AU2015100250B4 - High Load Triallate Emulsifiable Concentrate Formulations - Google Patents

High Load Triallate Emulsifiable Concentrate Formulations Download PDF

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AU2015100250B4
AU2015100250B4 AU2015100250A AU2015100250A AU2015100250B4 AU 2015100250 B4 AU2015100250 B4 AU 2015100250B4 AU 2015100250 A AU2015100250 A AU 2015100250A AU 2015100250 A AU2015100250 A AU 2015100250A AU 2015100250 B4 AU2015100250 B4 AU 2015100250B4
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triallate
trial
ninate
brown liquid
emulsion
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Ross Rainbird
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Imtrade Australia Pty Ltd
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Abstract

03/03/15,jb22520 innovation patent specification.doex,262 - 262 An emulsifiable concentrate formulation of iallate including: triallate wherein the triallate comprises at least about 600g/L of the emulsifiable concentrate for nul ation, and further comprising at least one agriculturally acceptable surfactant chosen from the set consisting of calcium alkylbenzenesulfonate in liquid concentrate form, alkylphenol ether sulphate/alkylamine ethoxylate salt. alcohol ether sulphate/alkylamine ethoxylate salt, alkylphenoil alkoxylates, fatty acid alkoxylates, alkoxylated triglycerides and EO/PO dibiock materials, wherein alkoxylate incliudes, eihoxylate, propoxylate and mixed ethoxylate propoxylate, including multi-block ethoxya/propoxyiate materials, and optionally further comprising at least one agiculturally acceptable solvent,

Description

03/03/15,jb22520 innovation patent specification.doex, 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.
03/03/15,jb22520 innovation patent specification.doex,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 [0006] The emulsifiers of the erulsifiable concentrates comprise at least one emulifier, which may bie a non-ionic surfactant, an ionic surfactant, or a bltnd of both typts of surfactans, 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 aides, alkox ylated fatty esters, alkoxylated oils, fatty esters, alkoxylated fatty acids, sorbitan derivatives, and the like. [00071 Typical ionic surfactants found, in em ulsifiers include alkylaryl sulfonates; aikvlarylsulfonic acids; carboxylated alcohol ethoxylates and alkylphenol ethoxylates; carboxylic a cids/fatt y acids; diphenyl sulfonate derivatives: olefin sulfonates; phosphate stirs; phosphorus organic derivatives; quaternary surfactants; sulfates and suifonates of oils and, fatty acids; sulfates and sulfonates of ethoxylated alkylphenols; sulfates of 03/03/15,jb22520 innovation patent specification.doex,3 -3 ethoxylated alcohols; sulfates of fatty esters; sulfonates of dodecyl and tridecyibenzenes; sulfonates of naphthalene and alkyl naphthalene; sulfonates of petroleum; sulfos uccinarnates; alkanolarnides; alkoxylated mines (with low EO values); sarcosine derived surfactants such as. ammonium lauroyl sarcosinate, and the like. [0008] Preferred emulsifiers may be alkoxylated alcohols and alkvphenols, 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 anine salts of ethoxylated alkyl phenol sulfates, e.g., that supplied under the trade nane WITCOLATE 1335 by Croipton Corporation, Witco Group. [p009] 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 cmusifier (surfactant) is preferably present at from about I 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 soiubility 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 soNents, such as vylenes; Co-C2 03/03/15,jb22520 innovation patent specification.doex,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-mnethyl pyrollidone; and ethers, such as dieth ylene glycol and dicthoxol. In addition, the solvent may include vegetable oils, methylated vegetable oils, petrol-oils, sugar esttrs of fatty acids, eg., sucrose esters, and the like, [0101] Preferred solvents may be C---C 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. o tional Iggleients [0013 Other addiives 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 sui table 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 trialate EC formulations contains at most 500g/L of trialiate active ingredient.
03/03/15,jb22520 innovation patent specification.doex,5 -5 which suggests that 500g/L represents an upper practical limit in the arnount 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 "riallate/solubilising rmoiety ratio" in a triallate EC, which may be calculated by dividing the weight of trial!ate active ingredient in a given weight of a triallate EC formulation by the weight of the siolublising 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 anounit of triallate formulation to a cultivation zone; 03/03/15,jb22520 innovation patent specification.doex,6 -6 2. The amount of high-quality packaging material that is utilized 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 flarnmability of triallate EC formulation; 6, The vapour pressure of solvent (frequently aroratic 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 tiallate in an EC formulation is associated with a lesser amount of solubilising moiety, ie., when the triallate/soiubilising inoiety ratio is greater.
03/03/15,jb22520 innovation patent specification.doex,7 -7 [0019] As an iflustration of pnor art, one rnay 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% 21- 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 + O.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 emu6 lsifiable concentrate formiulati of riallate including: triallate wherein the triallate comprises at least 600 giL of the ernulsifiable concentrate formulation, at least one solid, liquid-containing, or liquid agriculftraly acceptable surfacant, and, optionally, at least one agriculturally acceptable solvent; 03/03/15,jb22520 innovation patent specification.doex,8 wherein the liquid components of the emulsitiable concentrate fornulation form a solubilizing moiety for trialiate. [0023] The triallate may comprise at least 700 g/L of the emulsifiable concern trate formulation. [0024] The triallate may comprise at least 800 g/L of the emulsifiable concern trate 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 forrulation form a solubilising moiety for triallate, and wherein the triallate/solubili sing moiety weigh t ratio is greater than 2. [0028] According to another aspect of the invention there is provided an em tulsifiable concentrate formulation of triallate wherein the triallate/soiubilising moiety weight ratio is greater than 4. [0029] Accorchng to another aspect of the invention there is provided an emulsifiable concentrate formulation of triallate wherein the triallate/solubili sing rnoiety weight ratio is greater thwn 6.
03/03/15,jb22520 innovation patent specification.doex,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 mnoioethyl ether, dimiethyl 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 inven tioii 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. aikoxylates, alkoxylated triglycerides and EO/PO diblock materials, wherein alkoxyla-e includes thoxylate, propoxylate, and mixed ethoxylate-propoxylate. including multi-block ethoxylateipropoxyate 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 II EO (on an average basis) and the other block having 8-12 PO (on an average basis).
03/03/15,jb22520 innovation patent 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 alkoxyilaed 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 agriulturally acceptable surfactant includes at least one of a second surfactant chosen from the set consisting of calcium alkylbeizene sulfonic acid in liquid concentrate form, alkylphtenol ether sulphate/alkylaminc ethoxylate salt, and alcohol ether sulphate/alklamine ethoxylate salt. [0041] The at least one of a second surfactant may be chosen from the set consisting of calcium alkybenzene sulfonic acid salt in liquid form wberein the alkyl moiety, which may be straight or branched, is C-*Ci 4 alLyL. The alkyl moiety, which may be straight or branched. may be C 'C 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 CwC, alkyl, including tallowamine.
03/03/15,jb22520 innovation patent specification.doex, 11 - 11 [0043] The at least one of a second surfactant rnay 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 enul sifiable concentrate formulation; at least one solid, liquid -containing, or liquid, agr culturally acceptable surfactant; optionally, at least one agriculturally acceptable solvent; wherein the liquid components of the ernulsifiable concentrate formulation form ia 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 rnember of the set consisting of alkane compounds, aromatic compounds, alkylaryi compounds. alcohol-containing compounds, aldehyde-containig compounds, ether-contai ning compounds, ester-containing compounds, ketone containing compounds, actamcontaining compounds, amide-coaining compounds, chlorinated compounds. [0048] The agriculturally acceptable solvent may comprise at least one rnember of the set consisting of solvent naphtha (petroleum), heavy aromatic fraction, xylene, toluene. pyrroidones including N-alkylated pryrrolidones such as N.-methyl pyrrolidone, cyclohexanone, acetone, glycol ethers such as diethyleneglycol monornethyl ether (including the material sold under the trade name Carbitol), ethyleneglycolmonobutylethers (including the material sold 03/03/15,jb22520 innovation patent specification.doex,12 - 12 under the trade niame Butyl Glysolv), propylene glycol monoiethyl ether (including the material sold under the trade name Glysolv PM), methanol, ethanol, isopropanol, decanol, paraffin, hexane, acetic acid C-Cs branched alkyl ester ((including the material sold. under the trade name Exxate 700). [0049] An eriusifiable concentrate formulation according to the invention may include at least one agriculturally acceptable surfactant, wherein the curnulative amount (net of carrier solvent) of the at least one agriculturallyv acceptable surfactants is in the range from 40 to 200 g/L and preferably in the range frorn 60 to 1 50 g/L, mo re preferably, in the range from 80 to 110 g/L. [0050] The at least one agriculturally acceptable surfactant may cornrise a non-ionic surfactant. [0051] The at least one agriculturally acceptable non-ionic surfactan may be chosen from the categories in the set consisting of alkoxvlated block polymers. alkoxylated alcohols, aikoxylated alkylphenols, alkoxylated amines, alkoxylated aides, alkoxylated fatty enters, 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 NI 5, Teric N30), octyiphenol ethoxylate (inchiding materials sold under the trade name Teric X5, Terix X8, Teric XI0), alkoxylated alkylphenol (including materials sold under the trade name Termul 200, Orisurf 200), vegetable oil efioxylate (including materials sold under the trade name Termul 1284, Ternul 1285), tristyryl phenol ethoxylates (including material sold under the trade name Tennul 3150), alcohol ethoxylates such as tridecyl alcohol ~9EO (including rnaterial sold under the trade name Teric 3A9), Co-C 4 alcohols reacted with 2 moles EO (including material sold under the trade name Teric 12A2N), block copolyrers such as polyoxyethylene/pol yoxypropylene block copolymer 03/03/15,jb22520 innovation patent specification.doex,13 - 13 (including materials sold under the trade names Teric PF62 Teric PE64, Teric PE 68), and fatty amine higher-mole ethoxylates (such as taliowanine ethoxylates and oleyl amine ethoxylate) which have non-ionic ch aracteristics 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 consis ting of alkvlaryl sulfonates; alkylaryisulfonic acids; carboxylated alcohol ethoxylates and alkylphenol ethoxyl ates; carboxylic acids/fatty acids; diphenyl sulfonate deriv atives; 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: sulfon ates of dodecyl and tridecylbenzenes; sulfon ates of naphthalene and alkyl naphthalene; sulfonates of petroleum; sulfosuccinamates; alkoxylated aines; sarcosine derived surfactants such as, ammonium lauroyl sarcosinate; alkoxvlates as above other than ethoxvlates (such a propoxylates, butoxylates). [0055] The at least one agriculturally acceptable anionic surfactant may be chosen from the set consisting of linear and branched alkvlbenzenesuilphonates and salts thereof which may be provided as a non aqueous solution, (such as calcium C(1-C 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 Enipmin 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 03/03/15,jb22520 innovation patent specification.doex,14 - 14 PKiO), alkylphenol ether sulfate/tallowanine ethoxylate salts (including materials sold under the trade names Toximul TANS-5. Toxinmau TANS-6, Toximul TANS-8, Toxirnul TANS-15), and alcohol ether sulphate/tallowami ne ethoxylate salts (including materials sold. under the trade names Toximul TAABS-5, Toxinul TAABS-8). [0056] Alternatively, the at least one agriculturally acceptable surfactant is at least one cationic surfactant such as fatty amine lower-rnole ethoxylates (which may be incompatible with anionic surfactants). [0057j 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 zwitterionine surfactants include betaine surfactants. [05 8] 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 perfurne, 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 agriculturaly accepable solvent can be m-itinimised 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 aglrculturally acceptable surfactant but not agriculturally acceptable solvent, wherein the loading of triallate in the eimulsifiable concern trate: formulation is greater than 600 g/L.
