902.6 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4to n/a Specific gravity (temperature at 20C) 1.00 to 1.30 n/a <2mL cream after 30 min, trace off white milky emulsion Emulsion characteristics of oil after 30 min and complete 2ml of cream & oil @ Failed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min n/a Cold temp stability Dark yellow to brown liquid, brown liquid, (Accelerated Ageing) homogeneous, free from phase homogeneous, free from Passed separation in any format phase separation in any Viscosity0to2Ocsfra (temperature at 5C) 0 o20csn/a Viscosity 0t 0~~ (temperature at 20C) 0 o20csn/a Test parameter maintained within Long Term Performance required range after accelerated n/a General Rearksaging to approximate 2 years. PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # D9b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE_62 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 62 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :PE 62 : Recosol 150 28/08/13,jb20105 amended cap specification.docx,91 - 91 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4735.8 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 534.7 107 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 380.8 76 used: Ninate 60E (anionic surfactant) Block Co-polymer 251.7 50 used: PE 62 (non-ionic surfactant) Total 5903 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4 to 10 Specific gravity 100 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace off white milky emulsion, Emulsion characteristics of oil after 30 min and complete 4ml of cream & Failed re-emulsion after 24h oil@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase crystal forms @ bottom Failed separation in any format Viscosity (temperature at 5C) 0 to 2000cPs Viscosity to 2000cPs n/a (temperature at 20C) 0 Test parameter maintained within Long Term Performance required range after accelerated n/a General Remarks aging to approximate 2 years. I _I PASS or FAIL?
FAIL
28/08/13,jb20105 amended cap specification.docx,92 - 92 Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS AND COLD STAB FAILED Trial# D9c TRIALLATE 900 TRIALS Triallate active present at 900giL Trial details: Trial using PE 62 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 62 (90:10) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :PE 62 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 47364 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 532.0 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 569.8 114 used: Ninate 60E (anionic surfactant) Block Co-polymer 63.9 13 used: PE 62 (non-ionic surfactant) Total 5902.1 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 1 00 to 1.30 (temperature at 20C) - - n/a 28/08/13jb20105 amended cap specification.docx,93 - 93 <2mL cream after 30 min, trace off white milky emulsion, Emulsion characteristics of oil after 30 min and complete 3m! of cream e bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability Darkgyeo to bro liqid homogeneous, free from (Accelerated Ageing) separation in any format phase separation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial# D10a TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 64 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 64 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :PE 64: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4736.4 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.3 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) 28/08/13,jb20105 amended cap specification.docx,94 - 94 Block Co-polymer 443.6 89 used: PE 64 (non-ionic surfactant) Total 5900.8 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity n/a (temperature at 20C) 1.to 1.30 <2mL cream after 30 min, trace slightly hazy emulsion, Emulsion characteristics of oil after 30 min and complete 4ml of cream & Failed re-emulsion after 24h oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability Darkgyeo to bro liqid homogeneous, free from (Accelerated Ageing) separation in any format phase separation in any sepaatio in ny frmatformat Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # D10b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 64 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 64 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :PE 64: Recosol 150 28/08/13jb20105 amended cap specification.doex,95 - 95 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 47377 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 537 107 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 381.6 76 used: Ninate 60E (anionic surfactant) Block Co-polymer 254.4 51 used: PE 64 (non-ionic surfactant) Total 5910.7 RESULTS OF FORMULATION Remark Parameter Required Results S Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 100 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky white emulsion, 5m Emulsion characteristics of oil after 30 min and complete ml we emlsion, m Failed re-emulsion after 24h of cream & oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Ctemp stability homogeneous, free from phase homogeneous free from Passed geig) separation in any format phase separation in any format Viscosity n/a (temperature at 5C) 0 to 2000cPs Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL?
FAIL
28/08/13,jb20105 amended cap specification.docx,96 - 96 Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # D10c TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 64 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 64 (90:10) AnioniclNon-ionic surfactant/ Solvent used: Ninate 60E :PE 64: Recosol 150 FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4735.9 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 533.0 107 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 570.0 114 used: Ninate 60E (anionic surfactant) Block Co-polymer 65.7 13 used: PE 64 (non-ionic surfactant) Total 5904.55 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 28/08/13,jb20105 amended cap specification.docx,97 - 97 Specific gravity 1.00 to 1.30 (temperature at 20C) - n/a <2mL cream after 30 min, trace . Emulsion characteristics of oil after 30 min and complete milky white emulsion, 4ml Failed re-emulsion after 24h of cream & oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability Darkgyeo to bro liqid homogeneous, free from (Accelerated Ageing) homogenein any format phase separation in any separation ianfomtformat Viscosity n/a (temperature at 5C) 0 to 2000cPs Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial# D1Ia TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 68 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 68 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :PE 68 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4736.3 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.3 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid 189.5 38 in 2-ethyl hexanol 28/08/13,jb20105 amended cap specification.docx,98 - 98 used: Ninate 60E (anionic surfactant) Block Co-polymer 446.0 89 used: PE 68 (non-ionic surfactant) Total 5903.1 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4 to 10 n/a 1% aq. Solution Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Cold temp. stability homogeneous, free from phase Solidifies at room temp Failed (Accelerated Ageing) separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity 0 to 2000cPs n/a (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE MIXTURE SOLIDIFY AT ROOM TEMP 28/08/13,jb20105 amended cap specification.docx,99 - 99 Trial# D11b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 68 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 68 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :PE 68: Recosol 150 Trial # A15-t2 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 536.9 107 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 380.6 76 used: Ninate 60E (anionic surfactant) Block Co-polymer 250.6 50 used: PE 68 (non-ionic surfactant) Total 5903.6 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4to10 n/a Specific gravity 1.00 to 1.30 (temperature at 20C) - n/a <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.docx,100 - 100 Cold temp. stability Dark yellow to brown liquid, Forms crystal at room (Accelerated Ageing) homogeneous, free from phase temp Failed separation in any format Viscosity 0 to n/a (temperature at 5C) 2000cPs Viscosity 0 to n/a (temperature at 20C) 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE FORMED CRYSTALS AT ROOM TEMP Trial# D1Ic TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 68 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 68 (90:10) AnioniclNon-ionic surfactant Solvent used: Ninate 60E :PE 68: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4736.4 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 535.4 107 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 569.5 114 used: Ninate 60E (anionic surfactant) Block Co-polymer 63.5 13 used: PE 68 (non-ionic surfactant) Total 5904.8 28/08/13,jb20105 amended cap specification.docx,101 - 101 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance h yellow to brown liquid, Brown liquid Passed Appeaancehomogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4to1n Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, 5ml of Emulsion characteristics of oil after 30 min and complete cream & oil@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Forms crystal @ bottom Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS AND COLD STAB FAILED Trial # D12a TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using TSP 16 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : TSP 16 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : TSP 16 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4737.1 900 diisopropyl(thiocarbamate) 28/08/13,jb20105 amended cap specification.docx,102 - 102 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) Block Co-polymer 442.3 88 used: TSP 16 (non-ionic surfactant) Total 5900.3 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Forms crystals Failed separation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB
FAILED
28/08/13,jb20105 amended cap specification.docx,103 - 103 Trial # D12b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using TSP 16 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : TSP 16 (60:40) Anionic/Non-ionic surfactant Solvent used: Ninate 60E : TSP 16 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4763.1 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 533.5 106 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 385.0 77 used: Ninate 60E (anionic surfactant) Block Co-polymer 252.1 50 used: TSP 16 (non-ionic surfactant) Total 5933.7 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4tol1 n/a 1% aq. Solution Specific gravity 100 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, mI of Emulsion characteristics of oil after 30 min and complete cream & oil@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.docx, 104 - 104 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # D12c TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using TSP 16 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : TSP 16 (90:10) Anionic/Non-ionic surfactant Solvent used: Ninate 60E : TSP 16 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 43. 0 diisopropyl(thiocarbamate) 4736.5 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 532.5 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 570.2 114 used: Ninate 60E (anionic surfactant) Block Co-polymer 63.4 13 used: TSP 16 (non-ionic surfactant) 28/08/13,jb20105 amended cap specification.doex, 105 - 105 Total 5902.6 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4t10n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Crystal formed @ bottom Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # D13a TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 6400 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 6400 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : PE 6400: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4736.9 900 28/08/13,jb20105 amended cap specification.docx,106 - 106 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) Block Co-polymer 443.1 89 used: PE 6400 (non-ionic surfactant) Total 5900.9 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase forms crystal @ bottom Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB
FAILED
28/08/13,jb20105 amended cap specification.docx,107 - 107 Trial# D13b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 6400 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 6400 (60:40) Anionic/Non-ionic surfactant Solvent used: Ninate 60E : PE 6400 : Recosol 150 FORMULATION Component Amount, g Loading, glL (Chemical name) S-2,3,3-tricholoroallyl 4737 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 534.9 107 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 383.8 77 used: Ninate 60E (anionic surfactant) Block Co-polymer 251.4 50 used: PE 6400 (non-ionic surfactant) Total 5907.1 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4 to 10 n/a 1% aq. Solution Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a 28/08/13jb20105 amended cap specification.docx, 108 - 108 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase forms crystal @ bottom Failed (Ascceete Aseparation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial# D13c TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 6400 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 6400 (90:10) Anionic/Non-ionic surfactant Solvent used: Ninate 60E: PE 6400 : Recosol 150 Trial # IA17-t3 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 43. 9 diisopropyl(thiocarbamate) 4737.3 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 533.2 107 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 569.6 114 used: Ninate 60E (anionic surfactant) Block Co-polymer 64.3 13 used: PE 6400 (non-ionic surfactant) 28/08/13,jb20105 amended cap specification.docx,109 - 109 Total 5904.4 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase forms crystal @ bottom Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial# D14a TRIALLATE 900 TRIALS Triallate active present at 900giL Trial details: Trial using PE 6800 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 6800 (30:70) Anionic/Non-ionic surfactant Solvent used: Ninate 60E : PE 6800 : Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl 4736.9 900 28/08/13jb20105 amended cap specification.docx, 110 -110 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) Block Co-polymer 443.1 89 used: PE 6800 (non-ionic surfactant) Total 5900.9 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at - 1% aq. Solution 4tol1 n/a Specific gravity 1 00 to 1.30 n/a (temperature at 20C) -_-_n/a <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Solidifies at room temp Failed separation in any format Viscosity
--
(temperature at 5C) 0 to 2000cPs Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE IT SOLIDIFY AT ROOM TEMP 28/08/13,jb20105 amended cap specification.docx, 111 - 111 Trial # D14b TRIALLATE 900 TRIALS Triallate active present at 900giL Trial details: Trial using PE 6800 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 6800 (60:40) Anionic/Non-ionic surfactant Solvent used: Ninate 60E: PE 6800 : Recosol 150 FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl 4737.0 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 534.9 107 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 383.8 77 used: Ninate 60E (anionic surfactant) Block Co-polymer 251.4 50 used: PE 6800 (non-ionic surfactant) Total 5907.1 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4 to 10 Specific gravity 100 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.docx,112 - 112 Dark yellow to brown liquid, Acl etem stabiy homogeneous, free from phase forms crystal @ bottom Failed separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity 0 to 2000cPs n/a (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # D14c TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using PE 6800 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : PE 6800 (90:10) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: PE 6800: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4737.3 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 533.2 107 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 569.6 114 used: Ninate 60E (anionic surfactant) Block Co-polymer 64.3 13 used: PE 6800 (non-ionic surfactant) Total 5904.4 28/08/13,jb20105 amended cap specification-docx, 113 - 113 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4 to 10 Specific gravity (temperature at 20C) 1.00 to 1.30 n/a <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase forms crystal @ bottom Failed separation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # D15a TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 203 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Termul 203 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Termul 203 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4736.4 900 eg. Triallate Tech (95% purity) 28/08/13jb20105 amended cap specification.doex,114 -114 Solvent naphtha (petroleum), heavy aromatic 531.3 106 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 189.5 38 used: Ninate 60E (anionic surfactant) Block Co-polymer 443.2 89 used: Termul 203 (non-ionic surfactant) Total 5900.4 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 100 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete milky emulsion, 5mL Failed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS AND COLD STABILITY FAILED 28/08/13,jb20105 amended cap specification.docx, 115 - 115 Trial # D15b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 203 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Termul 203 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Termul 203 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4737.3 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 381.1 76 used: Ninate 60E (anionic surfactant) Block Co-polymer 254.5 51 used: Termul 203 (non-ionic surfactant) Total 5904.3 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4 to 10 n/a 1% aq. Solution4tl Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, 4mL Emulsion characteristics of oil after 30 min and complete cream@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.docx,116 - 116 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial# D15c TRIALLATE 900 TRIALS Triallate active present at 900giL Trial details: Trial using Termul 203 as non-ionic surfactants at varying concentration against Ninate 60E Ratio of N60E : Termul 203 (90:10) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Termul 203 : Recosol 150 FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl 4737.9 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.5 106 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 568.7 114 used: Ninate 60E (anionic surfactant) Block Co-polymer 64.7 13 used: Termul 203 (non-ionic surfactant) Total 5900.4 28/08/13,jb20105 amended cap specification.docx,117 -117 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at -- 1% aq. Solution 4to 10n/a Specific gravity (temperature at 20C) 1.00 to 1.30 n/a <2mL cream after 30 m, trace milky emulsion, 4mL Emulsion characteristics of oil after 30 min and complete cream@bottonm Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated g separation in any format phase separation in any sepaatio in ny frmatformat Viscosity 0 to 2000cPs nra (temperature at 5C) n/a Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED 28/08/13,jb20105 amended cap specification.doex,118 - 118 APPENDIX 2 #IE1b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 200 as non-ionic surfactants against Nansa EVM 7012E Ratio of Nansa EVM 7012E : Termul 200 (60:40) Anionic/Non-ionic surfactant Solvent used: Nansa EVM 7012E : Termul 200: Recosol 150 FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl 4732.9 901 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 567.2 114 used: Recosol 150 Calcium Dodecylbenzene Sulphonate in 2 ethylhexanol 377.3 76 used: Nansa EVM 70/2E (anionic surfactant) Alkoxylated alkyl phenol 252.0 50 used: Termul 200 (non-ionic surfactant) Total 5929.3 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.doex,119 -119 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Passed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: #IFlb TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 200 as non-ionic surfactants against Rhodacal 70 Ratio of Rhodacal 70 : Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Rhodacal 70 : Termul 200 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4743.7 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 569.6 114 used: Recosol 150 Calcium Dodecylbenzene Sulphonate in 2 ethylhexanol 376.8 75 used: Rhodacal 70 (anionic surfactant) Alkoxylated alkyl phenol 264.2 53 used: Termul 200 (non-ionic surfactant) Total 5954.15 28/08/13,jb20105 amended cap specification.doex, 120 - 120 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4 to 10 n/a 1% aq. Solution Specific gravity 100 to 1.30 n/a (temperature at 20C) 1.0t_13 / <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Passed separation in any format Viscosity to 2000cPs n/a (temperature at 5C) 0 Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a G Raging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: # IGib TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 200 as non-ionic surfactants against Rhodacal 70B Ratio of Rhodacal 70B: Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Rhodacal 70B : Termul 200 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4741.6 902 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 574.1 115 used: Recosol 150 362.9 73 28/08/13,jb20105 amended cap specification.docx,121 - 121 Calcium Dodecylbenzene Sulphonate in 2 ethylhexanol used: Rhodacal 70B (anionic surfactant) Alkoxylated alkyl phenol 254.3 51 used: Termul 200 (non-ionic surfactant) Total 5932.8 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Passed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: Trial # IH1b TRIALLATE 900 TRIALS Triallate active present at 900gIL Trial details: Trial using Termul 200 as non-ionic surfactants against Toximul TANS 5 Ratio of Toximul TANS 5 : Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Toximul TANS 5 : Termul 200: Recosol 150 28/08/13,jb20105 amended cap specification.docx,122 - 122 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4736 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531 106 used: Recosol 150 Alkylphenol ether sulfate/ tallow amine ethoxylated salts 385 77 used: Toximul TANS 5 (anionic surfactant) Alkoxylated alkyl phenol 256 51 used: Termul 200 (non-ionic surfactant) Total 5908 RESULTS OF FORMULATION Remark Parameter Required Results S Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4to1n Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 0.25ml of Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystal Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL?
