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Disclosure to Promote the Right To Information

Whereas the Parliament of India has set out to provide a practical regime of right to
information for citizens to secure access to information under the control of public authorities,
in order to promote transparency and accountability in the working of every public authority,
and whereas the attached publication of the Bureau of Indian Standards is of particular interest
to the public, particularly disadvantaged communities and those engaged in the pursuit of
education and knowledge, the attached public safety standard is made available to promote the
timely dissemination of this information in an accurate manner to the public.

“जान1 का अ+धकार, जी1 का अ+धकार” “प0रा1 को छोड न' 5 तरफ”

Mazdoor Kisan Shakti Sangathan Jawaharlal Nehru
“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 6940 (1982): Methods of Test for Pesticides and their

Formulations [FAD 1: Pesticides and Pesticides Residue
Analysis]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 : 6940"'·
ISIS: 6940 - 19821982
(Reaffirmed
( K~all1irlned- 2012)
1997 )

Indian Standard
~1ETHODS
OF TEST FOR
PESTICIDES AND THEIR FORMULATIONS

( First Revision)

FOlJl1h Reprint NOVEMBER 2002

UDC 632.951:620.1

© Copyright 1982

BUREAU OF INDIAN Sl'ANDARDS

MANAK BHA VAN, 9 BAHADIJR SHAI-I 7AFAR MARG
NEW I)ELI-I. 110002

Gr 8 Stptemher 1982
 IS ,6940· 1M2

Indian Standard
METHODS OF TEST FOR
PESTICIDES AND THEIR FORMULATIONS
( First Revision)

Pest Control Sectional Committee, AFCDC 6

Ch.srnuan R'p"s,ntinl
Dn K. D. }'AHARIA Directorate of Plant Protection, Quarantine &
S torage (Ministry of A g ric u I t u r e ),
Faridabad

~Innbt,s
DB H. L. BAMl Central Forensic Science Laboratory «(~cntral
Bureau of. Investigation), New Delhi
nit B. BANERJEB Tea Research Association, Calcutta
DR G. SATYA-NARAYANA (AlterrItJle)
SaRI S. K. BANERJEE Food Corporation of India, New Delhi
SHItI C. S. SnIvANN 1\ (Alle"",u)
Da N. K. BA8U The Alkali &t Chemical Corporation of India
Limited, Calcutta
SHRr S. R.
NKNE (Alternat,)
DR A. K. BBATNAOAR Hindustan Insecticide. Limited, New Delhi
SURI C. C. ABRAH AM (Alt"",,")
CRIBI' CHEMUlT Central Revenues Control Laboratory (Ministry
of Finance), New Delhi
SSRI S. KRI811NAMURTHY ( AII".rusl,)
CUIEI" PLANT PRO'l'XCTION OFFIOER Department of Agriculture, Government of
Maharashtra, Bombay
C HEll I 8 T I N 0 H A B Q E,
INsBOTICIDI:8 T B 8 TIN Q
LABORATORY ( Alt",.." )
SHRI V. G. DBSRPANDB Ciba-GeilY of India Limited, Bo~bay
SIIBI E. A. ALMEIDA ( Alternate)
SBRI OM. P. DUAMIJA Export Inspection CouDcil of I Ddia, New Delhi
SURI P. P. RANOA RAO (AlterMlI)

( c.,.,.,..tl.../M" 2 )

C Copyrit'" 1982
BUREAU OF INDIAN srrANDARDS
This publication i. protected under the lrulitJn Co/17r;,hl A" (XIV of 1957) aod
r~productio~ in whole or in part by any meaDS except with written perm_on or the
publisher .ball be deemed to be aD infrinlem~Dt of copynpt UDder the aaId Act.
 IS : 6940 • 1182
( Continued from pa" 1 )
MImIJ"s Rep,esenling
DR M. S. D.HATT National Malaria Eradication Programme, Delhi
DIREOTOR OJ' AOl\IOULTURlI: Department of Agriculture, Government of Uttar
Pradesh, Lucknow
DEPUTY DIREOTOR ( PLANT
PROTECTION) ( Alternate)
SSBI V. DORAIRAJ Plastic Containers Sectional Committee, MCPD
11, lSI
DRUGS CONTR.OLLER (INDIA) Indian Pharmacopoeia Committee ( Ministry of
Health & Family Welfare), New Delhi
SHut M. RAVIKANT (ALte,nal,)
SHlU G. D. GOKIIAr~lI: Bombay Chemicals Pvt Ltd, Bombay
SHUI V. V. KETKAR ( Alternate)
SHRI D. K.JAIN Punjab United Pesticides and Chemicals Limited,
Chandigarh
JOINT DIRECTOR OF AGRICULTURE, Department of Agriculture, Government of
( 1)14;V~14UPMgNT & rep) Karna taka, M ysore
D E PUT Y DIn E C TOR OJ'
AORJCULTURK PLANT
P IlOTECTloN (Alternate)
DR M. G.JOTWANI Entomology Division, Indian Agricultural
Research Institute (ICAR), New Delhi
DR. R. L. KALRA Punjab Agricultural University. Ludhiana
Dl~ R. P. CHAWLA (ALtunat,)
DR KALYAN SI~QH Chander Sekhar Azad Umversity of Agriculture &
Technology, Kanpur
DR KISHAN Sl.NOH Indian Institute of Sugarcane Research (leAR),
Lucknow t

DR K. K. BAJP AI ( Alternate)
DR K. KRl8UNAMURTHY Ministry of Agriculture ( Department of Food )
SUBJ G. N. BUARDWAJ (Alt"na', )
SURI S. G. KRISHNAN National Organic Chemical Industries Limited,
Bombay
DB J. S. VERMA ( Al,,,,,at, )
DR V. LAKSHMINARAYAN& Directorate of Plant Protection, QJarantine It
Storage ( Ministry of Agriculture), Faridabad
SHRt v.
C. BHARQAV& (AI'",1UJ")
SaRI S. K. LUTURA Directorate General of Technical Development,
. N~w Delhi
S1!RI S. C. BAJA'" ( AI'""a',)
DR J. C. MAJUMDAB BASF India Limited, New Delhi
DB B. P. CnANDRA8EKHAR (Al',rnat,)
SHRI S. K. MAJUMDAR Central Food Technological Research Inatitute
(CSIR), Mysore
SURI M. MUTHU (AII,rna,,)
SBBI O. N. MEHROTRA Ministry of Defence (R & D)
SaRI M. G. CBA1'TERJEE (~lt"tUJl')
SDRI K. S. MEHTA Bbarat Pulverising Mills·Pvt Limited, Bombay
SHRt S. CHATT~RJt ( Altmaal,)
SHBI L. S. MIRLE Alromore Limited, Bangalore
SHBI S. K. RAMAN ( All'","," )

( C..,i,.",d on"." 3S)

