Analysis Method of Cypermethrin Technical

Tagros Chemicals India Limited

Integrated Management

Department: Quality Control

Title: Analysis Method of Cypermethrin Technical for Assay and Related quality parameters

Prepared By

Signature

Designation Sr. Officer

I. PURPOSE:

The purpose of the procedure is to define the analysis

and related quality parameters.

II. SCOPE:

This procedure is applicable for analysis

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

IV. DOCUMENT REFRENCE:

Finished Goods Product Register

Finished Goods Worksheet –

V. PROCEDURE:

Wear all the personal protective equipments

1. Physical Appearance:

Take 20 ml of sample in a test tube,

present or not, compare

2. 10% solution in Toluene Test:

Weigh about 10.0 gm of sample in a 100 ml cone

with toluene (LR grade) and dissolve well.

or not.

3. Procedure for Assay Analysis:

a) Internal Standard:

Di-Octylphthlate of purity (Min

b) Reference Standard

Cypermethrin Technical of purity (Min

c) Preparation of Internal stock solution:

Weigh about 8 gm of Di

completely by using Chloroform (LR

dissolve the material by using chloroform (LR

solution carefully or

room temperature.

Tagros Chemicals India Limited-Cuddalore Doc No:

Integrated Management System Rev No:

Rev Date:

Analysis Method of Cypermethrin Technical for and Related quality parameters

Page No:

Reviewed By Approved By

Asst. Manager QA Head

The purpose of the procedure is to define the analysis method of Cypermethrin Technical for

and related quality parameters.

pplicable for analysis method of Cypermethrin Technical for Assay


ensure that the operations are carried out as per the procedure.

Finished Goods Product Register – Technical (FOR/QC/42)

– Cypermethrin Technical (FOR/QC/17).

Wear all the personal protective equipments

ple in a test tube, physically check the colour and any

compare with standard colour grade sample and fix the colour grade

% solution in Toluene Test:

.0 gm of sample in a 100 ml cone measuring cylinder and make

(LR grade) and dissolve well. Physically check the clarity and foreign particle

Analysis:

Octylphthlate of purity (Min-98.00%)

Standard:

ermethrin Technical of purity (Min – 95.00%)

Preparation of Internal stock solution:

gm of Di-Octylphthalate in a 150ml glass beaker. Dissolve the material

completely by using Chloroform (LR grade) and transfer into 2 lits

dissolve the material by using chloroform (LR grade) and make upto the mark. Dissolve the

or sonicate for 10minutes. Then allow the solution to retain

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Factory Head

Cypermethrin Technical for Assay

Cypermethrin Technical for Assay and related


check the colour and any visible foreign particles

and fix the colour grade.

er and make upto the mark

and foreign particle present

Octylphthalate in a 150ml glass beaker. Dissolve the material

) and transfer into 2 lits volumetric flasks. Then

upto the mark. Dissolve the

sonicate for 10minutes. Then allow the solution to retain and bring to





Prepared By

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d) Standard Preparation:

Weigh about 0.26gm of homogenized Cypermethrin reference standard in a separate 50ml

volumetric flask. Then dissolve the reference standard by using internal stock solution and

make upto the mark. Dissolve the solution

to retain and bring to

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 a

Dissolve the solution

room temperature. Perform a duplicate sample solution.

f) Injection sequence:

Blank, Standard-1, Sample

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



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Standard Preparation:

out 0.26gm of homogenized Cypermethrin reference standard in a separate 50ml


upto the mark. Dissolve the solution or sonicate for 10minutes. Then allow the sol

and bring to room temperature. Perform a duplicate standard solution.

Sample Preparation:


flask. Then dissolve the sample by using internal stock solution and make

Dissolve the solution or sonicate for 10minutes. Then allow the solution to retain

room temperature. Perform a duplicate sample solution.

Injection sequence:

1, Sample-1, Sample-2, Standard-2, Sample-1, Sample

Condition:

: Gas Liquid Chromatography

: FID

: 5% Dexil 300 ss 2 mtrs.

: 260°C

: 270°C

: 280°C

: 30 ml/min

: 30 ml/min

: 300 ml/min

: 10 min

: 2 - 3 min

: 4 - 5 min

: Internal Standard Method

Cypermethrin content for each sample injection, the following e

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Factory Head

out 0.26gm of homogenized Cypermethrin reference standard in a separate 50ml


sonicate for 10minutes. Then allow the solution

room temperature. Perform a duplicate standard solution.


nd make upto the mark.