03/03/15,jb22520 innovation patent specification.doex,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 trialIate/solvent ratio, the more restricted are the ranges of utilizable agricuituIrly acceptable solvents and agriculturally acceptable surfactants. [0062] The density of the emulsifiable concentrate is at least 1.05 g/ml, preferably 1I 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 trialate, including the steps of: adding an agriculturally acceptable solvent for triallate to a clean ernpty formulation ves;ek 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 character stics, foam persistence, and active constituent content. [0064] Formulations incorporating diluted enmusifiable 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 gronwell, 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.
03/03/15,jb22520 innovation patent specification.doex,16 - 16 [0065] Enulsifiable concentrate formulations according to aspects of the present invention are physically compatible with a range of other agricultural chernical formulations including those supplied under the trade names ChemAg Chlorsulfuron 750. Imtrade Mandate 750 WG Selective Herbicide, intrade Trifluralin 480 EC Herbicide, Eradicator 450 MIPA based, Glypihosate 888 WG, MONZA, Roundup Max, Eradicator 540, Eradicator 510, and Glyphosate 360. [0066] The current industry standard at 500 gIL was established by the initial market entrants and maiaintaned 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 subius0sions 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 emi sifi able 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/iabeliing/storage/transport There will also be less environmental impact through reduced solvent use.
03/03/15,jb22520 innovation patent specification.doex,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 PREFERR ED 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 emulsitiable concentrate according to the invention was made by mixing the following components. Component Sour'ce Parts by Weight (g/L) TrialIae 95% technical 947,4 Aromatic solvent 150 Recochem of Perth 106.3 (e.., Recosol 150) Australia Anionic surfactant e.g,, calcium Manufactiud by Stepan 76,2 Co--C4 alky lbnzenesulfonate (Correponds to (60 solid in 40%< 2-ethylhexanol) i5.7 - olid (c,g- Ninate 60E) surfactant) 03/03/15,jb22520 innovation patent specification.doex,18 - 18 Non-ionic surfactant; e.g., Manufactured by 50.1 alkoxylated alyklyphenol e.g., Huntsrnn Terrmul 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] n Ex ample 1, the fornulation procedure for a 10,000L batch, inclusive of quality control measures, was as follows, with the steps being identified numerically as ,1. 1.2, 1.3 and so on. [0073] 1,1I 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'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: 03/03/15,jb22520 innovation patent specification.doex,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 1L of product, ensuring it is representative. [0079] 1.7 Sub-sample 250mL from the original 1L 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 03/03/15,jb22520 innovation patent specification.doex,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.
03/03/15,jb22520 innovation patent specification.doex,21 - 21 [0086] 1.13 Catalogue and store a retention sample of approximately 200g. Tests to Confirn- the Suitahiihv of the Formiulatdon of Ex-,amle I [0087] For the test methods identified by the prefix CIPAC, refer to international Pesticides Analytical Council (CIPAC) published methodology. The Brookfield viscoimtetr used for ieasiurin.g viscosity of this formulation and the other formulations identified in the other Examples and Trials identified in this specification including in Appendices I 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 outcorne Observed outcome appearance visual homogeneous liquid homogeneous liquid assay validated chromatographic 875 --- 925 g/L complies rnethod, 98-102% accuracy, linearity R > 0.99 pH (I CIPAC MT 7153 4 --- 10 77 Spec Gravity CIPAC MT 3.1 1.00 - 3.00 1. 185 (SG) Erulsion CIPAC MT 47.2 2 ml cream and < complies characteristics trace oil after 30 min, complete resiusjpe nsion after 24 hIrs Persistent (I PAC NT 47.2< 60 nI after min 12rl (1 nin) foaming cold stability visual no phase separation complies 03/03/15,jb22520 innovation patent specification.doex,22 - 22 viscosity Brookfield viscometer 0 2000 cps 35 cPs 20C( viscosity 50C 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 [0088] The following triallate emulsifiabIe conctntrate forrmulation according to the invention was made by mixim 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) Huntsrnan Block co-polymer Manufactured by 170.0 (e~g. T ec PE64) 1-untsmnan [1089] in ite above fonrulation triallate is present at 0.95x806,0 = 766 parts by weight. [0090] in Exarnple 2, the forrmilation of a nominally 10,0001 batch of product, inclusive of quality control measures, is as follows, with the steps being identified nuinerically as 1,L 1.2, 1.3, and so on. [009 1] 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 03/03/15,jb22520 innovation patent specification.doex,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'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 1L of product, ensuring it is representative. [0096] 1.6 Sub-sample 250mL from the original 1L 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) 03/03/15,jb22520 innovation patent specification.doex,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 03/03/15,jb22520 innovation patent specification.doex,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. Dings [01061 Drawings relating to the validation method for the active constituent and llustrating a trial are identified as follows: 10107] FiL. 1 is a chromatogram of a sample identified as Trialiate A standard. [0108] Fig. 2 is a chromatogram of a sample identified as Triallate 900EC Validation Blank 1. [0109] Fig. 3 is a cbromatogram of a sample identified as Triallate Validation Spike Blank 1. [011o0 Fig. 4 is a cbromatogram of a sample identified as Triallate 900EC Validation Spike Blank 2 [oi 11] Fig. 5 is a chromatogram of a sample identified as Triallate 900EC Validation Spike Blank 3.
03/03/15,jb22520 innovation patent specification.doex,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 Trialiate 900EC Validation Linearity 4. [0116] Fig. 10 is a chromatogram of a sample identified as Triallate 900EC Validation Linearity 5. 10117] Fig. 1 is a chromatogran of a sample identified as Triallate 900EC Validation Linearity 6. 101 181 Fig. 12 is a chromatogran of a sample identmified as Triallate 900EC Validation Precision 1. 101191 Fig. 13 is a chromatogram of a sarnple identified as Triallate 900EC Validation Precision 2. 101201 Fig. 14 is a chromatogram of a sarnple 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.
03/03/15,jb22520 innovation patent specification.doex,27 - 27 [I23] Fig, 17 is a graph of Gas Chromatograrn response versus Triallate concentration. [0124] Fig. 18 is a bar graph of herbicide control. Ti as [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 R150, 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 03/03/15,jb22520 innovation patent 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.
03/03/15,jb22520 innovation patent specification.doex,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 03/03/15,jb22520 innovation patent 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-16-EO N Pluronic PE 6400 PE/PO/PE block copol N Pluronic PE 6800 PE/PO/PE block copol N 03/03/15,jb22520 innovation patent specification.doex,31 -31 TABLE C Name Termul 200 Nonylphenol 9 EO/10PO, 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 03/03/15,jb22520 innovation patent specification.doex,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 N10 Huntsman nonylphenolethoxlate Teric N13 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 03/03/15,jb22520 innovation patent specification.doex,33 - 33 Varying Non-lonic Surfactant and Surfaclant Ratio [19281 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 C 10 C alkylbenzenesulfonte, near, 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, CYAS #64742-94-5, supplied by Recochem, Perth. Australia). [0129j 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: Terul 200 (alkylphenol poly-ether EO/PO (ethyl eneoxide/propyene oxide) block copolymer, 9 mol EO, 10 mol PO, CAS #37251-69-7 CHECK, HLB=16.1, manufactured by Huntsman), Teric N2 (nonylpbenol 2-EO HLB=5.71, manufactured by Huntsman), Teric N8 (nonylphenol 8-EO, HLB=12.3, manufactured by Huntsman), Teric N13 (nonylphenol 13-EO, HLB=14.4. manufactured by H-un-tsmnan), Teric N20 (nonylphenol 20-EO. HLB=16, manufactured by H[untsman), Termul 1284 (castor oil PEG 36 CAS #61791-12--6, HLB=126, im-a nufactured 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), 03/03/15,jb22520 innovation patent specification.doex,34 - 34 Teric PE 68 (EO/PO block copolvmer, 150 Moles O, HILB = 29 CAS # 9003-11-6, manufactured by Hunitsman), 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=15I, 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 I to the specification of Austrian Provisional Patent Appication No. 201290279 [013 1] 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 'fables, 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 0 C HLB - Hydrophilic Lipophilic Balance P? - Pas F-Fail 03/03/15,jb22520 innovation patent specification.doex,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 PAS 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 B4 Teric N8 FAIL F P F P P B5 Teric N13 A F F F B6 Teric N20 Fi P C. Castor Oil Ethoxylates Code Trade Name E CTS E CTS E CTS C7 Termul 1284 FAIP P P C8 Termul 1285 FAL 03/03/15,jb22520 innovation patent specification.doex,36 - 36 D. Block Co-polymer Code Trade Name E CTS E CTS E CTS D9 PE62 VAIL F P F Fp D1O PE64 FAIL F 1 F p D1I PE68 FASL F F F D12 TSP16 FAIL F F F D13 PE6400 FAIL D14 PE6800 FAL F D15 Termul 203 FAIL F F P P Varvjng 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 etffier sulphonate, or branched alcohol ether sulphAc, were prepared. The anionic surfactants used have the following 1B1.3 values: Nansa EVM 70/2E, 113=9, Rhodacal 70, HLB=8,6; Rhodacal 70B, HLL=86; Thximul TAABS 5, HLB=9, Toximul TAABS 8, HLB=10. More detaUs 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 rmost of the forrmulations gav e satisfactory results for emulsion characteristics but unsatisfactory results for cold temperature stability.
