Classifications

• • A—HUMAN NECESSITIES
  • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
  • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
  • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
  • A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
  • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels

Definitions

• This disclosure concerns the use of dibenzylidene sorbitol (DBS) or chemical derivatives of DBS as rheology modifiers useful in preparing stable oil dispersion (OD) compositions of agrochemical products.
• DBS dibenzylidene sorbitol
• OD oil dispersion
• An agrochemical active ingredient such as a herbicide, insecticide, or fungicide, or a herbicide safener, can rarely be used in its originally
• Agrochemical products generally consist of two parts, the active ingredient and the co-formulants or inert ingredients combined together in a formulation.
• the combination of these two parts into the final product is conducted with two primary goals in mind: (1) maintaining the stability of the product during storage and (2) providing an easy and effective way to use the product upon dilution in a carrier such as water or oil, and spray application to an area to be treated.
• Agrochemical formulations are generally designed based on customer needs and the physiochemical properties of the active ingredient(s), for example, the solubility of the active ingredient in water and other non-aqueous solvents.
• Liquid formulations include emulsifiable concentrates (EC), suspension concentrates (SC), soluble liquids (SL), liquid flowables (F) and oil dispersions (OD).
• EC formulations consist of oil-soluble active ingredient(s) dissolved in non-aqueous solvent(s) to which are added emulsifying agents.
• the basic components of an agricultural OD formulation are the solvent or oil phase and the dispersed solid phase. These basic components may include active ingredients, petroleum or naturally derived solvents, safeners, rheology additives, emulsifiers, dispersants and other co-formulants that help deliver the desired attributes of the product.
• Rheology additives provide physical stability to the formulation by increasing the viscosity of the liquid phase in order to prevent insoluble active ingredient particles from falling out of suspension and forming a layer at the bottom of the storage container. This phenomenum, known as sedimentation, can result in difficulties in the delivery and use of the product if the sedimented layer of particles forms a hard pack that is difficult to disperse and re- suspend.
• a related physical instability of liquid formulations is syneresis. Syneresis in an OD formulation is generally measured as the amount of top- clearing due to phase separation.
• the amount and severity of sedimentation that occurs in an OD formulation over time may be measured with a pourability test. This test is conducted by pouring the OD formulation out of a container in a controlled manner and measuring the amount of the formulation remaining in the container. The pourability value is the per cent by weight of material remaining in the container.
• Rheology additives used to control sedimentation also known as thickeners, anti-caking agents, viscosity modifiers or structuring agents, generally provide the increased viscosity to the OD formulation.
• rheology additives have a shear thinning capability that allows the gel network they form to easily breakdown upon application of a small external force. This shear thinning allows the OD formulation to maintain its viscosity and physical stability while at rest, but allows this viscosity to quickly dissipate when external force is applied so that the product can be easily poured or pumped from its container, mixed in a carrier such as water and applied to an area where it is needed.
• Rheology additives used in products today to add viscosity come in many forms and chemistries. They can be mineral or derived from minerals (e.g., organoclays, fumed silica), swellable polymers (e.g., polyamides or hydrogenated caster oils), associative thickeners which form structures by themselves (e.g., EO/PO block co-polymers), or they can be steric dispersants (e.g., comb polymers such as polyvinylpyrrolidinones or polyacrylates). These rheological or structuring agents provide long term stability when the product is at rest or in storage.
• minerals e.g., organoclays, fumed silica
• swellable polymers e.g., polyamides or hydrogenated caster oils
• associative thickeners which form structures by themselves (e.g., EO/PO block co-polymers)
• steric dispersants e.g., comb polymers such as poly
• Agrochemical products generally have to be diluted and properly dispersed in water prior to application.
• An emulsifier system may be included in the OD formulation to help disperse the oil-based, water immiscible formulation in water.
• An emulsifier system commonly includes a mixture of non-ionic and anionic surfactants in order to accommodate variations in water hardness and temperature encountered in various locations.
• clays, organoclays such as bentonite, hectorite or gibbsite clays, which are also known as hydrophobically modified clays, hydrogenated castor oils, castor oil derivatives, polyamides, polar, oxidized waxes, and hydrophobized fumed silica may be used as rheology aids in nonaqueous solvents.
• organic sulfates are commonly used.
• High molecular weight polymers such as ethyl cellulose, cellulose acetobutyrate and man-made polymers such as polyacrylates, polystyrenes and polyisobutylenes may also be used to build viscosity in organic solvents.
