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FORM 2
THE PATENTS ACT, 1970 (39 of 1970)
THE PATENTS RULES, 2003
PROVISIONAL SPECIFICATION
(See Section 10 and Rule 13)
1. Title of the Invention:-
Chemically Stable Solid Formulation of Monocrotophos having Enhanced Shelf Life and Process for Preparation Thereof
2. Applicants:-
(a) Name: CHEMINOVA INDIA LTD.
(b) Nationality: An Indian National
(c) Address: 7th Floor, Keshava Building, Bandra-Kula Complex,
Bandra East, MUMBAI - 400 051, Maharashtra, INDIA
3. Preamble to the Description:-
Provisional Specification:
The following specification describes the nature of the Invention.

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Title of the Invention:
Chemically Stable Solid Formulation of Monocrotophos having Enhanced Shelf Life and Process for Preparation Thereof.
Field of the Invention:
5 The present invention relates to a chemically stable solid formulation of Monocrotophos having enhanced shelf life and process for preparation thereof. Particularly it relates to a chemically stable solid formulation of Monocrotophos having enhanced shelf life of one and half year or more, and a process for preparation thereof. More particularly it relates to a chemically stable water soluble
10 powder, or chemically stable water dispersible powder, or chemically stable water soluble granular, or chemically stable water dispersible granular formulation of Monocrotophos having enhanced shelf life of one and half year or more, and a process for preparation thereof. Background of the Invention:
15 The Monocrotophos is commercially available insecticide, which can be systematically taken up by a plant so that insects, which feed and/or which live on the plants are killed, in addition to those insects which directly ingest or are contacted by the insecticide. The solid formulations are generally known to be more stable and easy to be
20 packed, stored and transported because the solid formulations can be prepared without a solvent. Therefore, the main object of the present invention is to have Monocrotophos formulation in solid form.
The main problem in making solid formulation of Monocrotophos is its poor chemical stability due to catalytically driven degradation of Monocrotophos - the
25 active ingredient [hereinafter may also be referred to as AI] with carriers, fillers and base materials used in preparation of the solid formulation thereby shortening, drastically, the shelf life of Monocrotophos solid formulation. The AI degradation results in reduction of activity of the active ingredient meaning thereby the degradation problem renders the formulation useless for the desired purpose such
30 as insecticides, etc. Therefore, AI degradation of solid form of Monocrotophos formulation possesses serious problem for its storage, which appears to be the main reason for non-availability of solid form of Monocrotophos formulation. The another problem of solid formulations is that these comprise fillers and base materials which are generally not soluble in water, that is will have higher insoluble
35 matter / sediments, and therefore, cannot be made available as water soluble formulations, and hence, such solid formulations are always less preferred due to
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their higher insoluble matter / sediments which poses a serious problem of chocking of spray nozzles thereby making such solid formulations less acceptable for use as spray formulation, and hence, cannot be easily applied on plants after dilution in water in a spray tank.
5 In US patent application no. 10/410,354, a reference has been made to solid form of Monocrotophos formulation. This patent application discloses that a formulation consisting of Monocrotophos and essentially an ester as active ingredients and an inert carrier is possible and can be formulated in general including as wettable powders, dusts, granules, fumigants formulations, etc. However, no disclosure
10 about activity and stability of disclosed formulations when comprising Monocrotophos has been made in this application. Further, there is no indication whether the Monocrotophos, without disclosed ester, but with defined carriers can result in chemically stable solid form of Monocrotophos formulation. It is observed from the formulation examples discussed in this application that chemically stable
15 solid form of Monocrotophos formulation even with defined ester may not be possible.
In co-pending Indian patent application no. 1003/MUM/2006, a chemically stable solid formulation of Monocrotophos comprising one or more saccharides is disclosed. However, it has been observed that it has shelf life of about one year or
20 so. Further, its efficacy has been found to be less than the desired level. It has been observed that commercial viability of introducing a solid formulation of Monocorotophos comprising one or more saccharides with a shelf life of one year or so is however not clear as goods having expired date could become very serious problem for disposal. Further, it has also been observed that its materials cost is
25 higher which renders it commercially less acceptable.
Need of the Invention:
Therefore, there is a need to develop an improved and chemically more stable solid formulation of Monocrotophos having enhanced efficacy and shelf life of one and half year or more so that it does not suffer from serious problem for its disposal
30 and still being commercially viable. Objects of the Invention:
The main object of present invention is to provide an improved and chemically more stable solid formulation of Monocrotophos having enhanced efficacy and shelf life of one and half year or more so that it does not suffer from serious problem for its
35 disposal and still being commercially viable.
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Another object of the present invention is to provide an improved and chemically stable solid Monocrotophos formulation having enhanced shelf life of one and half year or more and still having reduced materials cost, which does not suffer from the disadvantage of catalytically driven degradation of the active ingredient, and
5 therefore, has enhanced shelf life of active ingredient and improved activity of the active ingredient meaning thereby the formulation is useful for the desired purpose as insecticides, etc with longer shelf life, which is desirable.
Still another object of the present invention is to provide an improved Monocrotophos formulation in solid form comprising reduced insoluble matter /
10 sediment so as to have more acceptability as spray formulation.
Yet another object of the present invention is to provide an improved and chemically stable Monocrotophos formulation in the form of water soluble powder, or water dispersible powder, or water soluble granules, or water dispersible granules.
15 This is another object of the present invention to provide an improved Monocrotophos formulation which is relatively more stable and can be easily packed, stored and transported without major loss of activity and stability of the active ingredient over a desired period of time varying upto one and half year or more.
20 This is still an object of the present invention to provide an improved Monocrotophos formulation in solid form which avoids use of undesired carriers, base materials, fillers etc. thereby making the disclosed formulation more economical and more easy to be formulated in-addition to being more stable. This is yet an object of the present invention to provide a process for preparation of
25 an improved and chemically stable Monocrotophos formulation, particularly chemically stable solid form of Monocrotophos formulation.
The other objects and advantages of the present invention will become apparent from the following description of the invention.
Brief Description and Nature of the Invention:
30 The solid form of Monocrotophos formulation has been found to be chemically unstable due to catalytically driven degradation of the active ingredient meaning thereby the shelf life of solid form of Monocrotophos formulation is greatly reduced. The reduced activity of the active ingredient [Monocrotophos] of solid form of Monocrotophos formulation due to catalytically driven degradation of
35 Monocrotophos makes the formulation useless for the desired purpose as
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insecticides, etc. for desired duration. The un-stability of the Monocrotophos formulation possesses serious problem for its storage and then transportation. The present invention is based on the observation that if chemical stability of the monocrotophos formulation, particularly of solid form of monocrotophos
5 formulation can be increased, then the problem of un-stability of the monocrotophos formulation, particularly of solid form of monocrotophos formulation can be easily overcome. It is understood that formulation of monocrotophos with known carriers, fillers and base materials cannot overcome this problem.
10 It has been surprisingly observed that if Monorotophos can be formulated with ammonium sulphate, the active ingredient degradation is drastically reduced and its shelf life is enhanced to one and half year or more. It has also been observed that when one or more stabilizers selected from a group comprising Methyl Para hydroxy Benzoate, Di Ethylene Glycol Mono Butyl Ether and Di Propylene Glycol
15 are employed alongwith ammonium sulphate, then its chemical stability has been found surprisingly very high for shelf life of one and half year or more. However, in order to have solid form of Monocrotophos formulation, the first need is to develop a mechanism to convert liquid form Monocrotophos into solid form Monocrotophos without disturbing its activity. It has been observed that if liquid
20 form Monocrotophos is mixed with an absorbent, preferably with silica, more preferably with precipitated silica, then it converts to a solid form Monocrotophos, which has been found to be convenient for formulating with ammonium sulphate which optionally may comprise one or more stabilizers selected from a group comprising Methyl Para hydroxy Benzoate, Di Ethylene Glycol Mono Butyl Ether
25 and Di Propylene Glycol.
Accordingly, the present invention relates to an improved and chemically stable Monocrotophos formulation having enhanced efficacy and shelf life of one and half year or more and still having low materials cost, particularly it relates to an improved and chemically stable solid form of Monocrotophos formulation, more
30 particularly it relates to an improved and chemically stable and water soluble powder, or chemically stable and water dispersible powder, or chemically stable and water soluble granular, or chemically stable and water dispersible granular forms of Monocrotophos formulation comprising Monocrotophos as active ingredient and ammonium sulphate which optionally may comprise one or more
35 stabilizers selected from a group comprising Methyl Para hydroxy Benzoate, Di Ethylene Glycol Mono Butyl Ether and Di Propylene Glycol as stabilizing agents.
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In one of the preferred embodiments of the present invention, it relates to an improved and chemically stable Monocrotophos formulation having enhanced efficacy and shelf life of one and half year or more and still having low materials cost, particularly it relates to an improved and chemically stable solid form
5 Monocrotophos formulation, more particularly it relates to an improved and chemically stable and water soluble powder, or chemically stable and water dispersible powder, or chemically stable and water soluble granular, or chemically stable and water dispersible granular forms of Monocrotophos formulation comprising Monocrotophos as active ingredient and ammonium sulphate wherein
10 liquid form Monocrotophos is mixed with an absorbent, preferably with silica, more preferably with precipitated silica convert it to a solid form Monocrotophos, and which optionally may comprise one or more stabilizers selected from a group comprising Methyl Para hydroxy Benzoate, Di Ethylene Glycol Mono Butyl Ether and Di Propylene Glycol as stabilizing agents.
15 In accordance with the present invention, the absorbent is preferably selected from the group comprising silica, silicate or mixture thereof. The absorbent is preferably silica, more preferably precipitated silica which absorbs the liquid form active ingredient and converts it into a solid form active ingredient and makes it suitable for formulating with ammonium sulphate to produce desired chemically stable solid
20 Monocrotophos formulation.
In accordance with preferred embodiment of the present invention, the Monocrotophos formulation may further comprise one or more surfactants. The surfactants may be selected from a group comprising napthalene phenol formaldehyde condensate [Tysperse DN], aryl alkyl sulphonate and aryl sulphonic
25 acid formaldehyde condensate, sodium salt of phenol sulphonic acid condensate, sodium salt of sulphated fatty alcohol, sodium ligno sulphonates, napthalene sulphonic acid formaldehyde condensate, or mixtures thereof. The preferred surfactant is Tysperse DN. In accordance with the present invention, the surfactant is so selected, which can
30 also act as dispersing agent, or as wetting agent or as dispersing agent and wetting agent thereby resulting in improvement of spreading properties of the formulation. The advantage of selecting Tysperse DN is that it has been found to act as dispersing agent as well as wetting agent. Further, Tysperse DN has been found to be strong suspending agent and capable of keeping water insoluble matter [silica]
35 in suspension form causing less sediment on dissolution in water thereby has been
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surprisingly found to avoid the chocking problem of the spray nozzles when the presently disclosed formulation is used as spray formulation.
In accordance with one of the preferred embodiments of the present invention, the Monocrotophos formulation may optionally also comprise one or more binding
5 agents. The binding agent may be selected from a group comprising vinyl acetate copolymer, hydroxy propyl methyl cellulose, polyvinyl alcohol, polyvinyl pyrrolidone, polyvinyl pyrrolidone co-polymer, polyacrylic acid, carbo methoxy cellulose, casein, gelatin, acacia, synthetic glue, xanthan gum, guar gum, gum arabic, lignin, or mixture thereof.
10 In accordance with another preferred embodiment of the present invention, the Monocrotophos formulation may optionally also comprise one or more coating agents. The coating agent may be selected from a group comprising sugar, polyvinyl alcohol, lignosulphonates, starch, cellulose derivatives, methyl cellulose, hydoxy propyl methyl cellulose, alginates, or mixture thereof.
15 In accordance with still another preferred embodiment of the present invention, the Monocrotophos formulation may optionally also comprise one or more additional active ingredient which may be selected from the group comprising fungicide, insecticide, any other such substance or mixture thereof. The fungicide may be selected from the group comprising carbendazim,
20 hexaconazole, mancozeb, thiram, captafol, captan, maneb, Propiconazole, tricyclazole, tebuconazole, chlorothalonil, zineb, ziram, methyl thiophanate, or mixture thereof.