2
 IS : 6940 • 1'82
( Contimudfrom pal' 2 )

Members Representing
SHBtJ. M. MUDI Pesticides Formulators Alsociation of India
( S. S. I ), Bombay
DR S. R. BAROOAH (AltpntJl,)
DB A. L. MO()K~RJEE Cyanamid India Limited, Bombay
SHRIJ. P. PABllCB (Allerna', )
DR S. K. MUKERJEB Agricultaral Chemicals Division, Indian
Agricultural Research Institute (leAR ).
New Delhi
Dn N. K. Roy (Alternat,)
SHRII.NARsARBDDY Department of Agriculture, Government of
Andhra Pradesh, Hyderabad
SHItI C. DHARMA RAO ( Alt"nat,)
SHIU G. NATARAJAN' Indofil Chemicals Limited, Bombay
DR L. RAMAKJUSHN AN ( Alternate )
DR V. N. NIGAM Ministry of D{~ft~nce (DGI)
SHat P. N. AOARWAL (Alternate)
SHaI M. M. PAHAJ.IA Department of Agriculture, Government of
Gujarat, Ahmadabad
SURI J
R. G. ADEJ A ( Altemat« )
DR S. Y. PANDIT Bayer (India) Limited, Bombay
SHIll C. G. DUARNE ( Alternate )
DB P. S. PlIAOXE Sandoz (India) Limited, Thane
Sn ru A. V. Nvrtr (Alt,rnal,)
SRRI S. M. PLtADHAN Metal Containers Sectional Committee, MCPD 12,
lSI
SARI Y. A. PJ(A1HI :\N Rallis India Limiu-d, Bombay
DR Z.J. KAPA1JIA (Alternat,)
SHut D. N. V. Rs o Tata Chemicals Limited, Mithapur
SHRt C. NEELKAN'f AN(Alt"nate)
SJI;CltETAR Y Central Insecticides Board, Directorate of Plant
Protec-tion, Quarantine & Storage ( Ministry
of Agricu lture ), Faridabad
DR. R. C. GUPTA ( AltlTnate)
Ds K. N. SlIltlVASTAVA Pesticides Association of India, New Delhi
Da]. C. MA,JUMDAR (Alternatl)
SHRIA. C. SHROFF Excel Industries Limited, Bombay
Suur P. V. KANGO ( Alter1ltJI, )
On K. S. SlNOII Indian Veterinary Research Institute (leAR),
Izatnagar
S. C. SRIVASTAVA ( Alternate )
SllRI
MAJ GEN R. R. SUBRAMANIAN Directorate General Armed Forces Medical
Services ( Ministry of Defence), New Delhi
COL P. S. GILL (Allnnate)
SBRIN.S.VE~KATARAMAN Department of Agriculture, Government of
Tamil Nadu, Madras
DR R. V. VENKATARATNAM Regional Research Laboratory ( (~SIR ).
Hyderabad
DR S. NAOA.DUSDAN RAO ( Alternat« )
DR P. R. VENKATE8WARAN Union Carbide ( India) Limited. New Delhi
DR K. N. SHRIVA8TAVA (Alternate)

( Continu,d on pal' 34 )

33
IS : 6940 • 1982
( Continu*, from """ S3)

MnnHrs R,/W,smlinl
SUI E. a: VIOCAJBJI Paper &. Flexible
Committee, MCPD 14, lSI
Packagil1l Sectional
SnRI N. G. W AGLB Pest Control (India) Private Limited, Bombay
SBRI M. R. BA..IIXAR ( Al',rnal, )
DR B. L. W~TTAL National Institute or Communicable Diseues.
Delhi
SUR) G. C. JOSHI (~l'"n", )
SHRIT.PUBBANANDAK, Direct.' Genual, lSI (&-t!IJi&io M,mNr)
Director ( Agri &. Food)
St"IIary
SURI M. L. KUMAR
Deputy Director (Agri & Food) J lSI
 AMENDMENT NO.1 SEPTEMBER 1988
TO
IS : 6940 - 1982 ME1'HODS OF TEST FOR
PESTICIDES AND THEIR FORMULATIONS
( First Revision)
( Page 20, clause 11.4.2 ) - Substitute the foJlowing for the existing
clause:
'11.4.2 Procedure - Weigh accurately 2 g of the material and pour
uniformly and quickly in the beaker containing 100 ml of the standard
hard water ( see 11.2.2.1). Start the stop-watch simultaneously. Note
the time when the bulk material is completely submerged into water.'
( Page 26" clause 13.5.4 ) - Substitute the following for the existing
clause:
'13.5.4 Electrometric Procedure for Determination of Acidity or
Alkalinity.
13.5.4.1 Reagents
a) Methyl alcohol - distilled.
b) Sodium hydroxide - 0'05 N.
c) Hydrochloric acid - 0·05 N.
13.5.4.2 Apparatus
a) lJH meter.
13.5.4.3 Procedure - Weigh accurately about 2 g of the sample in a
conical flask. Add 25 ml methyl alcohol and stir for 5 minutes. Filter
through a Buchner funnel into the filter flask. Rinse the conical flask
and the Buchner funnel with methyl alcohol (3 x 5 rnl ). Transfer the
combined methyl alcohol extracts to the titration vessel rinsing the filter
flask with 10 1111 of methyl alcohol. Add 10 rnl of distilled water and
titrate electrometrically with sodium hydroxide solution or hydrochloric
acid to pH 5 at 27~C. Calculate the acidity or alkalinity whatsoever by
the factor given in 13.5.2.3 or 13.5.3.3.

(AFCDC 6)

Printed at New India Printing Press, Khurja, India

 AMENDMENrr NO. 2 ()CTOBER 2003
'ro
IS 6940: 1982 Ml~rrHODS OF T~=Sl' FOR PES1'ICII)F~S
ANI) TH~:IR ~"ORMULA TI()NS
( First Revision)

( Page 22, clause 13.3.2.3, after line It ) --- Insert "close the cylinder with
the stopper and invert it sharply to give 10 complete cycles within 20 seconds'.

( FAI) 1 )

Reprography Unit. 81S. New Delhi, India

 IS I 6940 - 1982

Indian Standard
METHODS OF TEST FOR
PESTICIDES AND THEIR FORMULATIONS
( First Revision)
o. FOR E W 0 R D
0.1 This Indian Standard was adopted by the Indian Standards
Institution on 26 February 1982, after the draft finalized by the Pest
Control Sectional Committee had been approved by the Agricultural and
Food Products Division Council and the Chemical Division Council.
0.2 This standard was originally published in 1973 and an amendment
was issued subsequently. Since then a number of Indian Standards on
pesticides have been published and references made in those standards to
the methods of test prescribed in this standard. In the light of experience
gained during the last few years, it became necessary to issue revised
version of this standard. This revised version covers comprehensively
the general analytical details and methods which were not covered in the
original standard. Besides, general methods of test for g-ranules have
also been included.
0.3 About 200 Indian Standard specifications for technical grade
pesticides and their formulations have been published. The standards
for technical grade pesticides include insecticides, fungicides, herbicides,
rodenticides, and fumigants. The Indian Standard specifications for
different kinds of formulations for the above pesticides include emulsifiable
concentrates, water dispersible powders, dusting powders, granules, seed
dressing formulat ions and concentrates such as bait concentrates and
ready-to-use concentrates of certain pesticides themselves, All these
standards for the technical grade as well as for the formulations include
certain methods of test that .are COrn mon to all these standards. With a
view to avoid the repetition and to provide an easy reference, it was
found desirable to publish this standard as applicable generally to various
technical grade pesticides and their formulations,
0.3.1 While preparing this standard , due consideration has been given
to the methods of test as arrived at in the WHO specification; and also
the methods of test, prepared by the Collaborative Analytical Pesticides
Committee of the Food and Agricultural Organization.

3
IS : 6940 - 1982

0.4 In reporting the result of a test or analysis made in accordance with

this standard, if the final value, observed or calculated, is to be rounded
off, it shall ~e done in accordance with IS : 2-1960*.

1. SCOPE
1.1 This standard specifies general methods of test for technical grade
pesticides and their different formulations.

2. Q,UALITY OF REAGENTS
2.1 Unless specified otherwise, pure chemicals and distilled water (see IS:
1070-1 977t ) shall be employed in tests.
NOTE - C Pure chemicals • shall mean chemicals that do not contain impunities
which affect the results of analysis.

SECTION 1 GENERAL METHODS OF TEST FOR

PESTICIDES. TECHN leAL GRADE
3. GENERAL
3.1 There are several methods which are generally applicable to all
technical grade pesticides and they are given under various clauses.
4. DETERMINATION OF MOISTURE CONTENT
4.0 General - For the determination of moisture content, two methods,
namely, the Karl Fisher method (see 4.1) and the Dean and Stark
method ( see 4.2) have been specified. The Karl Fisher method may be
followed if the expected moisture content is below 1·0 percent and the
Dean and Stark method in cases where the expected moisture content is
1·0 percent and above.
4.1 Karl Fischer Method - The procedure for determining moisture
content by this method shall be in accordance with IS : 2362-1973:.
NO"I'lI: - All necessary precautions shall be taken in order to avoid any possible
hazards due to oxidation, while determining moisture content in mercaptan based
pesticides.