Sample-2.

sample injection, the following equation.





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Relative response factor

A = Area of Cypermethrin peak from the

B = Weight of Di-Octylphthalate (IS) stock solution

C= Purity of Di-Octylphthalate.

D = Area of Di-Octylphthalate peak of the

E = Weight of Cypermethrin in

G = Purity of the Cypermethrin

Total Cypermethrin content (

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-Octylphthalate (IS) stock solution.

J = Weight of sample.

C = Purity of Di-Octylphthalate.

F = Relative response factor

4. Procedure for Cis-Trans Isomer Analysis:

a) Standard Preparation:

Weigh about 100mg of Cypermethrin standard (known cis

volumetric flask and make

sonicate for 10minutes. Then allow the solution to retain

b) Sample Preparation:

Weigh about 100mg of sample in a 10ml volumetric flask and make

Mobile Phase. Dissolve the solution

and bring to room temperature.



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A x B x C Relative response factor (F) =

D x E x G

A = Area of Cypermethrin peak from the standard solution.

Octylphthalate (IS) stock solution

Octylphthalate.

Octylphthalate peak of the standard solution.

of Cypermethrin in standard solution.

G = Purity of the Cypermethrin reference standard.

H x B x C Total Cypermethrin content (% w/w) = ___________

I x J x F

= Area of Cypermethrin peak in the sample solution.

Octylphthalate peak in the sample solution

Octylphthalate (IS) stock solution.

of sample.

Octylphthalate.

F = Relative response factor.

Trans Isomer Analysis:

Standard Preparation:

Weigh about 100mg of Cypermethrin standard (known cis + trans

volumetric flask and make upto the mark by using Mobile Phase. Dissolve the solution


Sample Preparation:

Weigh about 100mg of sample in a 10ml volumetric flask and make

Mobile Phase. Dissolve the solution or sonicate for 10minutes. Then allow solution to retain

room temperature.

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= Area of Cypermethrin peak in the sample solution.

+ trans isomer ratio) in a 10ml

upto the mark by using Mobile Phase. Dissolve the solution or

room temperature.

Weigh about 100mg of sample in a 10ml volumetric flask and make upto the mark by using

sonicate for 10minutes. Then allow solution to retain





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c) Instrument condition

Instrument

Column

Mobile Phase

Ratio

Flow

Detector

Injection size

Retention time

Calculation:

A + BCis Isomer = ------------------

A + B + C + D

Trans Isomer = 100

First peak (A)

Second peak (B)

Third peak (C)

Fourth peak (D)

Procedure for Moisture Content:

Procedure:

Take about 5 ml of sample in a glass beaker (W

reweight the beaker again (W

(Titrate Value). Conduct the duplicate test to get concordance value.

Calculation:

T.VMoisture content = ________________

10



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condition:

: HPLC

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

: Hexane: Di-Ethyl ether

: 98 :02

: 1.50 ml / min

: UV 280 nm

: 20µl

: 7.0 – 12.0 min (CIS + Trans Isomers)

A + B ------------------ x 100 A + B + C + D

Trans Isomer = 100 - Cis Isomer

: First peak of Cis Isomer.

: Second peak of Cis Isomer.

: First peak of Trans Isomer.

: Second peak of Trans Isomer

Moisture Content:

Take about 5 ml of sample in a glass beaker (W1). Then transfer the sample into

reweight the beaker again (W2). Then titrate against KFR solution. Note down

Conduct the duplicate test to get concordance value.

T.V x water equivalent ___________________

x (W1 - W2)

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, 250mm x 4.6 mm ID.

transfer the sample into KFR vessel and

down the volume as T.V





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Procedure for Acidity:

Reagents Required:

0.02N Sodium Hydroxide Solution

Methyl red indicator

Procedure:

Weigh accurately 10 gm of sample

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

Calculation:

Acidity (as H2SO4) = ______________________________



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Solution

gm of sample in a conical flask. Then add 25ml of acetone and 75ml of distilled


e down the burette volume as T.V

T.V x Normality of 0.02N NaOH x 49 Acidity (as H2SO4) = ______________________________

10 x Wt. of sample

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in a conical flask. Then add 25ml of acetone and 75ml of distilled


Analysis Method of Cypermethrin Technical

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