FAIL
28/08/13,jb20105 amended cap specification.docx, 123 - 123 Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # llib TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 200 as non-ionic surfactants against Toximul TANS 6 Ratio of Toximul TANS 6 : Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Toximul TANS 6 : Termul 200: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4740.5 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 532.5 106 used: Recosol 150 Alkylphenol ether sulfate/ tallow amine ethoxylated salts 383 77 used: Toximul TANS 6 (anionic surfactant) Alkoxylated alkyl phenol 251 50 used: Termul 200 (non-ionic surfactant) Total 5907 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 0.25ml of Passed re-emulsion after 24h cream@bottom 28/08/13jb20105 amended cap specification.docx,124 - 124 Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed (Ascceeted Aseparation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # IJ1b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 200 as non-ionic surfactants against Toximul TANS 8 Ratio of Toximul TANS 8 : Termul 200 (60:40) AnioniclNon-lonic surfactant Solvent used: Toximul TANS 8 : Termul 200: Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4738.5 898 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.5 106 used: Recosol 150 Alkylphenol ether sulfate/ tallow amine ethoxylated salts 381.5 76 used: Toximul TANS 8 (anionic surfactant) Alkoxylated alkyl phenol 260.5 52 used: Termul 200 (non-ionic surfactant) Total 5912 28/08/13,jb20105 amended cap specification.docx,125 - 125 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 100 to 1.30 n/a (temperature at 20C) 1.0t_13 / <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 0.30ml of Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed (Accelte Aseparation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # IKIb TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Termul 200 as non-ionic surfactants against Toximul TAABS 5 Ratio of Toximul TAABS 5 : Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Toximul TAABS 5 : Termul 200 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4737 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531 106 28/08/13,jb20105 amended cap specification.docx, 126 - 126 used: Recosol 150 Branched alcohol ether sulfate/ tallow amine ethoxylated salts 382 76 used: Toximul TAABS 5 (anionic surfactant) Alkoxylated alkyl phenol 252 50 used: Termul 200 (non-ionic surfactant) Total 5902 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at -- 1% aq. Solution 4to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 0.25ml of Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB
FAILED
28/08/13,jb20105 amended cap specification.docx,127 - 127 Trial # IL1b TRIALLATE 900 TRIALS Triallate active present at 900gIL Trial details: Trial using Termul 200 as non-ionic surfactants against Toximul TAABS 8 Ratio of Toximul TAABS 8 : Termul 200 (60:40) Anionic/Non-ionic surfactant Solvent used: Toximul TAABS 8 : Termul 200: Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl 4736.5 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 533 106 used: Recosol 150 Branched alcohol ether sulfate/ tallow amine ethoxylated salts 382 76 used: Toximul TAABS 8 (anionic surfactant) Alkoxylated alkyl phenol 257 51 used: Termul 200 (non-ionic surfactant) Total 5908.5 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4t10n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 0.80ml of Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, CA elemp stability homogeneous, free from phase Formed crystals Failed separation in any format 28/08/13,jb20105 amended cap specification.docx, 128 - 128 Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity 0 to 2000cPs n/a (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB
FAILED
28/08/13,jb20105 amended cap specification.docx,129 - 129 APPENDIX 3 Trial # Ela TRIALLATE 1050 TRIALS Triallate active present at 1050gIL Trial details: Trial using Termul 200 as non-ionic surfactants against Ninate 60E, varying Triallate concentration Ratio of N60E: Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 200: Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 5527.6 1050 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 0 0 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 356.3 69 used: Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 234.7 46 used: Termul 200 (non-ionic surfactant) Total 6118.6 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, Etrace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a 28/08/13jb20105 amended cap specification.docx, 130 - 130 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # Elb TRIALLATE 1000 TRIALS Triallate active present at 1000g/L Trial details: Trial using Termul 200 as non-ionic surfactants against Ninate 60E, varying Triallate concentration Ratio of N60E: Termul 200 (60:40) Anionic/Non-ionic surfactant Solvent used: Ninate 60E: Termul 200: Recosol 150 FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 5263.1 1000 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 149.7 30 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 383.4 75 used: Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 252.5 50 used: Termul 200 (non-ionic surfactant) Total 6048.7 28/08/13,jb20105 amended cap specification.docx, 131 -131 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L Triallate n/a pH at - 1% aq. Solution 4to10 n/a Specific gravity 100 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, Etrace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity
-
(temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # Elc TRIALLATE 950 TRIALS Triallate active present at 950g/L Trial details: Trial using Termul 200 as non-ionic surfactants against Ninate 60E, varying Triallate concentration Ratio of N60E: Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 200: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 5001.1 950 diisopropyl(thiocarbamate) 28/08/13,jb20105 amended cap specification.doex, 132 - 132 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 336 67 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 384.8 77 used: Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 252.9 50 used: Termul 200 (non-ionic surfactant) Total 5974.8 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L Triallate n/a pH aq. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, Etrace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB
FAILED
28/08/13,jb20105 amended cap specification.docx,133 - 133 APPENDIX 4 Trial # IA1 TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Recosol 150 as a solvent using the current formulation of surfactants Ratio of Ninate 60E: Termul 200 (60:40) AnioniclNon-ionic surfactant/ Solvent used: Ninate 60E: Termul 200: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2, 3, 3-tricholoroallyl diisopropyl 4737.3 900 (thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-Cl 6 alkylbenzene Sulphonic acid in 2-ethylhexanol 381.1 76 used: Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 252.4 50 used: Termul 200 (non-ionic surfactant) Total 5902.2 ______ RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate 900g/L Passed pH at 1% aq. Solution 4 to 10 7.16 Passed Specific gravity (temperature at 20C) 1.00 to 1.30 1.183 Passed <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom 28/08/13,jb20105 amended cap specification.docx,134 - 134 Persistent Foaming <60mL after 1 min 12ml in 1min Passed Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity (temperature at 5C) 0 to 2000cPs 72 cps Passed Viscosity (temperature at 20C) 0 to 2000cPs 34cps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA Trial # IIA1 TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Recosol 200 as a solvent using the current formulation of surfactants Ratio of Ninate 60E: Termul 200 (60:40) Anionic/Non-ionic surfactant Solvent used: Ninate 60E: Termul 200: Recosol 200 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2, 3, 3-tricholoroallyl diisopropyl 4734 899 (thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 528.5 106 used: Recosol 200 Calcium C10-C16 alkylbenzene Sulphonic acid in 2-ethylhexanol 390 78 used: Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 253.5 51 used: Termul 200 (non-ionic surfactant) Total 5906 28/08/13,jb20105 amended cap specification.docx,135 - 135 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate 899g/L Passed pH at4to1 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0t 0~~ (temperature at 5C) 0 to 2000cPs Viscosity 0t 0~~ (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks FAIL PASS or FAIL? Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STAB FAILED Trial # IIIA1 TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Xylene as a solvent using the current formulation of surfactants Ratio of Ninate 60E: Termul 200 (60:40) Anionic/Non-ionic surfactant Solvent used: Ninate 60E: Termul 200: xylene FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2, 3, 3-tricholoroallyl diisopropyl 4734.5 899 (thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 527.5 105 28/08/13,jb20105 amended cap specification.docx, 136 - 136 used: xylene Calcium C10-C1 6 alkylbenzene Sulphonic acid in 2-ethylhexanol 385 77 used: Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 257 51 used: Termul 200 (non-ionic surfactant) Total 5904 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate 899g/L Passed pH at 4 to 10 1% aq. Solution Specific gravity 1.00 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0t 0~~ (temperature at 5C) 0 to 2000cPs Viscosity 0t 0~~ (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? Description: AWAITS FURTHER
ANALYSIS
28/08/13jb20105 amended cap specification.docx,137 -137 Trial # IVA1 TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Toluene as a solvent using the current formulation of surfactants Ratio of Ninate 60E: Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Termul 200 : Toluene FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4739 898 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 529.5 106 used: toluene Calcium C10-C16 alkylbenzene Sulphonic acid in 2-ethylhexanol 390 78 used:Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 254.5 51 used: Termul 200 (non-ionic surfactant) Total 5913 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate 898g/L Passed pH at 1% aq. Solution 4 to 10 Specific gravity 1 00 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min 28/08/13,jb20105 amended cap specification.docx,138 - 138 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0t 0~~ (temperature at 5C) 0 to 2000cPs Viscosity 0t 0~~ (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STAB PASS or FAIL? FAILED Description: AWAITS FURTHER ANALYSIS Trial # VAI TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Dimethyl adipate as a solvent using the current formulation of surfactants Ratio of Ninate 60E: Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Termul 200 : Dimethyl adipate FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4732 897 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 535 107 used: dimethyl adipate Calcium C10-C16 alkylbenzene Sulphonic acid in 2-ethylhexanol 390.5 78 used:Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 254 51 used: Termul 200 (non-ionic surfactant) Total 5911.5 28/08/13,jb20105 amended cap specification.docx,139 - 139 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate 897g/L Passed pH at 1% aq. Solution 4tol1 Specific gravity 1.00 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0t 0~~ (temperature at 5C) 0 to 2000cPs Viscosity 0t 0~~ (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? Description: AWAITS FURTHER ANALYSIS Trial # VIA1 TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using NMP as a solvent using the current formulation of surfactants Ratio of Ninate 60E: Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Termul 200 : NMP FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4736.5 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 530 106 28/08/13,jb20105 amended cap specification.docx,140 - 140 used: N-Methyl-2-pyrrolidone Calcium C10-C16 alkylbenzene Sulphonic acid in 2-ethylhexanol 381.5 76 used:Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 250 50 used: Termul 200 (non-ionic surfactant) Total 5898 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate 900g/L Passed pH at 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0t 0~~ (temperature at 5C) 0 to 2000cPs Viscosity 0 to 2000cPs (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? Description: AWAITS FURTHER
ANALYSIS
28/08/13,jb20105 amended cap specification.docx, 141 - 141 Trial # VIlA1 TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using DGME as a solvent using the current formulation of surfactants Ratio of Ninate 60E: Termul 200 (60:40) Anionic/Non-ionic surfactant Solvent used: Ninate 60E : Termul 200: DGME FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 898 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 528.5 106 used: Diethylene Glycol Monoethyl ether Calcium C10-C16 alkylbenzene Sulphonic acid in 2-ethylhexanol 388 77 used:Ninate 60E (anionic surfactant) Alkoxylated alkyl phenol 259 52 used: Termul 200 (non-ionic surfactant) Total 5911 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate 898g/L Passed pH at - 1% aq. Solution 4tol1 Specific gravity 100 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min Dark yellow to brown liquid, Dark yellow to brown (Cctemp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format 28/08/13,jb20105 amended cap specification.docx,142 - 142 Viscosity
---
(temperature at 5C) 0 to 2000cPs Viscosity (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a General Remarks aging to approximate 2 years. PASS or FAIL? Description: AWAITS FURTHER
ANALYSIS
28/08/13,jb20105 amended cap specification.docx,143 - 143 APPENDIX 5 Trial # E4ia TRIALLATE 850 TRIALS Triallate active present at 850g/L Trial details: Trial using Termul 1284 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1284 (30:70) Anionic/Non-ionic surfactant Solvent used: Ninate 60E: Termul 1284: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4471.4 850 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 828.2 166 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 185.8 37 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 453.4 91 used: Termul 1284 (non-ionic surfactant) Total 5938.65 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 1.0t .0n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 2ml cream @ Failed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.docx,144 - 144 brown liquid, Cold temp. stability Dark yellow to brown liquid, homogeneous, free from Passed (Accelerated Ageing) homogeneous, fre from phase phase separation in any separation in any format format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity 0 to 2000cPs n/a (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # E4ib TRIALLATE 850 TRIALS Triallate active present at 850g/L Trial details: Trial using Termul 1284 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1284 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1284: Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl 4471.4 848 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 834.2 167 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 393.0 78 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 250.9 50 used: Termul 1284 (non-ionic surfactant) Total 5949.4 28/08/13,jb20105 amended cap specification.docx,145 - 145 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 848g/L Passed pH at 4 to 10 7.21 Passed 1 %aq. Solution4t1 Specific gravity 1.00 to 1.30 1.165 Passed (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 4mL Passed brown liquid, Cold temp. stability Dark yellow to brown liquid, homogeneous, free from Passed (Accelerated Ageing) homogeneous, fre from phase phase separation in any separation in any format format Viscosity 0 to 2000cPs 56.9cps Passed (temperature at 5C) prature at 20C) 0 to 2000cPs 31.2cps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA Trial # E4iia TRIALLATE 800 TRIALS Triallate active present at 800giL Trial details: Trial using Termul 1284 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1284 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1284: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4212.0 800 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 1087.9 218 28/08/13jb20105 amended cap specification.docx,146 - 146 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 186.2 37 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 453.2 91 used: Termul 1284 (non-ionic surfactant) Total 5939.25 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate n/a pH at 4 to 10 n/a 1% aq. Solution Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 3ml of cream Failed re-emulsion after 24h @ bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity 0 to 2000cPs n/a (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED 28/08/13,jb20105 amended cap specification.docx, 147 - 147 Trial # E4iib TRIALLATE 800 TRIALS Triallate active present at 800g/L Trial details: Trial using Termul 1284 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1284 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1284: Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl 4208.3 801 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 1086.6 218 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 378.2 76 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 253.3 51 used: Termul 1284 (non-ionic surfactant) Total 5926.3 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance a yellow to brown liquid, Brown liquid Passed Appearance homogeneous Pse Assay 825 to 875g/L Triallate 801 g/L Passed pH at 4 to 10 7.25 Passed 1% aq. Solution4to1 Specific gravity 1.00 to 1.30 1.149 Passed (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 4mL Passed 28/08/13,jb20105 amended cap specification.doex,148 - 148 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity 0 to 2000cPs 55.0cps Passed (temperature at 50) 0to20cs5.psPse perature at 200) 0 to 2000cPs 23.2cps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA Trial # E4iiia TRIALLATE 850 TRIALS Triallate active present at 850g/L Trial details: Trial using Termul 1285 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1285 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1285: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4469.3 850 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 833.1 167 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 