HCL Testing Procedure PDF

Download as pdf or txt
Download as pdf or txt
You are on page 1of 22
At a glance
Powered by AI
The document discusses specifications for hydrochloric acid and lists several amendments to the standard. It also discusses the role of the Bureau of Indian Standards (BIS).

The document is about specifications and standards for hydrochloric acid, including limits for characteristics like total acidity. It also lists several amendments that were made to the standard over time.

Amendments 1-5 are listed on various pages and modify aspects of the specification like test procedures and limits. Amendment 2 changes a limit from 800°C to 800% 25°C for example.

इंटरनेट मानक

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 265 (1993): Hydrochloric acid [CHD 1: Inorganic


Chemicals]

“!ा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”

Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
IS 265: 1993
(Reaffirmed 1995)

REAFFIRMED

~T~~Cf~f~Cf) aT1=~ - fqfu~ 1010

(:ql~ ~U~)

Indian Standard
HYDROCHLORIC ACID-SPECIFICATION
( Fourth Revision)
Third Reprint MAY 2002
( Incorporating Amendment No.1)

UDe 561·419

C BIS 1997

BUREAU OF INDIAN STANDARDS


MANAK BHAVAN, 9 BAHADUR SHAH ZAPAR MARG
NEW DELHI 110002

June 1993 Price Group 6


AMENDMENT NO. 2 AUGUST 1998
TO
IS 265: 1993 HYDROCHLORIC ACID -
SPECIFICATION
( Fourth Revision)

( Page 4, clause B-3.2, line 1 ) - Substitute '800 % 25°C' for '800°C'.

(CHD2)
Printed at Printograph, New Delli, Ph.: 5726847
AMENDMENT NO.3 AUGUST 2001
TO
IS 265: 1993 HYDROCHLORIC ACID -
SPECIFICATION
( Fourth Revision)

(Page 6, clause B-S.2.3.1, first sentence) - Substitute the following for the
existing sentence:
'Dilute 4.00 g technical grade material (10.00 g in case of boiler water grade) to
100 ml with water.'
(Page 7, clause B-6.2.4) ~ Substitute the following for the existing:
"B-6.2.4 The limit prescribed in Table 1 shall be taken as not having been
exceeded if any; blue colour produced on treating the material as in B-6.2.3 is
discharged by the addition of not more than 'O.025ml of 0.05 N' or'O.25 ml of
0.005N' sodium thiosulphate for chemically pure grade, not more thali'O.l25 ml
of 0.0005 N' sodium thiousulphate solution in the case of boiler water grade and
not more than '0.05 ml of 0.005 N' sodium thiosulphate solution in the case of
analytical reagent grade."

Printed at Printograph, New Delli, Ph.: 5726847

(CHD2)
AMENDMENT NO. 4 JANUARY 2003
TO
IS 265: 1993 lHYDROCHLOJi:UC ACID--
SPECnnCATION
( Fourth Revision)

( Poge .I. clause 5.1.1.3. second sentence ) - Substitute the (oi lowing for
the existing:

'They shall be placed in an upright position on saw dust. straw, chalk or dry
earth and the empty surrounding space shall also be tilled with the same material
to prevent movement or they may be packed ill therrnocol packing (upro 2.:'
litre) ..

( Page 2, Table I. 51 No. (v), col 4) - Substitute 'o.no.:;- ( :;0 1'1'111) • [ov
'0.001 (iOpplllJ".