4.2 DeaD and Stark Method

4.2.1 Apparatus
4.2.1.1 Distillation flask - made of hard glass with ~OO ml capacity
and provided with a ground-glass socket.

·Rult s for rounding otT numerical values (rezJised).

tSpccification for water for general laboratory use ( second. recision ).
:Detcrmination of moisture content by the Karl Fischer method (first revision).

4
 IS 16940-1_
"'2.1.2 Reflux condms,r - made of glass, water cooled, having the
outside diameter of the inner tube 16 to 17 rom, and that of the jacket 23
to 25 mm, The lower end of the condenser is provided with a ground-
glass cone. The tip of the condenser is ground at an angle of
approximately 30° from the vertical axil.
".2.1.3 Receiver (or trap) - made of hard glass and consisting
eueritially of an upper chamber, provided with a side-arm leading to the
distillation flask, and a cylindrical graduated portion, the lower end of
which is sealed. The opening of the upper chamber is provided with a
ground-glasa socket fitting the CODe of the condenser. The lower end of
the side-arm is provided with a ground-glass cone fitting the socket ofthe
distillation flask. The graduated portion has a capacity of 5 ml when
filled to the highest graduation mark. The scale covers the range 0 to
5 mi. with graduation marks at 0-1 mi. intervals. The error at any
indicated capacity should not exceed 0·02 mi.
et.2.1.4 Heat sour" - either an oil-bath or an electric heater provided
with a sliding rheostat or other means of heat control. The temperature
of the oil in the bath should not be very much higher than the boiling
point of petroleum naptha ( se« 4.2.2.2 ).
".2.1.5 Copper wi,e - long enough to extend through the condenser
with one end twisted into a spiral. The diameter of the spiral should be
such that it fits snugly within. the graduated portion of receiver and yet
can be moved up and down.

"2.2 ReGgents
4.2.2.1 Chromic acidcl,alling solution
4.2.2.2 One of the following solvents may be used:
a) P,trol,um nGphtAa - with a boiling range or 90 to 210°C;
b) ,,-H,P''''',
-boiling point around 9S·C; and
c) Tolunu- boiling point around tIO°C.

4.2.3 Jlroe,tlur, - Clean the entire apparatus (sle Fig. 1 ) with chromic
acid solution to minimize the adherence of water droplets to the sides of
the condenser and the receiverv Rinse thoroughly with distilled water and
dry completely before using.
Place an appropriate. amount of the sample accurately weighed into
the distiJlation flask. The amount of sample taken should be such that
the distillation flask is not more than one-third full; it should not contain
more than 1-8ml of water. Add sufficient volume of the solvent ( 100 to
200 ml) 80 that the sample shall be completely covered by the solvent
while the distillation is in progress. Swirl to mix and add pumice stone

5
IS: 6940- 1982

to ensure steady boiling. Assemble the apparatus and fill the receiver
with the solvent by pouring the solvent through the condenser until it
begins to overflow into the distillation flask. Attach a guard tube
containing "anhydrous calcium chloride at the top of the condenser to
prevent condensation of atmospheric moisture within the tube. In order
that the refluxing may be under control, wrap the distillation flask and
the tube leading to the receiver with asbestos fibre. Heat the flask at such
a rate that about 100 drops are distilled over, increase the distillation rate
to about 200 drops/min and continue heating until no more water is
collected. Purge the condenser occasionally during the distillation with
5-ml portions of the solvent in order to wash down any moisture adhering
to the walls of the condenser. The water in the trap may be made to
separate from the solvent by means of a copper wire, one end of which is
twisted into a helix. The copper wire if moved up and down in the
condenser and receiver occasionally causes the water to settle down at the
bottom of the trap. Reflux until the water level in the receiver remains
unchanged for 30 minutes and then shut off the source of heat. Flush the
condenser with the solvent, making use of the copper wire to disengage any
moisture droplets. Allow to stand for about 15 minutes and then read the
volume of water.
4.2.4 Calculation
100 V
Moisture content, percent by mass = -M--
where
V::..= volume in ml of water collected; and
M = mass in g of the material taken for the test.
4.2.5 Precision - The results of a duplicate determination of moisture
content of the material, percent by mass, should not vary by more than
± 0·05 from that of the first determination.
5. DETERMINATION OF RELATIVE DENSITY OP UQ,UID
PESTICIDES
5.1 Terminology - For the, purpose of pesticides, the relative density of
the material shall be the ratio of the mass in air of a given volume of
the material generally at 27°C to that of an equal volume of water at the
same temperature.
5.2 Apparatus
5.2.1 Relative Density Bottle- Castell Evans modification with ground-
in stopper and ground-on cap (see Fig. 2 ) or a Perkin type pyknometer
tube (see Fig. 3 and also IS : 5717-1970· ).

·Spccification for pyknometen.

6
FLASK
500m'

7
II. &NO -1.2

FlO. 2 SPBCIFIC GRAVITY BOn'LE (CASTELL EVANS MODInCATlON

WITH GR.OUND-IN STOP.... AND GIlOUND-ON CAP)

FlO. 3 PYKNOIIBTBIl TUB. (P••XIN'. TYPE)

8
 IS I 6940 • 1982
5.3 Procedure - Weigh a clean and dry relative density bottle or a
pyknometer of 25 ml capacity. Fill the tared relative density boule or
the pyknometer with freshly boiled water, place it in a bath maintained
at 27 ± -loe and allow sufficient time to attain the temperature of the
bath. Then insert the ground-in stopper which has also been brought
to 27 ± loe. Wipe off the excess from the stopper and place the cap in
position. Remove the relative density bottle or the pyknometer from the
bath, bring to room temperature and weigh. Empty the relative density
bottle or the pyknometer, clean and dry it, and then repeat the operation
with the material at 27 ± loe.

5.4 Calculation aad Report

5.4.1 Specify the temperature of testing ·in the report.
5.4.2 The relative density is calculated by the following formula:

Relative density at 27~C/27".C == ~ - A

-A
where
C == mass in g of the relative density bottle or the pyknometer
filled with the material at 27°C,
A = mass in g of the dry relative density bottle or the
pyknometer, and
B :=I mass in g of the relative density bottle or the
pyknometer filled with water at 27°C.

6. DETERMINATION OF MELTING POINT

6.1 Apparatus
6.1.1 Thermometer - A long-stem and short-bulb thermometer with a
range of 0 to 200°C or 100 to 200°C and with subdivisions of O"soC.
6.1.2 Bath and Heating Assembry - This consists of a suitable chamber
with a glass front. Inside, there is a long-necked flask (250-ml Kjeldahl
flask) three-fourths full with liquid paraffin and placed on a suitable
mounting for heating with a gas burner. The flask is loosely fitted with
a stopper which carries a thermometer. The chamber is provided with
appropriate illumination to observe the .melting of the material and the
reading of temperature.
6.2 Procedure - Take a small quantity of finely powdered substance
and dry the same in a vacuum desiccator over silica gel or phosphorus
pentoxide for 24 hours or according to the requirements given in the
9
IS I 6940 • 1_"
specification. Transfer the same in the capillary tube with one end sealed.
Ensure proper packing of the material in the tube by gently tapping it on
the table. The material in the capillary tube should be sufficient to cover
the entire length of the thermometer bulb. Introduce the filled capillary
tube into the heated bath at a temperature loGe below the expected
lower limit of the melting range. Attach the capillary tube with the
thermometer such that the material is very close to the bulb. Introduce
the thermometer in the bath in such a way that the thermometer bulb is
well below the surface of the liquid. Now heat slowly and carefully so
that the rise in bath temperature is about l°e per minute. Note the
temperature of initial melting (when first liquid drop appears) and
completion of melting (when no solid particle is left). Report the
temperature of melting point completion and the difference of tempera-
tures as melting range.
NOTE - Ensure that two consecutive deterrninations do not differ by more
than O·5~C.

7. DETERMINATION OF SOFTENING POINT

7.1 Outline of Method - The softening point of technical grade
pesticide is determined at a temperature when the test sample becomes
sufficiently fluid to drop from the thermometer used in the determination
of the softening point.