187.6 38 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 447.3 90 used: Termul 1285 (non-ionic surfactant) Total 5937.3 28/08/13,jb20105 amended cap specification.doex,149 - 149 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 850g/L Passed pH at 4 to 10 7.15 Passed 1 %aq. Solution4t1 Specific gravity 1.00 to 1.30 1.170 Passed (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 4mL Passed Dark yellow to brown liquid brown liquid, Cold temp. stability homogeneous, free from pl ase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format perature at 5C) 0 to 2000cPs 57.5cps Passed perature at 200) 0 to 2000cPs 33.8cps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA Trial # E4iiib TRIALLATE 850 TRIALS Triallate active present at 850g/L Trial details: Trial using Termul 1285 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1285 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1285: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4472.0 849 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) 825.9 165 28/08/13,jb20105 amended cap specification.docx, 150 - 150 Solvent naphtha (petroleum), heavy aromatic used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 390.5 78 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 254.1 51 used: Termul 1285 (non-ionic surfactant) Total 5942.5 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 849g/L Passed pH at 4 to 10 7.23 Passed 1% aq. Solution4tl tperatur at 20C) 1.00 to 1.30 1.165 Passed <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 4mL Passed Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase Passed (Accelerated Ageing) homogeneous, free from pae paesprto nay Pse separation in any format phase separation in any format Viscosity 0 to 2000cPs 55.Ocps Passed (temperature at 5C) perature at 20C) 0 to 2000cPs 30.Ocps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA 28/08/13,jb20105 amended cap specification.docx,151 - 151 Trial # E4iva TRIALLATE 800 TRIALS Triallate active present at 800g/L Trial details: Trial using Termul 1285 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1285 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1285: Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyi(thiocarbamate) 4216.8 798 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 1094.0 218 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 194.8 39 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 455.7 91 used: Termul 1285 (non-ionic surfactant) Total 5961.2 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 798g/L Passed pH at 1% aq. Solution 4tol1 7.13 Passed Specific gravity (temperature at 20C) 1.00 to 1.30 1.155 Passed <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 4mL Passed 28/08/13,jb20105 amended cap specification.docx, 152 - 152 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity (temperature at 5C) 0 to 2000cPs 53.9cps Passed perature at 200) 0 to 2000cPs 45.Ocps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA Trial # E4ivb TRIALLATE 800 TRIALS Triallate active present at 800g/L Trial details: Trial using Termul 1285 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1285 (60:40) AnioniclNon-ionic surfactant Solvent used: Ninate 60E: Termul 1285: Recosol 150 FORMULATION Component Amount, g Loading, glL (Chemical name) S-2,3,3-tricholoroallyl 4210.0 800 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 1086.9 217 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 384.6 77 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 259.0 52 used: Termul 1285 (non-ionic surfactant) Total 5940.35 28/08/13,jb20105 amended cap specification.docx,153 - 153 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 800g/L Passed pH at 4 to 10 7.07 Passed 1% aq. Solution4to1 Specific gravity 1.00 to 1.30 1.150 Passed (temperature at 200) <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 3mL Passed Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity 0 to 2000cPs 51.3cps Passed (temperature at 50) 0t 00~ 1.csPse perature at 200) 0 to 2000cPs 27.5cps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA 28/08/13,jb20105 amended cap specification.docx, 154 - 154 APPENDIX 6 Trial # E4ia TRIALLATE 850 TRIALS Triallate active present at 850g/L Trial details: Trial using Termul 1284 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1284 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1284: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4471.4 850 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 828.2 166 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 185.8 37 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 453.4 91 used: Termul 1284 (non-ionic surfactant) Total 5938.65 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity 1.00 to 1.30 la (temperature at 20C) - - n <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 2ml cream @ Failed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.doex,155 - 155 Dark yellow to brown liquid, brown liquid, Cold temp. stability Darkgyeo to bro liqid homogeneous, free from (Accelerated Ageing) homogeneous, fre from phase phase separation in any Passed separation in any format format Viscosity 0t 0~~ / (temperature at 5C) 0 to 2000cPs n/a Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED Trial # E4ib TRIALLATE 850 TRIALS Triallate active present at 850g/L Trial details: Trial using Termul 1284 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1284 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1284: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4471.4 848 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 834.2 167 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 393.0 78 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 250.9 50 used: Termul 1284 (non-ionic surfactant) Total 5949.4 28/08/13,jb20105 amended cap specificationdocx, 156 - 156 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 848g/L Passed pH at 1% aq. Solution 4tol1 7.21 Passed Specific gravity 1.00 to 1.30 1.165 Passed (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 4mL Passed Cold temp. stability Dark yellow to brown liquid, homognou free from (Cleatedp. staglin) homogeneous, free from phase haseseon in any Passed (Accelerated Ageing) separation in any format phase separation in any Viscosity - (temperature at 5C) 0 to 2000cPs 56.9cps Passed Viscosity (temperature at 20C) 0 to 2000cPs 31.2cps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA Trial # E4iia TRIALLATE 800 TRIALS Triallate active present at 800g/L Trial details: Trial using Termul 1284 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1284 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1284: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4212.0 800 eg. Triallate Tech (95% purity) 1087.9 218 28/08/13jb20105 amended cap specification.docx,157 - 157 Solvent naphtha (petroleum), heavy aromatic used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 186.2 37 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 453.2 91 used: Termul 1284 (non-ionic surfactant) Total 5939.25 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate n/a pH at 4 to 10 n/a 1% aq. Solution4o1 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 3ml of cream Failed re-emulsion after 24h @ bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE EMULSION CHARACTERISTICS FAILED 28/08/13,jb20105 amended cap specification.docx, 158 - 158 Trial # E4iib TRIALLATE 800 TRIALS Triallate active present at 800gIL Trial details: Trial using Termul 1284 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1284 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1284: Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4208.3 801 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 1086.6 218 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 378.2 76 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 253.3 51 used: Termul 1284 (non-ionic surfactant) Total 5926.3 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 801g/L Passed pH at 1% aq. Solution 4 to 10 7.25 Passed Specific gravity (temperature at 20C) 1.00 to 1.30 1149 Passed <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 4mL Passed 28/08/13,jb20105 amended cap specification.docx,159 - 159 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format mperatue at 50) 0 to 2000cPs 55.Ocps Passed Viscosity 0 to 2000cPs 23.2cps Passed (temperature at 200) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA Trial # E4iiia TRIALLATE 850 TRIALS Triallate active present at 850g/L Trial details: Trial using Termul 1285 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1285 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1285: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4469.3 850 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 833.1 167 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 187.6 38 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 447.3 90 used: Termul 1285 (non-ionic surfactant) Total 5937.3 28/08/13jb20105 amended cap specification.docx, 160 - 160 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 850g/L Passed pH at 1% aq. Solution 4tol1 7.15 Passed Specific gravity 1.00 to 1.30 1.170 Passed (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 4mL Passed Cold temp. stability Dark yellow to brown liquid, brown liquid, Codtm.saiiyhomogeneous, free from paePse (Accelerated Ageing) homogeneous, free from phase phase separation in any Passed separation in any format format Viscosity (temperature at 5C) 0 to 2000cPs 57.5cps Passed Viscosity (temperature at 20C) 0 to 2000cPs 33.8cps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA Trial # E4iiib TRIALLATE 850 TRIALS Triallate active present at 850giL Trial details: Trial using Termul 1285 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1285 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1285: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4472.0 849 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 825.9 165 28/08/13jb20105 amended cap specification.docx, 161 - 161 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 390.5 78 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 254.1 51 used: Termul 1285 (non-ionic surfactant) Total 5942.5 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 849g/L Passed pH at 723 Passed 1% aq. Solution 4to13 tempratu at 20C) 1.00 to 1.30 1.165 Passed <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 4mL Passed Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format perature at 5C) 0 to 2000cPs 55.Ocps Passed Viscosity (temperature at 20C) 0 to 2000cPs 30.0cps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA 28/08/13,jb20105 amended cap specification.docx, 162 - 162 Trial # E4iva TRIALLATE 800 TRIALS Triallate active present at 800g/L Trial details: Trial using Termul 1285 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1285 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1285: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4216.8 798 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 1094.0 218 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 194.8 39 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 455.7 91 used: Termul 1285 (non-ionic surfactant) Total 5961.2 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 798g/L Passed pH at 7.13 Passed 1% aq. Solution 4 to 10 Specific gravity 100 to 1.30 1.155 Passed (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 4mL Passed 28/08/13,jb20105 amended cap specification.docx,163 - 163 brown liquid, Cold temp. stability Dark yellow to brown liquid, homogeneous, free from Passed (Accelerated Ageing) homogeneous, fre from phase phase separation in any separation in any format format Viscosity 0 to 2000cPs 53.9cps Passed (temperature at 5C) Viscosity 0 to 2000cPs 45.Ocps Passed (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA Trial # E4ivb TRIALLATE 800 TRIALS Triallate active present at 800g/L Trial details: Trial using Termul 1285 as non-ionic surfactants against Ninate 60E varying Triallate concentration Ratio of N60E: Termul 1285 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E: Termul 1285: Recosol 150 FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl 4210.0 800 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 1086.9 217 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 384.6 77 used: Ninate 60E (anionic surfactant) Castor Oil Ethoxylates 259.0 52 used: Termul 1285 (non-ionic surfactant) Total 5940.35 T 28/08/13,jb20105 amended cap specification.doex, 164 - 164 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 800g/L Passed pH at 1% aq. Solution 4 to 10 7.07 Passed Specific gravity 1.00to 1.30 1.150 Passed (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no cream @ Passed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min 3mL Passed Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) homogen fre frmas phase separation in any separation in any format format Viscosity (temperature at 5C) 0 to 2000cPs 51.3cps Passed Viscosity Passed (temperature at 20C) 0 to 2000cPs 27.5cps Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: SOLUTION TRIAL MEETS ALL CRITERIA 28/08/13,jb20105 amended cap specification.docx, 165 - 165 APPENDIX 7 Trial # E6a TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using combination of Teric PE62 and PE 64 as non-ionic surfactants with Triallate tech Ratio of N60E: Teric PE62 : Teric PE64 (60:24:16) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Teric PE62 : Teric PE64: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4743.4 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 563.3 113 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 380.7 76 used: Ninate 60E (anionic surfactant) Block Co-polymer used: PE 62 (non-ionic surfactant) 154.8 31 Block Co-polymer used: PE 64 (non-ionic surfactant) 104.2 21 Total 5946.2 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L Triallate n/a pH at - 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 (temperature at 20C) - n/a <2mL cream after 30 min, trace milky emulsion, 4mL Emulsion characteristics of oil after 30 min and complete cream@bottom Failed re-emulsion after 24h 28/08/13,jb20105 amended cap specification.docx, 166 - 166 Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0t 0~~ / (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD TEMP AND EMULSION CHARACTERISTICS FAILED Trial # E6b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using combination of Teric PE62 and PE 68 as non-ionic surfactants with Triallate tech Ratio of N60E: Teric PE62 : Teric PE68 (61:34:5) Anionic/Non-ionic surfactant Solvent used: Ninate 60E : Teric PE62 : Teric PE68: Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4743.8 896 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 574.1 114 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 397.6 79 used: Ninate 60E (anionic surfactant) Block Co-polymer used: PE 62 (non-ionic surfactant) 223.9 45 Block Co-polymer 34.7 7 28/08/13,jb20105 amended cap specification.docx,167 - 167 used: PE 68 (non-ionic surfactant) Total 5974.0 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion 3mL Emulsion characteristics of oil after 30 min and complete cream@botom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a temperature at 5C) 0 to 2000cPs Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a __ging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD TEMP AND EMULSION CHARACTERISTICS FAILED Trial # E6c TRIALLATE 900 TRIALS Triallate active present at 900giL Trial details: Trial using combination of Teric PE62 and TSP16 as non-ionic surfactants with Triallate tech Ratio of N60E: Teric PE62 : TSP 16 (61:24:15) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Teric PE62 : TSP16 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4735.7 891 28/08/13,jb20105 amended cap specification.doex, 168 - 168 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 564.1 112 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 430.0 85 used: Ninate 60E (anionic surfactant) Block Co-polymer used: PE 62 (non-ionic surfactant) 166.5 33 Block Co-polymer used: TSP 16 (non-ionic surfactant) 104.5 21 Total 6000.7 RESULTS OF FORMULATION Remark Parameter Required Results S Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace milky emulsion, 3mL Emulsion characteristics of oil after 30 min and complete cream@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity (temperature at 5C) 0 to 2000cPs Viscosity (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD TEMP AND EMULSION CHARACTERISTICS FAILED 28/08/13,jb20105 amended cap specification.docx, 169 - 169 Trial # E6d TRIALLATE 850 TRIALS Triallate active present at 900g/L Trial details: Trial using combination of Teric PE62 and PE64 as non-ionic surfactants with Triallate tech Ratio of N60E: Teric PE62 : Teric PE64 (29:43:28) Anionic/Non-ionic surfactant Solvent used: Ninate 60E : Teric PE62 : Teric PE64: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4469.1 849 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 834.5 167 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 186.1 37 used: Ninate 60E (anionic surfactant) Block Co-polymer 272.9 55 used: PE 62 (non-ionic surfactant) Block Co-polymer 176.0 35 used: PE 64 (non-ionic surfactant) Total 5938.5 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L Triallate n/a pH at 4t10n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, 3mL Emulsion characteristics of oil after 30 min and complete cream@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a 28/08/13jb20105 amended cap specification.docx, 170 -170 Dark yellow to brown liquid, Ao elem p. tabiiy homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD TEMP AND EMULSION CHARACTERISTICS FAILED Trial # E6e TRIALLATE 800 TRIALS Triallate active present at 900g/L Trial details: Trial using combination of Teric PE62 and PE64 as non-ionic surfactants with Triallate tech Ratio of N60E: Teric PE62 : Teric PE64 (30:42:28) Anionic/Non-ionic surfactant Solvent used: Ninate 60E : Teric PE62 : Teric PE64: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4210.5 800 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 1093.5 219 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 191.0 38 used: Ninate 60E (anionic surfactant) Block Co-polymer 267.0 53 used: PE 62 (non-ionic surfactant) Block Co-polymer 178.0 36 used: PE 64 (non-ionic surfactant) Total 5940.0 28/08/13,jb20105 amended cap specification.docx,171 - 171 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance h yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L Triallate n/a pH at n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky emulsion, 3mL Emulsion characteristics of oil after 30 min and complete cream@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD TEMP AND EMULSION CHARACTERISTICS FAILED Trial # E6f TRIALLATE 800 TRIALS Triallate active present at 900gIL Trial details: Trial using combination of Teric PE62 and PE68 as non-ionic surfactants with Triallate tech Ratio of N60E: Teric PE62 : Teric PE68 (30:59:11) Anionic/Non-ionic surfactant Solvent used: Ninate 60E : Teric PE62 : Teric PE68 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4210.5 800 eg. Triallate Tech (95% purity) 28/08/13jb20105 amended cap specification.docx,172 - 172 Solvent naphtha (petroleum), heavy aromatic 1093.0 219 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 191.0 38 used: Ninate 60E (anionic surfactant) Block Co-polymer 378.5 76 used: PE 62 (non-ionic surfactant) Block Co-polymer 67.0 13 used: PE 68 (non-ionic surfactant) Total 5940.0 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L Triallate n/a pH at n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity 0t 0~~ / (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD TEMP