• soaps such as aluminum stearate and magnesium stearate may be used to build viscosity.
• Natural clay products are generally layered silicates that can be effective thickeners for a wide range of applications. In order to make them dispersible in non-aqueous solvents, however, the clay surface is usually treated with quaternary ammonium. These modified clays are known as organoclay thickeners. These strongly agglomerated particles need to be wetted first and then separated by shear forces. High shear mixing is desirable for this process. Activators like alcohols can penetrate in between the clay layers and help make them form loose stacks for ease of application. The typical rheology curve of clay particle modified OD formulation shows strong shear-thinning and thixotropic behavior. At low shear stress, the clay structure may show some resistance to the flow.
• these micronized powders have to be dispersed into a gel form without complete dissolution in the solvent.
• the first step is swelling of the crystalline particles by the solvent using shear and heat to provide swollen particles that become fully separated and dispersed.
• the activating temperature is dependent on the solvent type. Care has to be taken not to exceed the activation temperature otherwise the castor oil derivatives will completely dissolve, lose their thickening properties and recrystallize upon cooling. Usually a pre-gel can be made for easier use of these materials.
• the third type of rheology modifiers that require polar interactions to build up a three-dimensional network are those based on fumed silica.
• Fumed silica either hydrophilic or hydrophobic, is composed of nano-size primary silica particles connected together to form chain shaped segregates. Due to its extremely high surface area and wide solvent compatibility, fumed silica products are widely used in formulating industrial and consumer products. Although both hydrophilic and hydrophobic fumed silica can be used in OD formulations as thickening agents, hydrophobic silica generally provides rheology properties that are easier to control in non-aqueous formulations than does hydrophilic silica.
• Rheology additives used in OD formulations to insure that suspended particles of active ingredients are not susceptible to irreversible sedimentation may be used alone or in combination with other rheology additives. It is very common to combine one or more rheology additives in a single OD formulation to obtain the desired rheological properties and, at the same time, minimize any adverse interactions that may occur between ingredients.
• the proper choice and amounts of OD thickeners can enhance the thickening efficacy and application range of a particular formulation. Factors to consider in the selection of rheology additives for the design of a stable OD system are the type of solvent, the interactions with emulsifiers, the robustness in activation of the thickeners, and the temperature sensitivity of the final system.
• DBS is derived from the sugar alcohol D-glucitol and benzaldehyde and is marketed by Milliken Chemical as Millithix® 925s. DBS has been investigated for use as a gelling agent in personal care products such as antipersperants and cosmetics, and also in biomedical materials and electronic devices. DBS has also seen use as a clarifying agent for polyolefin derived plastics (Millad® 3905). The morphological characteristics of DBS have been described by D. J. Mercurio and R. J.
• NX8000 CAS 882073-43-0
• Milliken Chemical a new DBS-type product known as NX8000 (CAS 882073-43-0) has been marketed by Milliken Chemical as a clarifying agent for plastics and its structure is shown below
• OD formulations of agrochemical products and offers improved performance and compatibility with the increasingly complex products being developed today.
• inventive compositions for producing stable OD formulations of agrochemical products that are suitable in controlling undesired vegetation, insects and plant diseases, the inventive composition comprising a solvent, dibenzylidene sorbitol or an analog of dibenzylidene sorbitol, and an agricultural active ingredient.
• the present invention relates to the use of dibenzylidene sorbitol or analogs of dibenzylidene sorbitol as rheology additives with improved
• the solvent of the present disclosure is generally an organic, water immiscible solvent and may comprise one or more of petroleum distillates such as aromatic hydrocarbons derived from benzene, such as toluene, xylenes, other alkylated benzenes and the like, and naphthalene derivatives, aliphatic
• hydrocarbons such as hexane, octane, cyclohexane, and the like, mineral oils from the aliphatic or isoparaffinic series, and mixtures of aromatic and aliphatic hydrocarbons; halogenated aromatic or aliphatic hydrocarbons; vegetable, seed or animal oils such as soybean oil, rape seed oil, olive oil, castor oil, sunflower seed oil, coconut oil, corn oil, cotton seed oil, linseed oil, palm oil, peanut oil, safflower oil, sesame oil, tung oil and the like, and Ci-C6 mono-esters derived from vegetable, seed or animal oils; dialkyl amides of short and long chain, saturated and unsaturated carboxylic acids; C -Cn esters of aromatic carboxylic acids and dicarboxylic acids, and C C ⁇ esters of aliphatic and cyclo-aliphatic carboxylic acids.
