Analysis Method of Cypermethrin Technical

Tagros Chemicals India Limited-Cuddalore

Doc No:

L3/SOP/QC/184

Integrated Management System

Rev No:

00

Department:

Quality Control

Rev Date:

05.06.2008

Title:

Analysis Method of Cypermethrin Technical for Assay and Related quality parameters

Page No:

Page 1 of 5

I. PURPOSE: The purpose of the procedure is to define the analysis method of Cyperme hrin Technical for Assay and related quality paramet rs. II. SCOPE: This procedure is applicabl

for analysis method of Cypermethrin Technical for Assay and related

quality parameters. III. RESPONSIBILITY: It is the responsibility of th e 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 Re ister – 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 i a test tube, physically check the colour and an y visible foreign particles present or not, compar with standard colour grade sample and fix the colour grade.

2.

10% solution in Toluene Test: Weigh about 10.0 gm of sample in a 100 ml cone measuring cylinder

nd make upto the mark

with toluene (LR grade) and dissolve well. Physically check the clarity an d foreign particle present or not. 3.

Procedure for Assay nalysis: a) Internal Standard: Di-Octylphthlate of purity (Min-98.00%) b) Reference Standar : Cypermethrin Technical of purity (Min – 95.00%) c) Preparation of Inte nal stock solution: Weigh about 8 gm of Di-Octylphthalate in a 150ml glass beake r. Dissolve the material completely by using Chloroform (LR grade) and transfer into 2 lits volumetric flasks. Then dissolve the materi l by using chloroform (LR grade) and make upto the mark. Dissolve the solution carefully or sonicate for 10minutes. Then allow the soluti n to retain and bring to room temperature.

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Tagros Chemicals India Limited-Cuddalore

Doc No:

L3/SOP/QC/184

Integrated Management System

Rev No:

00

Department:

Quality Control

Rev Date:

05.06.2008

Title:

Analysis Method of Cypermethrin Technical for Assay and Related quality parameters

Page No:

Page 2 of 5

d) Standard Preparation: Weigh about 0.26g

of homogenized Cypermethrin reference standard in a separate 50ml

volumetric flask. Then dissolve the reference standard by using int ernal stock solution and make upto the mark. Dissolve the solution or sonicate for 10minutes. Then allow the solution to retain and bring to room temperature. Perform a duplicate standar solution. e) Sample Preparatio : Weigh about 0.26g

of homogenized Cypermethrin sample in a separate 50ml volumetric

flask. Then dissolve the sample by using internal stock solution a nd make upto the mark. Dissolve the solutio 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, ample-1, Sample-2, Standard-2, Sample-1, Sam ple-2.

g) Instrument Conditi n: Instrument

: Gas Liquid Chromatography

Detector

: FID

Column

: 5% Dexil 300 ss 2 mtrs.

Temperatures: Oven Temp

: 260°C

Injector Temp

: 270°C

Detector Temp

: 280°C

Gas Flow Rates: Rates: Nitrogen Flow

: 30 ml/min

Hydrogen flow

: 30 ml/min

Zero Air flow

: 300 ml/min

Run Time

: 10 min

Retention Time: Internal Standard

: 2 - 3 min

Cypermethrin

: 4 - 5 min

Calculation Method

: Internal Standard Method

Calculation: Calculate the Cyper ethrin content for each sample injection, the following equation.

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Doc No:

L3/SOP/QC/184

Integrated Management System

Rev No:

00

Department:

Quality Control

Rev Date:

05.06.2008

Title:

Analysis Method of Cypermethrin Technical for Assay and Related quality parameters

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Page 3 of 5

AxBxC Relative response f ctor (F) = DxExG

A = Area of Cyperm thrin peak from the standard solution. B = Weight of Di-Oc ylphthalate (IS) stock solution C= Purity of Di-Octyllphthalate. D = Area of Di-Octyl phthalate peak of the standard solution. E = Weight of Cyper methrin in standard solution. G = Purity of the Cy ermethrin reference standard. HxBxC Total Cypermethrin ontent (% w/w) = ___________  IxJxF Where, H = Area of Cypermethrin peak in the sample solution. I = Area of the Di-Octylphthalate peak in the sample solution B = Weight of Di-Oc ylphthalate (IS) stock solution. J = Weight of sampl . C = Purity of Di-Oct lphthalate. F = Relative respon e factor.

4.

Procedure for Cis-Tra s Isomer Analysis: a) Standard Preparation: Weigh about 100m

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 Preparatio : Weigh about 100mg of sample in a 10ml volumetric flask and mak upto the mark by using Mobile Phase. Diss lve the solution or sonicate for 10minutes. Then allow solution to retain and bring to room temperature.

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Doc No:

L3/SOP/QC/184

Integrated Management System

Rev No:

00

Department:

Quality Control

Rev Date:

05.06.2008

Title:

Analysis Method of Cypermethrin Technical for Assay and Related quality parameters

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Page 4 of 5

c) Instrument conditi n: Instrument

: HPLC

Column

: Hypersil Silica 5micron (NP), 250mm x 4.6 mm ID.

Mobile Phase

: Hexane: Di-Ethyl ether

Ratio

: 98 :02

Flow

: 1.50 ml / min

Detector

: UV 280 nm

Injection size

: 20µl

Retention time

: 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)

: First peak of Cis Isomer.

Second peak (B)

: Second peak of Cis Isomer.

Third peak (C)

: First peak of Trans Isomer.

Fourth peak (D)

: 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 (W2). Then titrate against KFR solution. Note

own 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 (W1 - W2)

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Doc No:

L3/SOP/QC/184

Integrated Management System

Rev No:

00

Department:

Quality Control

Rev Date:

05.06.2008

Title:

Analysis Method of Cypermethrin Technical for Assay and Related quality parameters

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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 acet one and 75ml of distilled water and few drops of methyl red indicator and titrate against 0.02N NaO

up to orange to yellow

color change. Note down th burette volume as T.V Calculation: T.V x Normality of 0.02N NaOH x 49 Acidity (as H2SO4) = ______________________________  10 x Wt. of sample

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