FAILED
28/08/13,jb20105 amended cap specification.docx,173 - 173 Trial # E6g TRIALLATE 800 TRIALS Triallate active present at 900g/L Trial details: Trial using combination of Teric PE62 and TSP16 as non-ionic surfactants with Triallate tech Ratio of N60E: Teric PE62 : TSP16 (30:42:28) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Teric PE62 : TSP16 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4210.5 800 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 1093.5 219 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 191.0 38 used: Ninate 60E (anionic surfactant) Block Co-polymer used: PE 62 (non-ionic surfactant) 267.0 53 Block Co-polymer 36 used: TSP16 (non-ionic surfactant) 178.0 Total 5940.0 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L Triallate n/a pH at n/a 1% aq. Solution 4to1n Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.docx,174 - 174 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD TEMP
FAILED
28/08/13,jb20105 amended cap specification.doex, 175 - 175 APPENDIX 8 Trial # E3a TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E: Teric N2: Teric N8 (30:21:49) Anionic/Non-ionic surfactant Solvent used: Ninate 60E: Teric N2iTeric N8: Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4742.0 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 526.8 105 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 187.9 38 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 127.3 25 used: Teric N2 (non-ionic surfactant) Nonyl Phenol ethoxylates 319.5 64 used: Teric N8 (non-ionic surfactant) Total 5903.35 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 1.0ml of Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.docx,176 - 176 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystal Failed separation in any format Viscosity n/a (temperature at 5C) 0 to 2000cPs Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # E3b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E : Teric N2 : Teric N8 (30:42:28) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Teric N21Teric N8: Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4730.7 899 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 532.8 107 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 191.9 38 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 177.0 35 used: Teric N2 (non-ionic surfactant) Nonyl Phenol ethoxylates 269.5 54 used: Teric N8 (non-ionic surfactant) Total 5901.7 28/08/13,jb20105 amended cap specification.docx,177 - 177 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4to1n Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 1.0ml of Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystal Failed separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # E3c TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E : Teric N2 : Teric N13(30:28:42) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Teric N2/Teric N13 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4739.5 901 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 525.2 105 used: Recosol 150 28/08/13,jb20105 amended cap specification.docx, 178 - 178 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 186.5 37 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 182.2 36 used: Teric N2 (non-ionic surfactant) Nonyl Phenol ethoxylates 266.5 53 used: Teric N13 (non-ionic surfactant) Total 5899.8 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH aq. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 2.Oml of Failed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystal Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB AND EMULSION CHARACTERISTICS FAILED 28/08/13,jb20105 amended cap specification.docx, 179 - 179 Trial # E3d TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E : Teric N2 : Teric N20(30:42:28) AnioniclNon-ionic surfactant/ Solvent used: Ninate 60E : Teric N2/Teric N20 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4740.1 898 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 532.1 106 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 195.8 39 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 268.1 53 used: Teric N2 (non-ionic surfactant) Nonyl Phenol ethoxylates 183.2 37 used: Teric N20 (non-ionic surfactant) Total 5919.25 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 2.Oml of Failed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, homogeneous, free from phase Formed crystal Failed separation in any format 28/08/13,jb20105 amended cap specification.docx,180 - 180 Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB AND EMULSION CHARACTERISTICS FAILED Trial # E3e TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E : Teric N2 : Teric N8(60:30:10) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Teric N2/Teric N8 : Recosol 150 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl 4729.5 901 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 523.7 105 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 376.3 75 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 190.4 38 used: Teric N2 (non-ionic surfactant) Nonyl Phenol ethoxylates 67.6 14 used: Teric N8 (non-ionic surfactant) Total 5887.4 28/08/13,jb20105 amended cap specification.docx, 181 - 181 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH aq. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 8.Oml of Failed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystal Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB AND EMULSION CHARACTERISTICS FAILED Trial # E3f TRIALLATE 900 TRIALS Triallate active present at 900giL Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E : Teric N2 : Teric N8(60:32:8) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Teric N2/Teric N8 : Recosol 150 FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl 4732.5 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 521.0 104 used: Recosol 150 28/08/13,jb20105 amended cap specification.docx,182 - 182 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 384.2 77 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 204.7 41 used: Teric N2 (non-ionic surfactant) Nonyl Phenol ethoxylates 58.4 12 used: Teric N8 (non-ionic surfactant) Total 5900.65 RESULTS OF FORMULATION Remark Parameter Required Results S Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4 to 10 n/a 1% aq. Solution4o1 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 5.Oml of Failed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (clatep sAiity homogeneous, free from phase Formed crystal Failed (Accelerated Ageing) separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB AND EMULSION CHARACTERISTICS FAILED 28/08/13,jb20105 amended cap specification.docx,183 - 183 Trial # E3g TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E : Teric N2 : Teric N13(60:32:8) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Teric N2/Teric N13 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4740.6 898 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 522.6 104 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 386.0 77 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 213.6 43 used: Teric N2 (non-ionic surfactant) Nonyl Phenol ethoxylates 53.6 11 used: Teric N13 (non-ionic surfactant) Total 5916.3 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4 to 10 n/a 1 %aq. Solution4tl Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 5.0ml of Failed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystal Failed separation in any format 28/08/13.jb20105 amended cap specification.docx,184 - 184 Viscosity 0t 0~~ / (temperature at 5C) 0 to 2000cPs n/a Viscosity 0t 0~~ / (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB AND EMULSION CHARACTERISTICS FAILED Trial # E3h TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E : Teric N2 : Teric N13(60:34:6) AnioniclNon-ionic surfactant Solvent used: Ninate 60E : Teric N2/Teric N13 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4740.7 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 529.1 106 used: Recosol 150 Calcium C1 0-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 383.8 77 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 220.8 44 used: Teric N2 (non-ionic surfactant) Nonyl Phenol ethoxylates 39.7 8 used: Teric N13 (non-ionic surfactant) Total 5913.95 28/08/13,jb20105 amended cap specification.docx, 185 - 185 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4t10n/a 1%aq. Solution 4to1n Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 8.0ml of Failed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystal Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB AND EMULSION CHARACTERISTICS FAILED Trial # E3i TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E : Teric N2 : Teric N20(60:34:6) Anionic/Non-ionic surfactant Solvent used: Ninate 60E : Teric N2/Teric N20 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4733.6 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 521.7 104 used: Recosol 150 28/08/13,jb20105 amended cap specification.docx, 186 - 186 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 377.5 76 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 223.4 45 used: Teric N2 (non-ionic surfactant) Nonyl Phenol ethoxylates 42.7 9 used: Teric 20 (non-ionic surfactant) Total 5898.8 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4 to 10 n/a 1% aq. Solution4tl Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 2.Oml of Failed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystal Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB AND EMULSION CHARACTERISTICS FAILED 28/08/13,jb20105 amended cap specification.docx, 187 - 187 Trial # E3j TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E : Teric N2 : Teric N20(60:36:4) AnioniclNon-ionic surfactant/ Solvent used: Ninate 60E : Teric N2/Teric N20 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4738.7 900 eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 527.2 105 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 378.9 76 used: Ninate 60E (anionic surfactant) Nonyl Phenol ethoxylates 230.4 46 used: Teric N2 (non-ionic surfactant) Nonyl Phenol ethoxylates 26.9 5 used: Teric 20 (non-ionic surfactant) Total 5902 RESULTS OF FORMULATION Remark Parameter Required Results s Appearance Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 875 to 925g/L triallate n/a pH at 4to10 n/a 1% aq. Solution Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 5.Oml of Failed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystal Failed separation in any format II 28/08/13,jb20105 amended cap specification.docx,188 - 188 Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB AND EMULSION CHARACTERISTICS FAILED 28/08/13,jb20105 amended cap specification.docx,189 - 189 APPENDIX 9 Trial # E5a TRIALLATE 900 TRIALS Triallate active present at 900gIL Trial details: Trial using Teric PE62 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Teric PE62 : n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4500.0 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Block Co-polymer 500.1 used: PE 62 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, homogeneous homogeneous Assay 875 to 925g/L Triallate pH at 4 to 10 1% aq. Solution Specific gravity 1.00 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete re-emulsion after 24h Persistent Foaming <60mL after 1 min Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase separation in any format Viscosity 0t 00p (temperature at 5C) 0 to 2000cPs Viscosity 0t 00p (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated aging to approximate 2 years. General Remarks PASS or FAIL? Description: 28/08/13,jb20105 amended cap specification.docx, 190 - 190 Trial # E5b TRIALLATE 900 TRIALS Triallate active present at 900g/L Trial details: Trial using Teric PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Teric PE64: n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4501.1 eg. Triallate Tech (95% purity) Block Co-polymer 501.1 used: PE 64 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, homogeneous homogeneous Assay 875 to 925g/L Triallate pH at 4 to 10 1% aq. Solution Specific gravity 1.00 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete re-emulsion after 24h Persistent Foaming <60mL after 1 min Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase separation in any format Viscosity 0t 0~~ (temperature at 5C) 0 to 2000cPs Viscosity 0 to 2000cPs (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated aging to approximate 2 years. General Remarks PASS or FAIL? Description: 28/08/13,jb20105 amended cap specification.docx,191 - 191 Trial # E5c TRIALLATE 800 TRIALS Triallate active present at 800g/L Trial details: Trial using Teric PE62 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Teric PE62: n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4001.1 eg. Triallate Tech (95% purity) Block Co-polymer 1001.1 used: PE 62 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, homogeneous homogeneous Assay 875 to 925g/L Triallate pH aq.Solution 4 to 10 Specific gravity 1.00 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete re-emulsion after 24h Persistent Foaming <60mL after 1 min Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase separation in any format Viscosity 0t 0~~ (temperature at 5C) 0 to 2000cPs Viscosity 0t 0~~ (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated aging to approximate 2 years. General Remarks PASS or FAIL? Description: 28/08/13,jb20105 amended cap specification.docx, 192 -192 Trial # E5d TRIALLATE 800 TRIALS Triallate active present at 800g/L Trial details: Trial using Teric PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Teric PE64: n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4002.1 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Block Co-polymer 1001.5 used: PE 64 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, homogeneous homogeneous Assay 875 to 925g/L Triallate pH at 4 to 10 1% aq. Solution Specific gravity 1.00 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete re-emulsion after 24h Persistent Foaming <60mL after 1 min Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase separation in any format Viscosity 0t 0~~ (temperature at 5C) 0 to 2000cPs Viscosity 0t 0~~ (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated aging to approximate 2 years. General Remarks PASS or FAIL? Description: 28/08/13,jb20105 amended cap specification.doex,193 - 193 Trial # E5e TRIALLATE 700 TRIALS Triallate active present at 700giL Trial details: Trial using Teric PE62 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Teric PE62: nla FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroalyl diisopropyl(thiocarbamate) 3500.1 eg. Triallate Tech (95% purity) Block Co-polymer 1501.0 used: PE 62 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, homogeneous homogeneous Assay 875 to 925g/L Triallate pHaq. Solution 4 to 10 Specific gravity 1.00 to 1.30 (temperature at 20C) 1 <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete re-emulsion after 24h Persistent Foaming <60mL after 1 min Cold temp, stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase separation in any format Viscosity 0t 0~~ (temperature at 5C) 0 to 2000cPs Viscosity 0t 0~~ (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated aging to approximate 2 years. General Remarks PASS or FAIL? Description: 28/08/13,jb20105 amended cap specification.doex, 194 - 194 Trial # E5f TRIALLATE 700 TRIALS Triallate active present at 700g/L Trial details: Trial using Teric PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Teric PE64: n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 3500.1 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Block Co-polymer 1501.0 used: PE 64 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, homogeneous homogeneous Assay 875 to 925g/L Triallate pH at4to1 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete re-emulsion after 24h Persistent Foaming <60mL after 1 min Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase separation in any format Viscosity 0 to 2000cPs (temperature at 5C) 0t 00~ Viscosity 0t 0~~ (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated aging to approximate 2 years. General Remarks PASS or FAIL? Description: 28/08/13,jb20105 amended cap specification.docx, 195 - 195 APPENDIX 10 Trial # E6a TRIALLATE 900 PATENT TRIALS Triallate active present at 850g/L Trial details: Trial using Teric PE62 as non-ionic surfactants with Triallate tech AnioniclNon-ionic surfactant/ Solvent used: n/a : Teric PE62: n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4474.2 856 eg. Triallate Tech (95% purity) Block Co-polymer 1426.7 287 used: PE 62 Total 5900.8 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 4 to 10 n/a 1 %aq. Solution4tl Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, traces of Failed re-emulsion after 24h oil@top,0.5ml of solidified cream &oi l@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity 0 to 2000cPs n/a (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. FAIL General Remarks FAIL PASS or FAIL? 28/08/13,jb20105 amended cap specification.docx,196 - 196 Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE EMULSION CHARACTERISTICS FAILED Trial # E6b TRIALLATE 900 PATENT TRIALS Triallate active present at 850g/L Trial details: Trial using Teric PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Teric PE64: n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4474.2 856 eg. Triallate Tech (95% purity) Block Co-polymer 1426.7 287 used: PE 64 Total 5900.8 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years.