• the above solvents may be mixed with one or more polar solvents such as, but not limited to, ethers like tetrahydrofuran and the like, alkylene glycol mono- or dialkyl ethers such as ethylene glycol monoethyl ether and the like, amides such as dimethylacetamide or N-methylpyrrolidone and the like, ketones such as methylethyl ketone and the like, nitriles such as butyronitrile and the like, sulfoxides or sulfones such as dimethyl sulfoxide or sulfolane and the like, mono- or polyhydric alcohols having 2 to 12 carbon atoms, and alkylene carbonates such as propylene or butylene carbonate and the like.
• polar solvents such as, but not limited to, ethers like tetrahydrofuran and the like, alkylene glycol mono- or dialkyl ethers such as ethylene glycol monoethyl ether and
• the solvent of the present disclosure may comprise, with respect to the total composition, from about 200 g/L to 999 g/L, preferably from about 300 g/L to 950 g/L.
• the DBS of the present disclosure is used as a rheology additive to build viscosity in agrochemical OD formations thru formation of a gel. This helps keep the dispersed active ingredient suspended in the solvent and inhibits settling and sedimentation of the active ingredient which can contribute to formulation instability and inferior performance of the product.
• DBS may be dispersed and properly activated in the solvent prior to the addition of other components.
• the resulting mixture containing the activated DBS in the form of a gel generally shows good shear thinning properties.
• DBS may comprise, with respect to the total composition, from about 0.1 g/L to 100 g/L, preferably from about 0.1 g/L to 50 g/L.
• DBS may be used in combination with one or more existing rheology additives that are commonly used in agrochemical OD formulations to provide improved physical stability by inhibiting sedimentation.
• Suitable rheology additives to use with DBS may comprise one or more of a clay, a modified clay, a silica or a fumed silica, a hydrogenated castor oil, a castor oil derivative, a polyamide and a polyester.
• the DBS used in a combination with suitable rheology additives may comprise, with respect to the total composition, from about 0.1 g/L to 100 g/L, preferably from about 0.1 g/L to 50 g/L.
• the suitable rheology additives used in combination with DBS may comprise, with respect to the total composition, from about 0.1 g/L to 200 g/L, preferably from about 0.2 g/L to 100 g/L.
• analogs of DBS may be used alone, in combination with DBS, or in combination with one or more existing rheology additives used in agricultural OD formulations to provide physical stability by increasing the viscosity of such formulations.
• These analogs may comprise the following structures
• ⁇ and Ar 2 are the same or different mono- or polysubstituted phenyl rings groups.
• the substituted phenyl groups may contain one or more substituents selected from, but not limited to, C Qo alkyl, Ci-Cw haloalkyl, Ci-Cw alkoxy, C Cio haloalkoxy, Ci-Cw alkylthio, Ci-Cw haloalkylthio, Ci-Cw
• the agrochemical active ingredients of the present disclosure may be selected from the groups of herbicides, insecticides and fungicides.
• the active ingredients may be present as dispersed solids that have very low solubility in the solvent or they may be completely soluble or partially soluble in the solvent.
• Preferred dispersible active ingredients are generally higher melting solids (>50 °C) with low solubility ( ⁇ 10 g/L) in the solvent phase.
• Preferred soluble or partially soluble active ingredients are generally lower melting solids ( ⁇ 150 °C) with moderate to high solubility in the solvent phase (> 10 g/L).
• the dispersed solid herbicide active ingredients of the present invention include, but are not limited to sulfonamides, sulfonylureas, arylpyridine carboxylic acids and analogs, arylpyrimidine carboxylic acids and analogs, anilides, imidazolinones and carbazones. Also, alkali metal salts or amine salts of benzoic acids, phenoxyalkanoic acids, pyridinecarboxylic acids and
• pyridyloxycarboxylic acid herbicides may also comprise the dispersed active ingredients of the present invention.
• Herbicides which are especially suitable for dispersion in the solvent phase are triasulfuron, tribenuron, metasulfuron, thifensulfuron, flupyrsulfuron, iodosulfuron, rimsulfuron, nicosulfuron, cinosulfuron,
• R is H or halo and X is halo.