The additional insecticide may be selected from the group comprising chlorpyriphos, quinalphos, acephate, dichlorvos, dimethyl, phenthoate, malathion,
25 ethion, fenvelarate, cypermethrin, permethrin, cyhalothrin, deltamethrin, cycloprothrin, or mixture thereof.
It has been surprising observed that when Monocrotophos in absorbed form on silica is formulated with ammonium sulphate with or without one or more stabilizers selected from a group comprising Methyl Para hydroxy Benzoate, Di
30 Ethylene Glycol Mono Butyl Ether and Di Propylene Glycol, it does not suffer from the disadvantage of catalytically driven degradation of the active ingredient even on storage, and therefore, it has been found to have unexpectedly better efficacy and shelf life of the active ingredient and surprisingly improved activity/efficacy and stability of active ingredient meaning thereby the presently disclosed formulation
35 has been found to have shelf life of one and half year or more and hence being useful for desired purpose as insecticides, etc. for a longer duration. Furthermore,
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the materials costs are reduced compared to conventionally available Monocrotophos formulations.
It has been further observed that ammonium sulphate with or without one or more stabilizers in the Monocrotophos formulation of the present invention wherein
5 Monocrotophos is preferably taken in absorbed form on silica and formulated with ammonium sulphate with or without one or more stabilizers enhances water soluble matter of the formulation.
The enhanced water soluble matter in the presently disclosed formulation has been observed to overcome problem of chocking of spray nozzles thereby the presently
10 disclosed formulation is expected to be more acceptable for use as spray formulation, and hence can be easily applied on plants after dilution in water in a spray tank.
The presently disclosed formulation in water soluble powder form or in water soluble granular form has better solubility in water. However, after dissolution in
15 water, the spray solution form of the formulation may contain certain amount of insoluble silica, which is employed as absorbent, as insoluble matter/sediments. However, it has been observed that the advantages of silica as absorbent overcome disadvantage of it being in insoluble form, therefore, the insoluble nature of silica does not pose serious problem within its selected range as described herein.
20 Further, as described herein, the presently selected surfactant, preferably Tysperse DN has been found to be strong suspending agent and capable of keeping water insoluble matter [silica] in suspension form causing less sediment on dissolution in water thereby has been surprisingly found to avoid chocking problem of spray nozzles when presently disclosed formulation is used as spray formulation.
25 If the additional active ingredients are insoluble or less soluble in water, then presently disclosed formulation is made available as chemically stable water dispersible powder or as chemically stable water dispersible granules. The presently disclosed Monocrotophos formulation has been observed to have more than about 50% water soluble matter, that is more than about 50% solubility.
30 The addition of additional active ingredients has been observed to result in lowering of solubility of Monocrotophos.
It has also been surprisingly observed that when Monocrotophos in absorbed form on silica is formulated with ammonium sulphate with or without one or more stabilizers, ammonium sulphate also acts as carrier, filler and base material,
35 thereby in accordance with the present invention no additional carrier, filler and base material is required to be mixed with the formulation meaning thereby making
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the presently disclosed formulation more economical and more easy to be formulated by avoiding use of undesired carriers, base materials, fillers etc. It has also been observed that use of fillers, carriers and base materials in a formulation may also reduce solubility of the formulation, therefore, it can be said
5 that absence of fillers, carriers and base materials in the present formulations helps in increase in solubility of the present formulation.
The solid form of chemically stable water soluble powder, or chemically stable water dispersible powder, or chemically stable water soluble granules, or chemically stable water dispersible granules of the presently disclosed Monocrotophos
10 formulation have been found to have additional advantages of ease of packaging, storing and transportation even without major loss of activity and stability of the active ingredient over a desired period of time varying upto one and half year or more. The presently disclosed solid form Monocrotophos formulation which can be made
15 available as chemically stable water soluble powder, or chemically stable water dispersible powder, or chemically stable water soluble granules, or chemically stable water dispersible granules has been found to have advantage of being capable of dissolved or dispersed in water and sprayed thereby it has been found to have advantage of overcoming disadvantages of water insolubility and chocking
20 during spraying.
In accordance with the present invention, the Monocrotophos formulation can be made available with desired activity of the active ingredient. For example, Monocrotophos formulation can be made available with the activity varying from about 5% to about 50% of the active ingredient, preferably with the activity varying
25 from about 15% to about 40% of the active ingredient, more preferably with the activity varying from about 20% to about 35% of the active ingredient. In accordance with one embodiment of the present invention, the Monocrotophos formulation comprises at least about 5%, preferably from about 5% to about 90% of ammonium sulphate of the total formulation.
30 In accordance with another embodiment of the present invention, the Monocrotophos formulation comprises from about 10% to about 40% of ammonium sulphate of the total formulation.
In accordance with preferred embodiment of the present invention, the Monocrotophos formulation comprises from about 20% to about 35% of ammonium
35 sulphate of the total formulation.
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In accordance with another preferred embodiment of the present invention, the Monocrotophos formulation comprises about 30% of ammonium sulphate of the total formulation.
In accordance with another embodiment of the present invention, the
5 Monocrotophos formulation comprises at least about 5% to about 15% of stabilizer which is preferably selected from a group comprising Methyl Para hydroxy Benzoate or Di Ethylene Glycol Mono Butyl Ether or Di Propylene Glycol or combination thereof. In accordance with the present invention, the Monocrotophos formulation
10 comprises at least about 5% of Monocrotophos of the desired activity and at least about 5% of ammonium sulphate and the balance being absorbent while taking care that the amount of silica is restricted upto about 50% of the total formulation. The percent amount referred is with reference to amount of the total-formulation. In accordance with one embodiment of the present invention, the Monocrotophos
15 formulation comprises Monocrotophos of the desired activity in an amount varying from about 5% to about 70% of the total formulation and ammonium sulphate in an amount varying from about 5% to about 90% of the total formulation and the balance being absorbent while taking care that the amount of silica is restricted upto about 50% of the total formulation.
20 In accordance with one embodiment of the present invention, the Monocrotophos formulation comprises Monocrotophos of the desired activity in an amount varying from about 5% to about 70% of the total formulation and ammonium sulphate in an amount varying from about 10% to about 40% of the total formulation and the balance being absorbent while taking care that the amount of silica is restricted
25 upto about 50% of the total formulation.
In accordance with one embodiment of the present invention, the Monocrotophos formulation comprises Monocrotophos of the desired activity in an amount varying from about 5% to about 50% of the total formulation and ammonium sulphate in an amount varying from about 20% to about 35% of the total formulation and the
30 balance being absorbent while taking care that the amount of silica is restricted upto about 50% of the total formulation.
In accordance with one embodiment of the present invention, the Monocrotophos formulation comprises Monocrotophos of the desired activity in an amount varying from about 5% to about 50% of the total formulation and ammonium sulphate in
35 an amount of about 30% of the total formulation and the balance being absorbent
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while taking care that the amount of silica is restricted upto about 50% of the total formulation.
In accordance with one of the preferred embodiments of the present invention, the Monocrotophos formulation may additionally comprise one or more auxiliaries
5 selected from the group comprising surfactants, binding agents, coating agents, or mixtures thereof in an amount so that the total amount of these auxiliaries does not exceed more than about 10% of the total formulation.
In accordance with ,another preferred embodiment of the present invention, the Monocrotophos formulation may additionally comprise one or more additional
10 active ingredient selected from the group comprising fungicide, insecticide, any other such substance or mixture thereof in any amount, preferably in an amount so that the total amount of these additional active ingredients varies upto about 10% of the total formulation so that the desired activity of the Monocrotophos is not suppressed.
15 In one embodiment, the present invention relates to a process for preparation of chemically stable Monocrotophos formulation comprising absorbing weighed quantity of liquid Monocrotophos on weight quantity of absorbent to result in formation of powder of Monocrotophos followed by mixing the powder of Monocrotophos with weighed quantity of ammonium sulphate form Monocrotophos
20 formulation which can be made available as chemically stable water soluble powder or chemically stable water dispersible powder.
In another embodiment, the present invention relates to a process for preparation of chemically stable Monocrotophos formulation comprising absorbing weighed quantity of liquid Monocrotophos on weight quantity of absorbent to result in
25 formation of powder of Monocrotophos followed by mixing the powder of Monocrotophos with weighed quantity of ammonium sulphate to form Monocrotophos formulation which is then mixed with water to result in dough which is extruded through an extruder. On drying the extrudates in a fluid bed drier, the present formulation can be made available as chemically stable water
30 soluble granules or chemically stable water dispersible granules.
It may be noted that the present formulation is made available as chemically stable water dispersible powder or as chemically stable water dispersible granules when the additional active ingredient is either insoluble or less soluble in water. The homogeneous mixing of the ingredients while blending results in formation of
35 homogeneous, chemically stable, water soluble powder or homogeneous, chemically stable, water dispersible powder form of the formulation. The mixing while
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granulating results in formation of chemically stable, water soluble granules or water dispersible granules.
In accordance with preferred embodiment of the present invention, one or more of auxiliaries and/or additional active ingredients may also be mixed in the
5 Monocrotophos formulation while formulating powder or granules of Monocrotophos with ammonium sulphate of the present invention. The term granules, as employed herein, is intended to include solid pellets, granules, grains and the like. In accordance with present invention, the term granules, as employed herein, is intended to include a granule wherein
10 Monocrotophos forms core of the granule and the ammonium sulphate forms a coating over the core of the granule, and a granule wherein ammonium sulphate forms core of the granule and Monocrotophos forms a coating over the core of the granule, and a granule wherein no such discrete core or coating is formed, that is, the granule having a substantially uniform composition.
15 The granules may have any particle size, preferably may have particle size varying from about 0.1mm or more, more preferably from about 0.1mm to about 2.0mm diameter.
The term chemically stable, as employed herein, means that the activity of the active ingredient does not fall more than 10%, preferably more than 7% of the
20 originally selected activity of the active ingredient, and such drop in activity of the active ingredient is calculated after about one year at ambient storage. The active ingredient referred herein is Monocrotophos and the additional active ingredient referred herein is selected from the group comprising fungicide, insecticide, any other such substance or mixture thereof.
25 It has been observed that drop in activity of the active ingredient of the formulation in accordance with present invention is well within the limits for shelf life of one and half year or more. It has been found to have less than 4% drop in activity of the active ingredient over a period of one and half year or more. In one embodiment, the activity of the active ingredient is checked for testing purpose by Bureau of
30 Indian standards - IS specification no. 8025 : 1990.
It may be noted that the scope of the present invention is not restricted by the manner of mixing ammonium sulphate, other auxiliaries and additional active ingredients, which may be mixed in. any manner. The present invention is now described with the help of following examples, which
35 are illustrated in following tables wherein compositions of various formulations prepared in accordance with present invention have been disclosed.
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Table no. 1 illustrates nine formulations prepared in accordance with present invention using ammonium sulphate and initial activity of Monocrotophos is increased from left to right side of the table. The tenth formula-J illustrates a standard formulation prepared without ammonium sulphate.
5 Each formulation was analyzed for drop in activity of active ingredient -Monocrotophos [MCP] after one and half year ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than 4% of the originally selected activity of the active ingredient. However, the standard
10 formulation-J prepared without incorporating ammonium sulphate of the present invention was 13% after one and half year ambient storage.
Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 100% water soluble matter. However, the standard formulation - J shows about
15 68.49% of water soluble matter.
Table no. : 1
Stability of different concentrations of MCP AI with ammonium sulphate