03/03/15,jb22520 innovation patent specification.doex,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 IE1 Nansa EVM 70/2E Pp IF1 Rhodacal 70 IG1 Rhodacal 70B PP B. Alkyl phenol ether sulphate / Summary 60:40 tallowamine ethoxylated salts of Results (b) Code Trade Name E CTS IH1 Toximul TANS 5 Fa P Ill Toximul TANS 6 F IJi Toximul TANS 8 F C. Branched alcohol ether sulphate/tallowamine ethoxylated salts Code Trade Name E CTS IK1 Toximul TAABS 5 F ILl Toximul TAABS 8 F 03/03/15,jb22520 innovation patent specification.doex,38 - 38 Vat inlLoading Oily [134] In each formuiaion of this set of trials, tb anionic sufactant 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 10f) 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 rnay be an upper triallate limit for the invention, TAB LE 3 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 Ela Termul 200 (Triallate 1050) FA iLF Etb Termul 200 (Triallate 1000) FAIL F Etc Termul 200 (Triallate 950) FAI F 03/03/15,jb22520 innovation patent specification.doex,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 6OE, 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 (diethylenegiycoimonoethylether). Recosol solvents are graded and identified according to their nniniun flaslhpoints in Fahrenheit, More details of these trials are set out in Appendix 4 to the specification of Australian Provisional Patemn Application No. 2012902790. [0137] Satisfactory fornulations were obtained with the solvents Recosol 150, xvlene, dinethyl 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. TABLE4 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 IA1 Recosol 150 PA SS P P IIA1 Recosol 200 FA L P 03/03/15,jb22520 innovation patent specification.doex,40 -40 IIIA1 Xylene PASS P P IVA1 Toluene FA VA1 Dimethyl adipate VIA1 NMP VIIA1 DGME PASS Varjn~ L idngand Nondlonic Surfaictant [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 Rtcosol 150 solvent. Termul 1284 and 'ermul 1285 are castor oil ethoxylates. More details of these trials are set out in Appendix 5 to the specification of Australian Provisional Patent A pplication No. 2012902790. [0139] Tennul 1285 provided saisfactory 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 Ternml 1285 differ in the degree of ethoxylation of the castor oil parent material on which they are based, with Terrnul 1285 being more highly ethoxylated than Termul 1284.
03/03/15,jb22520 innovation patent specification.doex,41 - 41 TABLE1 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) PA SS F P P P E4ii Termul 1284 (Triallate 800) PASS F E4iii Termul 1285 (Triallate 850) E4iv Termul 1285 (Triallate 800) [0140] In this set of trials all triallate formulaions contained [riallate a loading of 900 g/L. In each formuilaton of the trials, a single non-ionic surfactant was used: Terrnml 200 (alkylphenol poly-ether EO/PO block copolymier, 9 mol EO, 10 mol P0, CAS #37251-69-7 CHECK, manufactured by Hndunt and distibuted by ISM, Perth). In each formlation in thi s set of trials, a single solvent was used, namely, Recosol 150. The reference anionic surfactant was (hat supplied under the trade naime Ninate 60E, More detafls of these trials are set out in Appendix 6 to the specificaion of Australian Provisional Patent Application No, 2012902790.
03/03/15,jb22520 innovation patent specification.doex,42 - 42 [0141] The alternative anionic surfactants used were those identified by the trade names as follows: Nansa EVM 70/2E (calciurn Cio-C a linear alkyl benzene sulphonate. 70% in 2-ethyihexanol 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), Toxirnul TA NS 5 (aikylphenol ether suiphate/alowanine ethoxilate, HLB 8, supplied by Stepan), Toximul TANS 6 (alkylphenol ether sulphate/tallowamine ethoxylate, HLB 10, supplied iby Stepan), Toxirml T ANS 8 (alkylphenol ether suiphate/taflowarnne ethoxylate, HLB 12, supplied by Stepan), Toximul TAABS 5 (branched alcohol ether sulphattllowarine ethoxylated sals, supplied by Stepan), and Toximul TAABS 8 (branched alcohol ether suilphate/tallowamine ethoxylated salts, supplied by Stepan) [0112] Throughout this set of trials, the ratio of anionic to non-ionic surfactants was fixed at 60:40. [0113] 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 alkylbenztne sulphonate type. and, the non-ionic surfactant was Termul 200, and the ratio of surfactants was 60:40.
03/03/15,jb22520 innovation patent specification.doex,43 - 43 [0144] Trialate 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 alkylbenzenesuifonate 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 trialiate loadings of 800 g/L and 700 g/L, as was Toxinud TAABS 5. Other anionic surfactants were effective at one triallate loading but not the other. TAB LE 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 P P> P 9B Nansa EVM 70/2E P PP 9C Rhodacal 70 9D Rhodacal 70B 03/03/15,jb22520 innovation patent specification.doex,44 - 44 B. Alkyl phenol ether sulphate / Summary tallowamine ethoxylated salts of Results Code Trade Name E CTS E CTS 9E Toximul TANS 5 P 9F Toximul TANS 6 P 9G Toximul TANS 8 Pas C. Branched alcohol ether sulphate/tallowamine ethoxylated salts Code Trade Name E CTS E CTS 9H Toximul TAABS 5 Pass P 91 Toximul TAABS 8 FF P F Varyng on ioic uraaats ithi Deire Hvropili - ipohilic Balance [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 TSP1 6). combinations to achieve desired bydrophili c i pophilic balance (HLB) values, and a solvent, were prepared with varying loadings of triallate. For prefteTtd formulations the system iHLB is in the range 11-14, built up from components with 1-Ls identified previous. 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.
03/03/15,jb22520 innovation patent specification.doex,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) FA E6c Triallate 900 (PE62 : TSP16) F F u E6d Triallate 850 (PE62 : PE64) FA UL F F E6e Triallate 800 (PE 62 : PE64) FA L F E6f Triallate 800 (PE 62 : PE68) FI VL F F E6g Triallate 800 (PE62 : TSP16) FL F (:onitbii' atin fVvn on kicSuacaatD hrntixd S ulfactan t Rados0 [0147] At loadings of about 900 g/L of triallate, and using varying combinations of anionic surfactant, being calciun alkyl benzvl sulphon ate (supplied under the trade name Ninate 60E) and a blend of non-ionic surfactants, being nonyl phenol ethoxylates in v arying 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.
03/03/15,jb22520 innovation patent specification.doex,46 - 46 More details of these trials are set out in Appendix 8 to the specification of Au stralian Provisional Patent Application No. 2012902790. TABLE 8 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): FAl, E3a Teric N8 (64 g/L) N60E (38 g/L): Teric N2 (35 g/L): E3b Teric N8 (54 g/L) N60E (37 g/L): Teric N2 (36 g/L): FA F E3c Teric N13 (53 g/L) N60E (39 g/L): Teric N2 (53 g/L): FF 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): FF E3e Teric N8 (14 g/L) N60E (77 g/L): Teric N2 (41 g/L): F E3f Teric N8 (12 g/L) N60E (77 g/L): Teric N2 (43 g/L): E3g Teric N13 (11 g/L) 03/03/15,jb22520 innovation patent specification.doex,47 - 47 N60E (77 g/L): Teric N2 (44 g/L): E3h Teric N13 (8 g/L) N60E (76 g/L): Teric N2 (45 g/L): E3i Teric N20 (9 g/L) N60E (76 g/L): Teric N2 (46 g/L): E3j Teric N20 (5 g/L) Aceptable Slvnt [0148] Trials using anionic surfactant, being calcium alkyl benzyl sulphonate (supplied under the trade name Ninate 60E), and non-ionic surfacant, being. Bock Co-polyrner (such as that supplied under the trade names PE62 or PE63), without using any agriculturally acceptable sovents and varying the triallate loading froi 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; iriallate 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
_ILK
03/03/15,jb22520 innovation patent specification.doex,48 -48 Triallate 900 g/L F A E5a Teric PE62 at 256 g/L Triallate 900 g/L E5b Teric PE64 at 256 g/L Triallate 800 g/L E5c Teric PE62 at 339 g/L Triallate 800 g/L p E5d Teric PE64 at 344 g/L Triallate 700 g/L E5e Teric PE62 at 428 g/L Triallate 700 g/L Ef Teric PE64 at 433 g/L Minim-al -Solvent Formul ations [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 Terrnul 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 terns 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 terns of cold temperature 03/03/15,jb22520 innovation patent specification.doex,49 - 49 stability and emulsion characeri sticsf for some block co-polymers and block co-poiymer combinations, but not for another block co-polymer. and, the block co-polymer-no-ionic surfactant combinations used. [015 1] At a loading of 700 g/L trallate, 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. AI 800 and 700 g/L triallate loading, formulations were obtained where the PE surfactant series (EO/PO blocl copoiymter), and blends thereof, acted as solvent as wil 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 E7a E8a P PE 64 E6b F n/a F E7b E8b PE 62:PE 64 (50:50) E6c E7c E8c PE 62:PE 64 F (25:75) E6d N E7d E8d Termul 203 E6e F n/a F E7e FAIL n/a F E8e F n/a F Termul 203:PE n/a 62:PE 64 (10:27:63) E6f E7f E8f 03/03/15,jb22520 innovation patent specification.doex,50 -50 Termul 203:PE F n/a n/a n/a 62:PE 64 (20:30:50) E6g E7g E8g Termul 203:PE n/a n/a n/a 62:PE 64 (30:34:36) E6h E7h '" E8h Termul 203:PE n/a n/a n/a 62:PE 64 (40:37:23) E6i E7i E8i Termul 203:PE n/a n/a n/a VN 62:PE 64 (50:40:10) E6j E7j E8j _Comlpatibility ' ni [) 152] Compatibility tials using a trial lat emulsifiable concentrate formulation according to Example 1 of the present invention, a commercially available agricultiua chemical fornulation (identified by the trade name under which it is supplied) and water were carried out. The results are set out in fable 11L TABLE iI 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 03/03/15,jb22520 innovation patent specification.doex,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 03/03/15,jb22520 innovation patent specification.doex,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/L 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 4 (+47) 106 76 50 IIIA 1 Campaign 899 Xylene Ninate 60E Termul 200 4 (+47) 105 77 51 VIAl Campaign 900 n-methyl-2- Ninate 60E Termul 200 4 (+47) pyrrolidone 76 50 106 03/03/15,jb22520 innovation patent specification.doex,53 - 53 VIIA1 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 03/03/15,jb22520 innovation patent specification.doex,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 03/03/15,jb22520 innovation patent specification.doex,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 03/03/15,jb22520 innovation patent 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.
03/03/15,jb22520 innovation patent specification.doex,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.
03/03/15,jb22520 innovation patent specification.doex,58 - 58 Wheat 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 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 FEl (see above) and CA500 were applied to pots containing herbicide susceptible ryegrass biotype SLR4 buried at 1cm depth. FE l 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.
03/03/15,jb22520 innovation patent specification.doex,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 FE1 85 +/- 1.8 890 ml/ha FE1 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.
03/03/15,jb22520 innovation patent specification.doex,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.