28/08/13,jb20105 amended cap specification.docx, 197 -197 General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E6c TRIALLATE 900 PATENT TRIALS Triallate active present at 850g/L Trial details: Trial using Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Teric PE62 :Teric PE64: nla FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4474.2 856 eg. Triallate Tech (95% purity) Block Co-polymer 713.3 144 used: PE 62 Block Co-polymer 713.3 144 used: PE 64 Total 5900.8 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 4t10n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 1 ml of solidify Failed re-emulsion after 24h oil&cream@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability Darkgyeo to bro liqid liquid, homogeneous, free (Accelerated Ageing) homogeneous, fre from phase from phase separation in Passed separation in any format ayfra any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0t 00~ Viscosity 0t 0~~ / (temperature at 20C) 0Io200~
/
28/08/13,jb20105 amended cap specification.doex,198 -198 Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER ANALYSIS BECAUSE EMULSION CHARACTERISTICS FAILED Trial # E6d TRIALLATE 900 PATENT TRIALS Triallate active present at 850g/L Trial details: Trial using Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Teric PE62 :Teric PE64 : n/a HLB value: 13.0 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4474.2 856 eg. Triallate Tech (95% purity) Block Co-polymer 356.7 72 used: PE 62 Block Co-polymer 1070.0 215 used: PE 64 Total 5900.8 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at n/a 1% aq. Solution 4to1n Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 2mt of Failed re-emulsion after 24h traces of oil@top Persistent Foaming <60mL after 1 min n/a 28/08/13,jb20105 amended cap specification.docx,199 - 199 Dark yellow to brown liquid Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0t 0~~ / (temperature at 5C) 0 to 2000cPs n/a Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE EMULSION CHARACTERISTICS FAILED Trial # E6e TRIALLATE 900 PATENT TRIALS Triallate active present at 850g/L Trial details: Trial using Termul 203 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : n/a FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4474.2 856 eg. Triallate Tech (95% purity) Block Co-polymer 1426.7 287 used: Termul 203 Total 5900.8 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h 28/08/13jb20105 amended cap specification.docx,200 -200 Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity 0t 0~~ / (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E6f TRIALLATE 900 PATENT TRIALS Triallate active present at 850giL Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.1 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroally diisopropyl(thiocarbamate) 4474.2 856 eg. Triallate Tech (95% purity) Block Co-polymer 142.5 29 used: Termul 203 Block Co-polymer 385.0 78 used: Teric PE 62 Block Co-polymer 899.2 181 used: Teric PE 64 Total 5900.8 28/08/13,jb20105 amended cap specification.docx,201 - 201 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 n/a Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E6g TRIALLATE 900 PATENT TRIALS Triallate active present at 850g/L Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.1 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4474.2 856 eg. Triallate Tech (95% purity) Block Co-polymer 285.0 57 used: Termul 203 28/08/13,jb20105 amended cap specification.docx,202 - 202 Block Co-polymer 428.3 86 used: Teric PE 62 Block Co-polymer 713.3 144 used: Teric PE 64 Total 5900.8 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at n/a 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o20csn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 to 2000cPs n/a (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED 28/08/13,jb20105 amended cap specification.docx,203 - 203 Trial # E6h TRIALLATE 900 PATENT TRIALS Triallate active present at 850gIL Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.0 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4474.2 856 eg. Triallate Tech (95% purity) Block Co-polymer 427.5 86 used: Termul 203 Block Co-polymer 485.0 98 used: Teric PE 62 Block Co-polymer 513.3 103 used: Teric PE 64 Total 5900.0 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) 0Io200~ 28/08/13,jb20105 amended cap specification.docx,204 - 204 Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E6i TRIALLATE 900 PATENT TRIALS Triallate active present at 850giL Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: nla HLB value: 13.0 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4474.2 856 eg. Triallate Tech (95% purity) Block Co-polymer 570.8 115 used: Termul 203 Block Co-polymer 527.5 106 used: Teric PE 62 Block Co-polymer 328.3 66 used: Teric PE 64 Total 5900.8 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) 28/08/13,jb20105 amended cap specification.docx,205 - 205 <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 to 2000cPs n/a (temperature at 20C) Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E6j TRIALLATE 900 PATENT TRIALS Triallate active present at 850g/L Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.1 FORMULATION Component Amount, g Loading, giL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4474.2 856 eg. Triallate Tech (95% purity) Block Co-polymer 713.3 144 used: Termul 203 Block Co-polymer 570.8 115 used: Teric PE 62 Block Co-polymer 142.5 29 used: Teric PE 64 Total 5900.8 28/08/13,jb20105 amended cap specification.docx,206 - 206 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at n/a 1% aq. Solution 4to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 5C o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E7a TRIALLATE 900 PATENT TRIALS Triallate active present at 800g/L Trial details: Trial using Teric PE62 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Teric PE62 : n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4209.2 805 eg. Triallate Tech (95% purity) Block Co-polymer 1693.3 341 used: PE 62 Total 5902.5 28/08/13,jb20105 amended cap specification.docx,207 - 207 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 4t10n/a 1% aq. Solution 4to1n Specific gravity 1.00 to 1.30 n/a (temperature at 20C) Milky emulsion, no <2mL cream after 30 min, trace separation, traces of Emulsion characteristics of oil after 30 min and complete cream@top, 0.5ml of Failed re-emulsion after 24h solidified cream&oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0 to 2000cPs n/a (temperature at 50) Viscosity 0t 0~~ / (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks FAIL PASS or FAIL? Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE EMULSION CHARACTERISTICS FAILED Trial # E7b TRIALLATE 900 PATENT TRIALS Triallate active present at 800g/L Trial details: Trial using Teric PE64 as non-ionic surfactants with Triallate tech AnioniclNon-ionic surfactant Solvent used: nla : Teric PE64: nla FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4208.3 805 eg. Triallate Tech (95% purity) 28/08/13,jb20105 amended cap specification.docx,208 - 208 Block Co-polymer 1689.2 340 used: PE 64 Total 5897.5 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at n/a 1% aq. Solution 4to1n Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, oil@top, Iml Passed re-emulsion after 24h of cream&oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0 to 2000cPs n/a temperature at 50C) 0 to 2000cPs n/a Viscosity 0 o2Ocsn/a (temperature at 20C) 0t 00~ Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: AWAITS FURTHER ANALYSIS Trial # E7c TRIALLATE 900 PATENT TRIALS Triallate active present at 800g/L Trial details: Trial using Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Teric PE62 :Teric PE64: nla FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4210.8 806 eg. Triallate Tech (95% purity) 28/08/13,jb20105 amended cap specification.docx,209 - 209 Block Co-polymer 843.3 170 used: PE 62 Block Co-polymer 844.2 170 used: PE 64 Total 5898.3 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH aq. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, oil@top, 0.1ml Passed re-emulsion after 24h of cream&oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0t 0~~ / (temperature at 5C) 0 to 2000cPs n/a Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: AWAITS FURTHER ANALYSIS Trial # E7d TRIALLATE 900 PATENT TRIALS Triallate active present at 800g/L Trial details: Trial using Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Teric PE62 :Teric PE64 : n/a HLB value: 13.0 28/08/13,jb20105 amended cap specification.docx,2 10 -210 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4210.8 805 eg. Triallate Tech (95% purity) Block Co-polymer 421.7 85 used: PE 62 Block Co-polymer 1267.5 255 used: PE 64 Total 5900.0 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, oil@top, 1ml Passed re-emulsion after 24h of cream&oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown Cold temp. stability Dark yellow to brown liquid, liquid, homogeneous, free (Accelerated Ageing) homogeneous, fre from phase from phase separation in Passed separation in any format ayfra any format Viscosity (temperature at 5C) 0 to 2000cPs n/a Viscosity
-
(temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: AWAITS FURTHER
ANALYSIS
28/08/13jb20105 amended cap specification.docx,211 - 211 Trial # E7e TRIALLATE 900 PATENT TRIALS Triallate active present at 800giL Trial details: Trial using Termul 203 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4210.8 805 eg. Triallate Tech 95% purity) Block Co-polymer 1690.8 340 used: Termul 203 Total 5901.7 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity n/a (temperature at 5C) 0 to 2000cPs Viscosity 0t 0~~ / (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED 28/08/13,jb20105 amended cap specification.doex,212 -212 Trial # E7f TRIALLATE 900 PATENT TRIALS Triallate active present at 800gIL Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.1 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4210.0 806 eg. Triallate Tech (95% purity) Block Co-polymer 168.3 34 used: Termul 203 Block Co-polymer 456.7 92 used: Teric PE 62 Block Co-polymer 1063.3 214 used: Teric PE 64 Total 5898.3 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at n/a 1% aq. Solution 4to1n Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation rea@top, Failed re-emulsion after 24h cream&oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format 28/08/13,jb20105 amended cap specification.docx,213 -213 Viscosity n/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE EMULSION CHARACTERISTICS FAILED Trial # E7g TRIALLATE 900 PATENT TRIALS Triallate active present at 800g/L Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: nla : Termul 203 : Teric PE62 :Teric PE64: nla HLB value: 13.1 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4212.5 805 eg. Triallate Tech (95% purity) Block Co-polymer 342.5 69 used: Termul 203 Block Co-polymer 505.0 102 used: Teric PE 62 Block Co-polymer 842.5 170 used: Teric PE 64 Total 4212.5 805 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4tol1 n/a 28/08/13,jb20105 amended cap specification.doex,214 -214 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o20csn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E7h TRIALLATE 900 PATENT TRIALS Triallate active present at 800g/L Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.0 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) 4210.8 805 Block Co-polymer used: Termul 203 506.7 102 Block Co-polymer used: Teric PE 62 574.2 116 Block Co-polymer used: Teric PE 64 608.3 122 Total 5900.0 28/08/13,jb20105 amended cap specification.docx,2 15 -215 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E7i TRIALLATE 900 PATENT TRIALS Triallate active present at 800g/L Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.0 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4209.2 805 eg. Triallate Tech (95% purity) Block Co-polymer 678.3 137 28/08/13,jb20105 amended cap specification.docx,216 -216 used: Termul 203 Block Co-polymer 623.3 126 used: Teric PE 62 Block Co-polymer 387.5 78 used: Teric PE 64 Total 5898.3 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o20csn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E7j TRIALLATE 900 PATENT TRIALS Triallate active present at 800giL Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.1 28/08/13,jb20105 amended cap specification.docx,217 -217 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4213.3 806 eg. Triallate Tech (95% purity) Block Co-polymer 842.5 170 used: Termul 203 Block Co-polymer 675.8 136 used: Teric PE 62 Block Co-polymer 171.7 35 used: Teric PE 64 Total 5903.3 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 4tol1 n/a 1% aq. Solution Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED 28/08/13,jb20105 amended cap specification.docx,218 -218 Trial # E8a TRIALLATE 700 TRIALS Triallate active present at 700g/L Trial details: Trial using Teric PE62 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Teric PE62: n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 3688.3 705 eg. Triallate Tech (95% purity) Block Co-polymer 2215.8 446 used: PE 62 Total 5904.2 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity (temperature at 20C) 1.00 to 1.30 n/a <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, no Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? Description: AWAITS FURTHER ANALYSIS 28/08/13,jb20105 amended cap specification.docx,219 -219 Trial # E8b TRIALLATE 700 TRIALS Triallate active present at 700g/L Trial details: Trial using Teric PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Teric PE64: n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 3685.8 705 eg. Triallate Tech (95% purity) Block Co-polymer 2216.7 446 used: PE 64 Total 5902.5 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, 0.1ml Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: AWAITS FURTHER
ANALYSIS
28/08/13,jb20105 amended cap specification.doex,220 -220 Trial # E8c TRIALLATE 700 TRIALS Triallate active present at 700g/L Trial details: Trial using Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Teric PE62 :Teric PE64: n/a FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 3684.2 704 eg. Triallate Tech (95% purity) Block Co-polymer 1110.8 223 used: PE 62 Block Co-polymer 1110.8 223 used: PE 64 Total 5905.8 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4tol1 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, traces Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL?