7.2 Apparatus
7.2.1 H,aling Vesul>« a glass beaker, 1 000 ml capacity.
7.2.2 Stirre - capable of mixing the liquid thoroughly.
7.2.3 Thermometer - 0 to 200°C with loe subdivisions.
7.2.4 Sample-Melting Bath - an oil-bath maintained at 125 ± loe.
7.2.5 Test- Tubes - provided with rims; 175 mm long and 22 mm
outs ide 'dia meter.

7.3 Procedure
7.3.1 Place sufficient material which, when melted, will fill in one-third
or one-half of 50-mt beaker. Place the beaker in a sample-melting bath
for 4 to 8 minutes until the material is niched completely. The melted
sample shall be clear and free of crystals.
7.3.2 Weigh the thermometer to the nearest 0·01 g and warm over a
flame or hot-plate until it is heated to about 50°C. Immediately dip the
thermometer vertically into the melted sample until the shoulder of the
bulb is covered. Lift the thermometer from the sample, hold it in a

10
 IS : 6940 • 1'82
vertical position keeping the bulb on the top, rotate until the sample
solidifies and weigh. The mass of the sample on the thermometer bulb
should be between 0·50 and 0-55 g. If there is insufficient material on
the thermometer, dip it again into the melted sample to pick up the
desired quantity of the material. If the bulb of the thermometer has
picked up too much sample repeat the operation. Allow the thermometer
and the sample to cool until they reach approximately room temperature
which takes about 15 minutes.

7.3.3 Adjust the heating vessel containing liquid paraffin to 110 to

111"C. Insert the thermometer carrying the sample in the test-tube
supporting it with a notched rubber or cork stopper so that the lower end
of the bulb is about 25 mm from the bottom of the tube. Place the tube
in the vessel so that the bonom of the tube is about 25 mm above the
bottom of the vessel. The bottom of the thermometer bulb is thus 50 mm
above the bottom of. the beaker and the top of the bulb about 25 rom
below the level of the liquid in the vessel. Stir the vessel continuously
during the test with a motor stirrer.

7.3.3.1 Observe the thermometer carrying the sample inside the test-
tube and record the temperature of the softening point from the
thermometer, when the first drop of the melted material falls from the
end of the bulb.

7.3.4 Repeat the operation specified in 7.3.3 and 7.3.3.1 until the
results agree within 10C (see Note ).
No'rlC- Two or more samples may be placed in the veasel durin. the ..me
operation.

8. DETERMINATION OF SETTING POINT

8.1 Apparatus ( see Pil_ 4 )
8.1.1 Boiling Tube A - a 20 ± 0·1 mm thick-walled, 20 X 2-5 em tube
fitted with a cork collar at 6 to 7 em below the top edge of the tube, the
collar fitting tightly in the boiling tube B (see 8.1.3 ).

8.1.2 Gloss Stirrer -of length sufficient for tube A, and with its one
end bent at right angle in the form of a ring so as to permit a
thermometer to pass through the ring.

8.1.3 Boiling Tube B - 15 X 4 em,

I.I.t Thermometer - A long-stem and short-bulb thermometer with a

range of 0 to 200°C and with subdivisions at one-tenth of a degree.

11
IS I 6940 • 1982

f~
..._ l

All dimensions in mi'[ljm erres,

FIG. 4 APltARATUS FOR THft: Dl~TERl\I1NATIUN OF SETTING POINT

8.2 Procedure
8.2.1 Place in the boiling tube A, a sufficient amount of the sample to
give, when rnclted, a depth of liquid of approximately 7·S em. Melt
carefully by immersing the tube to a depth of 10 CIn in an oil-bath
maintained at 14 to 15CtC above the anticipated minimum setting point
of the test material,
8.2.2 Insert this boiling tube, oy means of a cork collar, to wit.hin 1-3
em of the bottom of the boiling tube B immersed to a depth of 10 ern in
an oil-bath maintained at about 10°C below the anticipated setting point.
Place the stirrer in the inner boiling tube. The thermometer is then
clamped in a central position with its bulb 2·5 em from the bottom of the

12
 IS I 6940 • 1182
tube. The temperature of the melt should be approximately 10°0 higher
than the anticipated setting point at this stage.

8.2.3 Stir at the rate of about two strokes per second by moving the
stirrer up and down until the material begins to thicken, at this point stir
vigorously, working into the melt portions of the material solidified on the
walls of the tube. Stop stirring when the temperature ceases dropping
and remains constant for some time (see Note ). Record this temperature
as the setting point.
~OT. - In some instances, there rna y be a slight rise in the temperatdre of the
material; in such a case, record the highest .teady temperature AI the .etting point.

8.2.3.1 Apply corrections as necessary for the thermometer

calibration and the emergent stem.

8.2.3.2 Emergent -stem corrections - The correction for the emergent

stem in mercury-filled thermometers, to be added to the temperature
reading, is calculated from the following formula:
0·00015 N( T-I)
where
N = number of degrees on the scale of the t~rlllemeter
between the top of the inner boiling tube and the level
of the rnercu rv,
T = temperature reading, on the thermometer in the melt,
and
t· = t~mperatureof the stem at the mid-point of the exposed
mercury thread.

9. DETERMINATION OF MATERIAL INSOLUBLE IN

ACETONE
9.1 Procedure - Weigh 109 of the material into a clean and dry
250-ml Erlenmeyer flask, fitted with a ground-glass joint. Add 150 ml of
dry acetone and warm under reflux until all soluble material is dissolved.
Filter 'the solution using a tared. Gooch or sintered-glass crucible of
porosity No.3,. and wash well with more solvent. Dry at 110°0 (or
30 minutes, cool, and then weigh,

9.1.1 For phenyl mercury acetate technical and other similar products
containing up to 5 percent matter insoluble in acetone, weigh 2 g of
material and proceed in .accordance with 9.1.
13
IS I &940 • 1982

9.2 Calca1atioD
100m
Matter insoluble in acetone, percent by mass = --1.1-
where
m :I::: mass in g of the residue obtained after drying, and
M :::II mass in « of the material taken for the test.

SECTION 2 GENERAL METHODS OF TEST FOR

PESTICIDAL FORMULATIONS
10. GENERAL
10.1 The pesticidal formulations, which are commonly used, are water
dispersible powders. dusting powders, emulsifiable concentrates and
granules.

11. METHODS OF TEST FOR WATER DISPERSIBLE POWDERS

11.1 Sieving Test After Accelerated Storage/Without Pretreat-
meat (8~~ Appeadlz A )
11.1.1 ApptJ1alus
11.1.1.1 B,ak" - of 6·0 to 6'5 em and 250 ml capacity.
11.1.1.2 Pressure asstmbly - a piston or disc, loosely fitting in the
beaker and so formed or weighed as to exert an even pressure of
25 K/eml •
11.1.1.3 Test siew - specified IS Sieve [ see IS : 460 ( Part I )-1978· ]
prepared for the test by removing any film, grease or other water..
repellent material and then by drying.
11.1.1.4 Rubber hose - of about 10 mm internal diameter.

11.1.2 Procedure
11.1.2.1 Ace,lerated sto,ale - Weigh about 20·0 ± 0-5 g of the material
in the beaker. Gently' level the surface of the material in the beaker
with the help of a paper strip. a camel hair brush or a feather. Place the
pressure assembly over the surface of the material in the beaker and
place it in an oven maintained at 54 ± 1~C for 24 hours. Take out the
beaker from the oven. remove the pressure assembly and allow the
material in the beaker to come down to room temperature in a closed

·Specification for telt sieves: Part I Wire elotn telt sieve. (s""ruJ "uisio" ).