03/03/15,jb22520 innovation patent specification.doex,61 - 61 APPENDIX I Trial # Ala 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 (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 C10-16 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%) *Haq. Solution MT 75.3 4 to 10 n/a (eperatugaty20C) CIPAC MT 3.1 1.00 to 1.30 n/a 03/03/15,jb22520 innovation patent specification.doex,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 Dark yellow to brown liquid brown liquid, Cold temp. stability MT75.3 homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) separation in any format phase separation in any format Viscosity MT 192 0 to2Ocsn/a (temperature at 5C) to 2000cPs (temperature at 20C) MT 192 0 to 2000cPs n/a Test parameter maintained within Long Term Performance Various as per above required range after accelerated n/a aging to approximate 2 years. I General Remarks 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: 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 4737.3 900 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) 03/03/15,jb22520 innovation patent specification.doex,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. Solution 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 Passed Persistent Foaming <60mL after 1 min 12ml in 1 min Dark yellow to brown liquid brown liquid, Cold temp. stability homar eow free fro phase homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format Viscosity 0 to 2000cPs 72cps Passed (temperature at 5C) Viscosity 0 to 2000cPs 34cps Passed (temperature at 20C) 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# Aic 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 03/03/15,jb22520 innovation patent specification.doex,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 C10-16 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 pHaq. Solution 4 to 10 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 milky emulsion, 5mL Failed re-emulsion after 24h cream@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) seaaini n omtphase separation in any format 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 03/03/15,jb22520 innovation patent specification.doex,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) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Teric N2 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4736.3 900 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) 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 pHaq. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) 03/03/15,jb22520 innovation patent specification.doex,66 - 66 <2mL cream after 30 min, trace clear emulsion, 5ml Emulsion characteristics of oil after 30 min and complete oil&cream@bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability hooeeufe rmpae homogeneous, free from Pse Ahetemetabishomogeneous reafrom Passed (Accelerated Ageing) separation in any format 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 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) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Teric N2 : Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4737.0 900 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) 03/03/15,jb22520 innovation patent specification.doex,67 - 67 Nonyl Phenol ethoxylates 252.1 50 used: Teric N2 (non-ionic surfactant) Total 5901.6 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 4to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace clear emulsion, 5ml Emulsion characteristics of oil after 30 min and complete oil&cream@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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format 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 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 03/03/15,jb22520 innovation patent specification.doex,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 4t10n/a 1%aq. Solution 4to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace clear emulsion, 5ml Emulsion characteristics of oil after 30 min and complete oil&cream@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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format 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 03/03/15,jb22520 innovation patent specification.doex,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 4737.1 900 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 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 pHaq. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) 03/03/15,jb22520 innovation patent specification.doex,70 - 70 <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 hooeeufe rmpae homogeneous, free from Pse Ahetemetabishomogeneousmrehasom Passed (Accelerated Ageing) separation in any format phase 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 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 4736.3 900 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 381.1 76 used: Ninate 60E (anionic surfactant) 03/03/15,jb22520 innovation patent specification.doex,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 4to 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 homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format 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 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 03/03/15,jb22520 innovation patent specification.doex,72 - 72 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4737.1 900 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 568.6 114 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 4t10n/a 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, 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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) 03/03/15,jb22520 innovation patent specification.doex,74 - 74 <2mL cream after 30 min, trace milky emulsion, 4.5ml of Emulsion characteristics of oil after 30 min and complete cream & oil@bottomFailed 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 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 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) 03/03/15,jb22520 innovation patent specification.doex,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 4t10n/a 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, 2.1ml 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 Passe (Accelerated Ageing) homraognos freen formase phase separation in any d format 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 EMULSION CHARACTERISTICS FAILED Trial # B5c 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 (90:10) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Teric N13 : Recosol 150 03/03/15,jb22520 innovation patent specification.doex,76 - 76 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4736.3 900 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 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 pHaq. 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, 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 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format Viscosity 0t 0~~ / (temperature at 5C) 0 to 2000cPs n/a 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.
03/03/15,jb22520 innovation patent specification.doex,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 900g/L 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 4737.1 899 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 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 paq. Solution 4 to 10 n/a 03/03/15,jb22520 innovation patent specification.doex,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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format 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 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) 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 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 3ml 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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format Viscosity 0t 0~~ / (temperature at 5C) 0 to 2000cPs n/a 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 # 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 03/03/15,jb22520 innovation patent specification.doex,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, g/L (Chemical name) S-2,3,3-tricholoroallyl 4738.3 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.5 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid 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 pHaq. 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, 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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format Viscosity 0t 0~~ / (temperature at 5C) 0 to 2000cPs n/a Viscosity 0 to 2000cPs n/a (temperature at 20C) 0t 00~ / 03/03/15,jb22520 innovation patent specification.doex,8 1 - 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 # C7a 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-t1 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4738.0 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.5 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid 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 03/03/15,jb22520 innovation patent specification.doex,82 - 82 Assay 875 to 925g/L triallate n/a pHaq. 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, 1.7ml of Emulsion characteristics of oil after 30 min and complete cream & oil@bottom Passed 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 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 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 4739.1 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 534.9 107 used: Recosol 150 380.1 76 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 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, unstable, forms crystal @ Failed (Accelerated Ageing) homogeneous, free from phase bottom Fie separation in any format 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
FAILED
03/03/15,jb22520 innovation patent specification.doex,84 - 84 Trial # C7c 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 (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 4737.7 899 diisopropyl(thiocarbamate) 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 paq. 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, 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 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from Passed (Accelerated Ageing) homaraiogeno, f formhase phase separation in any sepaatio in ny frmatformat 03/03/15,jb22520 innovation patent specification.doex,85 - 85 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 EMULSION CHARACTERISTICS FAILED Trial # C8a 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 (30:70) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E :Termul 1285 : Recosol 150 FORMULATION (Choemiponea e) Amount, g Loading, g/L 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 03/03/15,jb22520 innovation patent specification.doex,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 paq. 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, 0.25ml of Emulsion characteristics of oil after 30 min and complete cream & oil@bottom Passed re-emulsion after 24h 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 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 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 4738 896 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) 03/03/15,jb22520 innovation patent specification.doex,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 paq. Solution 4 to 10 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 0 to 2000cPs n/a (temperature at SC)_________________ 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
FAILED
03/03/15,jb22520 innovation patent specification.doex,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/L (Chemical name) S-2,3,3-tricholoroallyl 4737.1 898 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 541.0 108 used: Recosol 150 Calcium C10-16 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 pHaq. 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, 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 03/03/15,jb22520 innovation patent specification.doex,89 - 89 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) seaaini n omtphase 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 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 4737.1 900 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) Block Co-polymer 444.6 89 used: PE 62 (non-ionic surfactant) Total 5902.6 03/03/15,jb22520 innovation patent specification.doex,90 - 90 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 pHaq. Solution 4 to 10 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 2ml of cream & oil @ 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 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 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 03/03/15,jb22520 innovation patent specification.doex,91 - 91 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4735.8 899 diisopropyl(thiocarbamate) 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 4t10n/a 1%aq. Solution 4to 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 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 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 03/03/15,jb22520 innovation patent specification.doex,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 900g/L 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 4736.4 900 diisopropyl(thiocarbamate) 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 pHaq. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) 03/03/15,jb22520 innovation patent specification.doex,93 - 93 <2mL cream after 30 min, trace off white milky emulsion, Emulsion characteristics of oil after 30 min and complete 3ml of cream @ bottom Failed re-emulsion after 24h Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, brown liquid, Cold temp. stability hooeeufe rmpae homogeneous, free from Pse Ahetemetabishomogeneous reafrom Passed (Accelerated Ageing) separation in any format 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 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 4736.4 900 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) 03/03/15,jb22520 innovation patent specification.doex,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 4t10n/a 1%aq. Solution 4to 10 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <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 homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format 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 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 03/03/15,jb22520 innovation patent specification.doex,95 - 95 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4737.7 899 diisopropyl(thiocarbamate) 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 pHaq. 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 white emulsion, 5ml Emulsion characteristics of oil after 30 min and complete of 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) seaaini n omtphase separation in any format 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 03/03/15,jb22520 innovation patent specification.doex,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) 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 4735.9 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 533.0 107 used: Recosol 150 Calcium C10-16 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 pHaq. Solution 4 to 10 n/a 03/03/15,jb22520 innovation patent specification.doex,97 - 97 Specific gravity 1.00 to 1.30 n/a (temperature at 20C) <2mL cream after 30 min, trace milky white emulsion, 4ml Emulsion characteristics of oil after 30 min and complete of 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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format 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 EMULSION CHARACTERISTICS FAILED Trial# D11a 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 4736.3 899 diisopropyl(thiocarbamate) 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 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 Solidifies at room temp Failed separation in any format 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 MIXTURE SOLIDIFY AT ROOM TEMP 03/03/15,jb22520 innovation patent specification.doex,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 # IA15-t2 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4735.5 899 diisopropyl(thiocarbamate) 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 pHaq. Solution 4 to 10 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 03/03/15,jb22520 innovation patent specification.doex,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 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. I General Remarks PASS or FAIL? FAIL Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE FORMED CRYSTALS AT ROOM TEMP Trial# D11c 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) 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 4736.4 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 535.4 107 used: Recosol 150 Calcium C10-16 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 03/03/15,jb22520 innovation patent specification.doex,101 - 101 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 pHaq. 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, 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 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 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) eg. Triallate Tech (95% purity) 03/03/15,jb22520 innovation patent specification.doex,102 - 102 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 paq. Solution 4 to 10 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 Forms 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 STAB