• Additional herbicides which are especially suitable for dispersion in the solvent phase are alkali metal or amine salts of dicamba, 2,4-D, MCPA, 2,4- DB, aminopyralid, picloram, clopyralid, fluroxypyr and triclopyr, and alkali metal salts of bromoxynil and ioxynil.
• the amines are comprised of primary, secondary or tertiary alkylamines, alkanolamines, alkylalkanolamines or
• alkoxyalkanolamines wherein the alkyl and alkanol groups are saturated and contain C C 4 alkyl groups individually.
• the alkali metals are comprised of sodium and potassium.
• the solvent dispersible herbicide may comprise, with respect to the total composition, from about 1 g/L to 700 g/L, preferably from about 5 g/L to 500 g/L. It is commonly known that this concentrated formulation may be diluted from 1 to 2000 fold at point of use depending on the agricultural practices.
• a further embodiment of the present disclosure comprises the addition of solvent soluble or partially solvent soluble active ingredients and safeners.
• active ingredients and safeners may include one or more of a herbicide, an insecticide, a fungicide and a herbicide safener, but are not limited to, esters of carboxylate, phosphate, or sulfate pesticides.
• Suitable soluble or partially soluble herbicide active ingredients of the present invention include, but are not limited to benzoic acid herbicides such as dicamba esters, phenoxyalkanoic acid herbicides such as 2,4-D, MCPA or 2,4- DB esters, aryloxyphenoxypropionic acid herbicides such as clodinafop, cyhalofop, fenoxaprop, fluazifop, haloxyfop and quizalofop esters,
• pyridinecarboxylic acid herbicides such as aminopyralid, picloram and clopyralid esters, pyridyloxycarboxylic acids such as fluroxypyr and triclopyr esters, and nitrile herbicides such as bromoxynil and ioxynil and esters thereof.
• Suitable soluble or partially soluble herbicide safeners of the present disclosure may comprise, but are not limited to, cloquintocet mexyl, benoxacor, cyometrinil, cyprosulfamide, dichlormid dicyclonon, dietholate, fenchlorazole ethyl, fenclorim, flurazole, fluxofenim, furilazole, isoxadifen ethyl, mefenpyr diethyl, mephenate, naphthalic anhydride, oxabetrinil and derivatives and analogs thereof.
• the solvent soluble or partially solvent soluble herbicide active ingredients or herbicide safeners of the present invention may comprise, with respect to the total composition, from about 1 g/L to 700 g/L, preferably from about 5 g/L to 500 g/L.
• Additional agricultural active ingredients of the present disclosure may include insecticides and fungicides. These active ingredients may be present as dispersed solids, or soluble or partially soluble active ingredients.
• Suitable insecticide active ingredients of the present disclosure include, but are not limited to, antibiotic insecticides, macrocyclic lactone insecticides (for example, avermectin insecticides, milbemycin insecticides, and spinosyn insecticides), arsenical insecticides, botanical insecticides, carbamate insecticides (for example, benzofuranyl methylcarbamate insecticides,
• dimethylcarbamate insecticides dimethylcarbamate insecticides, oxime carbamate insecticides, and phenyl methylcarbamate insecticides
• diamide insecticides desiccant insecticides, dinitrophenol insecticides, fluorine insecticides, formamidine insecticides, fumigant insecticides, inorganic insecticides, insect growth regulators (for example, chitin synthesis inhibitors, juvenile hormone mimics, juvenile hormones, moulting hormone agonists, moulting hormones, moulting inhibitors, precocenes, and other unclassified insect growth regulators), nereistoxin analogue insecticides, nicotinoid insecticides (for example, nitroguanidine insecticides, nitromethylene insecticides, and pyridylmethylamine insecticides), organochlorine insecticides, organophosphorus insecticides, oxadiazine insecticides, oxadiazolone insecticides, phthalimide insecticides, pyr
• insecticides that can be employed beneficially in combination with the invention disclosed in this document include, but are not limited to, the following 1,2-dichloropropane, 1,3-dichloropropene, abamectin, acephate, acetamiprid, acethion, acetoprole, acrinathrin, acrylonitrile, alanycarb, aldicarb, aldoxycarb, aldrin, allethrin, allosamidin, allyxycarb, alpha- cypermethrin, alpha-endosulfan, amidithion, aminocarb, amiton, amitraz, anabasine, athidathion, azadirachtin, azamethiphos, azinphos-ethyl, azinphos- methyl, azothoate, barium hexafluorosilicate, barthrin, bendiocarb, benfuracar
• Suitable fungicide active ingredients of the present disclosure may also be combined with other fungicides to form fungicidal mixtures and synergistic mixtures thereof.