PASS
28/08/13,jb20105 amended cap specification.docx,221 -221 Description: AWAITS FURTHER ANALYSIS Trial # E7d TRIALLATE 700 TRIALS Triallate active present at 700g/L Trial details: Trial using Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Teric PE62 :Teric PE64: n/a HLB value: 13.0 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroalyl diisopropyl(thiocarbamate) 3685.0 705 eg. Triallate Tech (95% purity) Block Co-polymer 555.8 112 used: PE 62 Block Co-polymer 1660.0 334 used: PE 64 Total 5900.8 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4to 10 Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, traces of Passed re-emulsion after 24h oil@top, traces of cream@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homogeneous, free from phase liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) 0t 00~ / Viscosity 0t 0~~ / (temperature at 20C) 0Io200~
/
28/08/13,jb20105 amended cap specification.docx,222 - 222 Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? PASS Description: AWAITS FURTHER ANALYSIS Trial # E7e TRIALLATE 700 TRIALS Triallate active present at 700giL Trial details: Trial using Termul 203 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 3690.0 704 eg. Triallate Tech (95% purity) Block Co-polymer 2222.5 447 used: Termul 203 Total 5912.5 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity n/a (temperature at 5C) 0 to 2000cPs Viscosity n/a (temperature at 20C) 0 to 2000cPs 28/08/13,jb20105 amended cap specification.doex,223 - 223 Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E8f TRIALLATE 700 TRIALS Triallate active present at 700g/L Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.1 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 3689.2 705 eg. Triallate Tech (95% purity) Block Co-polymer 220.8 44 used: Termul 203 Block Co-polymer 599.2 120 used: Teric PE 62 Block Co-polymer 1399.2 281 used: Teric PE 64 Total 5908.3 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at - 1% aq. Solution 4tol1 n/a Specific gravity n/a (temperature at 20C) 1.00 to 1.30 28/08/13,jb20105 amended cap specification.docx,224 - 224 <2mL cream after 30 min, trace Milky emulsion, no Emulsion characteristics of oil after 30 min and complete separation, cream@top' Failed re-emulsion after 24h cream o ttom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability liquid, homogeneous, free (Accelerated Ageing) homogeneous, free from phase from phase separation in Passed separation in any format ayfra any format Viscosity 0t 0~~ / tem erature at 5C) 0 to 2000cPs n/a Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE EMULSION CHARACTERISTICS FAILED Trial # E8g TRIALLATE 700 TRIALS Triallate active present at 700giL Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.1 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 3691.7 705 eg. Triallate Tech (95% purity) Block Co-polymer 447.5 90 used: Termul 203 Block Co-polymer 666.7 134 used: Teric PE 62 Block Co-polymer 1107.5 222 used: Teric PE 64 Total 5913.3 28/08/13,jb20105 amended cap specification.docx,225 - 225 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid' Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity n/a (temperature at 20C) 1.00 to 1.30 <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity n/a (temperature at 5C) 0 to 2000cPs Viscosity (temperature at 20C) 0 to 2000cPs n/a Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E8h TRIALLATE 700 TRIALS Triallate active present at 700g/L Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: nla : Termul 203 : Teric PE62 :Teric PE64: nla HLB value: 13.0 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 3686.7 705 eg. Triallate Tech (95% purity) Block Co-polymer 665.8 134 28/08/13,jb20105 amended cap specification.docx,226 - 226 used: Termul 203 Block Co-polymer 753.3 152 used: Teric PE 62 Block Co-polymer 793.3 160 used: Teric PE 64 Total 5899.2 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 4 to 10 n/a 1% aq. Solution Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Aol etem stabiy homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 to 2000cPs n/a (temperature at 5C) Viscosity n/a (temperature at 20C) to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED Trial # E8i TRIALLATE 700 TRIALS Triallate active present at 700g/L Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.0 28/08/13,jb20105 amended cap specification.doex,227 - 227 FORMULATION Component Amount, g Loading, gIL (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 3690.0 704 eg. Triallate Tech (95% purity) Block Co-polymer 887.5 178 used: Termul 203 Block Co-polymer 819.2 165 used: Teric PE 62 Block Co-polymer 515.8 104 used: Teric PE 64 Total 5912.5 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at n/a 1% aq. Solution 4to1n Specific gravity (temperature at 20C) 1.00 to 1.30 n/a <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity n/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED 28/08/13,jb20105 amended cap specification.docx,228 -228 Trial # E7j TRIALLATE 700 TRIALS Triallate active present at 700g/L Trial details: Trial using Termul 203, Teric PE 62 and PE64 as non-ionic surfactants with Triallate tech Anionic/Non-ionic surfactant/ Solvent used: n/a : Termul 203 : Teric PE62 :Teric PE64: n/a HLB value: 13.1 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 3686.7 704 eg. Triallate Tech (95% purity) Block Co-polymer 1113.3 224 used: Termul 203 Block Co-polymer 885.8 178 used: Teric PE 62 Block Co-polymer 220.8 44 used: Teric PE 64 Total 5906.7 RESULTS OF FORMULATION Parameter Required Results Remarks Appearance Dark yellow to brown liquid, brown liquid, Passed homogeneous homogeneous Assay 875 to 925g/L Triallate n/a pH at 1% aq. Solution 4 to 10 Specific gravity (temperature at 20C) 1.00 to 1.30 n/a <2mL cream after 30 min, trace Emulsion characteristics of oil after 30 min and complete n/a re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystals Failed separation in any format Viscosity 0 to 200cPs n/ (temperature at 5C) 0t 00~ 28/08/13,jb20105 amended cap specification.docx,229 - 229 Viscosity 0 o2Ocsn/a (temperature at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING BECAUSE COLD STABILITY FAILED 28/08/13,jb20105 amended cap specification.docx,230 -230 APPENDIX 11 i-k N C -e a sa n g TN -en u 1,A 2 7,5 742 SA on S g- sa F-a ,E a p :444 C;8 19o S - Ct ya~g I 7
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28/08/13,jb20105 amended cap specification.docx,234 -234 iC IETiOD TR A' L TE ,ust Aerded N4 Decerher '1 ePas cf: AMhl: 1 C1 221) Reagents SeA i An ytical gradeaene Anaytc Standard = A class Triisa star ac mineral Snard = Analyas grade diethy! pbthatate (CEP) Standard Sclution = Accurate welgh approximately 0G*g c'Traltate standard o a 100crm vo lr.etic ask.Acu lyweig ap.oximately o19 inrtern stndare Ito the flaA and dI Lte to uCre wth solvert Mix thoroagy Sample Preparation Accuatly wegh si-e samp - contain approximately 0.1g ' Talate. transfer til qatnt~v. ynto a m vo'metric flsk Accu vtely wC'up P7i iy O 11: i ' i;re standard the fas and diute to volume with solvent Mix thoroughly. Gas Chromatography Aralyse the ,aple soluon agarst the standard soluton Pm each sol to erthe same operating conditions. Operating paramerws are as fIlows' 1 'isn-rSmadu G-2010 2. Oolumrn EC,5 3 Camier gas NiMtre 4 Temper ures- - lrletLiner 260*C Deteor_______ 2BO*C Counr @ uHedin Ii0"C for 31 minutes Cotann @ Ramping 10Crm- Ut fo 7 m oues okCafumw @ Holding 250"C for 0 minutes Assay Determlrtlor Appride peak retention times are as listed'. .. at 1.so..ent 2.4 minutes (lerielw Standard -iterral standard 5.3 minutes | Tlate |arget 7.6 rnutes MeA lat caletoo of the target content Is as follows, Scr x Ar xISm x s /( XISSaMLs iscsd where: ______ ________________ 5tibrevIation Extension 7 concentration of target in standard ca___ concentation of target sample concntratin W intemai standard in standard r' MILconcentration of internal standard in sample target peak area of in standard target peak area afin sample T internall standard peak area in standard - internal standard peak ar on sarnple 28/08/13,jb20105 amended cap specification.doecx,235 -235 Au17 IOcanet KWINANA WA 66 Ah hnatoais Dhow &n TFi20. 14.5:8P Drrre 21 4:$A i Sme ID 101.Mtd: Sarnis TypeLnknown frinVolan : 100 DOa Nast C iCart~nM~aaPrject\T !laru024d 1 g Method Nase ~ C -GCacenv DFwjtctt l Vfrlm-nex Trnaluaemet.-od vad 0 97.o Trnahae (Amndud I ,!41. L xiraul tandard in ncr~nc The chromatogram is shown in Fig. 1. Ta Cnb ch he - 11ri a et ie Aren Aats fllgh Heitt Mark 1E# CgNae I S.309 223495 63083 101301 64.6 I DEP 2 7.669 13 91 16917 4642 '00 tiuliste TatM 3$428 00. 1594 10 28/08/13,jb20105 amended cap specification.docx,236 -236 The Imtrade T*=2 Austalia -K - NAW^ PO;A 95CMOW 65 Samj U) : 2010 11 IsTDlAmoum ;r DataNam : C Mskioa mDr4elct Ti r*ul 01012148*Lged Mtx!Nnm : C(; \D~onazs ojecltnaUactTrih.1gcm Trials u:w x vauaam:i BhkV1 0.6C/ fom tintk 112y/ DE Pknenstndard inace The chromatogram is shown in Fig. 2. Pet? al ChanS -tchme I Peak# Re Tin Area Arn% heigh H k* Mrk I4W Cp Narr 8 2192 100.0 %XM 100 00 DE? 7'o i2 9 00.0 99868 10000 28/08/13,jb20105 amended cap specification.docx,237 -237 tz r. Ocpbr O(8 94 19 0333 A trlia p " MW6W tFacradee;&(0) 9419 753 A 0lmDtt &Tia :2 201/ E4 6.:4 PM vi t -A m Sacpk .Nc Trallae 90CC Vajdao Spike Hiark Sampc D :201312I451 Sampk Typc; :1r rw njconVolm : 000 DNamse -CV2CzutonDa?dcl Triallatct201012I45B1gcd TDnese nonI Spikdllum 1 0200 fnnlaion bhca+Qij33' Ttiall I.998 LDEP mstandrd n0etn The chromatogram is shown in Fig. 3. Peak Table Cand1 - Cwmel I Peakt Rtne Ac Aret% }k#g~ kti% Wrk (D Ip Nr 1 539 218913 6L972 974 71571 I DEP 2 7649 98451 31 2 4 76 9.429 2trira Tui 1734* X 113998 10000 28/O8/13,jb20105 amended cap specification.doex,238 -238 I t 'X '"' "' cs Australia5 (,(,M( WA691 7 I 1,t N..:r Adlii )v a"' t ~T:Ifr9(J d $cB Nlctac Nary':. ~ ~ ~ j ~ 1 ~± Sp LW B~utk 2 -&2 J . 0,mt~ "l'F, I~~O Vi~JW r1,r The chromatogram is shown in Fig. 4. PekThLe1 Claom1 L C_1Adun,d E R .- C, inr Mut An". t v Mini ID; mp .__ ~ .6f ......... .. . 42 439: 3vQ 9 2I&IAue Ta~~~~II ~ 1525 j eJO W249 S .07 28/08/13,jb20105 amended cap specification.docx,239 -239 Telepk n.. (00) 9419 793 7Australia ' S ^KANAW 1O x 11COMO WA Mi2 AysisDa&Tm 201/ :14634:8 PM L~rNit, : AdinI Saria Name :ti1rsue,0D Vaiida2 Spie lank 3 Sampi : 2002lt43 Samp age ype Unknown S1AjaVunte : O Dal Nae : C-CAPia I ra wI me a 1 $14 cet Mehtd Na CAaoa2 jj n: -e [Desription] Spiked Bluio:st 0.33 pf Rrmln l n 1.266g/L Trndii we I.19/ DE? inteamal adsud in anfltmc The chromatogram is shown in Fig. 5. Pcak Ttble CharuwII - Chaa Peak# RetTime Arm Armt Hcighr Heig% Mrk IDI CanpdNrm I 5.309 22070 5S9S 99182 5&71t4 DL? 2 7.67 I16 66 41342 Z2.l 41.286 2 IrnC le Tota A826 OOKJ l 1711 $^twU.00 28/08/13,jb20105 amended cap specification.doex,240 - 240 Intrade TelcpLo:" 9410 Australi OrxtKWAANA WA 6167 IU x 3x C0MO WA 6952 Analysis Date & *nc 210 /fl14 3:3r34 PM vizi : 2 Sa:>::Nae Triallase ete va e tiLEriy samipe D :201012llt Sampin Typo Unknown Injertion Voiume l$TD A K:1:>urat Dnaw lec: C:XGCmolu i P~aajcaTnnlis&e'0 10124L tgod Method Nam . C.P&Csl& r adt~fl&petD riadTrialngnrn Tralate re d nuhdurmn: Liacx*it-a 0.L 4 iallailed i .097/1 LDE? in sr-ml1dard irn acmoe The chromatogram is shown in Fig. 6. Pek Table m C diaanl - ChameltI I# 1.. 4 i Arne Arna% Ieight HEgbr% Mark Ri CmpdNme 1 5.307 216165 7A441 9523 727 1 DEP 2 7466? 91001 29.559 373 27 678 2 tIsrill Txa 307866 100.000 134346 l u1 A0 28/08/13,jb20105 amended cap specification.docx,241 -241 Imtrade Tpe)9 U /4Facsimile: (38 94.9 7f16 as17 Ocan htcct KWLJANA WA 6167 HOB I95 C UMOWA5 Ai:adysbDnee& Time :02'1.74 34:35 PM Vi i '2 Spt Name Tidallare 9EC Whaa Linrity2 Scipe iD2Ofl 4L2 arown inoeun Vume I.0L Data Na C:'~k t~Aionn ~aa1ec l ialWa2O1 14L2.gcd Method Narme C:WCs-lutonatdc~jct in MT ag roDescrnpio Tri~dlniw r#edx validnag: Linafry 2- 98l Tdait t 109$5 DRP mnsmai srtardrd in actne The chromatogram is shown in Fig. 7. Peak Tacea Chianned - Citai I Perk* RetTIma Arm An% TEdf Hkrt% Mark mD# CmpdNamns 1 53A 2126:4 67.62 2492 69.7:14 1 OPE 2 7-6 10430M 32378 42638 30234 aUe t 22162 00100 140935 100.000 28/08/13,jb20105 amended cap specification.doex,242 - 242 (0) 919 0333 acnmid e {kf00 9419 7516 I7AOscar Str KWINANA WA 6 167 - P I 395 CAMO WA 6952 Ana'.s Dale& Tm 21 1 2uL4.3:57:36 PM User Nrcn Admi, ViaiS : Sampl Nam. nTrijta* IC a n irAreiy3 Sample I) : 2$101 14,3 Sarnple Type :Urknwm bsjetnt Voine :DLI ISTD AmourAt Dana Nimr - CW~isJlutici atai~wjert1\TriJliate\2O1012I4L3.gcd Methodi Nwurc C C:23CalkIc id?rujc1\TriaJ Trialuae gan Trialiste method validamt: Linearit 3 -0904 Thaint ,0.i tgL DEP inmtd samdard in ecvAme The chromatogram is shown in Fig. 8. PeekTaihnril- Cone I Pcds# RtT A Arca% heir Heigh % Mari TD* Caipdwnir 126 644 1 9,010 661 2 .666I | 11a91 35s,2 4814$ 1677tra:: Tutd 336451 00 T I 487 0[ i 28/08/13,jb20105 amended cap specification.docx,243 - 243 :08)94 333 Facslie (0) 99 7f 7 t Oc SIrmK WINANA WAf 67 N, IfI ox 95 lOMO WA"L 6952r AnTyis Daie & Time 21C2/14 4:09:3 PM Vialk : SaipL Narna Trajale 9U0: VIlidation LinemIty 4 aalpD :20102 4,.4 T aipe Type ;^ W own kjecion Volume ; O.0 150D Aiirantb Hilt'- I14 Upl ' b TOW Nam: C I Illn .h3>te et ;a rrs2pI{ 1 AiA aed Muhod Nam : C .G~oltodnDamiGefte Yi rbsAralacti: fTlecpiornl Trill methd vnJidatio: innrty 4 -I1 O0g/L ITrate - 1.95g'L DEP ir-:J a#rdend ijn rewncm The chromatogram is shown in Fig. 9. Peak Tt abt Chnal - Chanrel I IPEM RaImeh Arem Asen% Ueight Height% Mark IDN Cmpd Name I 5,36 2179O3 61.212 99220 64165 1 DEP 2 7667 112 Mfl 37.7* 5417 Th5 2 trinate 34%610 IX)10~t 15;4W XM 28/08/13,jb20105 amended cap specification.docx,244 - 244 Australia 4i4a" S ' K ANA WA1 P6 Bo 39 COM) WA 6952 Analsis Dtc & Timn 2010124 42 :0tPM User Nn A drnia V inY -5 pr Nim- Triate 9X.'C Vidation Eierity C STnrple ID :s 2o10 4 .5 Pmrtp Ty-l peffnd : Unkanwn ISTTlS Am40 D N" C K2lt.3 tn cictITriua2 I214L5acd icibod Nam: :C:'C'solutidmfriecilTriallWiTrile m Triiaihtc medhad validatica: iiwmrity 5 -1L 104g&7 Trinate + 1 A1954 DEP iatnt. standard in acctcae The chromatogram is shown in Fig. 10. Pea' Table Clwmel - Chmnrne I Penkf RtTinm An Ariu% Height Heigit% Mak 101 Capd Nma 1 3'6 21724 59850 97733 61931 1 DEP 2 7.6t Iev$ 4Ot %90 60076 31. 