Page No.

1/4 FC-PF-277

PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD, NIPHM, HYDERABAD

Sr. No. in Scope NABL/ NON NABL

Flow chart for analysis of Suspensibility of Deltamethrin WP formulation

Date of Analysis

Execution Execut
Sl. No. Step
ed By
1. Sample No.
2. Name of Sample
3. Procedure R1 R2
3.1. Preparation of Standard
Purity of standard %
3.1.1
%
Weigh 0.05 g a.i. of standard in a 50 ml g
3.1.2
volumetric flask g
3.1.3 Note down the S.No. of balance log book.
Dissolve and dilute up to the mark with a
3.1.4 mixture of 1,4-dioxan and iso-octane (20 :
80)
Pipette out 2 mL of standard solution (3.2.4)
into a 10 mL volumetric f lask and make up
3.1.5
to the mark with a mixture of 1,4-dioxan and
iso-octane (20 : 80)
3.2 Preparation of suspension:
3.2.1 Weigh 0.05 g a. i. sample in a 100 ml beaker
3.2.2 Note the serial No. of balance log book
3.2.3 Add standard hard water 342 ppm (at least
twice the mass of the material taken for test)
at 30 ± 10C
3.2.4 Allow to stand for 30 sec. & stir by hand for
30 sec. with a glass rod.
3.2.5 Transfer the slurry to the stoppered
measuring cylinder (250 ml) and any residue
by washing with small quantity of hard
water (342 ppm)
3.2.6 Add hard water (342 ppm) up to the mark
3.2.7 Close the cylinder with the stopper and
invert it sharply through 30 complete cycles
within 1 min.
Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow chart for analysis of
Document No. : FC-PF-277 Document Name : suspensibility of Deltamethrin WP
formulation, % by mass
Revision No. : 00 Issue Date : 01/06/2014
Revision Date : -- Next Revision Date : 01/06/2016
Prepared By Checked By Approved By Issued By

Mrs.T. Sridevi Dr. Nirmali Saikia Dr. Abhay Ekbote Mr. C. V. Rao
(Deputy Quality Manager) (Technical Manager) (Director PM) (Quality Manager)
Page No. 2/4 FC-PF-277

PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD, NIPHM, HYDERABAD

3.2.8 Allow the cylinder to stand at rest for 30

min. at 30±10C
3.2.9 Withdraw suspension (nine-tenths) from the
cylinder within 10 to 15 sec by dipping the
nozzle of the glass tube using suction
through filtration flask
Suspension including sediment at the
3.2.10 bottom of the cylinder (one - tenth of the
suspension)
3.3 Preparation of Sample
Transfer the bottom 25 mL of sediment to a
3.3.1 250 mL separating funnel.
Extract the sample with mixture iso-octane :
3.3.2 1,4-dioxane(80 :20) thrice using 25 mL each
time.
Collect the organic solvent layer in a 500 mL
GG stoppered conical flask passing through a
3.3.3
funnel plugged with cotton and filled
anhydrous Na2SO4
Evaporate the solvent on a rotary vaccum
3.3.4
evaporator at 85°C to less than 5 mL
Quantitatively transfer the content to a 50
mL volumetric flask using a mixture of 1,4-
3.3.5
dioxan and iso-octane (20 : 80) and make up
to the mark.
Filter the sample through sample filtration
3.3.6 kit using 0.45µm membrane filters and inject
the sample.
4. HPLC Parameters
4.1 Column
4.1.1 S.S. Packed with Lichrosorb silica 60-80
mesh
4.1.2 Length: 25 cm
4.1.3 I.D.: 4.6 mm
4.2 Mobile Phase
4.2.1 Dioxan: iso-octane (5 : 95)
4.2.2 Flow Rate: 1.5 ml/min
4.3 Detector: Ultra-violet
4.4 Wave Length: 254 nm
4.5 Injection Volume: 20 µl

Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow chart for analysis of
Document No. : FC-PF-277 Document Name : suspensibility of Deltamethrin WP
formulation, % by mass
Revision No. : 00 Issue Date : 01/06/2014
Revision Date : -- Next Revision Date : 01/06/2016
Prepared By Checked By Approved By Issued By

Mrs.T. Sridevi Dr. Nirmali Saikia Dr. Abhay Ekbote Mr. C. V. Rao
(Deputy Quality Manager) (Technical Manager) (Director PM) (Quality Manager)
Page No. 3/4 FC-PF-277

PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD, NIPHM, HYDERABAD

5. Result
Sample chromatogram no.
Standard chromatogram no.
6. Calculations:
Deltamethrin content in (g), Where,
in bottom 25 mL of sediment is = A1 = Area of Deltamethrin in sample solution
A2 = Area of Deltamethrin in standard solution
A 1 x M1 X P M1 = Weight of Deltamethrin standard taken in g.
= ------------------ P = Purity of Deltamethrin standard
A2 x 5 X 100

% Suspensibility = 1000 X (M-m) Where,

--------------------- M = Mass in ‘g’ of pesticide present in the
9XM sample taken for the preparation of
suspension
m = Mass in ‘g’ of pesticide found in the suspension
1/10th of sediment remaining in the graduated
cylinder

Result:
Sl. No. Name of test Result Unit Method of Analysis

Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow chart for analysis of
Document No. : FC-PF-277 Document Name : suspensibility of Deltamethrin WP
formulation, % by mass
Revision No. : 00 Issue Date : 01/06/2014
Revision Date : -- Next Revision Date : 01/06/2016
Prepared By Checked By Approved By Issued By

Mrs.T. Sridevi Dr. Nirmali Saikia Dr. Abhay Ekbote Mr. C. V. Rao
(Deputy Quality Manager) (Technical Manager) (Director PM) (Quality Manager)
Page No. 4/4 FC-PF-277

PESTICIDE FORMULATION & RESIDUE ANALYTICAL CENTRE, PMD, NIPHM, HYDERABAD

1. Suspensibility % IS: 6940-1982

Remark / Reference :

Name
Analyzed by Dated signature

Name
Checked by
Dated signature

Name of the Laboratory : Pesticide Formulation & Residue Analytical Centre, PMD, NIPHM, Hyderabad
Flow chart for analysis of
Document No. : FC-PF-277 Document Name : suspensibility of Deltamethrin WP
formulation, % by mass
Revision No. : 00 Issue Date : 01/06/2014
Revision Date : -- Next Revision Date : 01/06/2016
Prepared By Checked By Approved By Issued By

Mrs.T. Sridevi Dr. Nirmali Saikia Dr. Abhay Ekbote Mr. C. V. Rao
(Deputy Quality Manager) (Technical Manager) (Director PM) (Quality Manager)