• the fungicidal compounds of the present disclosure are often applied in conjunction with one or more other fungicides to control a wider variety of undesirable diseases.
• the presently claimed compounds may be formulated with the other fungicide(s), tank mixed with the other fungicide(s) or applied sequentially with the other fungicide(s).
• Such other fungicides may include 2- thiocyanatomethylthio)-benzothiazole, 2-phenylphenol, 8-hydroxyquinoline sulfate, ametoctradin, amisulbrom, antimycin, Ampelomyces quisqualis, azaconazole, azoxystrobin, Bacillus subtilis, benalaxyl, benomyl, benthiavalicarb- isopropyl, benzylaminobenzene- sulfonate (BABS) salt, bicarbonates, biphenyl, bismerthiazol, bitertanol, bixafen, blasticidin-S, borax, Bordeaux mixture, boscalid, bromuconazole, bupirimate, calcium polysulfide, captafol, captan, carbendazim, carboxin, carpropamid, carvone, chloroneb, chlorothalonil, chlozolinate, Coniothyrium
• thiochlorfenphim thiophanate, thioquinox, tioxymid, triamiphos, triarimol, triazbutil, trichlamide, urbacid, XRD-563, and zarilamid, IK- 1140, and any combinations thereof.
• the insecticide or fungicide active ingredients of the present disclosure may comprise, with respect to the total composition, from about 1 g/L to 700 g/L, preferably from about 5 g/L to 500 g/L.
• the surface-active agents can be anionic, cationic or nonionic in character and can be employed as emulsifying agents, wetting agents, suspending agents, or for other purposes.
• Surfactants conventionally used in the art of formulation and which may also be used in the present formulations are described, inter alia, in "McCutcheon's Detergents and Emulsifiers Annual", MC Publishing Corp., Ridgewood, New Jersey, 1998 and in "Encyclopedia of Surfactants", Vol. I- III, Chemical publishing Co., New York, 1980-81.
• Typical surface-active agents include salts of alkyl sulfates, such as diethanolammonium lauryl sulfate; alkylarylsulfonate salts, such as calcium dodecylbenzenesulfonate; alkylphenol-alkylene oxide addition products, such as nonylphenol-Cig ethoxylate; alcohol- alkylene oxide addition products, such as tridecyl alcohol-C ⁇ ethoxylate; soaps, such as sodium stearate; alkylnaphthalene-sulfonate salts, such as sodium dibutylnaphthalenesulfonate; dialkyl esters of sulfo succinate salts, such as sodium di(2-ethylhexyl) sulfo- succinate; sorbitol esters, such as sorbitol oleate; quaternary amines, such as lauryl trimethylammonium chloride; polyethylene glycol esters of fatty
• composition of the present disclosure may optionally include one or more additional inert ingredients such as antifoam agents, adjuvants, stabilizers, fragrants, sequestering agents, neutralizing agents, buffers, corrosion inhibitors, dyes, odorants and other commonly used ingredients.
• additional inert ingredients such as antifoam agents, adjuvants, stabilizers, fragrants, sequestering agents, neutralizing agents, buffers, corrosion inhibitors, dyes, odorants and other commonly used ingredients.
• the effective amount of the OD formulation of the present disclosure to be employed in a typical agricultural application often depends upon, for example, the type of plants, the stage of growth of the plant, severity of environmental conditions, the weeds, insects or fungal pathogens to be controlled and application conditions.
• a plant in need of protection from weeds or insects, or disease pathogen control or elimination is contacted with an amount of the OD formulation diluted in a carrier such as water that will provide an amount from about 1 to about 40,000 ppm, preferably from about 10 to about 20,000 ppm of the active ingredient.
• the contacting may be in any effective manner.
• any exposed part of the plant e.g., leaves or stems may be sprayed with the active ingredient in mixture with a suitable amount of a diluent or carrier such as water.
• compositions of the present invention may be applied to the plant foliage or the soil or area adjacent to the plant. Additionally, the compositions of the present invention may be mixed with or applied with any combination of agricultural active ingredients such as herbicides, insecticides, bacteriocides, nematocides, miticides, biocides, termiticides, rodenticides, molluscides, arthropodicides, fertilizers, growth regulators, and pheromones.