14
 IS I 69to • 1912
container taking care to avoid unnecessary exposure of the sample to
atmospheric humidity.
Formulations of water dispersible powders based on organo-
phosphorus compounds should be placed in 100 ml wide-mouthed neutral
glass bottle fitted with a vinyl plastic cap and placed in an oven at
temperature and duration as mentioned in Appendix A. Cool the bottle
in a closed container before removing the cap. After accelerated storage
treatment, the sample should not be exposed to heat,' bright lunshine
or high atmospheric humidity.
11.1.2.2 Sievin,( - At the completion of 3 hours of cooling weigh
accurately about 10·0 g of the treated material (se, 11.1.2.1 ) into a wide-
mouth bottle ( provided with a cork or rubber stepper) and add 100 ml
of tap water. Allow to stand for 30 seconds, then stir for 30 seconds with
a 4 to 6 mm diameter glass rod, at not more than 4 rev/., making no
deliberate attempt to break any lumps. Transfer the slurry immediately
to the sieve rinsing with tap water. Wash the material on the sieve with
an oscillating moderately vigorous spray of tap water iSluing out of the
rubber hose at the rate of 4 to 5 l/min. Continue wuhing for
10 minutes or until no more solid particles of the material pall through
the sieve. Transfer the residue retained on the sieve to a tared Gooch
crucible, dry to constant mass in an oven at a temperature not exceeding
55°C. cool and then weigh. Find the mass of the dry residue,
11.1.3 Calculation
Material passing through specified
IS Sieve, percent by mass = 100 ( 1 - :- )

where
m ::::I mass in g of the dry residue obtained (see 11.1.2.2 ») and
M = mass in g of the material taken for the test.
11.2 S.spe.slbllity Test After Accelerated Storale/Wltlaoat
PretreatmeDt (666 Appeadis A )
11.2.1 Apparatus
11.2.1.1 Beaker- See 11.1.1.1.
11.2.1.2 Pressure assembl" - See 11.1.1.2.
11.2.1.3 Graduated 'ylinder - of capacity 250 ml with ground gla.a
stopper. The distance between 0- and 250-ml marks shall be
21·0 :i: 0-5 em with a clearance of 6·0 to 8·0 em between 25Q-ml mark
and the neck of the cylinder ( see IS : 878-1975*).

• Specification for graduated measuring cylinden (firsl "Disia).

15
IS : 6940 • 1982
11.2.1.4 Glass tube - About 40 em long, of an internal diameter of
about 5 rom, drawn at one end to an openingof2 to:3 mm diameter, with
the other end connected to a vacuum pump

11.2.2 Reagent
11.2.2.1 Standard hard water - Dissolve 0-3040 g of calcium chloride
anhydrous and 0-139 0 g of magnesium chlori Je hexahydrate in distilled
water and make up to one litre in a volumetric flash.
NOT. - Standard hard water is defined aa 'water', which provides a hardneu of
342 ppm, calculated as calcium carbonate,

11.2.3 Procedure
11.2.3.1 Accelerated storage - Carry out accelerated storage test as
prescribed in 11.1.2.1.
11.2.3.2 SusPtnsibililJ test - Weigh accurately into a IOO-ml beaker,
quantity of the treatedJuntreated material ( see 11.2.3.1 and Appendix A )
which could form 250 rnl of suspension. Add a volume of the standard
hard water at 30 ± loe equal to at least: twice the mass of the material
taken for test. Allow to stand for 30 seconds and then stir by hand for
30 seconds with a glass rod 4-6 mm in diameter at not more than, 4 rev/s
making no deliberate attempt to break up any lumps. Transfer the
slurry to the graduated cylinder. Wash any residue in the beaker with
small quantities of standard hard water at 30 ± 1°C. Transfer the
washings to the cylinder. Fill the cylinder to the 250-ml mark with
standard hard water at 30 ± 1°C _ Close the cylinder with the stopper
and invert it sharply through 30 complete cycles within one minute,
thermalJy insulating the cylinder from the hands to maintain the
temperature of the contents at 30 ± IQC during the operation. Allow the
cylinder to stand at rest for 30 minutes in a waterbath maintained at
30 ± 1°C.. (The bench on which the cylinder is placed should be
protected from vibrations. ) At the end of the settling period ( 30 minutes),
dip the nozzle of the glass tube into the supernatant liquid contained in
the cylinder and withdraw nine-tenths ( 225 rnl ) of the suspension within
10 to 15 seconds, using the vacuum pump_ During its withdrawal, the
suspension should be disturbed as little as possible, which could be
achieved by maintaining the nozzle of the glass tube just below the
sinking top level of the suspension. Discard the suspension so withdrawn.
The sediment at the bottorn of the cylinder shall not exceed 25 rnl,
NOT. - Should "'XCf~l,ive flocculation occur during the rest, tbe material shall
be deemed unsatisfactory. Excessive flocculation in this context means either
curdling up of the suspension in the entire column or the appearance of the
transparent liquid accompanied by total or partial curdling up.

16
 IS ,6940 -1982
11.2.3.3 Proceed with the retained one-tenth of the suspension.
including the sediment for the determination of active ingredient in
accordance with the guidelines given in Appendix A.
11.2.4 Calculation

S uspensiibili
I uv, percent
b y mass = 1 000 (M
-----9 - m)
M---
where
M .= 1l1aSS in g of pesticide present in the material taken for
the preparation of the suspension (see 11.2.3.2), and
m = mass in g of pesticide found in the suspension including
the sediment remaining in the graduated cylinder
( see 11.2.3.3 ).

11.3 Acidity or Alkalinity Test

11.3.1 Qpalitalil'c Test
11.3.1.1 Procedure - Take about 0'5 g of the material in a test-tube
and mix with about I ml of water. Test the mixture for acidity or
alkalinity with a litmus paper. Determine the acidity (see 11.3.2) or
the alkalinity (see 11.3.3 ), as the case may be.
11.3.2 Determination oj Acidity
11.3.2.1 Reagents
a) Methyl red indicator solution-aqueous - one percent ( mlu ).
b) Bromocresol purple indicator solution - one percent (m/v) in ethyl
alcohol.
c) Standard sodium hydruxide solution - 0·05 N.
d) Standard hydrochloric acid - 0·05 N.

11.3.2.2 Procedure - Weigh accurately 10·0 g of the material into a

dry conical flask, add ~5 ml of acetone and mix. Warm the flask gently
to effect the solution of the active ingredient present. Add 75 ml of
water and let it stand for an hour. Filter the supernatant aqueous
extract and take 50 ml filtrate. Titrate immediately with the standard
sodium hydroxide solution using methyl red or bromocresol purple as the
indicator. Alternatively, the end point may be determined electro-
metrically ( see 13.5.4 ).
Carry out a blank determination on an aliquot of 50 ml made from
25 ml acetone and 75 ml water.
17
IS : 6HO· 1982
11.3.2.3 Calculation

Acidity ( as H.SO, ), percent by mass -= 4'9 X 2( Y- 1I ) N

M
where
v = volume in ml of the standard sodium hydroxide
. solution required for the test with the material,
v = volumeinml of the standard sodium hydroxide solution
required for the blank determination,
}I = normality of the standard sodium hydroxide solution,
and
M = mass in g of the material taken for the test.

In case the blank shows alkaline reaction, neutralize with the

standard hydrochloric acid and calculate the acidity as follows:
. . ( as H 2 SO"percent
Acidity ) b y mass - _.. X._... 2 ( VM», + vN2 )
= 4-9
where
v = volume in ml of the standard sodium hydroxide
solution required for the test with the material,
NI = normality of the standard sodiurn hydroxide solution,
v a::z volume in ml of the standard hydrochloric acid
required for the blank determination,
N. = normality of the standard hydrochloric acid, and
M = mass in g of the material taken for the test.

11.3.3 Determination of Alkalinity

11.3.3.1 Reagents
a) Methyl red indicater solution - aqueous, one percent ( mlo ).
b) Bromocresol purple indicator solution - one percent (mlv) in
ethyl alcohol.
c) Standard hydrochloric acid - 0·05 N.
d) S'andard sodium hydroxide solution - 0·05 N.

11.3.3.2 Procedure - Weigh accurately 10·0 g of the material into a

dry conical flask, add 25 ml of acetone and mix. Warm the flask gently
to effect the solution of the active ingredient present, Add 75 ml of

18
 IS I 6HO • 1982
water and let it stand for an hour. Filter the supernatant aqueous extract
and take 50 ml of filterate, Titrate immediately with the standard
hydrochloric acid using methyl red or bromocresol indicator as the
indicator. Alternatively, the end point may be determined electro-
metrically ( see 13.5.4)
Carry out a blank determination on 50 ml aliquot made from 25 ml
acetone and 75 ml water.