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula ' I Formula J
Monocrotophos AI in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50% 50%
Monocrotophos tech (73% AI) 6.85% 13.70% 20.54% 27.40% 34.25% 41.10% 47.95% 54.79% 68.49% 68.49%
Ammonium sulphate 93.15% 86.30% 79.46% 72.60% 65.75% 58.90% 52.05% 45.21% 31.51% ...
Ppt Silica (Sypernat 22 S) ... ... ... ... ... ... ... ... "- 31.51%
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophos AI after one and half year ambient storage 0.40% 0.85% 1.20% 1.50% 1.95% 2.50% 2.80% 3.20% 3.90% 13.0%
Water soluble matter 100% 100% 100% 100% 100% 100% 100% 100% 100% 68.49%
Table no. 2 illustrates eight formulations prepared in accordance with present
20 invention using ammonium sulphate and initial activity of Monocrotophos is
increased from left to right side of the table. The ninth formula-I illustrates a
standard formulation prepared without ammonium sulphate.
Each formulation was analyzed for drop in activity of active ingredient -
Monocrotophos [MCP] after one and half year ambient storage. It was observed that
25 the drop in activity of Monocrotophos of all formulations prepared in accordance
with present invention was well within the preferred value, that is, was less than
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4% of the originally selected activity of the active ingredient. However, the standard formulation prepared without incorporating ammonium sulphate of the present invention was 13% after one and half year ambient storage.
Each formulation was also analyzed for water soluble matter and it was observed
5 that all most all formulations, except formulation-H prepared in accordance with present invention shows about 75 to 95% water soluble matter. However, the standard formulation - I shows about 70.49% of water soluble matter.
Table no. : 2
Stability of different concentrations of MCP Al with ammonium sulphate