(CHD i)
Reprography Unit. BIS, New Delhi. L~jia
AMENDlvlENT NO. 5 A.UGUST 2003
'ro
IS 265: 1993 lHYDROCHLOJi:UC ACID--
SPECnnCATION
( Fourth Revision )

( Page 8, clause ;B-9.1 ) - ... Substitute the following for the existing:
'13··9.1 Take suitable quantity of material so that the test solution contains 1 to
I0 ~~g of arsenic. Evaporate on a steam bath until reduced to 15 ml, keeping the
liquid yellow by the addition, from ti111<: to time, a few drops of bromine
solution. Add 50 rnl of water and a few drops of stannous chloride
(approximately 1..5 rnl) solution "ild test arsenic by silver diethyl d.thiccarbamate
method as prescribed in IS 2.088:
(CHD I )
Reprography Unit, BIS, New Delhi. India
Acids, Alkalies and Halides Sectional Committee, CHD 002

FOREWORD

This Indian Standard (Fourth Revision) was adopted by the Bureau of Indian Standards, after the draft
finalized by the Acids, Alkalies and Halides Sectional Committee had been approved by the Chemical
Division Council.

Hydrochloric acid is used for acidification ( activation) of petroleum well, as chemical intermediate, in
ore reduction, food processing, pickling and metal cleaning, cleaning of membrane in the desalination
plants, as alcohol denaturant and in boiler water plants.
This standard was first published in 1950 and subsequently revised in 1962, 1976 and 1987. In this
revision a separate grade of hydrochloric acid used in boiler water plant has been incorporated.

A correlation table for relative density and percent by mass of hydrochloric acid has been given in
Annex A for information.
Hydrochloric acid is a hazardous chemical. Safety aspects relating to hydrochloric acid are covered in
IS 6164 : 1971 'Code of safety for hydrochloric acid'.
In the preparation of this standard, reference has been made to the following:
ISO 904-1976 Hydrochloric acid for industrial use - Determination of total acidity - Titrimetric
method ( International Organization for Standardization ).
ISO 907-1976 Hydrochloric acid for industrial use - Determination of sulphated ash - Gravi-
metric method ( International Organization for Standardization ).
ISO 908-1980 Hydrochloric acid for industrial use - Determination of oxidizing or reducing
substances content - Titrimetric method (International Organization for Standardization ).
ISO/R 909-1968 Hydrochloric acid for industrial use - Determination of iron content - 2, 2'-
bipyridyl spectrophotometric method (Tnternational Organization for Standardization ).
BS 976 : 1957 Density composition tables for aqueous solutions of hydrochloric acid (British
Standards Institution ).
BS 3993 : 1966 Specification for hydrochloric acid, commercial, Types I and 2 ( British Standards
Institution ).
For the purpose of deciding whether a particular requirement of this standard is complied with, the
final value, observed or calculated, expressing the result of a test or analysis, shall be rounded off in
accordance with IS 2 : 1960 ' Rules for rounding off numerical values ( revised) '. The number of signi-
ficant places retained in the rounded off value should be the same as that of the specified value in this
standard.
IS 265: 19~3