11.3.3.3 Calculation
. . 4·0 X 2 ( V - v) N
Alkalinity (as NaOH ), percent by mass = ~--- kl - - -

where
v ~ volume in rot of the standard hydrochloric acid
required for the test with the material,
v = volurne in fill of the standard hydrochloric acid
required for the blank determination,
N = normality of the standard hydrochloric acid, and
M = mass in g of the material taken for the test.

In case the blank shows acid reaction, neutralize with the standard
sodium hydroxide solution and calculate the alkalinity as follows:

Alkalinity ( as NaOH), percent by mass = 4·0 X 2 ( VNl

M
+ »x;)
where
v= volume in ml of the standard hydrochloric acid
required for the test with the material,
Xl = normality of the standard hydrochloric acid,
v == volume in ml of the standard sodium hydroxide
solution required for the blank determination,
N 2 = normality of the standard sodium hydroxide 101utioD.
and
M == mass in g of the material taken for the test.

11.4 Wettability Test

11.4.1 Apparatus

11.4.1.1 Beeker - See 11.1.1.1.

19
IS : 6940 • 1982
11.4.2 Procedure - Weigh accurately about 2 g of the material and pour
uniformly and quickly in the beaker containing 100 ml of the standard
hard water (see 11.2.2.1). Start the slop-watch simultaneously, Note
the time when the whole material is completely submerged into the
water.
12. METHODS OF TE'ST FOR DUSTING POWDERS
12.1 Test for Sieving Requiremeat for Particle Size
12.1.1 Apparatus
12.1.1.1 Test sieve - See 11.1.1.3.
12.1.2 Procedure
12.1.2.1 Dustingpowders - Weigh accurately 10·0 g of the material
and transfer it to the test sieve. Cover the sieve and screen the material
in a Ro-Tap or a. similar .'machine for 20 minutes, Two small square
rubber cubes are introduced along with the material on the sieve to
facilitate the breaking-up of any soft -lumps of the caked material. After
20 minutes stop the machine and brush the residue On the sieve into a
tared weighing dish. Weigh the dish and determine the mass of the
residue.
12.1.2.2 Granules - Weigh 100 g of the material and transfer to a
deck of sieves consisting of sieves of upper declared limit, lower declared
limit and a receiver. Screen for 15 minutes, Collect separately the fractions
retained on sieves. Weigh separately 'fractions retained on the sieve of
upper declared-limit and collected in the receiver. Determine the oversize
retained on the sieve of upperdeclared limit and that passing through the
sieve of lower declared limit.
12.1.3 CalcullJtiorl
Material passing through specified
m \
IS Sieve, percent by mass =1OOI- M
( )
where
m = mass in g of the material retained on the- test sieve, and
M = mass in g of the material taken for the test.
12.2 Test for Balk DeDliity After Compacting
12.2.1 Apparatus
12.2.1.1 Graduatedcylinder - of 100 ml capacity (Jee IS: 878·1975- ,
with internal diameter of 27 to 29 mm,

·Specification for graduated measuring cylinden (fi,,' ""ilM,.).

20
 IS : 69~ • 1982
12.2.1.2 Funnel - wide and short-stemmed.

12.2.2 Procedure
12.2.2.1 Bulk density before compacting - Rest the funnel over the top
edge of the tared graduated cylinder. Fill the cylinder to the lOO-ml
mark by pouring the material through the funnel, without tapping, and
level the powder with the minimum of disturbance. Leave the cylinder
untouched for 5 minutes and add tnorepowder if necessary, to bring the
contents to the IOO-rol mark, level again with the minirnum of
disturbance. Weigh the filled cylinder and calculate the bulk density
before compacting (Inass of the material/volume occupied by the
material ).

12.2.2.2 Bulk density after (rJlnpncling - Stopper the filled cylinder

(Str. 12.2.2.1 ), and drop it 20 times through a height of 15 em on to a
felt pad resting on a hard surface. Note the volume of the material after
compacting, Calculate the bulk density of the material after
compacting ( mass of the material/volume occupied by the material after
compacting ).

12.2.3 Test Eraluation - The value obtained in 12.2.2.2 shall not

exceed the value obtained in 12.2.2.1 by more than 60 percent.

12.3 Test for Acidity or Alkalinity- The test for acidity or alkalinity
determination shall be conducted on the same lines as given under 11.3.

13. METHODS OF TEST FOR EMULSIFIABLE CONCENTRATES

WATER SOLUBLE CONCENTRATES

13.1 Cold Test

13.1.1 Procedure --- Ta ke!)O m I of t he material in a lOO-lnl transparent
glass container and close it with a cork or stopper fitted with the thermo-
meter. Cool the material to 10°C (Sf.t~ Note) by placing the container
in ice cold water. \Vhen the temperature of the material in the container
reaches 1OO(~J add to it a small seeding crystal of the pesticide with
minimum opening of the stopper within the shortest possible duration of
time. In case the formulation has boon prepared from technical liquid
pesticides, there is no need to seed with crystal. Gently stir. the material
in the container at short intervals for one hour maintaining the
temperature of the material at 100(~. At the pod of one· hour, examine
the material for any turbidity or separated solid or oily matter or both.
NOTE - In case the purchaser spl.Jlritl,·s that the rest is required to he carried out
at ooe, the material in a containvr shall be cooled to O'JC by placiug the container in
a bath of crushed ice and the tvst carried out at O°C instead of 10°C.

21
IS , 6"0 • 1982
13.2 Flash PoiDt (Abel) - When determined by the method as
prescribed in IS : 1448 [P : 20 ]-1960·, the flash point of the material shall
be above 24·5~C.

13.3 Test for Em.l.joB Stability

13.3.1 Methods - Two methods are prescribed for the determination of
emulsion stability of the material. The method to be ernployed shall
depend upon the manufacturer's instructions for the preparation of the
diluted emulsion from the material. Method 1 shall be employed for
material which is required to be added to standard hard water for the
preparation of the diluted emulsion, while Method 2 shall be employed
for material to which standard hard water should be added to prepare
the diluted emulsion,

13.3.2 Melhod 1
13.3.2.1 Apparatus
a) Beaker - capacity 250 ml, with an internal diameter of 6-0 to
6-S em and marked at 100 ml,
b) Mohr-type pipett«,
c) Glass-rod - 4 to 6 mm in diameter and of a convenient length,
and
d) Graduated cylinder - capacity 100 ml,
13.3.2.2 Reagent
a) Standard hard water - See 11.2.2.1.
13.3.2.3 Procedure - Pour 75 to 80 ml of standard hard water,
brought to a temperature of 30 ± 1°C, in the beaker. By means of the
pipette add 5 ml of the concentrate if meant for public health use and
2 rnl of the concentrate if meant for agricultural use, while stirring with
a glass rod, at about 4 tevl«. The concentrate should be added to water
at the rate of 25 to 30 mIl min, with the point of the pipette 2 em inside the
beaker, the flow of the concentrate being directed towards the centre, and
not against the sides of the beaker. Make up to 100 ml with water with
continuous stirring and immediately pour into the clean and dry cylinder.
The stirring time should be 3 minutes from the beginning of the addition
of the concentrate until the emulsion is poured into the IOO-ml cylinder.
Keep at 30 ± 1°0 for one hour and examine for any creaming or
separation.