Name of the Weight percentage
ingredient Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I
Monocrotophos AI in formulation. 5% 10% 15% 20% 25% 30% 35% 40% 50%
Monocrotophos tech (73% AI) 6.85% 13.70% 20.54% 27.40% 34.25% 41.10% 47.95% 54.79% 68.49%
Ppt Silica (Sypernat 22 S) 5% 10% 15% 20% 22% 25% 25% 30% 29.51%
Ammonium sulphate 86.15% 74.30% 62.46% 50.60% 41.75% 31.90% 25.05% 13.21% ...
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2%
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophos AI after 1 'A yr ambient storage 0.60% 0.95% 1.50% 1.95% 2.50% 2.90% 3.30% 3.80% 13.0%
Water soluble matter 95.0% 90.0% 85.0% 80.0% 78.0% J5.0% 75.0% 70.00% 70.49%
10
Table no. 3 illustrates nine formulations prepared in accordance with present invention using ammonium sulphate and initial activity/of Monocrotophos is kept constant. The tenth formula-J illustrates a standard formulation prepared without ammonium sulphate.
15 Each formulation was analyzed for drop in activity of active ingredient -Monocrotophos [MCP] after one and half year ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance with present invention was well within the desired value, that is, was less than about 10.0% of the originally selected activity of the active ingredient. However, the
20 standard formulation prepared without incorporating Ammonium sulphate of the present invention was much higher that is 14.0% after one and half year ambient storage.
Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about
25 40 to 81% water soluble matter. However, the standard formulation - J shows about 36.25% of water soluble matter.
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The formulations disclosed in Table 3 confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show better stability even after one and half year of storage and very high water soluble matter.