09 2Ztrialkee_ Taal36.3233 100.Di 157109 1 DCUl 28/08/13,jb20105 amended cap specification.docx,245 - 245 LmtadeFacsimile (08) 941i9 75.l6 Astra ia I J5 CMC WA t,6 Analyst Dame& Trm 201./1 A4N: PM Use nName Adm Viei :6 Eamplc Nmrc Trizliste 900C Valite U neef 6 amlpl ID 2010121A4 Sampic ypc Unknown in:ction Ve- LOr I The Ahrmator mi hw nFg 1 Dara Nune CM l >ikn hjf t (uin TiZl I U! 14L6.gg Mer4hnx Name CWiCsuotYr t rojg r.Taaiaid4altrgo T ia.|he tred wasdanaca Linearity 6 - L4g*L Tria~me + .334 L DEV? imqad sicrkm in acbcnc The chromatogram is shown in Fig. 11. Peak TuibleChannel - Cianr I Pea'rA RctTinme Am Ares% Height Ikeight% Mark IN Cripd Nnm 1 tPO2 223658 56.317 W00SJ6 Stts 1 DIE? 7 766 173 480 4 . 7219 4L915 2 tidat -TJ~ m 31 1.000D 4'72225 1.00-to 28/08/13,jb20105 amended cap specification.docx,246 - 246 Imtrade 'r -s " 7 A t n SreetKWNAA W i Ana~vse Da"& Tirc : 2010/12:14 4:5:36 PM Uer Name Admk u-npe MNse: Trinile 900EC Yalidaion Precisinng Satap]CD :0124Pi Samie Typ ei n tt . 00 Dea NuncC:'LK'a namDaalosjee: Thialiar:J 0u: 1 . cd Meibud N a C:0- tonU'mrjcc TIiaflmie';iriantktin [Derripion Trisllatc mcthd validation: Pietciom 1 D(1l g/L i T n u+ .95j% DEP bItermel gwode Lnacon The chromatogram is shown in Fig. 12. tmt Arm Amii% icaiP I tig% Mark D Cm, Nae 1 537 2 7160 6-'231 98S39 64.193 I DE1' 2 6:S:795 7,769 54f25 31802 2 friaikze Total 34355 100.00 1 313 ( 10430 28/08/13,jb20105 amended cap specification.docx,247 - 247 Teskpone: (8) 9410tOWJ Inr Facuir-k (6O) 9 4 7516 s 17 Ocean Street KW.NANA WA C167 Box 394 COO WA 1 952 Annyr |Uate & Time :U1WlZ14 4:tt3VM User Narc A drri Sample Name Trzluc 9CEC VaEldatin PreJalon 2 SamplelID 12 1 2fP Srnpl Type 1SD Amnoum Da mIKin D hpc I Aralitc.211 12r"4 P2 ycd MatctdNa~nr :C.GCflior I~ et LaraallarqdTm4Ilatgi [Dcecripdi-1] Triafate method v'is tion: Precisin 2 -<* pylig Trinala.e + L095g1LWE iinia standard in astone The chromatogram is shown in Fig. 13. Pei ak: Clwumiel - CmAsnwl I PA Atcj% Hdghn Hear% Mrnk TD# Cmpd Na 508 212 62.20 97071 633 49 1 DE? 2 7.6 13J4. 793 S4727 36.1- 2 triallat Ti3429 0.00 IS180$ 10o.U4 28/08/13jb20105 amended cap specification.docx,248 - 248 LImtrade Fa*O "9 ;~ Australia """" -"*IA^ ^WA 67 A ~ ~ ~ ~ ~~r ui ass,- coi wA ' es: A1 J !1 Analysflater&fTm: - 701'12I4S51Qt16 PM Viat#:4 aup: NAm : Trillae 9OEC Validation Precisien 3 D 2 C : 20C 12 4P3 Sarnp' TCyp : Urdnown Injection Volure : .00 1D Amot ; l~als.Neas;i C:tshd~o in'rjctivraltse11714P3-ge Mtoo Name : OCeslnmaivnwrojectl\TriaMldTrisateum (Dcscription] Pnacsin 3 - LO1IL Triaia+ 1.095w1 DEP ntemal stWiard in aectore The chromatogram is shown in Fig. 14. Prak TauQiainc.A- Chaar: I PN&4 RetTime Ana Arcat% 1*rjiht HeightL Mark ID CmpdName 1 i301 21903J 62.249 99087 64.621 1 DP 2 132134 37 51 5422 5 2 tikn total 35 S67 1000 itiI Oxh 28/08/13,jb20105 amended cap specification.doex,249 - 249 ii (0 94 19 75 e 6 Australia ""-*''* K NNAWA 1 PO lika 195 COMOJ WA 6957 Anal & Thime :I012/14 :SO PM r Nsune di Vti$l :4 Samp$Nn Tria3ltae 900EC Vbdlsin Tht'i~iwm 4 Sempk D:201012]4P4 Smpl Type: Unkrown 4jci laVolume ;1, 0u [$0Amoa Dta1 Nam C9 GK so.;.a e rjea iI~flihsrie 12) 4.j ge Method Name : tJMil o;.Jomwraejo. bnldt'r ."rswi~Ja c icptinn ThI rialmit nitdgiron: Prcisnm4 - L.00OkgLTrislato 'IX,95ga . intmiel suri: inicar The chromatogram is shown in Fig. 15. Peak Tab Chanll Channel I ltk# RC:.1 Am Area% Hieight Hedght% Mark Kl# ) Cmpd Nana 5.3 217c9 62.237 9i027 64203 2 7.668 132 33 37.763 54636 33,797 2 irilelz Total 349900 I003). 152633 100.0(0) 28/08/13,jb20105 amended cap specification.docx,250 -250 FTphone:(0) M19 333 IFafde ctu94nie 91 7516 Austr a& .1? Cun Sntet KWINANA WA 61 6n PO Bx 395 COMO WA 6952 AJysd atn & Ttne :.201/1214 ) 34: PM UJr Narne :Admaar Vin# ;:4 Sample Nine : Ttrnilnrk 9IJOEC Vafduden PresidnaS Sorg LD : 20 31214P5 1gajeition Volname : 1.00 ISTD Amurnt Das Nor : KMi atngikttrjec11trisllat2 10 214P$.gcd %tvtnd Nane :C:'O nkPi atPrtocil\ riallaltTrieliScegcn 'Tria* redhod 1.. Jidati c Precision 5 -It.00.j Tie~Lute + L09%/L DEP ;itotal aardd it acetonc The chromatogram is shown in Fig. 16. lThak Table Cbnnel - Chaunel I Pe* R.The AJ*A Ast% Ueight R-gh% Mnrk If CFpdON 530* 215661 62.209 %6950 2 :fl flEP 7 66_ .i3 o 31. 9a i 446 .472 2 L __ilde Ti46jlT 10 A00 : t419 lot! 28/08/13jb20105 amended cap specification.docx,251 -251 APPENDIX 12 IMTRADE Confide nial pntacit P r-,a1nC t 17ET IL 20n2 17 API 2012.
28/08/13,jb20105 amended cap specification.docx,252 -252 FINDINGS 71ae @( 500 g ana applied as either Irade Avatar 00EC (Pmopose' n a Tr-aee 0C CRererenc=e cie di not arc a numbers or vsa bmass -educt WM sh low sown Kaspa peas reposenimg palse crops (Ta e I). Te ' ults sugest ha Imirade Avatar 90CEC is as safe to use on ba.w siwn Kaspa peas s made Tial atw 5000C herbicide. Table t Reduction in biomass and plant numbers vt two Ir7ad tr-ada herbicides Blomass reduction Reduction in plant numbers (K6) + Herbicide _ rate(visual estimate) standard error Reference 1.6 t/ha 0 4 ± 8E6 Proposed 890 mI/ha 0 4 ±42 Untreated 0 MATERIALS AND METHODS Shallow sown Kaspa peas (1 cm depth} were treated with 500 g aliha of tri -alate as Avatar Utra 900E C proposedd' or Tria late 5001 C referencel Rates: 1. 1.6 /ha 'Reference' 2.890 mi/ha 'Proposed' 3 Unsprayed Seed (6 per pot) were sown a 1cm depth in 10cm x 10cm pam and sprayed. The seed was then covered by 0Ci soil to simulate incorporation which is the ma common practice af applying pre-emergence herbicides in no -t agricult ure. Herbicide appliation was performed using a laboratory boom sprayer equipped with twin T jet fan nozzles at a speed of m . Output from the sprayer was calibrated at 110 1 ha' at a presure of 250 kPa. Using this testing procedure, volatiliation lasses wen minimised by the immediate and even incarporation of the herbicide. The experiment was conducted outdoors m a shade house in March-April 2012 as a randamised complete design with five replicatmors. Herbicide effects were measured 3 weeks after spraying, The number of pea seedlings that had emerged were counted and converted to reduction In plant numbers (Table 1). In addition, biarnass redutior was visually eWtirnted by compan to untreated plan (able Tirade consdaed 28/08/13,jb20105 amended cap specification.docx,253 -253 P Report Comparison of two Imtrade Triallate formulations: Imtrade Avatar Ultra 900 EC and Imtrade Triallate 500 EC on wheat safety and wild oat bioefficacy Cent: Imtrade Australia Trial Officer Dr Peter Boutsalis Date: 20 Novenber 2011 Executive Summary The trade Avatar Iltra 900 EiC and Imtrade TrilIate 500 EC h er tbicides offer equivalent efficacy on the target species at equal active equivalent application rates. Both products perftmed similarly in tIrns of In eir effct n n target spees . they displayed similar host crop safety cI racteristics. In ifct when applied at rats so as to deIver id etical amounts of kt actiVe igredien t (iallate). both pr ucts were Lquivalent in t rmts of hiefficacy and host c op sa ety.
28/08/13,jb20105 amended cap specification.docx,254 -254 Findings The effect oa ra e response of two pr ie-mrgent herbicide formulations on wh at safety and wild wat activity four weeks after apphcation was assessed The t wo formulations will be referred to as "proposed" nerbicide and ~eference herbiade. Details of the formulations are: "Proposed" - Innade Avatar Ultra 900 EC ilerbicd - Imtrade triallate 900g/L EC "Reference" - Imtrde Trialiate 500 IC Herbicide = itr triallate 500g/ EC Bloefflcacy: Both formula tions were highly of Uetive on wild oats with complete con rol achieved at haUth recommended raes (Figure 1). Efficacy tten observed in both pot and field trials does not alw ys correlate with yield losses as there are numerous factors apart rom herbicide efficacy that influences yAed. [n addition, herbicides are generally more act ive in pot triaLs due to optimum herbicide application, perfect growing conditions and the absence of stubble and other field factors which commonly hinder herbicide perfortan e. The mean percentage control of each herbicide on wild oats and wheat measured as a visual estimation of plant biomass reduction compared to untreated pots. The results are shown in Fig. 18. Error bars indicate the standard error of the means. Assessment was made 4 weeks after herbicide application.
28/08/13,jb20105 amended cap specification.docx,255 -255 3 Host Crop Safety: Ilelow 10% biom s r duc ton was ose rv at 400 g aijha oft te "propowd" herbicide compared to a statistically significant 15% tor the "reere h icide (Figure. A the recommended rates each product the difference on wheat safety wer nt statistical different Figure 1). Similady, at double the recommended rates of ch orrmu nation, tre were no statistically significant differences on whe- t safety. Thus there was a sigmicant diference ohserved between wheat and wild oat activity suggesting bot the "proposed" and "reference" formulations w uld be selective in a crop situaiiOn at the recommend rates "proposed" by lmtrade. Methods and Materials A pot trial was conducted by Plan; Science ConsultingIocated in Prospect, SA. The plant material asd was: Wheat varietyy Derrimut) and wid oats (Aveno strilis). Wheat was sown at 4cm depth and wild oats was sown at 2cm depth in A.55L pots containirg potting flux specially anared at the University of Adelaide. Five replicate pots were established for each herhicide treatment Standard error of the means wee calculated for 0ach herbicide trerment. Spraying was conducted in a cabinet sprayer located at the mversi ol Adelide,. Waite Campus. Th prayeroutpu was 00Ljha using twinT-Jet0 nozzleswith the boom moving at 3.6 km/. Each herbicide was sprayed onto th soil surface and hnen Scorporated immediately after sp saying to simulate an 18 system. The pots were kept outdoors in a shade-house and watered as required.
28/08/13,jb20105 amended cap specification.docx,256 -256 4 Appendm- taw Dat kdo'.aal put a Imn I ra w at tad r a" iki eats ad aI In asored a% a vimt ean SE f Iant bimanradadeaLcnire )aparedoua tedpaostsAasnrntwastade4wtskaafrterhideu pIlea. arr de seas~e cta WItD GATS n 'me 101 heta ____ ____ 0 2)uR m :."'4 o -Tv ex nCT 6 77- 28/08/13,jb20105 amended cap specification.docx,257 -257 IMTRADE Confidentidal Efficacy of Imtrade Avatar Ultra 900EC compared to lmtrade Triallate 500EC in combination with Imtrade Trifluralin 480EC on herbicide susceptible annual ryegrass activity. CLIENT: NEIL MCPHEE, IMTRADE Or Peter Boutslals, Plant Science Consulting 17 APRIL 2012 28/08/13,jb20105 amended cap specification.docx,258 -258 FINDINGS T -a late @ 500 g alha appild as a ihr Irntrace Avatar 900EC or rtrado Tri late 500C. herb do produced 85% corrol of herbicide susceptia ryegras buored at 1cm depth (Table 1) Addition of 175 Ltha a Triluralin 48020 horbictde to either ti-aate ou 4 -a resumed in the total control of ry oss. These resu s suggest thast cornritb of mrde Trituralin 480EC herbicide with ether irflrade Avitar 90EC or lmade Tri-allote S0EC wil rest in equal control of herblcde susceptibe Table 1, Percent control of herbicide susceptible ryegrass biotype (SLR4) with two Inrade tri-allate her idss an d corbrat ns w.i trade Trinurain 480EC. Control {%) + Herbicide rate standard error 6 L/ha Reference 85 2 1.6 L/ha Reference + L75 Lfha Influralin 48EC 100 ± 0 Proposed 890 nI/ha 85 1.8 Proposed 890 mi/ha + 15t/ha Trifluraln 480EC 98±16 Untreated Imtrade Conden al 28/08/13jb20105 amended cap specification.docx,259 -259 MATERIALS AND METHODS Herbicide suscop tiue ryegrass was tested wit h Avatar Ultra 900EC ('proposed ! u- Triallate Soar C'reference} comnblatons with Imtrade Trifluralin 480EC herbicide Rates* L 16 L/ha 'Reference' 2.1 5 t/ha 'Reference'+ 1.75 /ha lmtrade Tifluralin 480EC herbicide 3. 890 nd/ha 'Proposed' 4.890 ml/ha 'ProposedJ' - I 75Lha lmtrade Trifluralin 480C herbiade 5. Unsprayed Seed wa sown at 1cm depth in 10cm x 10cm pots and sprayed. The seed was then covered by 15cm soil to simulate incorporation which is the most common practice of applymg pre emergence herbicides in no-til agriculture. Herbicide application was performed using a laboratory boom sprayer equipped with twin 1 jet fan no:91 s at a speed of 1 ms" Output from the sprayer was calibrated at 110 L h& at a pressure of 250 kPa. Using this testing procedure, volatilisation losses were minimised by the immediate and even incorporation of the herbidde. The experiment was conducted outdoors in a shade hoaue in March-April 012 as a randomised complete design with five replications. Herbicide effects were measured 3 weeks after ,praying. Seedlngs were considered emerged if they had reached the 2-leaf stage at this time. Survival % was recorded by comparing the sur ving number of 2 leaved seedings in the sprayed treatments to the number present before spraying. Percentage control was calculated by subtracting % survival ftom 100 (Table 1)C

Claims (42)

1. An emulsifiable concentrate formulation of triallate including: as the sole active ingredient, triallate wherein the triallate comprises at least 600 g/L of the emulsifiable concentrate formulation, at least one solid, liquid-containing, or liquid agriculturally acceptable surfactant, and, optionally, at least one agriculturally acceptable solvent; wherein the liquid components of the emulsifiable concentrate formulation form a solubilizing moiety for triallate.
2. An emulsifiable concentrate formulation as claimed in claim 1 wherein the triallate comprises at least 700 g/L of the emulsifiable concentrate formulation.
3. An emulsifiable concentrate formulation as claimed in claim 1 wherein the triallate comprises at least 800 g/L of the emulsifiable concentrate formulation.