FAILED
03/03/15,jb22520 innovation patent specification.doex,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 4763.1 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 533.5 106 used: Recosol 150 Calcium C10-16 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 pHaq. 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, 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 03/03/15,jb22520 innovation patent specification.doex,104 - 104 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse 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 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 4736.5 900 diisopropyl(thiocarbamate) 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) Total 5902.6 03/03/15,jb22520 innovation patent specification.doex,105 - 105 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 paq. Solution 4 to 10 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 Crystal formed @ bottom Failed 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 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 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) 03/03/15,jb22520 innovation patent specification.doex,106 - 106 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 paq. Solution 4 to 10 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 forms crystal @ bottom 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 STAB
FAILED
03/03/15,jb22520 innovation patent specification.doex,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, g/L (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 pHaq. Solution 4 to 10 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 03/03/15,jb22520 innovation patent specification.doex,108 - 108 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase forms crystal @ bottom Failed separation in any format 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 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 4737.3 899 diisopropyl(thiocarbamate) 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) Total 5904.4 03/03/15,jb22520 innovation patent specification.doex,109 - 109 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 pHaq. Solution 4 to 10 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 forms crystal @ bottom Failed separation in any format 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 FAILED Trial# D14a 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 (30:70) 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 4736.9 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) 03/03/15,jb22520 innovation patent specification.doex, 110 -110 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 pHaq. Solution 4 to 10 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 Solidifies at room temp Failed separation in any format 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 IT SOLIDIFY AT ROOM TEMP 03/03/15,jb22520 innovation patent specification.doex, 111 - 111 Trial# D14b 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 (60:40) 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 4737.0 899 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 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 pHaq. Solution 4 to 10 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 03/03/15,jb22520 innovation patent specification.doex, 112 -112 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase forms crystal @ bottom Failed separation in any format 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 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 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 6800 (non-ionic surfactant) Total 5904.4 03/03/15,jb22520 innovation patent specification.doex, 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 pHaq. Solution 4 to 10 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 forms crystal @ bottom Failed separation in any format 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 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 4736.4 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) 03/03/15,jb22520 innovation patent specification.doex, 114 -114 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) 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 paq. Solution 4 to 10 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 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 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 EMULSION CHARACTERISTICS AND COLD STABILITY FAILED 03/03/15,jb22520 innovation patent specification.doex, 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 pHaq. 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, 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 03/03/15,jb22520 innovation patent specification.doex, 116 - 116 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) seaaini n omtphase 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 EMULSION CHARACTERISTICS FAILED Trial# D15c 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 (90:10) 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 4737.9 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.5 106 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid 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 03/03/15,jb22520 innovation patent specification.doex, 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 pHaq. 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, 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 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 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 03/03/15,jb22520 innovation patent 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 70/2E Ratio of Nansa EVM 70/2E : Termul 200 (60:40) Anionic/Non-ionic surfactant/ Solvent used: Nansa EVM 70/2E : Termul 200: Recosol 150 FORMULATION Component Amount, g Loading, g/L (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 pHaq. 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 03/03/15,jb22520 innovation patent specification.doex, 119 - 119 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Passed separation in any format 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? PASS Description: # IF1b 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 4743.7 899 diisopropyl(thiocarbamate) 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 03/03/15,jb22520 innovation patent 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 paq. 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 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Passed 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 PASS or FAIL? PASS Description: # IG1b 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 4741.6 902 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 574.1 115 used: Recosol 150 362.9 73 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Passed separation in any format 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? PASS Description: Trial # IH1b TRIALLATE 900 TRIALS Triallate active present at 900g/L 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 03/03/15,jb22520 innovation patent specification.doex,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 4t10n/a 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 crystal Failed separation in any format 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 03/03/15,jb22520 innovation patent specification.doex,123 - 123 Description: DID NOT CONTINUE ANY FURTHER TESTING, BECAUSE COLD STAB FAILED Trial # Ilb 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 4740.5 900 diisopropyl(thiocarbamate) 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 paq. 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, 0.25ml of Passed re-emulsion after 24h cream@bottom 03/03/15,jb22520 innovation patent specification.doex,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 separation in any format 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 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) Anionic/Non-ionic surfactant/ Solvent used: Toximul TANS 8 : Termul 200: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4738.5 898 diisopropyl(thiocarbamate) 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 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 separation in any format 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 FAILED Trial # IK1b 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 4737 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531 106 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 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 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
FAILED
03/03/15,jb22520 innovation patent specification.doex,127 - 127 Trial # ILlb TRIALLATE 900 TRIALS Triallate active present at 900g/L 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, g/L (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 paq. 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, 0.80ml 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 03/03/15,jb22520 innovation patent specification.doex,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
03/03/15,jb22520 innovation patent specification.doex,129 - 129 APPENDIX 3 Trial # Ela TRIALLATE 1050 TRIALS Triallate active present at 1050g/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 5527.6 1050 diisopropyl(thiocarbamate) 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 paq. 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 03/03/15,jb22520 innovation patent specification.doex,130 - 130 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 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 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, g/L (Chemical name) S-2,3,3-tricholoroallyl 5263.1 1000 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 149.7 30 used: Recosol 150 Calcium C10-16 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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 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 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) 03/03/15,jb22520 innovation patent 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 at 4t10n/a 1%aq. Solution 4to 10 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 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
FAILED
03/03/15,jb22520 innovation patent specification.doex,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) 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 4737.3 900 (thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 531.4 106 used: Recosol 150 Calcium C10-C16 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 pHaq. Solution 4 to 10 7.16 Passed Specific gravity 1.00 to 1.30 1.183 Passed (temperature at 200) <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 03/03/15,jb22520 innovation patent specification.doex,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 fromip oseparato re Passed (Accelerated Ageing) separation in any format fo hs eaaini any format perature at 50) 0 to 2000cPs 72 cps Passed perature at 200) 0 to 2000cPs 34cps Passed Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years. I 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 03/03/15,jb22520 innovation patent specification.doex,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 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 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 03/03/15,jb22520 innovation patent specification.doex,136 - 136 used: xylene Calcium C10-C16 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 Darkgeyelos toe bro liquid liquid, homogeneous, free Pse homogeneous, free fromaphasepa atr Passed (Accelerated Ageing) seaaini n omtfrom phase separation in any format Viscosity 0 to 2000cPs (temperature at 5C) 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 03/03/15,jb22520 innovation patent specification.doex,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 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 03/03/15,jb22520 innovation patent specification.doex,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 # VA1 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 03/03/15,jb22520 innovation patent specification.doex,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 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 Darkgeyelos toe bro liquid liquid, homogeneous, free Pse homogeneous, free fromaphasepa atr Passed (Accelerated Ageing) seaaini n omtfrom 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 03/03/15,jb22520 innovation patent specification.doex,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 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 fromip oseparato re Passed (Accelerated Ageing) separation in any format fo hs eaaini 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 03/03/15,jb22520 innovation patent specification.doex,141 - 141 Trial # VIA1 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, g/L (Chemical name) S-2,3,3-tricholoroallyl 4735.5 898 diisopropyl(thiocarbamate) 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 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 Darkgyeo to bro liqid liquid, homogeneous, free Passed (Accelerated Ageing) separation in any format from phase separation in __________________________________________any format_____ 03/03/15,jb22520 innovation patent specification.doex,142 - 142 Viscosity 0 to 2000cPs (temperature at 5C) 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 03/03/15,jb22520 innovation patent specification.doex,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 paq. 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, 2ml cream @ Failed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min n/a 03/03/15,jb22520 innovation patent specification.doex,144 - 144 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse 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 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 4471.4 848 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 834.2 167 used: Recosol 150 Calcium C10-16 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 03/03/15,jb22520 innovation patent specification.doex,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 paq. Solution 4 to 10 7.21 Passed Specific gravity 1.00 to 1.30 1.165 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 4mL Passed Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format perature at 50) 0 to 2000cPs 56.9cps Passed perature at 200) 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 4212.0 800 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 1087.9 218 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format 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 EMULSION CHARACTERISTICS FAILED 03/03/15,jb22520 innovation patent specification.doex,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, g/L (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 Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 801 g/L Passed pHaq. Solution 4 to 10 7.25 Passed Specific gravity 1.00 to 1.30 1.149 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 4mL Passed 03/03/15,jb22520 innovation patent specification.doex,148 - 148 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) seaaini n omtphase separation in any format perature at 50) 0 to 2000cPs 55.Ocps Passed 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 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 03/03/15,jb22520 innovation patent 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 paq. Solution 4 to 10 7.15 Passed Specific gravity 1.00 to 1.30 1.170 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 4mL Passed Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format perature at 50) 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 03/03/15,jb22520 innovation patent specification.doex,150 - 150 Solvent naphtha (petroleum), heavy aromatic 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 pHaq. Solution 4 to 10 7.23 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 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format Viscosity 0 to 2000cPs 55.Ocps Passed (temperature at SC) 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 03/03/15,jb22520 innovation patent specification.doex,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, g/L (Chemical name) S-2,3,3-tricholoroallyl 4216.8 798 diisopropyl(thiocarbamate) 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 pHaq. Solution 4 to 10 7.13 Passed Specific gravity 1.00 to 1.30 1.155 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 4mL Passed 03/03/15,jb22520 innovation patent specification.doex,152 - 152 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) seaaini n omtphase separation in any format perature at 50) 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) 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 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 03/03/15,jb22520 innovation patent specification.doex,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 Saq. Solution 4 to 10 7.07 Passed 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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format perature at 50) 0 to 2000cPs 51.3cps Passed 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 03/03/15,jb22520 innovation patent specification.doex,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 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 paq. 