• Methods of test for petroleum and its products: P: 20 Flash point by Abel
apparatus,

22
 IS 1"40 • 1'82
13.3.2.4 Report- Report the total volume in ml of the creamed
matter at the top and the sediment at the bottom in the cylinder.
13.3.3 Method 2
13.3.3.1 Apparatus
a) Beaker - Set 11.1.1.1,
b) Dropping funnel,
c) Glass rod - See 13.3.2.1 (c), and
d) Graduated cylinder - See 13.3.2.1 (d).
13.3.3.2 Reagen:
a) Standard hard water - See 11.2.2.1.
13.3.3.3 Procedure - Take 5 ml of concentrate if meant for public
health use and 2 ml of concentrate if meant for agricultural use. Pour
standard hard water at 30 ± 1Q(~ into t.he droping funnel, and a.dd it to
the mat.erial contained in the beaker at the rate of 15 to 20 mljmin,
During the audition, stir the contents of the beaker continuously with the
glass rod, and stop the addition of standard hard water just when the
volume of diluted emulsion in the beaker reaches 100 ml. Transfer the
diluted emulsion immediately to the clean and dry graduated cylinder.
Keep the cylinder with its contents at 30 ± 10(~ for one hour. After this
period} note the volume of the creamed matter at the top and the sediment
at the bottom, if any.
13.3.3.4 Report - Report the total volume in ml of the creamed
matter at the top and the sediment at the bottom in the cylinder.

13.4 Test for Ileat StabIlity

13.4.1 A1P1Jarat lls
13.4.1.1 Glass bottle -- of convenient size, with all air-tight glass
stopper.
13.4.1.2 Thermostat - capable of maintaining the temperature
at 54 ± 1°C.
13.4.2 Procedure
13.4.2.1 Pour the material into the glass bottle until it is about three-
fourths full. Stopper the bottle and seal it air-tight with sealing wax to
avoid any loss of the volatile solvent. Place the filled bottle in the
thermostat maintained at 54 ± 1O(~ for 24 hours. Remove the bottle from
the thermostat after 24 hours and cool its contents to rOOtH temperature.

23
IS : 6940 • 1982

13.4.2.2 Test the treated material for compliance with the

requirements of cold test. flash-point test and emulsion-stability test.
NOTE - This test is done on emulsifiable concentrates of certain pelticidea only.

13.5 Acidity or Alkalinity Test

13.5.1 OJlalitative Test
13.5.1.1 Procedure - Take about 0'5 ml of the material in a test tube
and mix with about one millilitre of water. Test the mixture for acidity
or alkalinity with a litmus paper. Determine, as the case may be, the
acidity (see 13.5.2 ) or the alkalinity ( see 13.5.3 ).
13.5.2 Determination of Acidity
13.5.2.1 Reagents
a) Metlryl red indicator solution - aq ueous one percent ( nl/v).
b) Bromocresol purple indicator solution- one percent (mIl) in ethyl
alcohol.
c) Standard sodium hydroxide solution -_... 0'05 N.
d) Standard hydrochloric acid - 0'05 N.

13.5.2.2 Procedure - Weigh accurately about 10 g of the material into

a dry conical flask and dilute with 100 ml of water. Titrate the contents
of the flask immediately with the standard sodium hydroxide solution
using methyl red or bromocresol. purple as the indicator. Alternatively,
the end-point may be determined potentiometrically (see 13.5.4 ).
Carry out a blank determination on 100 ml of water.

13.5.2.3 Calculation

Acidity ( as H 2S04 ), 4'9 ( V - v) N

percent by mass = ---kJ--

where
v= volume in ml of the standard sodium hydroxide solution
required for the test,
v = volume in ml of the standard sodium hydroxide solution
required for the blank determination,
N = normality of the standard sodium hydroxide solution,
and
M = mass in g of the material taken for the test.

24
 II. 6MO • 1982
In cue the blank determination shows alkaline reaction, neutralize
with the standard hydrochloric acid and calculate the acidity as follows:
Acidity ( as H.SO, ).
percent by mass =
4·9 ( V N
M+ D eM )
t

where
v = volume in ml of the standard sodium hydroxide IOlutioD
required for the teat,
NI - normality of the standard sodium hydroxide solution,
v = volume in ml of the standard hydrochloric acid required
for the blank determination,
N I = normality of the standard hydrochloric acid, and
M :::::I mass in g of the material taken for the test.

13.5.3 Determination of AlkalinitJ

13.5.3.1 Rlagents
a) Methyl red indicator solution - Aqueous one percent ( mil) ).
b) Bromocresol purple indicator solution - One percent (mlv) in ethYl
alcohol.
c) Standard hydrochloric acid - 0·05 N.
d) Standard sodium h7droxidt solution - 0·05 N.
13.5.3.2 Procedure - Weigh accurately about 10 g of the material into
a dry conical flask and dilute with 100 ml of water. Titrate the contents
of the flask immediately with the standard hydrochloric acid, using
methyl red or bromocresol as the indicator. Alternatively, the end-point
may be determined potentiometrically.
Carry out a blank determination with 100 ml of water.
13.5.3.3 Calculation
Alkalinity ( as NaOH ), 4·0 ( Y - v ) N
percent by mass M
where
V = volume in ml of the standard hydrochloric acid
required for the test,
v .. volume in ml of the standard hydrochloric acid
required for the blank determination,
25
IS ~ 6MO • 1912
N normality of the standard hydrechlerlc acid, and
at

M =- mass in g of the material taken for the test.

In case the blank determination showl an acid reacnen, neutralize
with the standard sodium hydroxide solution and calculate the alkalinity
as follows:
Alkalinity (as NaOH), 4·0 ( VNJ + vN.)
percent by mass - M
where
Y == volume in ml of the standarcl hydrochloric acid for the
test,
Nl -= 'Dormality of the standard hydrochloric acid,
v ... volume in 'ml of the standard sodium hydroxide
solution required for the blank determination,
NI = normality of the standard sodium hydroxide solution,
and
M == mass in g of the material taken for the telt..

13.5.4 Electrometric Procedure for Determmauo« ofAcidity or Alkalinity

63.5.4.1 Rtagents
a) Buffer-solutiora- Mix acetic acid ('100 ml of 2 N solution) and
sodium hydroxide (100 ml of IN solution) and make up to
one litre with demineralized water.
b) Acetone - distilled.
c) Sodium hJdroxide - 0·05 N.
d) HJdrochloric «id - 0-05 N.
13.5.4.2 Apparatus
a) pH meter.

13.5.4.3 Procedure>« Determine the apparent pH, at 20°0. of a

mixture of the acetone (50 ml) and buffer solution (5 ml ), with the
electrodes and pH meter to be used in the titration. Transfer 10 g of the
sample to the conical flask. Add acetone ( 75 ml ) and stir for 5. minutet.
Filter through a Buchner funnel into the filter flask. Rinse the conical
flask and the Buchner funnel with acetone (4 X 5 ml ), Transfer the
combined acetone extracts to the titration vessel rinsing the filter flask
with acetone ~ 5 ml ). Add distilled water (10 ml) and titrate
electrometrically with IOdium hy~roxide lolution or hydrochloric acid to
26
 IS I 6940 • 1982
the apparent pH of acetone/buffer mixture at 20°C. Calculate the acidity
or alkalinity whatsoever by the factor given in 13.5.2.3 or 13.5.3.3.

14. METHODS OF TEST FOR GRANULES

14.1 EDcapsalatioD
14.1.1 Attrition Test
14.1.1.1 Procedure - Take 100 g of the material and sieve it for 6
hours in 75-micron IS Sieve [sec IS : 460 (Part I )-1978* ] in a ro-tap
machine.
14.1.1.2 Collect the residue from the test sieve and determine its
active ingredient by the method prescribed in the relevant Indian
Standard.

14.1.2 Wattr Run-Off Test

14.1.2.1 Procedure - Take 10 g of the material in a 100 ml capacity
burette plugged with cotton/glass wool at the bottom and add 50 ml
water. Keep it for 15 minutes. Drain off the water after 15 minutes.
14.1.2.2 Determine active ingredient in the drained water so collected
( see 14.1.2.1 ) by the method prescribed in the relevant Indian Standard.

14.1.3 Wet Test for Encapsulation

14.1.3.1 Reagents
a) Solvent same as used for the determination of active ingredient,
b) Sodium sulphate - anhydrous.
14.1.3.2 Apparatus
a) Wide mouth bottle- 15 cm in length and 11 em in diameter.
b) Roller pot mill
c) Cloth piece - 30 X 15 CIn. Grey medium-B.