4. An emulsifiable concentrate formulation as claimed in claim I wherein the triallate comprises at least 850 g/L of the emulsifiable concentrate formulation.
5. An emulsifiable concentrate formulation as claimed in claim 1 wherein the triallate comprises at least 900 g/L of the emulsifiable concentrate formulation.
6. An emulsifiable concentrate formulation of triallate including: as the sole active ingredient, triallate, wherein the triallate comprises at least 600 g/L of the emulsifiable concentrate formulation; at least one solid, liquid-containing, or liquid, agriculturally acceptable surfactant; optionally, at least one agriculturally acceptable solvent; wherein the liquid components of the emulsifiable concentrate formulation form a 15/06/15,jb205((3) amended claims.docx,261 - 261 solubilising moiety for triallate, and wherein the triallate/solubilising moiety weight ratio is greater than 2.
7. An emulsifiable concentrate formulation of triallate as claimed in claim 1, wherein the triallate/solubilising moiety weight ratio is greater than 4.
8. An emulsifiable concentrate formulation of triallate as claimed in claim 1, wherein the triallate/solubilising moiety weight ratio is greater than 6.
9. An emulsifiable concentrate formulation of triallate as claimed in any one of claims 1 to 8, wherein said at least one optional agriculturally acceptable solvent for triallate comprises at least one member of the set consisting of petroleum-based aromatic hydrocarbons, diethyleneglycol monoethyl ether, dimethyl adipate, dimethyl succinate, n-methyl pyrrolidone, and xylene.
10. An emulsifiable concentrate formulation of triallate as claimed in claim 9 wherein said at least one optional agriculturally acceptable solvent is present in the range of from 0 to 400 g/L of the formulation.
11. An emulsifiable concentrate formulation of triallate as claimed in either claim 9 or claim 10 wherein the said at least one optional agriculturally acceptable solvent is present in the range of from 80 to 200 g/L of the formulation.
12. An emulsifiable concentrate formulation of triallate as claimed in any one of claims 9 to 11 wherein the said at least one optional agriculturally acceptable solvent is present in the range of from 80 to 120 g/L of the formulation. 15/06/15jb20 105((3) amended claims.docx.262 - 262
13. An emulsifiable concentrate formulation of triallate as claimed in claim 1, wherein the at least one solid, liquid-containing, or liquid agriculturally acceptable surfactant is at least one of a first surfactant chosen from the set consisting of alkylphenol alkoxylates, fatty acid alkoxylates, alkoxylated triglycerides and EO/PO diblock materials, wherein alkoxylate includes ethoxylate, propoxylate, and mixed ethoxylate-propoxylate, including multi-block ethoxylate/propoxylate materials.
14. An emulsifiable concentrate formulation as claimed in claim 13 wherein the at least one of a first surfactant is chosen from the set consisting of nonylphenol EO-PO diblock materials with one block having 7-11 EO (on an average basis) and the other block having 8-12 PO (on an average basis).
15. An emulsifiable concentrate formulation as claimed in claim 13 wherein the at least one of a first surfactant is chosen from the set consisting of alkoxylated triglycerides being alkoxylated castor oils (including castor oil 36 EO (on an average basis) and castor oil 54 EO (on an average basis)), and alkoxylated coconut oils.
16. An emulsifiable concentrate formulation as claimed in claim 13 wherein the at least one of a first surfactant is chosen from EO/PO diblock materials having EO block lengths in the range 12-35 and HLB values in the range 5-20.
17. An emulsifiable concentrate formulation as claimed in any one of claims 13 to 16 wherein the at least one of a first surfactant is present in the range of from 30 to 450 g/L of the formulation.
18. An emulsifiable concentrate formulation as claimed in any one of claims 13 to 16 wherein the at least one of a first surfactant is present in the range of 30 to 100 g/L of the formulation. 15/06/15,jb20105((3) amended claims.docx.263 - 263
19. An emulsifiable concentrate formulation as claimed in claim 1 wherein the at least one solid, liquid-containing or liquid agriculturally acceptable surfactant includes at least one of a second surfactant chosen from the set consisting of calcium alkylbenzene sulfonic acid in liquid concentrate form, alkylphenol ether sulphate/alkylamine ethoxylate salt, and alcohol ether sulphate/alkylamine ethoxylate salt.
20. An emulsifiable concentrate formulation as claimed in claim 19 wherein the at least one of a second surfactant is chosen from the set consisting of calcium alkylbenzene sulfonic acid salt in liquid form wherein the alkyl moiety, which may be straight or branched, is C 8 -C 1 4 alkyl.
21. An emulsifiable concentrate formulation as claimed in claim 20 wherein the alkyl moiety, which may be straight or branched, is Cio-C 12 alkyl.
22. An emulsifiable concentrate formulation as claimed in claim 19 wherein the at least one of a second surfactant is chosen from the set consisting of alkylphenol ether sulphate/alkylamine ethoxylate salt and alcohol ether sulphate/alkylamine ethoxylate salt, wherein the alkylamine moiety is C 14 -C 16 alkyl, including tallowamine.
23. An emulsifiable concentrate formulation as claimed in any one of claims 19 to 22 wherein the at least one of a second surfactant is present in the range of from 0 to 120 g/L of the formulation.
24. An emulsifiable concentrate formulation as claimed in any one of claims 19 to 22 wherein the at least one of a second surfactant is present in the range of from 30 to 100 g/L of the formulation. 15/06/15jb20 105((3) amended claims.docx.264 - 264
25. An emulsifiable concentrate formulation as claimed in claims 19 to 21 wherein the at least one of calcium alkylbenzene sulfonic acid is present, net of solvent, in the range from 15 to 60 g/L of the formulation.
26. An emulsifiable concentrate formulation of triallate as claimed in any one of the preceding claims, wherein the density of the emulsifiable concentrate formulation is at least 1.05 g/ml.
27. An emulsifiable concentrate formulation of triallate as claimed in the preceding claim, wherein the density of the emulsifiable concentrate formulation is at least 1.1 g/ml.
28. A method of preparing an emulsifiable concentrate formulation of triallate, having a composition as claimed in any one of claims 1 to 27, including the steps of: adding an agriculturally acceptable solvent for triallate to a clean empty formulation vessel; adding triallate which has been heated above its melting point to the formulation vessel in a series of addition steps each of which addition steps is followed by agitation of the contents of the formulation vessel; adding at least one agriculturally acceptable surfactant and additional agriculturally acceptable solvent, with the latter being used to clear residual surfactant from pumps or process lines used for the addition of the at least one agriculturally acceptable surfactant; agitating the resulting contents of the formulation vessel for at least 30 minutes; abstracting and testing a representative sample of the product according to a testing regime for specific gravity, pH 1% aqueous, emulsion characteristics, foam persistence, and active constituent content.
29. An emulsifiable concentrate formulation of triallate, wherein triallate is the sole active ingredient, including about 900 g/L triallate, about 106 g/L high flash-point aromatic hydrocarbon having a boiling range of 15/06/15jb20105((3) amended claims.docx.265 - 265 about 180 0 C - 210 C, about 46 g/L C 10 - C 16 linear alkylbenzene sulfonate (preferably calcium salt, preferably as 76 g/L of 60% solution in 2-ethyl hexanol), and about 50 g/L alkylphenol polyether EO/PO block copolymer (preferably 8-10 mol EO and 9-11 mol PO).
30. An emulsifiable concentrate formulation of triallate including: as the sole active ingredient, triallate, wherein the triallate comprises at least 600 g/L of the emulsifiable concentrate formulation; at least one solid, liquid-containing, or liquid, agriculturally acceptable surfactant; optionally, at least one agriculturally acceptable solvent; wherein the liquid components of the emulsifiable concentrate formulation form a solubilising moiety for triallate, and wherein the triallate/solubilising moiety weight ratio is greater than 2.
31. An emulsifiable concentrate formulation of triallate as claimed in claim 30, wherein the triallate/solubilising moiety weight ratio is greater than 4.
32. An emulsifiable concentrate formulation of triallate as claimed in claim 30, wherein the triallate/solubilising moiety weight ratio is greater than 6.
33. An emulsifiable concentrate formulation of triallate as claimed in any one of claims 30 to 32, wherein said an agriculturally acceptable solvent for triallate comprises at least one member of the set consisting of alkane compounds, aromatic compounds, alkylaryl compounds, alcohol-containing compounds, aldehyde-containing compounds, ether containing compounds, ester-containing compounds, ketone-containing compounds, lactam-containing compounds, amide-containing compounds, chlorinated compounds. 15/06/15jb20 105((3) amended claims.docx.266 - 266
34. An emulsifiable concentrate formulation of triallate as claimed in claim 33, wherein said an agriculturally acceptable solvent for triallate comprises at least one member of the set consisting of solvent naphtha (petroleum), heavy aromatic fraction, xylene, toluene, pyrrolidones, cyclohexanone, acetone, glycol ethers, ethyleneglycolmonobutylethers, propylene glycol monomethyl ether, methanol, ethanol, isopropanol, decanol, parrafins, hexane, acetic acid C 6 -C 8 branched alkyl ester.
35. An emulsifiable concentrate formulation as claimed in claims 30 to 34, wherein the at least one agriculturally acceptable surfactant comprises a non-ionic surfactant.
36. An emulsifiable concentrate formulation as claimed in the preceding claim, wherein said at least one agriculturally acceptable non-ionic surfactant is chosen from the categories in the set consisting of alkoxylated block polymers, alkoxylated alcohols, alkoxylated alkylphenols, alkoxylated amines, alkoxylated amides, alkoxylated fatty esters, alkoxylated oils, fatty esters, alkoxylated fatty acids, sorbitan derivatives.
37. An emulsifiable concentrate formulation as claimed in the preceding claim, wherein the at least one agriculturally acceptable non-ionic surfactant is chosen from the set consisting of nonylphenol ethoxylate, octylphenol ethoxylate, alkoxylated alkylphenol, vegetable oil ethoxylate, tristyryl phenol ethoxylates, alcohol ethoxylates, C 1 u-C 1 4 alcohols reacted with 2 moles EO, block copolymers such as polyoxyethylene/polyoxypropylene block copolymer, and fatty amine higher-mole ethoxylates which have non-ionic characteristics such as cloud point and compatibility with anionic surfactants. 15/06/15.jb2O 105((3) amended claims.docx.26 7 - 267
38. An emulsifiable concentrate formulation as claimed in any one of claims 30 to 33 wherein the at least one agriculturally acceptable surfactant comprises an anionic surfactant.
39. An emulsifiable concentrate formulation as claimed in the preceding claim, wherein the at least one agriculturally acceptable anionic surfactant is chosen from the categories in the set consisting of alkylaryl sulfonates; alkylarylsulfonic acids; carboxylated alcohol ethoxylates and alkylphenol ethoxylates; carboxylic acids/fatty acids; diphenyl sulfonate derivatives; olefin sulfonates; phosphate esters; phosphorus organic derivatives; sulfates and sulfonates of oils and fatty acids; sulfates and sulfonates of ethoxylated alkylphenols; sulfates of ethoxylated alcohols; sulfates of fatty esters; sulfonates of dodecyl and tridecylbenzenes; sulfonates of naphthalene and alkyl naphthalene; sulfonates of petroleum; sulfosuccinamates; alkoxylated amines; sarcosine derived surfactants such as, ammonium lauroyl sarcosinate; alkoxylates as above other than ethoxylates (such a propoxylates, butoxylates).
40. An emulsifiable concentrate formulation as claimed in the preceding claim, wherein the at least one agriculturally acceptable anionic surfactant is chosen from the set consisting of linear and branched alkylbenzenesulphonates and salts thereof which may be provided as a non-aqueous solution, (such as calcium Cio-C 14 alkylbenzenesulfonate), alkyl sulphates, alkyl ether sulfates, alkyl phosphates, alkyl ether phosphates, alkylphenol ether sulfate/tallow amine ethoxylate salts, and alcohol ether sulphate/tallow amine ethoxylate salts. 15/06/15,jb2O 105((3) amended claims.docx.268 - 268
41. An emulsifiable concentrate formulation as claimed in the preceding claim, wherein the at least one agriculturally acceptable surfactant is at least one cationic surfactant or at least one zwitterionic surfactant, or at least one cationic surfactant and at least one zwitterionic surfactant.
42. An emulsifiable concentrate formulation of triallate, containing, as the sole active ingredient, about 900 g/L of triallate, about 106 g/L of an agriculturally acceptable solvent being a petroleum-based aromatic hydrocarbon distillate fraction, about 50 g/L of a first agriculturally acceptable surfactant being an alkylphenol polyether EO/PO block copolymer, and a second agriculturally acceptable surfactant being a salt of an alkylbenzene sulfonic acid in 2 ethyl hexanol.
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US4276079A (en) * 1975-08-18 1981-06-30 Monsanto Company Synergistic herbicidal composition comprising N-(butoxymethyl)-6'-tert-butyl-2-chloro-o-acetotoluidide and triallate
EP0042688B1 (en) * 1980-06-19 1984-01-18 May & Baker Limited Weed control using 3-(4-isopropylphenyl)-1,1-dimethylurea in combination with s-2,3,3-trichloroallyl diisopropylthiocarbamate
US5045109A (en) * 1989-03-13 1991-09-03 Kumiai Chemical Industry Co., Ltd. High concentration herbicide formulation
US5180416A (en) * 1989-05-23 1993-01-19 Kumiai Chemical Industry Co., Ltd. Herbicidal composition comprising a liquid thiocarbamate herbicide, a solid herbicide, surfactant, and dry process silicic acid
US20030072776A1 (en) * 2000-01-06 2003-04-17 Jinxia Sun Emulsifiable concentrate compositions with silicone antifoams
WO2012024297A2 (en) * 2010-08-18 2012-02-23 Gowan Comercio Internacional E Servicos Limitada Improved processes for the control of undesired vegetative growth in crops

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Publication number Priority date Publication date Assignee Title
US4276079A (en) * 1975-08-18 1981-06-30 Monsanto Company Synergistic herbicidal composition comprising N-(butoxymethyl)-6'-tert-butyl-2-chloro-o-acetotoluidide and triallate
EP0042688B1 (en) * 1980-06-19 1984-01-18 May & Baker Limited Weed control using 3-(4-isopropylphenyl)-1,1-dimethylurea in combination with s-2,3,3-trichloroallyl diisopropylthiocarbamate
US5045109A (en) * 1989-03-13 1991-09-03 Kumiai Chemical Industry Co., Ltd. High concentration herbicide formulation
US5180416A (en) * 1989-05-23 1993-01-19 Kumiai Chemical Industry Co., Ltd. Herbicidal composition comprising a liquid thiocarbamate herbicide, a solid herbicide, surfactant, and dry process silicic acid
US20030072776A1 (en) * 2000-01-06 2003-04-17 Jinxia Sun Emulsifiable concentrate compositions with silicone antifoams
WO2012024297A2 (en) * 2010-08-18 2012-02-23 Gowan Comercio Internacional E Servicos Limitada Improved processes for the control of undesired vegetative growth in crops

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