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, 2ml cream @ Failed re-emulsion after 24h bottom Persistent Foaming <60mL after 1 min n/a 03/03/15,jb22520 innovation patent specification.doex,155 - 155 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse 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 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 4471.4 848 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 834.2 167 used: Recosol 150 Calcium C10-16 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 7.21 Passed Specific gravity 1.00 to 1.30 1.165 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 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 50) 0 to 2000cPs 56.9cps Passed perature at 200) 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 4212.0 800 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) 1087.9 218 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse 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 EMULSION CHARACTERISTICS FAILED 03/03/15,jb22520 innovation patent specification.doex,158 - 158 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, g/L (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 Dark yellow to brown liquid, Brown liquid Passed homogeneous Assay 825 to 875g/L Triallate 801 g/L Passed pHaq. Solution 4 to 10 7.25 Passed Specific gravity 1.00 to 1.30 1.149 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 4mL Passed 03/03/15,jb22520 innovation patent specification.doex,159 - 159 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) seaaini n omtphase separation in any format perature at 50) 0 to 2000cPs 55.Ocps Passed 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 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 03/03/15,jb22520 innovation patent specification.doex,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 paq. Solution 4 to 10 7.15 Passed Specific gravity 1.00 to 1.30 1.170 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 4mL Passed Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format perature at 50) 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) Solvent naphtha (petroleum), heavy aromatic 825.9 165 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 7.23 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 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format perature at SC) 0 to 2000cPs 55.Ocps Passed 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 03/03/15,jb22520 innovation patent specification.doex,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 4216.8 798 diisopropyl(thiocarbamate) 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 pHaq. Solution 4 to 10 7.13 Passed Specific gravity 1.00 to 1.30 1.155 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 4mL Passed 03/03/15,jb22520 innovation patent specification.doex,163 - 163 Dark yellow to brown liquid, brown liquid, Cold temp. stability homogeneous, free from phase homogeneous, free from Passed (Accelerated Ageing) seaaini n omtphase separation in any format perature at 50) 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) 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 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 03/03/15,jb22520 innovation patent 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 Saq. Solution 4 to 10 7.07 Passed 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 Passed (Accelerated Ageing) homraognos freen formase phase separation in any Pse format perature at 50) 0 to 2000cPs 51.3cps Passed 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 03/03/15,jb22520 innovation patent specification.doex,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 C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 380.7 76 used: Ninate 60E (anionic surfactant) Block Co-polymer 154.8 31 used: PE 62 (non-ionic surfactant) Block Co-polymer 104.2 21 used: PE 64 (non-ionic surfactant) 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 pHaq. 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, 4mL Emulsion characteristics of oil after 30 min and complete cream@bottom Failed re-emulsion after 24h I 03/03/15,jb22520 innovation patent specification.doex,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 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 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, g/L (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 223.9 45 used: PE 62 (non-ionic surfactant) Block Co-polymer 34.7 7 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 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 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 TEMP AND EMULSION CHARACTERISTICS FAILED Trial # E6c TRIALLATE 900 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: 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 03/03/15,jb22520 innovation patent specification.doex,168 - 168 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 564.1 112 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 430.0 85 used: Ninate 60E (anionic surfactant) Block Co-polymer 166.5 33 used: PE 62 (non-ionic surfactant) Block Co-polymer 104.5 21 used: TSP 16 (non-ionic surfactant) 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 pHaq. 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, 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 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 TEMP AND EMULSION CHARACTERISTICS FAILED 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 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 03/03/15,jb22520 innovation patent specification.doex,170 - 170 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 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 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 C10-16 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 03/03/15,jb22520 innovation patent specification.doex,171 - 171 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 pHaq. 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, 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 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 TEMP AND EMULSION CHARACTERISTICS FAILED Trial # E6f TRIALLATE 800 TRIALS Triallate active present at 900g/L 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) 03/03/15,jb22520 innovation patent specification.doex,172 - 172 Solvent naphtha (petroleum), heavy aromatic 1093.0 219 used: Recosol 150 Calcium C10-16 alkyl benzenesulfonic acid in 2-ethyl hexanol 191.0 38 used: Ninate 60E (anionic surfactant) Block Co-polymer 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 4t10n/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 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 TEMP
FAILED
03/03/15,jb22520 innovation patent specification.doex,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 267.0 53 used: PE 62 (non-ionic surfactant) Block Co-polymer 178.0 36 used: TSP16 (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 pHaq. Solution 4 to 10 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 03/03/15,jb22520 innovation patent specification.doex,174 - 174 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 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 TEMP
FAILED
03/03/15,jb22520 innovation patent 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 N2/Teric N8: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4742.0 900 diisopropyl(thiocarbamate) 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 pHaq. 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, 1.0ml of Passed re-emulsion after 24h cream@bottom Persistent Foaming <60mL after 1 min n/a 03/03/15,jb22520 innovation patent specification.doex,176 - 176 Cold temp. stability Dark yellow to brown liquid, (Accelerated Ageing) homogeneous, free from phase Formed crystal Failed separation in any format 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 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 N2/Teric N8: Recosol 150 FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl 4730.7 899 diisopropyl(thiocarbamate) 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 03/03/15,jb22520 innovation patent specification.doex,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 paq. 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, 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 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 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 2.0ml 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 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 03/03/15,jb22520 innovation patent specification.doex,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) 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 4740.1 898 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 532.1 106 used: Recosol 150 Calcium C10-16 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 4t10n/a 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, 2.0ml 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 03/03/15,jb22520 innovation patent specification.doex,180 -180 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 # 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, g/L (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 03/03/15,jb22520 innovation patent specification.doex,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 paq. 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, 8.0ml 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 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 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 900g/L Trial details: Trial using Ninate 60E as anionic surfactants against Teric N series combination Ratio of Ninate 60E : Teric N2 : Teric N8(60:32:8) Anionic/Non-ionic surfactant/ Solvent used: Ninate 60E : Teric N2/Teric N8: Recosol 150 FORMULATION Component Amount, g Loading, g/L (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 03/03/15,jb22520 innovation patent specification.doex,182 - 182 Calcium C10-16 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 pHaq. 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, 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 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 03/03/15,jb22520 innovation patent specification.doex,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 C10-16 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 4t10n/a 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, 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 03/03/15,jb22520 innovation patent specification.doex,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) 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 4740.7 899 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 529.1 106 used: Recosol 150 Calcium C10-16 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 03/03/15,jb22520 innovation patent specification.doex,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 paq. 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, 8.0ml 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 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 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 4733.6 900 diisopropyl(thiocarbamate) eg. Triallate Tech (95% purity) Solvent naphtha (petroleum), heavy aromatic 521.7 104 used: Recosol 150 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 2.0ml 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 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 03/03/15,jb22520 innovation patent specification.doex,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) 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 4738.7 900 diisopropyl(thiocarbamate) 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 4t10n/a 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, 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 03/03/15,jb22520 innovation patent specification.doex,188 - 188 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 03/03/15,jb22520 innovation patent specification.doex,189 - 189 APPENDIX 9 Trial # E5a TRIALLATE 900 TRIALS Triallate active present at 900g/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 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 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: 03/03/15,jb22520 innovation patent specification.doex,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 4501.1 diisopropyl(thiocarbamate) 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 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: 03/03/15,jb22520 innovation patent specification.doex,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 4001.1 diisopropyl(thiocarbamate) 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 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: 03/03/15,jb22520 innovation patent specification.doex,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: 03/03/15,jb22520 innovation patent specification.doex,193 - 193 Trial # E5e 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 3500.1 diisopropyl(thiocarbamate) 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 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: 03/03/15,jb22520 innovation patent 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 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: 03/03/15,jb22520 innovation patent specification.doex,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 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) 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 pHaq. 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, traces of Failed re-emulsion after 24h oil@top,0.5ml of solidified cream&oil@bottom Persistent Foaming <60mL after 1 min n/a Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homrene free f phase liquid, homogeneous re Passed (Accelerated Ageing) homraognos freen formase from phase separation in Pse any format 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 FAIL PASS or FAIL? 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 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 0t 0~~ / (temperature at 5C) 0 to 2000cPs n/a Viscosity 0 o2Ocsn/a temperaturee at 20C) 0 to 2000cPs Test parameter maintained within Long Term Performance required range after accelerated n/a aging to approximate 2 years.
03/03/15,jb22520 innovation patent specification.doex,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: 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 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 Haq. 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, 1ml 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 homrene free f phase liquid, homogeneous re Passed (Accelerated Ageing) homraognos freen formase from phase separation in Pse any format Viscosity 0t 0~~ / (temperature at 5C) 0 to 2000cPs n/a Viscosity 0 to 2000cPs n/a -(temperature at 20C) 0t 00~
/