Indian Standard
HYDROCHLORIC ACID - SPECIFICATION
( Fourth Revision)
1 SCOPE 5 PACKING AND MAJU{ING
This standard prescribes requirements and 5.1 Packing
methods of sampling and test for hydrochloric
5.1.1 The material shall be packed in containers
acid. as agreed to between the purchaser and the
2 REFERENCES supplier, and subject to .the relevant provisions
of Red Tariff No. 18 of 1960 issued by the
The Indian Standards listed below are necessary Indian Railways Conference Association with
adjuncts to this standard: any alterations or additions made thereafter.
IS No. Title 5.1~1.1 When hydrochloric acid is supplied in
screw-stoppered stone bottles, glass carboys,
266: 1993 Sulphuric acid ( third revision) polyethylene carboys-or hard-rubber drums, the
1070 : 1992 Reagent -grade water (third containers shall be fitted with leak-proof stop-
revision) pers.
1260 Pictorial marking for handling 5.1.1.2 Hydrochloric acid of analytical reagent
(Part 1 ) : 1973 and labelling of goods (first grade shall be supplied in glass bottles or poly.
revision) ethylene containers or glass carboys fitted 'with
tight-fitting H~PE or other suitable stoppers:
2088: 1983 Methods for determination of The use of HDPE or other suitable caps over
arsenic ( second revision) the stopper is recommended.
4905 : 1968 Methods for random sampling 5.1.1.3 The bottles and jars shall be packed in
suitable pent-top packing cases. They shall be
3 GRADES placed in an upright position on saw dust, straw,
chalk or dry earth, and the empty surrounding
There shall be following four grades of hydro- space shall also be filled with the same material
chloric acid: to prevent movement. Carboys shall be packed
a) Technical grade ( Tech ), in suitable iron hampers or wooden crates, the
interspace being sufficiently stuffed with whiting
b) Chemical pure grade (CP ), kiselguhr or other non-combustible absorbent
c) Analytical reagent grade ( AR ), and material.
d) Boiler water grade ( BW ). S.2 Marking
4 REQUIREMENTS - 5.2.1 The packages shall be suitably marked in
4.1 Description red letters not less than 25 mm high showing
the name of the acid; indication of the source of
4.1.1 Technical Grade and Boiler Water Grade manufacture; and the'grade and mass of the
The material shall be a clear, colourless or light material. They shall prominently display the
yellow liquid free from dirt and other visible words 'CORROSSIVE, HANDLE WITH CARE'.
impurities. 5.2.2 In case of analytical reagent grade, tae
actual analysis of the material with resp-ect to
4.1.2 Chemically Pure and Analytical Reagent the characteristics laid down. in col 6 of Table-I
Grade 'shall also appear on the label.
The material shall be a colourless fuming liquid 5.2.3 The packages shall be labelled as shown
free from dirt and other visible impurities. in Fi~. 15 ofIS 1260 ( Part 1 ) : 1973.
4.2 The material 'shall also complY' with the 6 SAMPLING
requirements given in Table 1 when tested
according to the methods prescribed in Representative sample of the material ~hall be
Annex a.Reference to .the relevant clause of drawn and conformity of a lot to the standard
AnnexB is' given in col 7 of Table 1. determined as prescribed in AnnexC.

1
IS 265 _: 1993

Table 1 Requirements for Hydrochloric Acid


i Clauses 4.2, 5.2.2, B-4.3.3, B-5.2.4, B-7.2.2, B-8.4, B-10.3, C-4,2, C-5.I and C-5.2 )

SINo. Characteristic Requirement, "Grade Method of Test,


,------ ------ -_ ........ _-----------_.-..... Ref to Cl No.
BW Tech CP AR in Annex B
(1) (2) (3) (4) (5) (6) (7)
i) Total acidity (as HCI ), 30'0 30'0 32'0 32'0 B-2
percent by mass, Min
ii) Residue on ignition, 0'01 0'1 0'01 00005 B-3
percent by mass. Max ( 5 ppm)
iii) Sulphates (as H2S04 ), 0'1 0'1 0'02 0'0002 B·4
percent by mass, Max ( 2 ppm)
iv) Iron (as Fe), percent 0'002 0'005 0'0001 0'00004 B-5
by mass, Max ( 20 ppm) (50 ppm) ( 1 ppm) ( 0'4 ppm)
v) Free chlorine and bro- 0'0005 0'001 0'001 00002 B-G
mine (asCl ), percent (5 ppm) ( 10 ppm) ( 10 ppm) ( 2 ppm)
by mass, Max
vi) Sulphites ( as SOs ), 0'05 0'05 0'04 0'0001 B-7
percent by mass, Max ( 1 ppm)
vii) Heavy metals ( as Pb ), 0'002 0'0005 0'000 08 B-8
percent by mass, Max ( 5 ppm) (O'S ppm)
viii) Arsenic ( as As J, per- 0'000 5 0'0002 0'000002 B-9
cent by mass, Max (5 ppm) (2 ppm) (O'02ppm)
ix) Ammonium compounds 0'0003 B·I0
( as NH4 ), percent by ( 3 ppm)
mass, Max
x) Mercury (as Hg ), ppm, 3 3 0'03 B-ll
Max

