Tagros Chemicals India Limited Limited-Cuddalore Integrated Management System Department: Title: Quality Control Analysis Method

of Cypermethrin Technical for Assay and Related quality parameters

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L3/SOP/QC/184 00 05.06.2008 Page 1 of 5

I. PURPOSE: The purpose of the procedure is to define the analysis method of Cypermethrin Technical for Assay and related quality parameters. II. SCOPE: This procedure is applicable for analysis method of Cypermethrin Technical for Assay and related pplicable quality parameters. III. RESPONSIBILITY: It is the responsibility of the officer / Junior officer to execute the operation and the Sr.Officer to ensure that the operations are carried out as per the procedure. IV. DOCUMENT REFRENCE: Finished Goods Product Register – Technical (FOR/QC/42) Finished Goods Worksheet – Cypermethrin Technical (FOR/QC/17). V. PROCEDURE: Wear all the personal protective equipments 1. Physical Appearance: Take 20 ml of sample in a test tube, physically check the colour and any visible foreign particles ple present or not, compare with standard colour grade sample and fix the colour grade grade. 2. 10% solution in Toluene Test: % Weigh about 10.0 gm of sample in a 100 ml cone measuring cylinder and make upto the mark .0 er with toluene (LR grade) and dissolve well. Physically check the clarity and foreign particle present or not. 3. Procedure for Assay Analysis: a) Internal Standard: Di-Octylphthlate of purity (Min Octylphthlate (Min-98.00%) b) Reference Standard Standard: Cypermethrin Technical of purity (Min – 95.00%) ermethrin c) Preparation of Internal stock solution: Weigh about 8 gm of Di Octylphthalate in a 150ml glass beaker. Dissolve the material Di-Octylphthalate completely by using Chloroform (LR grade) and transfer into 2 lits volumetric flasks. Then ) dissolve the material by using chloroform (LR grade) and make upto the mark. Dissolve the solution carefully or sonicate for 10minutes. Then allow the solution to retain and bring to room temperature.

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Tagros Chemicals India Limited Limited-Cuddalore Integrated Management System Department: Title: Quality Control Analysis Method of Cypermethrin Technical for Assay and Related quality parameters

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L3/SOP/QC/184 00 05.06.2008 Page 2 of 5

d) Standard Preparation: Weigh about 0.26gm of homogenized Cypermethrin reference standard in a separate 50ml out volumetric flask. Then dissolve the reference standard by using internal stock solution and make upto the mark. Dissolve the solution or sonicate for 10minutes. Then allow the sol solution to retain and bring to room temperature. Perform a duplicate standard solution. e) Sample Preparation: Weigh about 0.26gm of homogenized Cypermethrin sample in a separate 50ml volumetric flask. Then dissolve the sample by using internal stock solution and make upto the mark. and Dissolve the solution or sonicate for 10minutes. Then allow the solution to retain and bring to room temperature. Perform a duplicate sample solution. f) Injection sequence: Blank, Standard-1, Sample Sample-2, Standard-2, Sample-1, Sample 1, Sample-1, Sample-2. g) Instrument Condition: Instrument Detector Column Temperatures: Oven Temp Injector Temp Detector Temp Gas Flow Rates: Nitrogen Flow Hydrogen flow Zero Air flow Run Time Retention Time: Internal Standard Cypermethrin Calculation Method Calculation: Calculate the Cypermethrin content for each sample injection, the following e equation. : 2 - 3 min : 4 - 5 min : Internal Standard Method : 30 ml/min : 30 ml/min : 300 ml/min : 10 min : 260°C : 270°C : 280°C : Gas Liquid Chromatography : FID : 5% Dexil 300 ss 2 mtrs.

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Tagros Chemicals India Limited Limited-Cuddalore Integrated Management System Department: Title: Quality Control Analysis Method of Cypermethrin Technical for Assay and Related quality parameters

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L3/SOP/QC/184 00 05.06.2008 Page 3 of 5

AxBxC Relative response factor (F) = DxExG

A = Area of Cypermethrin peak from the standard solution. B = Weight of Di-Octylphthalate (IS) stock solution Octylphthalate C= Purity of Di-Octylphthalate. Octylphthalate. D = Area of Di-Octylphthalate peak of the standard solution. Octylphthalate E = Weight of Cypermethrin in standard solution. G = Purity of the Cypermethrin reference standard. HxBxC Total Cypermethrin content ( w/w) = ___________ (% IxJxF Where, H = Area of Cypermethrin peak in the sample solution. I = Area of the Di-Octylphthalate peak in the sample solution Octylphthalate B = Weight of Di-Octylphthalate (IS) stock solution. Octylphthalate J = Weight of sample. C = Purity of Di-Octylphthalate. Octylphthalate. F = Relative response factor factor.

4. Procedure for Cis-Trans Isomer Analysis: Trans a) Standard Preparation: Weigh about 100mg of Cypermethrin standard (known cis + trans isomer ratio) in a 10ml volumetric flask and make upto the mark by using Mobile Phase. Dissolve the solution or sonicate for 10minutes. Then allow the solution to retain and bring to room temperature. b) Sample Preparation: Weigh about 100mg of sample in a 10ml volumetric flask and make upto the mark by using Mobile Phase. Dissolve the solution or sonicate for 10minutes. Then allow solution to retain and bring to room temperature.

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Tagros Chemicals India Limited Limited-Cuddalore Integrated Management System Department: Title: Quality Control Analysis Method of Cypermethrin Technical for Assay and Related quality parameters

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L3/SOP/QC/184 00 05.06.2008 Page 4 of 5

c) Instrument condition condition: Instrument Column Mobile Phase Ratio Flow Detector Injection size Retention time : HPLC : Hypersil Silica 5micron (NP), 250mm x 4.6 mm ID. , : Hexane: Di-Ethyl ether : 98 :02 : 1.50 ml / min : UV 280 nm : 20µl : 7.0 – 12.0 min (CIS + Trans Isomers)

Calculation: A+B Cis Isomer = ------------------ x 100 A+B+C+D Trans Isomer = 100 - Cis Isomer First peak (A) Second peak (B) Third peak (C) Fourth peak (D) : First peak of Cis Isomer. : Second peak of Cis Isomer. : First peak of Trans Isomer. : Second peak of Trans Isomer

Procedure for Moisture Content: Procedure: Take about 5 ml of sample in a glass beaker (W 1). Then transfer the sample into KFR vessel and reweight the beaker again (W 2). Then titrate against KFR solution. Note down the volume as T.V (Titrate Value). Conduct the duplicate test to get concordance value. Calculation:

T.V x water equivalent Moisture content = ________________ ___________________ 10 x (W 1 - W 2)

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Tagros Chemicals India Limited Limited-Cuddalore Integrated Management System Department: Title: Quality Control Analysis Method of Cypermethrin Technical for Assay and Related quality parameters

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L3/SOP/QC/184 00 05.06.2008 Page 5 of 5

Procedure for Acidity: Reagents Required: 0.02N Sodium Hydroxide Solution Methyl red indicator Procedure: Weigh accurately 10 gm of sample in a conical flask. Then add 25ml of acetone and 75ml of distilled water and few drops of methyl red indicator and titrate against 0.02N NaOH up to orange to yellow color change. Note down the burette volume as T.V e Calculation: T.V x Normality of 0.02N NaOH x 49 Acidity (as H2SO4) = ______________________________ 10 x Wt. of sample

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