03/03/15,jb22520 innovation patent 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 Haq. 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, 2ml of Failed re-emulsion after 24h cream &oil@bottom, traces of oil@top Persistent Foaming <60mL after 1 minn/ 03/03/15,jb22520 innovation patent specification.doex,199 - 199 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 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 # 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, 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: 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 pHaq. Solution 4 to 10 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 03/03/15,jb22520 innovation patent specification.doex,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 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 STABILITY FAILED Trial # E6f 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 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 03/03/15,jb22520 innovation patent specification.doex,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 paq. Solution 4 to 10 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 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 # 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 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 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 STABILITY FAILED 03/03/15,jb22520 innovation patent specification.doex,203 - 203 Trial # E6h 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: 13.0 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 pHaq. Solution 4 to 10 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 to 2000cPs (temperature at 5C) 0t 00~ / 03/03/15,jb22520 innovation patent specification.doex,204 - 204 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 # E6i 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: 13.0 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 pHaq. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) 03/03/15,jb22520 innovation patent specification.doex,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 to 2000cPs n/a (temperature at 50) Viscosity 0t 0~~ / temperaturee 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 # 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, 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: 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 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 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 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 n/a 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 hooeeufe rmpae liquid, homogeneous,' free (Accelerated Ageing) homon free frmas from phase separation in Passed 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 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 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) 4208.3 805 eg. Triallate Tech (95% purity) 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 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 homrene free f phase liquid, homogeneous re Passed (Accelerated Ageing) homraognos freen formase from phase separation in Pse any format 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? 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: n/a FORMULATION Component Amount, g Loading, g/L (Chemical name) S-2,3,3-tricholoroallyl diisopropyl(thiocarbamate) 4210.8 806 eg. Triallate Tech (95% purity) 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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 homrene free f phase liquid, homogeneous re Passed (Accelerated Ageing) homraognos freen formase from phase separation in Pse any format 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? 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 03/03/15,jb22520 innovation patent specification.doex,210 - 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 pHaq. 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, 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) seaaini n omtfrom phase separation in any format 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? PASS Description: AWAITS FURTHER ANALYSIS 03/03/15,jb22520 innovation patent specification.doex,211 -211 Trial # E7e TRIALLATE 900 PATENT TRIALS Triallate active present at 800g/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, 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 pHaq. Solution 4 to 10 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 0t 0~~ / temperaturee at 5C) 0 to 2000cPs n/a Viscosity 0t 0~~ / temperaturee 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 03/03/15,jb22520 innovation patent specification.doex,212 - 212 Trial # E7f 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: 13.1 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 pHaq. 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, 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 homrene free f phase liquid, homogeneous re Passed (Accelerated Ageing) homaraiogeno, f formhase from phase separation in any format 03/03/15,jb22520 innovation patent specification.doex,213 - 213 Viscosity 0 to 2000cPs n/a -(temperature at 50) 0t 00~ / 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 # 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: 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) 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 pHaq. Solution 4 to 10 n/a 03/03/15,jb22520 innovation patent 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 0t 0~~ / temperaturee at 5C) 0 to 2000cPs n/a Viscosity 0t 0~~ / temperaturee 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 # 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 03/03/15,jb22520 innovation patent specification.doex,215 - 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 pHaq. Solution 4 to 10 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 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 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 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 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 STABILITY FAILED Trial # E7j 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: 13.1 03/03/15,jb22520 innovation patent specification.doex,217 - 217 FORMULATION Component Amount, g Loading, g/L (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 pHaq. Solution 4 to 10 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 to 2000cPs n/a (temperature at 5C) Viscosity 0t 0~~ / temperaturee 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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 Dark yellow to brown liquid, Dark yellow to brown Cold temp. stability homrene free f phase liquid, homogeneous re Passed (Accelerated Ageing) homraognos freen formase from phase separation in Pse 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 PASS or FAIL? Description: AWAITS FURTHER ANALYSIS 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. 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, 0.1 ml 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 homrene free f phase liquid, homogeneous re Passed (Accelerated Ageing) homraognos freen formase from phase separation in Pse any format 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? PASS Description: AWAITS FURTHER ANALYSIS 03/03/15,jb22520 innovation patent 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, g/L (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 pHaq. 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, 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 homrene free f phase liquid, homogeneous re Passed (Accelerated Ageing) homraognos freen formase from phase separation in Pse any format 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? PASS 03/03/15,jb22520 innovation patent specification.doex,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-tricholoroallyl 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 pHaq. 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, 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 liquid, homogeneous re Passed (Accelerated Ageing) homraognos freen formase from phase separation in Pse any format Viscosity 0 o2Ocsn/a (temperature at 5C) 0 to 2000cPs Viscosity 0 to 2000cPs n/a -(temperature at 20C) 0t 00~
/
03/03/15,jb22520 innovation patent specification.doex,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 700g/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, 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 pHaq. Solution 4 to 10 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 0t 0~~ / temperaturee at 5C) 0 to 2000cPs n/a Viscosity 0 to 2000cPs n/a (temperature at 20C) 0t 00~
/
03/03/15,jb22520 innovation patent 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 pHaq. Solution 4 to 10 n/a Specific gravity 1.00 to 1.30 n/a (temperature at 20C) 03/03/15,jb22520 innovation patent specification.doex,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 2m o om cream&oil @bottom 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~~ / (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 EMULSION CHARACTERISTICS FAILED Trial # E8g 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) 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 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 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 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 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: 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) 3686.7 705 eg. Triallate Tech (95% purity) Block Co-polymer 665.8 134 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 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 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 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 03/03/15,jb22520 innovation patent specification.doex,227 - 227 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 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 pHaq. Solution 4 to 10 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, (Cleated. stain) homogeneous, free from phase Formed crystals Failed (Accelerated Ageing) separation in any format 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 STABILITY FAILED 03/03/15,jb22520 innovation patent specification.doex,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 pHaq. Solution 4 to 10 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 to 2000cPs (temperature at 5C) 0t 00~ / 03/03/15,jb22520 innovation patent specification.doex,229 - 229 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 03/03/15,jb22520 innovation patent specification.doex,230 -230 APPENDIX 11 L tA oH a T X a. 1 9 s&
-
.. tb s -M Jsm _ * - 0 k i -- -- -- -- b 7 x 03/03/15 ,j522520 innovation patent specification.docx,231 - 231 'N' .St-4k. fY 4PP 00 03/03/15,jb22520 innovation patent specification.doex,232 - 232 1 a5 6S ---- ---- . ..... v. n ts ~ t 8I a~ 4)*~W' ~ilH~' c
§
03/03/15 ,j522520 innovation patent specification.docx,233 - 233 . ... . . D -, P; TM cu Qu. P z 5 : 1~ i ,: en a Z .i& ... . n4W ''....* '4 ' 03/03/15 ,j522520 innovation patent specification.docx,234 - 234 Rsspn*'t Re: A4flZlM 220 A ~ - &Is h~s ttta wts m-r &'uli A tc*toe~ w yxiri~h Cg at hat ta& - - -- -- - -- - - -- ---- --- ---- -- -- r &. ... . " ' , ' ' , wetg~ isuthzs~t &tw * ~ snt~na om t--------------~h~ 13pera ~ QHokrry' 1,rsC E14} r1t3patit~ r -------- ..... ----------------------------- -. -~m ---------- ...............................---- ----------- CL2stk fga ji m -m 4.Mm pea ------- _ _ -2 & ------ -- -----C- .... ..... .... ..... ..... .... .... --- -- 4UStar tard a ...... ......- L . i ..... a -- a-------------------------L R X ------ _ _ _ _ -r n e l k --- -- .. ... .. -- --- --- ---r t-- -.. .... ... .. .... ... ... ... -------- ~o -a t-- --- --- --- ......... d. ..................... r-----------------------------------d ----------- t-------------- .* ...... n -------- Ii3tar Rt P adr 03/03/1 5,j522520 innovation patent specification.docx,235 -235 I \% ra-11-, rade ;tz r= n& A17rli CkM $ftMW KWTNAN4 WA W6" IMIE~~C(( IW t O A OM A~~&Th N fl0V +4tfAw h14 NIVm 1 Th4mm The chrornatgraim is shown iii En:y 1 2t _~lt fl1ZWlI V442\" M ________ 03/03/1 5,j522520 innovation patent specification.docx,236 -236 wn C OW :, 4A ASt uAx ~ r a. t, "N"" The ~ ~ ~ ~ 94Sj chomtoyrrAi sow i Fg-) 03/03/1 5,j522520 innovation patent specification.docx,237 -237 K Ausffali t3WA24W K'3AW\ W A V The chromawogram is shoxvn in Fig. 3. 2 ~ ~ fH A.2 3W &7 03/03/15,jb22520 innovation patent specification.doex,238 - 238 ntrade ***7**" \ K ~ Atftria ~ h A61 sItm Xamss AiekTypet ThmeeCr 6t4P s~ectctstVss TaAWWVmA4Sn S The chromatogram is shown in Fig, 4. ?uk Thk Cume1 - Chomt ]I Ped Ka l ge Arts Arm Hdegft r4ht% M JP* md a - 2 2221s flD421 10t 6.94 2 D .__... _... .. .. .- . . _...._ 2. . I3 mas moi mza *co- M 03/03/15 ,j522520 innovation patent specification.docx,239 - 239 I T Autra d;o~~ k~tf4 63J ~§P Oil SolM OM OA 12 The chromawogram is shoxvn in Fig. 5, Thks I ------- M yv $464 61 u;%9 1 1 --- -- - ~~41 M9 4tA Th _____ 2 .
03/03/15 ,j522520 innovation patent specification.docx,240 - 240 w'Austia Q k 5CO C W 2 A-WtYsO? )W&t~~M2f4 P StD~ aw m CV ,~s Lt Uw~t4 I M,~f~~# i~ The chiromaiogram is shown in [Fig. 6. C aJ Th tw I- ' RtM ", AHnb k29.O$t5u U 03/03/15 ,j522520 innovation patent specification.docx,241 - 241 E&I §MWA W A 61 The chromatoayram is shown in Fig. 7 .P~~~~~si~~~~*~ .11' n l~ 4 t ~ ~ ~ Ml D ~ .............. 6 h74 I s~ ......................... 2 03/03/15,jb22520 innovation patent specification.doex,242 - 242 TnatIe (%)419 0333 Esimk,(8 ME49 716 A ai Ocem St&e KWINANA WA 67 PO fi 39S COMO IWA 67 AnaysDe& T & 2§142I4 3-7:M PM Uer lNam di Swp VMI The chromawgram is shoxvn in Fig. 8, ......... VV .0 l a1 ...... T . A. : Da9 4 N4e C:M a tiw\a ,,t1\, l Alen14t..d Medd N : '4Matle~1Mojait ~fdatt~dt6aeg 2 Di se1dp2~ $~m 2Al 03/03/15,jb22520 innovation patent specification.doex,243 - 243 PchAss (08) 94.9 7516 r u AKWTNANA WA 667 PO( 3 (tA-OMO WA 6fl Aayds Da & T4c : 201002/4 4:09:31 PM U -m Mi4 4 d' Sh c-oamp o New is shwin ig 9t :t adg a~ Sap l 2010214L4 igjkao volm : 309 hiete~ Naat : C±4OattAeW'bwim Mti cb 4 inen The chromatogram is shown in Fig, 9. Peek 'Tabe (2em -Ctsmd Pek#R> Tom~ Ass Ans% Ikdgt HeigtX Mis EM CmpdName $30 2 9910 4 MJ5 I DP . 34 tE7fl 5$417 3+ 2ri T % 7 .. 10 . 1...........l 03/03/15 ,j522520 innovation patent specification.docx,244 - 244 lirnrade zz Atralia Pm k N T2~ 2fl/4 t2 41 PM The c2omPga is shxni Fg Th hoak o na is shoAn in ~ ktA Y 10. XM211Z4 $9,SO 97 a% 1. IJEP --- _ _ _ _ _ _ _ ----- 60---07--- - ---- ---- ---- 6 ............. - ------- 03/03/15 ,j522520 innovation patent specification.docx,245 - 245 U'wgl NZ WS lqlq~l \ThRIfi"L tw V WNN U i "W6 ,4 itsmI Wt34ypeW 6, The chromawogram is shoxvn inl Fig. I1I I LAI~ =Mfg J 5017~ 1 n S 17"xi4,1K 43. rn& wteoolJ 03/03/15 ,j522520 innovation patent specification.docx,246 - 246 -Qkk Austrafia " gw_ &xt396CflW.) WA X~~ Tr ha *z~waMW&:~t "m wx"", ' IS-Mt a ~ T~e!t~f~ ~d~i di~ *tbsv M t~~ JAit ~~t 9~~DEPT mr 6fel 2 "K_______ --------- ......... ..........
03/03/15 ,j522520 innovation patent specification.docx,247 - 247 Alnatad t 395k--' CUOWO WA W2 ISf A"a."M~u tt The chromawgrnam is shoxvn in Fig . 13. T~MV $Sfl~ 1 ID# CKIP da 9 -3XO t g4 k -- - - - - - - - - - - - - - - - - - - - - - - - - - - - -- - - - - - - - - - - - - - - - -~ -- - - - - - -- - - - - - - 03/03/15,jb22520 innovation patent specification.doex,248 - 248 TmtaieTih4:(nX)9419 ?f16 0ms S5* K W1NANA WA 6 6 PO ox393COO'A 95 Airym Da&e & Ta t w~ f2d7/4 $: 0t06 PM~ UTMN1e: Anl*~ a~dti ~t*~ Vintt : 4A The chromao : 20ishown in T2h4 14P inec Vkirn : 000grMA~D -- STD--- A9&34 a -N :------ CM-2 10 Metoe one e C~eimmadmetaTiama~ 03/03/15 ,j522520 innovation patent specification.docx,249 - 249 Llzus ij Nam WA 41 The hriatpyra is& shwn in F*O@C 15.~i~ NwI% RcMM&A K ~ 3kP 21~ "r~a Th -h o at a a is sh- in-- -Fig---------- ----------- -3:-,-- --- 6------- 4 , 15.----
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TZW314 X"I A, M 526 tcAII* 03/03/15,jb22520 innovation patent specification.doex,250 - 250 - e :i:0 9497 AGeIa BSEt XWNA)RA WA 6 t -P0 3m 3 COMO WA 6912 AmlssDat & Tixms 201294 a 3M:0 PM. Saeh ot < alat 9O0EC Vastidtii. Paitsam 5 4&cik V\urgm The chromaToram ispshown in Fignow 1 6 fISTDl CAnntl rn;it im~~~ew' 0G 20 9zdtWhJtlm \2024Pge T e c r r a g a i s s o -i i . 1 6. ..... . -- 03/03/15,jb22520 innovation patent specification.doex,251 - 251 APPENDIX 12 Safety of Imtrade Avatar Ultra 90GEC compared to Imtrade Triallate 500EC on shallow sown pulses (Kaspa peas), CLIENT NEIL MCPHEE, JMTRADE Or Petfr Butsas, Plapt Sciane consuting IY APAR2 Z 03/03/15,jb22520 innovation patent specification.doex,252 - 252 FINDNGS ,;awe up to g a As either lstmle A.; DEGC (Prp ce rade ai-MIte COOEC (le~tra)' herbicie did not aoe perAt imere vicisa bicnxss duitr e4 shsf w Kaspa peas re esereitg ptdse cro (Tatie * i Th ss its riigged that ta&k Avatar 900EC is as sate to use on aak sow : Kaspa pa a mret% Tri5k/ts 50%C h r>a Tabte 1, Redsai 0 mas and plan r ars w o m rii -L-------- - - - - --- egwona oa mdewath re ated w ith ios00 n plstnute (IX) ats r ~- --------- --- --------- ,- -------.-.............