• agricultural active ingredients such as herbicides, insecticides, bacteriocides, nematocides, miticides, biocides, termiticides, rodenticides, molluscides, arthropodicides, fertilizers, growth regulators, and pheromones.
• a pre-gel of DBS is first prepared by dispersing and activating the DBS in the solvent with shear mixing and heat. Following cooling to room temperature, the pre-gel of DBS is then added with mixing to a mixture previously formed by shear mixing the active ingredient and any other ingredients with the solvent.
• An example of a stable OD formulation of the present disclosure in which sedimentation of the dispersed active ingredient is retarded by DBS comprises: a) a solvent comprising, with respect to the total composition, from about 200 g/L to about 999 g/L of Aromatic 200ND; b) a rheology additive comprising, with respect to the total composition, from about 0.1 g/L to about 100 g/L of dibenzylidene sorbitol; c) an active ingredient comprising, with respect to the total composition, from about 1 g/L to about 200 g/L of pyroxsulam; d) optionally, other inert formulation ingredients.
• ExxonMobil was made by dispersing 1.5g of DBS into 98.5g of Aromatic 200 under high shear, heating the mixture to 50-55°C for 15 minutes, and cooling the mixture to room temperature under low shear mixing. The resulting mixture should be semi-clear to clear in appearance and show highly thixotropic gel properties.
• compositions of the present disclosure shown in Table 1 were prepared using the following procedure: 1) the amount of solvent shown in Table 1 was charged into a glass beaker equipped with a mechanic stirrer; 2) the 1.5% DBS pre-gel was added into the beaker under constant mixing; 3) the active ingredient was then added to the mixture; 4) the mixture was stirred until homogeneous and then sonicated for 10 minutes to furnish the test sample. All samples were stable to sedimentation after 24 hours at room temperature by visual inspection.
• Table 1 Compositions of the present disclosure for evaluation of stability to sedimentation.
• samples 7 and 8 were prepared with the ingredients shown and by the following procedure.
• Aromatic 200ND was first charged into a glass beaker equipped with a mechanic stirrer. Bentone 38 powder was then added to the beaker under high shear to ensure complete dispersion of the powder.
• Samples 9 and 10 were exposed to a variety of temperature conditions including 54 °C and 40 °C constant temperatures, and -10 °C /40 °C cycling over one day, in order to evaluate their storage stability.
• the chemical assays were measured after storage for 2 weeks and formulations 9 and 10 were found to be chemically stable with no loss of the active ingredient being detected under all storage conditions.
• the samples were also compared on the basis of their yield stress which is known to be an indicator of rheology structure strength and hence the stability of the formulations. The higher the yield stress value the stronger the gel strength and hence better formulation stability.
• the yield stress was measured using an AR1000 rheometer from TA Instruments equipped with a 4 mm cross-hatched plate.
• the viscosity-stress curve was obtained by running the steady state shear by operating the rheometer from the lowest torque possible with the equipment up to 10,000 micro Newton meters ( ⁇ ).
• the yield stress was then calculated by the software on the rheometer as the onset stress value measured in Pascals (Pa) to drive the sample to flow.
• the yield stress was then calculated by the software on the rheometer as the onset stress value measured in Pascals (Pa) to drive the sample to flow.
• the pourability of a particular OD formulation is a measure of the amount of sedimentation that occurs over time and how resistant that sediment is to being poured from the container in which it is stored.
• the pourability value can be measured by use of CIPAC method MT 148.1, Pourability of Suspension Concentrates. In this method, the suspension concentrate is allowed to stand for a defined period of time and then subjected to a standardized pouring procedure. The amount of material remaining in the container after pouring is determined and reported as the wt of material remaining in the container. The wt of material remaining after pouring is known as the pourability value.
• a glass bottle containing a sample of Formulation 10 was allowed to stand at room temperature for 24 hours and then the contents of the bottle were poured out following CIPAC method MT 148.1.
• the residual amount of Formulation 10 remaining in the bottle after pouring was found to be 1.77 wt of the original amount, thereby giving a pourability value of 1.77% for Formulation 10.
• compositions or methods may include numerous compounds or steps not mentioned herein. In other embodiments, the compositions or methods do not include, or are substantially free of, any compounds or steps not enumerated herein. Variations and modifications from the described embodiments exist. Finally, any number disclosed herein should be construed to mean approximate, regardless of whether the word "about” or “approximately” is used in describing the number. The appended embodiments and claims intend to cover all those modifications and variations as falling within the scope of the invention.

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