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Table no. : 3

Stability of MCP 25% Al with different concentrations of Ammonium sulphate

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I Formula J
Monocrotophos AI in formulation 25% 25% 25% 25% 25% 25% 25%i 25% 25% 25%
Monocrotophos tech (73% Al) 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25%
Ppt Silica (Sypernat 22 S) 58.75% 53.75% 48.75% 43.75% 38.75% 33.75% 28.75% 22.00% 18.75% 63.75%
Ammonium sulphate 5% 10% 15% 20% 25% 30% 35% 41.75% 45.0% -
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2% 2%
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophos AI after l'/2 yr. Ambient storage 10.0% 8.9% 7.0% 6.1% 5.1% 4.2% 3.5% 2.5% 2.3% 14.0%
Water soluble matter 41.25% 46.25% 51.25% 56.25% 61.25% 66.25% 71.25% 78.0% 81.25% 36.25%
Table no. 4 illustrates eight formulations prepared in accordance with present
10 invention wherein the initial activity of Monocrotophos is increased from left to right. The ninth formulation-I illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 4 also comprise one or more of fungicides described hereinabove. Each formulation was analyzed for drop in activity of active ingredient - Monocrotophos [MCP] after one and half year
15 ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than 4% of the originally selected activity of the active ingredient. However, the standard formulation prepared without incorporating ammonium sulphate of the present invention was 13% after one and
20 half year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 38 to 70% water soluble matter. The formulations disclosed in Table 4 also confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show better
25 stability even after one and half year of storage and very high water soluble matter. The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is, fungicide.
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Table no.: 4
Stability of different cone, of MCP Al + different cone, of Fungicides Al with Ammonium sulphate

Name of ' V/eight percentage
The ingredient Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I
Monocrotophos Al in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50%
Monocrotophos Tech (73% Al) 6.85% 13.70% 20.54% 27.40% 34.25% 41.10% 47.95% 54.79% 68.49%
Ppt Silica (Sypernat 22 S) 5% 10% 15% 20% 22% 25% 25% 30% 29.51%
Ammonium sulphate 44.05% 37.46% 30.88% 24.28% 20.70% 16.12% 14.53% 7.95% -
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2%
Fungicide 42.10% 36.84% 31.58% 26.32% 21.05% 15.78% 10.52% 5.26% -
Total % 100% 100% / 100% 100% 100% 100% 100% 100% 100%
Drop in Monocrotophos Al after one and half year ambient storage 0.7% 1.10% 1.7% 2.2% 2.7% 3.0% 3.5% 4.0% 13.0%
Water soluble matter 52.90% 53.16% 53.42% 53.68% 56.95% 59.22% 64.48% 64.74% 70.49%
5 In accordance with one embodiment, the fungicide may be selected from a group comprising Carbendazim, Hexaconazole, Mancozeb, Thiram, Captafol, Captan, Maneb, Propiconazole, Tricyclazole, Tebuconazole, Chlorothalonil, Zineb, Ziram, Methyl Thiophanate or combination thereof.
Table no. 5 illustrates eight formulations prepared in accordance with present
10 invention wherein the initial activity of Monocrotophos is increased from left to right. The ninth formulation-I illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 5 also comprise one or more of additional active ingredient - insecticides described here in above. Each formulation was analyzed for drop in activity of active ingredient - Monocrotophos
15 [MCP] after one and half year ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than about 4% of the originally selected activity of the active ingredient. However, the standard formulation prepared without incorporating Ammonium sulphate of the present
20 invention was 13% after one and half year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 51 to 65% water soluble matter. The formulations disclosed in Table 5 also confirm that Monocrotophos formulations comprising ammonium sulphate within preferred
25 range, that is 10% or more show better stability even after one and half year of storage and very high water soluble matter. The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is, insecticide.
16

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Table no.: 5
Stability of different conc. Of MCP Al + different conc. Of Insecticides Al with Ammonium sulphate

Name of Weight percentage
the ingredient Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I
Monocrotophos AI in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50%
Monocrotophos tech (73% AI) 6.85% 13.70% 20.54% 27.40% 34.25% 41.10% 47.95% 54.79% 68.49%
Ppt Silica (Sypernat 22 S) 5% 10% 15% 20% 22% 25% 25% 30% 29.51%
Ammonium sulphate 42.68% 36.26% 29.86% 23.43% 20.01% 15.61% 14.18% 7.78%
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2%
Insecticide 43.47% 38.04% 32.60% 27.17% .21.74% 16.29% 10.87% 5.43% -
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop in Monocrotophos AI after one and half year ambient storage 0.6% 1.0% 1.6% 2.1% 2.6% 3.0% 3.4% 3.9% 13.0%
Water soluble matter 51:53% 51.96% 52.40% 52.83% 56.26% 58.71% 64.13% 64.57% 70.49%
In accordance with one embodiment, the insecticide may be selected from a group
5 comprising Chlorpyriphos, Quinalphos, Acephate, Dichlovos, Dimethyl, Phenthoate, Malathion, Ethion, Fenvalerate, Cypermethrin, Permethrin, Cyhalothrin, Deltamethrin, Cycloprothrin or combination thereof. Table no. 6 illustrates eight formulations prepared in accordance with present invention wherein initial activity of Monocrotophos is increased from left to right.
10 The ninth formulation-I illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 6 also comprise one or more of additional active ingredient - insecticides and auxiliaries - binding agent and coating agent described hereinabove. Each formulation was analyzed for drop in activity of active ingredient - Monocrotophos [MCP] after one and half year
15 ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance with present invention was well within the preferred value, that is, was less than about 4% of the originally selected activity of the active ingredient.. However, the standard formulation prepared without incorporating ammonium sulphate of the present invention was 13% after one and
20 half year ambient storage. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 51 to 65% water soluble matter. The formulations disclosed in Table 6 also confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show better
25 stability even after one and half year of storage and very high water soluble matter.
17

MCP2
The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is, insecticide.
Table no.: 6

5

Stability of different cone, of MCP AI + different cone, of insecticides AI with Ammonium sulphate and binding agent / coating agent

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I
Monocrotophos AI in formulation 5% 10% 15% 20% 25% 30% 35% 40% 50%
Monocrotophos Tech (73% AI) 6.85% 13.70% 20.54% 27.40% 34.25% 41.10% 47.95% 54.79% 68.49%
Ppt Silica (Sypernat 22 S) 5% 10% 15% 20% - 22% 25% 25% 30% 28.51%
Ammonium sulphate 41.68% 35.26% 28.86% 22.43% 19.01% 14.61% 13.18% 6.78% -
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2%
Binding Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5%
Coating Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5%
Insecticide 43.47% 38.04% 32.60% 27.17% 21.74% 16.29% 10.87% 5.43% -
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophosAI afterOne and half yearAmbient storage 0.7 % 0.9% 1.5% 2.2% 2.6% 3.1% 3.5% 3.9% 13.0%
Water soluble matter 51.53% 51.96% 52.4% 52.83% 56.26% 58.71% 64.13% 64.57% 71.49%
in accordance with one embodiment, the binding agent may be selected from a group comprising Poly Vinyl Alcohol, Poly Vinyl Pyrrolidone, Poly Vinyl Pyrrolidone
10 Co- polymer, Polyacrylic Acid, Carbo Methoxy Cellulose, Casein, Gelatin, Acacia, Synthetic Glue, Xanthan gum, Guar Gum, Gum Arabic, Lignin or combination thereof.
In accordance with one embodiment, the coating agent may be selected from a group comprising Starch, Cellulose Derivatives, Methyl Cellulose, Hydroxy propyl
15 methyl cellulose, Alginates or combination thereof.
In accordance with one embodiment, the insecticide may be selected from a group comprising Chlorpyriphos, Quinalphos, Acephate, Dichlovos, Dimethyl, Phenthoate, Malathion, Ethion, Fenvalerate, Cypermethrin, Permethrin, Cyhalothrin, Deltamethrin, Cycloprothrin or combination thereof.
20 Table ho. 7 illustrates eight formulations prepared in accordance with present invention wherein initial activity of Monocrotophos is increased from left to right. The ninth formulation-I illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 7 also comprise one or more of additional active ingredient - fungicides and auxiliaries - binding agent and
25 coating agent described hereinabove.
Each formulation was analyzed for drop in activity of active ingredient -Monocrotophos [MCP] after one and half year ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance
18