L 1.6 Ua e A &c6 ------ ----------- .... -- 1... --------- 2rpoe 890 ml/a 0 oposed'_ MATERtA1LS AND METOOS Shallow' sor fsjapa J.c eth a- retdwt 0 ua of tr- a a AvY4aa 28S90 MI/ha PpsdJ 3. Orprayed Seed (6 per pot) were sown at Ian depth in l0cm x 1cm pms and sprayed he seed Ws then covered by 0,M sod to simuate incorporaton which is the mis Common practice a -appl.ig pre-ernergpnce herbicides in ne-tO agriculture Herbcde apphetion was peeromed using a laboratory boon sprayer equipped wt M I je fan nozes at a !peed of 1 n& Output front the sprayer was calibrated at 110 L ha at a pressre of 250 kPra. srsg this testing proMdure, vdatation losses wet mirnimised by the immediate and even in.orportion of wa bericidar The experiment was conducted d outdoors in a shade house in March-Agri 2012 as a randomisd complete design with five replatsns. Herb.dke ftects were measured 3 weeks after spraying The number of pea se-edlings that had emerged was to ed an converted to reduction I: par urnbrs (Table t t addition. bomanducios w isualy estimated by com-parng to untreated plants (Tabe ln rads Q:MaIt 03/03/15,jb22520 innovation patent specification.doex,253 - 253 Report Comparison of two Imtrade Triallate formulations: intnde Avatar Ultra 900 EC and trade Triaflate 500 EC on wheat safety and wild oat bioefficacy cJeenlmrade Andrali Tria Officer Dr eter Beutsaii Dte 20 November 201 Execudve Sumnmary ne imeraedo Avar Ulnr 9{o EC and Irmtrade Traalate 500 EC heroicdes offer qivilent efficacy on the target species at eua active equihle apphtaton r tits. Both prodore pet&:med similarig in ierm dithetr effect on nodargettipecies - e they disptlsyed shimia*-t host crop -iafety characteristics Ia effect wh en applied att ratni sto as to dtnvitr identkat amonts of the active ingedient :(triallatr). both pradwts were equivialent in at-erm d bionfficacy and hatcrop eaety. ~fac tt!,Aata< .:.taoittt 03/03/15,jb22520 innovation patent specification.doex,254 - 254 Find wings The effect of a rate response of two preemergent herbicide formulations on wheat safety and wild oat aWdvity, four weeks after applicaton was assessed The two formutiAons will be refe rred to as "proposed" rbidde ard ~reference" herbicide Details of the formuaions are: "Proposed" Imtrade Avatar Utra 9N0 EC Herbicide Imtade tsdAtr 900g/L EC Imtrade Triaitate 500 EC Herbicide 1a trade triallate 500g/L EC Bioefiacy: Both formuktions were hugh y ef ectve on wild oauts with complete conLtrol achieved at half the recommended rntes (Figure 1. Efficey often observed in both por and feWd trials does not aways correte with yield losses as there are numerous factors apart from herbicide efficacy that influences yield, i addition herbkides are generally more active in pot trials due to optimum herbicide application perfect growmg conditOns and the absence of stubble and other field factors whWIh commonly hinder herbicide perfostance, 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 rnade 4 weeks after herbicide application.
03/03/15,jb22520 innovation patent specification.doex,255 - 255 Hast Crop Safety; Below 10% biOmIass redaction was observed at 400 g aha of he proposed ' herbicide ampared to a :tSticalty sg rnm t for the ^reference erbicde (Figure 1. At the teomm ended rates of each product. the differences on wheat sety were not stattsticaly de r:nt (Figure 1J iimiary, at double the recommended rates af each formuiatijon, there were o a tattstically significant diFferences on wheat safety, Thus there was a pfgntle difference seed between wheat and wiid o activity suggestsing both the "pu psed''and "reference" M formuiatiotts would be selective irn a crop s§Watihan at. the recommended rat es "prepoed" M by Imtrade. NiethoDs and MaterdFs A pot trial was conducted by Plat Se meo Consulting located ir Prospect, SA The pliant material used war Wheat (vanery Derrinut) and wdd oats (A vena soris Wheat was sawn at Acm depth and wid oats wa awn at 2cm depth mn 55L potn ontaning potting mix specially formurated at the Unersity MtAdelade. Fe replicate pots were ess Ablished 6> oach herbicide treatment. Standard error ofthe mean were calmiatd for each hethicide treat tent. Spraygx was conducted m&r cabinet sprayer located at thet navrsisyvofAdeiade, Waie Camprt T1he spt yer nutpt twas OOL./ha using twin T-let 001 nozzles with t he boom mavug at 3.6 kn/h Each herbicide was sprayed onto the sod surface and then it cor'porated irsmediatey after spraying to te an 185 syst em. The por were kept outdoors in a s'hade-house and watered as required, 03/03/15 ,j522520 innovation patent specification.docx,256 - 256 iict~tt~ nit a'tptt a aaa~tt~pOa~tt~ $a-ltI4~da ti v44ait &lt.]t<'aat~a~I$Iflt a t'sittt ~ttt ~(tiitiet -- ai ai ------- t --- --- ----- t4 .. .. . ------- -no~~ ~ ------- e t ~ a t i t a s M ' a rt d t a tt ~ a Kotat~~~~~~~~~~~~~ot... t.tt :t 1~r~~$tht tt C - P ttp a a'-"-- '-'------------ _ _ _ _ I -------------- h------~ L~ '' ~ '- ' '~ ......... -t t -t ---- 1 ~ ~ l .... ....... i ~ a ~ t C 1< 03/03/15,jb22520 innovation patent specification.doex,257 - 257 ~MTRAM~Cnl4~ Efficacy of Imtrade Avatar Ultra 900EC compared to Imtrade Triallate 500EC in combination with Imtrade Trifiuralin 480EC on herbicide susceptible annual ryegrass activity. CLIENT: NEIL MCPHEE, IMTRADE DT Patar 9outras, PlasItne iu 17 APRIL 2012 03/03/15,jb22520 innovation patent specification.doex,258 - 258 FINDINGS Th..-age gj g apM appIlod a edthe imrade AvWtW TKV)tN or 1atea Tudiame 500EC hetrbicid. pbduit B% coreto &hMide use yess bied at i em dpabo 4 Addeon T 115 U latoade Thd lra 480EC Itbice to either thf& trnsatal suited ri tie 14|I o n0 of y Tgaheass ses:Jst PAugessMt 1t CO>tnasal d TNT tUTtde f 4IC tic1otetft Wodfk Ans W00!EC IMiade T-slate 00EC mli ses-in w eqput ckt of bWttls suacept& Ta*Ae 1. Pecsmtcttwi M Iesce asseepe rg~e tAoatypeSt4 il o ItIod~t ie e ustides amt cart rs IomdaTdto~in 480EQ stndrd ro gvrbkde ----------- j ---- .. .---- Salm [Ufhe Rferec 1-6 qN Refer c L 75 /h Trfjnb 4ACO Propmed 3$90i/i Pwee SSO nMh .51heTisah4OCs ±6 --------- --- ._ns I ------ te --- -- - ---- ----- -. ....... ---- -.... -------------------- Im---s .... - --- - --- ---- ---- n---- ---- !--- 03/03/15,jb22520 innovation patent specification.doex,259 - 259 MATERIALS AND METHODS Nernde suscep1tle ryegrass was tested wtth Avatsr Lt41 900EC t popmedi o TrialthY e 50XWC Ureferencef) combinatkas witt lmtradte Tifkean 480EC hetticdde L. 1.6 L/ha $eference' 2.1. tAa %eferenc+ 1.75 L/he imtrade Tritlrahn 480EC herbicide 2. 890 mI/he rropolsed' 4, 90 mI/ha 'Proptaed' + L5 L/ha trade Triflrahn 480C herbicde . Umprayed Se-ed wa:s wn at 1cm depth in 0ukm x 10cm pots and sprayed. The seed was then covered by msd to simulate incorporation which is the most common pratte o apply pre eml3ergete herbicddes in nrol agritsdure. HerAcide apphcation was performed usls a laboratory boom sprayer equipped with twin 2 jet fan mstdes at a speed of I ms' Output from the sprayer was calibrated at 110 1, ho' at a pressure of 250 kPa. Using this testing procedure, Voitasation losses ere mimrsed by the immediate and even incorpor tior of the herbicide. The expedment was coducteel outdoors i a shade touse on March -Aprl 2012 as a randomised complete design with five replctis. Hericide effects were measured 3 weeks after spraying Seedlings were crisidered emerged if they had reached the -leaf stage at ts time. .ryia % was recorded by c paang she sorviv ing number of 2 leaved seedngs m the sprayed treatments to the number present before ;prayng. Percentage control w as calclated by subtf acting % survival from 100 ITable mtade CaMh&er.Sd

Claims (5)

1. An emulsifiable concentrate formulation of triallate including: as the sole active ingredient, triallate wherein the triallate comprises at least about 600g/L of the emulsifiable concentrate formulation. and further comprising at least one agriculturally acceptable surfactant chosen from the set consisting of calcium alkylbenzenesulfonate in liquid concentrate form. alkylphenol ether sulphate/alkylamine ethoxylate salt. alcohol ether sulphate/alkylamine ethoxylate salt., 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, and optionally further comprising at least one agriculturally acceptable solvent.
2. A formulation according to claim I wherein wherein the liquid components of the emulsifiable concentrate form a solubilising moiety for triallate and wherein the ratio of triallate/solubilising moiety is greater than about 2.
3. A formulation according to claims I or 2 wherein the agriculturally acceptable solvent 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.
4. A formulation according to claims 1, 2. or 3 wherein the at least one agriculturally acceptable surfactant comprises calcium alkylbenzenesulfonate. and said calcium alkylbenzenesulfonate is present. net of solvent in an amount of at least about 15 g/L. 23/06115,jb22520 amended claims.docx,261 -261
5. A formulation according to claims 1. 2. 3 or 4 wherein the agriculturally acceptable solvent comprises a petroleum derivative present at less than about 400g/L, and comprising an agriculturally acceptable surfactant such as calcium alkylbenzenesulfonate in an amount. net of solvent, of less than about 120g.
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