14.1.3.3 Procedure - Moisten the cloth piece with 6 ml water and

place it in the glass bottle. Place 100 g of the material in it and close
the bottle. Rotate the bottle on a roller mill at 50 RPM for two and a
half hours. Take out the cloth and remove all granules adhering to the
cloth by jerking the cloth. Place the cloth piece in a 250-ml beaker.
Add 100 ml methylene chloride or any other specified solvent into the
beaker and let it stand for 30 minutes, then swirl the cloth piece with the

·Specification for teat sieves: Part I Wire cloth test sieves ( secondrevision).

27
IS : 6940 • 1982
help of a glass rod and decant the extract through a bed of anhydrous
sodium sulphate contained in a funnel fitted with a cotton plug. into a clean
250-ml round bottom flask. Wash the cloth twice with 50-ml portions
of methylene chloride each time and decant the washings through the
same sodium sulphate bed into the same flask. Add one drop of diethylene
glycol and attach the ftask to a rotary vacuum evaporator with vacuum
pre-set at 50 mm of Hg, Immerse the flask in a 45°0 waterbath and strip
the solvent to complete dryness. Add 2 ml of specified solvent to the flask
and swirl to effect complete dissolution. Transfer the contents of the flask
to a 10-ml volumetric flask and rinse the flask repeatedly with small
portions of specified solvent. Transfer washings to the same lO-ml
volumetric flask and make up the volume. Determine the active content
in this solution by the method prescribed in the relevant Indian
Standard.

14.1.3.4 Calculation
. M X 10
1 M·-
Active content released. percent by mass = __
I
where
M1 = concentration of active content in solution, and
M. = active content in granules.
14.1.4 Liquid Holding Capacity ( LHC )
14.1.4.1 Principle - This characteristic determines the maximum
loading of a technical formulation that can be put on a given type
of blank granule.
14.1.4.2 Procedure - Make up a mixture of heavy aromatic naphtha
and cyclohexanone to a relative density of 1·000 ( alternatively a mixture
of monochlorobenzene and xylene can be used). Fill this mixture of
organic solvents in a .burette.
Take 20 g of sample in a 250-ml bottle. Add solvent mixture from
burette drop by drop, into the centre of the sample, shake the bottle.
Continue to add solvent. shaking the bottle till some particles of the sample
begin to stick on the sides of the bottle.

14.1.4.3 Calculation
Liquid holding capacity, M
percent by mass M1 + M X 100
where
M = mass of solvent, in g, used; and
M1 =:II mass of blank granules taken for the tesL

28
 APPENDIX A
( Clauses 11.1 and] 1.2)
ACCELERATED STORAGE, CONCENTRATIONS OF ACTIVE INGREDIENTS REQ,UlRED
FOR SUSPENSIBILITY AND TREATMENT OF SUSPENSION INCLUDING SEDIMENT

51.. FORMULATION CONCENTRATION SUSPENSI3ILITY/ TREATMENT OF SUSPE~SION AND SEDIMENT

No. SIEVING TEST

( 1) (2) (3) (4) (5)

i) BHC \VDP 0·5 percent After accelerat- Shake vigorously the remaining one tenth
gamma m]o ed storage at suspension including sediment with
54 ± l°e for sufficient acetone. Make the volume to
I\j
24 hours 250 ml. Take a suitable aliquot and
<.0 determine the active ingredient by the
hydrolysable chlorine method prescribed
in ..A ppendix A of IS : 561:-1978.

ii) Carbaryl \\TDP 0·5 percent m]o After accelerat- Shake vigorously the remaining one tenth
ed storage at suspension including sediment with
54 ± 1°C for sufficient methanol and make up the
24 hours volume to 250 ml in the suspensibilitv
cylinder. Take a suitable aliquot for the
determination of active content by the
method prescribed in Appendix A of ;;
IS : 7121-1973.
I
iii) Carbendazim 0-5 percent mlo After accelerat- Filter the sediment including suspension a
\\tDP ed storage at using distilled water. Dissolve the sediment •
54 ± 1°C for in a mixture of acetic acid and acetic
24 hours anhydride (90: 10), making the volume i
 to 100 ml using same mixture. Take fIJ
suitable aliquot in a ground-glass flask and
stopper it. Reflux on a water ba th for 10 ~
'0
minutes and then proceed by the method as Q
-..
prescribed in Appendix A of IS : 841-6-1975. I

iv) Copper oxychlo- 0·5 percent ml» Without pre-"] Transfer quantitatively the remaining
...co
CD
ride WDP treatment I suspension and sediment to an Erlenmeyer N

~ flask and determine the active ingredient

v) Cuprous-oxide 0·5 percent mlo \Vithout pre- f by the method prescribed in Appendix A of
\VDP treatment J IS : 1506-1977.
vi) DDT \\tDP 2·5 percent m.u After accelerat- Shake vigorously the remaining one tenth
ed storage at suspension including sediment with sufficient
54 ± loe acetone and make the volume to 250 ml,
Take suitable aliquot and determine the
tJ:) active ingredient content by the method
o prescribed in Appendix A of IS : 565·1975.
vii) Diazinon lVDP 0·5 percent mlo After accelerat- Transfer the retained one tenth of
ed storage at suspension including sediment, to a 250 rnl
54 ± I~C for separating funnel. Rinse the cylinder
24 hours twice with 50 ml portions of petroleum
ether (b.p. 40·60°C), adding the rinsings
to separating funnel. Shake and drain the
aqueous layer into a second 250 ml
separating funnel. Add to the second
separating funnel 100 ml of light petroleum
and 10 ml of saturated sodium chloride
solution and shake again. Let the phases
separate and then discard the aqueous
phase. Combine the petroleum ether
extracts and then proceed as per Appendix A
of IS : 2862-1964.
 viii) Endosulfan 0·25 percent m]» After accelerat- Transfer the suspension including sediment
\VDP ed storage at to the reaction flask. Wash the cylinder
54 ± r-c thrice with methanol using a quantity of
not more than 100 ml, and then determine
the active ingredient content by the method
prescribed in Appendix A of IS: 4324-
1967.

ix) Malathion 2·5 percent m.v After accelerat- Instead of 250 ml suspension 100 ml
\\rDP ed storage at suspension is prepared. After 30 minutes
90 ± 2°C 25 ml aliquot is withdrawn from the level
of 50 rnl, Malathion content is determined
in this aliquot. Details of the procedure are
given in Amendment No. 2 issued to
IS : 2569-1978.
~
~

x) ~Iancozeb O· 5 percent ml» After accelerat- Transfer quantitatively the retained one
\VDP ed storage at tenth portion of suspension including
54 ± loe for sediment to a reaction flask, wash the
24 hours cylinder with minimum quantity of water
and add washings to the reaction flask.
Proceed for the determination of active
ingredient content by the method prescrib-
ed in Appendix A of IS : 8707-1978.
;
xi) Sulphur wet- O·5 percent mlu After accelerat- Transfer the remaining one tenth suspension
table powder ed storage at including sediment, quantitatively, using
54 ± l°C for the minimum amount of water, to a 300-ml =
~
24 hours conical flask and determine the active •
ingredient content by the method prescrib-
.-
ed in Appendix A of IS : 3383-1975. =:'"
 xii) Tbiram WDP 0-5 percent m'» After aecelerat- Transfer the remaining one tenth suspension CIJ
ed storage at including sediment, quantitatively, using
....
54 ± laC minimum amount of water to a reaction
flask and then determine the. active
ingredient by the method prescribed in
'i•
Appendix A of IS : 4766-1968. ...
xiii) Zineb WDP 0·5 percent m'u After accelerat- Transfer the retained one tenth suspension,
I
ed storage at including sediment, quantitatively, using
54 ± 1°C for minimum quantity of water to a reaction
24 hours flask and then proceed by the method
prescribed in Appendix A of IS : 3898-1981 .

xiv) Ziram WDP 2-5 percent ml» After accelerat- Transfer the retained one tenth suspension
ed storage at including sediment, quantitatively, using
~
34 ± i-c for minimum quantity of water to a reaction
~ 54 hours flask and determine the active ingredient
content by the method prescribed in
Appendix A of IS : 3900-1975.
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