MCP2
with present invention was well within the preferred value, that is, was less than about 4.1% of the originally selected activity of the active ingredient. However, the standard formulation prepared without incorporating ammonium sulphate of the present invention was 13% after one year ambient storage. Each formulation was
5 also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows about 52 to 65% water soluble matter. The formulations disclosed in Table 7 also confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show better stability even after one and half year of
10 storage and very high water soluble matter. The drop in water soluble matter in formulations A-D is observed due to higher concentration of additional active ingredient, that is. fungicide.
Table no.: 7
Stability of different cone, of MCP AI + different cone, of fungicide AI with Ammonium sulphate

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formula E . FormulaF Formula G Formula H Formula 1
Monocrotophos AI in formulation 5% 10% .15% 20% 25% 30% 35% 40% 50%
Monocrotophos Tech (73% AI) 6.85% 13.70% 20.54% 27.40% 34.25% 41.10% 47.95% 54.79% 68.49%
Ppt Silica (Sypernat 22 S) 5% 10% 15% 20% 22% 25% 25% 30% 28.51%
Ammonium sulphate 43.05% 36.46% 29.88% 23.28% 19.70% 15.12% 13.53% 6.95 -
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2%
Binding Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5%
Coating Agent 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5% 0.5%
Fungicide 42.1% 36.84% 31.58% 26.32% 21.05% 15.78% 10.52% 5.26% -
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophosAI afterone and half Yearambient Storage 0.60% 1.00% 1.55% 2.3% 2.65% 3.20% 3.45% 4.10% 13.0%
Water soluble matter 52.90% 53.16% 53.42% 53.68% 56.95% 59.22% 64.48% 64.74% 71.49%
in accordance with one embodiment, the Fungicides may be selected from a group comprising Carbendazim, Hexaconazole, Mancozeb, Thiram, Captafol, Captan, Maneb, Propiconazole, Tricyclazole, Tebuconazole, Chlorothalonil, Zineb, Ziram,
20 Methyl Thiophanate or combination thereof.
In accordance with one embodiment, the binding agent may be selected from a group comprising Poly Vinyl Alcohol, Poly Vinyl Pyrrolidone, Poly Vinyl Pyrrolidone Co- polymer, Polyacrylic Acid, Carbo Methoxy Cellulose, Casein, Gelatin, Acacia, Synthetic Glue, Xanthan gum, Guar Gum, Gum Arabic, Lignin or combination
25 thereof.
19

MCP2
In accordance with one embodiment, the Coating agent may be selected from a group comprising Starch, Cellulose Derivatives, Methyl Cellulose, Hydroxy propyl methyl cellulose, Alginates or combination thereof.
Table no. 8 illustrates nine formulations prepared in accordance with present
5 invention using ammonium sulphate and initial activity of Monocrotophos is kept constant. The tenth formula-J illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 8 also comprise different concentrations of binding agents described here in above. Each formulation was analyzed for drop in activity of active ingredient -
10 Monocrotophos [MCP] after one and half year ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance with present invention was well within the desired value, that is, was less than about 2.6% of the originally selected activity of the active ingredient. Each formulation was also analyzed for water soluble matter and it was observed
15 that each formulation prepared in accordance with present invention shows 78% water soluble matter. However, the standard formulation - J shows about 36.25% of water soluble matter.
The formulations disclosed in Table 8 confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show
20 better stability even after one and half year of storage and very high water soluble matter. However, the standard formulation prepared without incorporating ammonium sulphate of the present invention was 14.0% after one and half year ambient storage.
Table no.: 8
25 Stability of MCP 25% Al with Ammonium sulphate and different concerntration of binding agent.

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D FormulaE Formula F Formula G Formula H Formula I Formula J
Monocrotophos Al in formulation 25% 25% 25% 25% 25% 25% 25% 25% 25% 25%
Monocrotophos tech (73% Al) 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25%
Ppt Silica ' (Sypernat 22 S) 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 63.75%
Ammonium sulphate 41.70% 41.65% 41.50% 41.25% 40.75% 39.75% 38.75% 37.75% 36.75% ...
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2% 2%
Binding Agent . 0.05% 0.1% 0.25% 0.5% 1.0% 2.0% 3.0% 4.0% 5.0% ...
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophosAl after one and halfyearAmbient storage 2.40% 2.60% 2.50% 2.55% 2.40% 2.60% 2.50% 2.45% 2.60% 14.00%
Water soluble matter 78.00% 78.00% 78.00% 78.00% 78.00% 78.00% 78.00% 78.00% 78.00% 36.25%
20

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The binding agents in these formulations are same as stated for formulations described in table 6.
Table no. 9 illustrates ten formulations prepared in accordance with present invention using ammonium sulphate and initial activity of Monocrotophos is kept
5 constant. The tenth formula-J illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 9 also comprise , different concentrations of coating agents described here in above. Each formulation was analyzed for drop in activity of active ingredient -Monocrotophos [MCP] after one and half year ambient storage. It was observed that
10 the drop in activity of Monocrotophos of all formulations prepared in accordance with present invention was well within the desired value, that is, was less than about 2.6% of the originally selected activity of the active ingredient. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows 78%
15 water soluble matter. However, the standard formulation - J shows about 36.25% of water soluble matter.
The formulations disclosed in Table 9 confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show better stability even after one and half year of storage and very high water, soluble
20 matter. However, the standard formulation prepared without incorporating ammonium sulphate of the present invention was 14.0% after one and half year ambient storage.
Table no.: 9
25 Stability of MCP 25% Al with Ammonium sulphate and different concerntration of coating agent.

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I Formula J
Monocrotophos Al in formulation 25% 25% 25% 25% 25% 25% 25% 25% 25% 25%
Monocrotophos tech (73% Al) 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25%
Ppt Silica (Sypernat 22 S) 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 63.75%
Ammonium sulphate 41.70% 41.65% 41.50% 41.25% 40.75% 39.75% 38.75% 37.75% 36.75% ...
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2% 2%
Coating Agent 0.05% 0.1% 0.25% 0.5% 1.0% 2.0% 3.0% 4.0% 5.0% ...
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophosAl after one and halfyearAmbient storage 2.50% 2.40% 2.45% 2.50% 2.45% 2.50% 2.60% 2.45% 2.55% 14.00%
Water soluble matter 78.00% 78.00% 78.00% 78.00% 78.00% 78.00% 78.00% 78.00% 78.00% 36.25%
The coating agents for these formulations are same as for formulations described in table 6.
21

MCP2
Table no. 10 illustrates nine formulations prepared in accordance with present invention using Ammonium sulphate and initial activity of Monocrotophos is kept constant. The tenth formula-J illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 10 also comprise
5 different concentrations of stabilizer- Methyl Para Hydroxy Benzoate described here in above.
Each formulation was analyzed for drop in activity of active ingredient -Monocrotophos [MCP] after one and half year ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance
10 with present invention was well within the desired value, that is, was less than 2.5% of the originally selected activity of the active ingredient. Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows 63% to 78% water soluble matter. However, the standard formulation - J shows about
15 36.25% of water soluble matter.
The formulations disclosed in Table 10 confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show better stability even after one and half year of storage and very high water soluble matter. However, the standard formulation prepared without incorporating
20 ammonium sulphate of the present invention was 14.0% after one and half year ambient storage.
Table No. : 10
Stability of MCP 25% Al with Ammonium sulphate and different concerntration of stabilizer -:Methyl Paraben.

Name of the Weight percentage
ingredient Formula A Formula B Formula C Formula D FormulaIE Formula F Formula G Formula H Formula I Formula J
Monocrotophos AI in formulation 25% 25% 25% 25% 25% 25% 25% 25% 25% 25%
Monocrotophos tech (73% AI) 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25%
Ppt Silica (Sypernat 22 S) 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 63.75%
Ammonium sulphate 41.75% 40.75% 38.75% 35.75% 33.75% 31.75% 29.75% 27.75% 26.75% ._
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2% 2%
Methyl Paraben *** (Stabilizer) — 1% 3% 6% 8% 10% 12% 14% 15% —
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophosAI after one and halfyearAmbient storage 2.50% 2.40% 2.35% 2.30% 2.15% 2.07% 2.10% 2.20% 2.15% 14.00%
Water soluble matter 78% 77% 75% 72% 70% 68% 67% 64% 63% 36.25%
25
*** Methyl Paraben = Methyl Para - hydroxy benzoate
22

MCP2
Table no. 11 illustrates nine formulations prepared in accordance with present invention using ammonium sulphate and initial activity of Monocrotophos is kept constant. The tenth formula-J illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 11 also comprise
5 different concentrations of stabilizer- Di Ethylene Glycol Mono Butyl Ether ( Butyl Carbitol) described here in above.
Each formulation was analyzed for drop in activity of active ingredient -Monocrotophos [MCP] after one and half year ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance
10 with present invention was well within the desired value, that is, was less than 2.5% of the originally selected activity of the active ingredient.
Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows 78% water soluble matter. However, the standard formulation - J shows about 36.25%
15 of water soluble matter.
The formulations disclosed in Table 11 confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show better stability even after one and half year of storage and very high water soluble matter. However, the standard formulation prepared without incorporating
20 ammonium sulphate of the present invention was 14.0% after one and half year ambient storage.
Table No. : 11
Stability of MCP 25% Al with Ammonium sulphate and different concerntration of stabilizer -:Butyl carbitol.

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I Formula J
Monocrotophos Al in formulation 25% 25% 25% 25% 25% 25% 25% 25% 25% 25%
Monocrotophos tech (73% Al) 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25%
Ppt Silica (Sypernat 22 S) 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 63.75%
Ammonium sulphate 41.75% 40.75% 38.75% 35.75% 33.75% 31.75% 29.75% 27.75% 26.75% ...
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2% 2%
Butyl Carbitol *** (Stabilizer) — 1% 3% 6% 8% 10% 12% 14% 15% ...
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophosAl after one and halfyearAmbient storage 2.50% 2.40% 2.45% 2.30% 2.25% 2.17% 2.20% 2.30% 2.35% 14.00%
Water soluble matter 78% 78% 78% 78% 78% 78% 78% 78% 78% 36.25%
*** Butyl Carbitol = Diethylene glycol mono butyl ether
23

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Table no. 12 illustrates nine formulations prepared in accordance with present invention using ammonium sulphate and initial activity of Monocrotophos is kept constant. The tenth formula-J illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 12 also comprise
5 different concentrations of stabilizer- Di Propylene Glycol described here in above. Each formulation was analyzed for drop in activity of active ingredient -Monocrotophos [MCP] after one and half year ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance with present invention was well within the desired value, that is, was less than
10 2.5% of the originally selected activity of the active ingredient.
Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows 78% water soluble matter. However, the standard formulation - J shows about 36.25% of water soluble matter.
15 The formulations disclosed in Table 12 confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show better stability even after one and half year of storage and very high water soluble matter. However, the standard formulation prepared without incorporating ammonium sulphate of the present invention was 14.0% after one and half year
20 ambient storage.
Table No. : 12
Stability of MCP 25% Al with Ammonium sulphate and different concerntration of stabilizer -:Dipropylene Glycol.

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I Formula J
Monocrotophos Al in formulation 25% 25% 25% 25% 25% 25% 25% 25% 25% 25%
Monocrotophos tech (73% Al) 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25% 34.25%
Ppt Silica (Sypernat 22 S) 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 22.00% 63.75%
Ammonium sulphate 41.75% 40.75% 38.75% 35.75% 33.75% 31.75% 29.75% 27.75% 26.75% ...
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2% 2%
Dipropylene Glycol (Stabilizer) — 1% 3% 6% 8% 10% 12% 14% 15% ...
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophosAl after one and halfyearAmbient storage 2.50% 2.45% 2.45% 2.45% 2.40% 2.39% 2.40% 2.45% 2.45% 14.00%
Water soluble matter 78% 78% 78% 78% 78% 78% 78% 78% 78% 36.25%
25 Table no. 13 illustrates eleven formulations prepared in accordance with present invention using ammonium sulphate and initial activity of Monocrotophos is varied from 10% to 40%. The twelfth formula-L illustrates a standard formulation
24

MCP2
prepared without ammonium sulphate. The formulations illustrated in Table 13
also comprise different concentrations of stabilizer- Methyl Para Hydroxy Benzoate
(Methyl Paraben ) described here in above.
Each formulation was analyzed for drop in activity of active ingredient -
5 Monocrotophos [MCP] after one and half year ambient storage. It was observed that
•the drop in activity of Monocrotophos of all formulations prepared in accordance
with present invention was well within the desired value, that is, was less than 4%
of the originally selected activity of the active ingredient.
Each formulation was also analyzed for water soluble matter and it was observed
10 that each formulation prepared in accordance with present invention shows 60% to
89% water soluble matter. However, the standard formulation - J shows about
36.25% of water soluble matter.
The formulations disclosed in Table 13 confirm that Monocrotophos formulations
comprising ammonium sulphate within preferred range, that is 10% or more show
15 better stability even after one and half year of storage and very high water soluble
matter. However, the standard formulation prepared without incorporating
ammonium sulphate of the present invention was 14.0% after one and half year
ambient storage.
Table No.: 13
20 Stability of different conc.of MCP AI with different concerntration of stabilizer -: Methyl Paraben.

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I Formula J Formula K Formula L
MonocrotophosAl informulation 10% 10% 10% 10% 25% 25% 25% 25% 40% 40% 40% 25%
Monocrotophos tech (73% AI) 13.70% 13.70% 13.70% 13.70% 34.25% 34.25% 34.25% 34.25% 54.79% 54.79% 54.79% 34.25%
Ppt Silica (Sypemat 22 S) 10% 10% 10% 10% 22% 22% 22% 22% 30% 30% 30% 63.75%
Ammonium sulphate 73.30% 69.30% 64.30% 59.30% 40.75% 36.75% 31.75% 26.75% 12.21% 8.21% 3.21% ...
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2% 2% 2% 2%
Methyl Paraben *** (Stabilizer) 1.0% 5.0% 10.0% 15.0% 1.0% 5.0% 10.0% 15.0% 1.0% 5.0% 10.0% ...
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophos AI after one and half year Ambient storage 0.90% 0.85% 0.80% 0.85% 2.40% 2.30% 2.07% 2.35% 3.60% 3.90% 4.0% 14.00%
Water soluble matter 89% 85% 80% 75% 77% 73% 68% 63% 69% 65% 60% 36.25%
*** Methyl Paraben = Methyl Para - hydroxy benzoate
25
25

MCP2
Table no. 14 illustrates eleven formulations prepared in accordance with present invention using ammonium sulphate and initial activity of Monocrotophos is varied from 10% to 40%. The twelfth formula-L illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 14
5 also comprise different concentrations of stabilizer- Di Ethylene Glycol Mono Butyl Ether ( Butyl Carbitol) described here in above.
Each formulation was analyzed for drop in activity of active ingredient -Monocrotophos [MCP] after one and half year ambient storage. It was observed that/ the drop in activity of Monocrotophos of all formulations prepared in accordance
10 with present invention was well within the desired value, that is, was less than 4% of the originally selected activity of the active ingredient.
Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows 70% to 90% water soluble matter. However, the standard formulation - J shows about
15 36.25% of water soluble matter.
The formulations disclosed in Table 14 confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show better stability even after one and half year of storage and very. high water soluble matter. However, the standard formulation prepared without incorporating
20 ammonium sulphate of the present invention was 14.0% after one and half year ambient storage.
Table No.: 14
Stability of different conc.of MCP AI with different concerntration of stabilizer-: Butvl Carbitol.
Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I Formula J Formula K Formula L
MonocrotophosAl informulation 10% 10% 10% 10% 25% 25% 25% 25% 40% 40% 40% 25%
Monocrotophos Tech (73% AI) 13.70% 13.70% 13.70% 13.70% 34.25% 34.25% 34.25% 34.25% 54.79% 54.79% 54.79% 34.25%
Ppt Silica (Sypernat 22 S) 10% 10% 10% 10% 22% 22% 22% 22% 30% 30% 30% 63.75%
Ammonium sulphate 73.30% 69.30% 64.30% 59.30% 40.75% 36.75% 31.75% 26.75% 12.21% 8.21% 3.21% —
TysperseDN 2% 2% 2% 2% 2% 2% 2% 2% 2% 2% 2% 2%
Butyl Carbitol *** (stabilizer) 1.0% 5.0% 10.0% 15.0% 1.0% 5.0% 10.0% 15.0% 1.0% 5.0% 10.0% —
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophos AI after one and half year Ambient storage 1.0% 0.90% 0.85% 0.80% 2.40% 2.30% 2.17% 2.25% 3.70% 4.0% 4.0% 14.00%
Water soluble matter 90% 90% 90% 90% 78% 78% 78% 78% 70% 70% 70% 36.25%
25 *** Butyl Carbitol = Diethylene glycol mono butyl ether
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MCP2
Table no. 15 illustrates eleven formulations prepared in accordance with present invention using ammonium sulphate and initial activity of Monocrotophos is varied from 10% to 40%. The twelfth formula-L illustrates a standard formulation prepared without ammonium sulphate. The formulations illustrated in Table 15
5 also comprise different concentrations of stabilizer- Di Propylene Glycol described here in above.
Each formulation was analyzed for drop in activity of active ingredient -Monocrotophos [MCP] after one and half year ambient storage. It was observed that the drop in activity of Monocrotophos of all formulations prepared in accordance
10 with present invention was well within the desired value, that is, was less than 4% of the originally selected activity of the active ingredient.
Each formulation was also analyzed for water soluble matter and it was observed that each formulation prepared in accordance with present invention shows 70% to 90% water soluble matter. However, the standard formulation - J shows about
15 36.25% of water soluble matter.
The formulations disclosed in Table 15 confirm that Monocrotophos formulations comprising ammonium sulphate within preferred range, that is 10% or more show better stability even after one and half year of storage and very high water soluble matter. However, the standard formulation prepared without incorporating
20 Ammonium sulphate of the present invention was 14.0% after one and half year ambient storage.
Table No.: 15
Stability of different conc.of MCP AI with different concerntration of stabilizer- Dipropylene Glycol.

Name of the ingredient Weight percentage
Formula A Formula B Formula C Formula D Formula E Formula F Formula G Formula H Formula I Formula J Formula K Formula L
Monocrotophos AI in formulation 10% 10% 10% 10% 25% 25% 25% 25% 40% 40% 40% 25%
Monocrotophos tech (73% AI) 13.70% 13.70% 13.70% 13.70% 34.25% 34.25% 34.25% 34.25% 54.79% 54.79% 54.79% 34.25%
Ppt Silica (Sypernat 22 S) 10% 10% 10% 10% 22% 22% 22% . 22% 30% 30% 30% 63.75%
Ammonium sulphate 73.30% 69.30% • 64.30% 59.30% 40.75% 36.75% 31.75% 26.75% 12.21% 8.21% - 3.21% —
Tysperse DN 2% 2% 2% 2% 2% 2% 2% 2% 2% 2% 2% 2%
Dipropylene Glycol ( stabilizer) 1.0% 5.0% 10.0% 15.0% 1.0% 5.0% 10.0% 15.0% 1.0% 5.0% 10.0% —
Total % 100% 100% 100% 100% 100% 100% 100% 100% 100% 100% 100% 100%
Drop inMonocrotophos AI after one and half year Ambient storage 1.0% 0.95% 0.85% 0.90% 2.45% 2.45% 2.39% 2.45% 3.80% 4.0% 4.0% 14.00%
Water soluble matter 90% 90% 90% 90% 78% 78% 78% 78% 70% 70% 70% 36.25%
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MCP2
It may be noted various modifications are possible for the formulations illustrated in the Tables provided herein without deviating from the intended scope of present invention. Therefore, in one embodiment the present invention includes all formulations which can be prepared without deviating from its scope.
5 It may be noted that the term water soluble powder or granules as employed herein means a formulation in which the active ingredient is fully dissolved in spray solution despite the fact that the spray solution may contain a certain amount of insoluble silica which is very low in the Monocrotophos formulation disclosed in the present invention and the term water dispersible powder or granules means a
10 formulation in which the active ingredient is not fully dissolved in the final spray solution, but it is dispersed.
The amounts or volumes of various ingredients described herein and in the Tables are with reference to the total weight or total volume of the formulation and are taken in a way so as to have a total of 100%. These amounts may, however, vary
15 within the permissible limits of practically allowable ranges of each ingredient of the present formulation.,
The word "about" appearing before various values is intended to include practically
permissible limits of variations in respective value.
Dated this 20th day of April, 2007.
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