ANNEX A
( Foreword)
CORRELATION TABLE FOR RELATIVE DENSITY
AND PERCENT BY MASS OF HYDROCHLORIC ACID

Relative Density at 25°C Percent by Mass Relative Density at 25°C Percent by Mass
(I) (2) 1'095 19·9
1·000 0'6 1'100 20'8
1;005 1'6 1'105 21'8
1·010 2'6 1'1l0 22'8
1·015 3'6 HIS 23'8
1'020 4'7 1'120 24,7
1,025 5'7 I:L25 25~7
1·030 6·7 1'130 26'7
1'035 7'8 1'135 27'7
1·040 8'8 1,140 28'7
1'045 9'9 1'145 29'7
1'050 10'9 1·150 30'7
1,055 11'9 1'155 31'7
1'060 12'9 1'160 32'1
JM)65 ia-B t·~ ~
1'070 14'9 1'170 34'8
1'075 15'9 1,175 35'9
1'080 16'9 1'180 36'9
1,085 17'9 1-185 38'0
1'090 18'9 1'188 38'7
( see Note)
NOTE - This is the saturation value at 25°C.
2
IS 265: 1993

ANNEX B
( Clause 4.2 )
METHODS OF TEST FOR HYDROCHLORIC ACID

B-1 QUALITY OF REAGENTS sample to a conical flask and dilute to 100 ml with
water. If the sample was weighed in the ampoule,
B-l.l Unless specified otherwise, pure chemical place it into the conical flask containing 200
and distilled water (see IS 1070: 1992) shall ml of cold water. Stopper the flask and while
be used in tests. cooling, shake to break the ampoule containing
NOTE - 'Pure chemicals' shall mean chemicals that the test portion. Keep cooling and shaking until
do not contain impurities which affect the results of the vapours are completely absorbed. Remove
analysis. the stopper and rinse it with water, collecting
B-2 DETERMINATION OF TOTAL ACIDITY atheglass washings in the conical flask. By means of
rod, mince the fragments of the ampoule
B-2.0 Outline of the Method and in particular the capillary which may have
remained .intact inspitc of shaking. Withdraw
A known mass of the acid is carefully dissolved the glass rod and wash it with water, collecting
in water and titrated against standard alkali the washings in the conical flask.
using methyl orange indicator.
B-2.3.3 Add two drops of methyl orage indica-
B-2.1 Apparatus .tor to the solution in the beaker or flask and
B-2.1.1 Lunge-Rey Pipette titrate to the end' point with standard sodium
hydroxide solution.
Lunge~Rey pipette shall be of shape and dimen-
sions as shown in Fig. 1. If this pipette is not
available; a weighing bottle of a glass ampoule
of the type shown in Fig. 2 may be used.
B-2.2 Reagents
B-2.2.1 Standard Sodium Hydroxide Solution-
1 N.
B-2.2.2 Methyl Orange Indicator Solution
0'05 g.of methyl orange dissolved in 100 ml of
water.
B-2.3 Procedure I
I
B-2.3.1 If Lunge-Rey pipette or an ordinary 1
I
weighing bottle is used for weighing the sample, I
accurately weigh about 2 to 3 g of the material 140 I
I
in it. I
85 ii'
If a glass ampoule is used, take sufficient amount I I I
I I,
of sample in a beaker or flask. Slightly heat on I ,',
flame, the bulb of the glass ampoule, previously
weighed to the nearest 0'1 mg. Immerse the
i I
I
I
II
II
II
capillary end of the ampoule into the beaker. or I II
I I:
flask containing the test sample and ensure that I II
the bulb is filled up to about two-thirds of its I II
volume during cooling (2 to 3 ml approxi- I ::
I I'
mately). Withdraw the ampoule and carefully I I'
I
wipe the capillary end with filter paper. Seal
the capillary end in an oxidizing flame without
loss of glass. Remove the glass ampoule from
the flame and allow to cool. Wash the capillary
1llRtwipeccaref'utly with filter 'paper. weigfi the
ampoule to the nearest 0'1 mg and calculate
by difference the mass of the test portion.
)3-2.3.2 If the sample was weighed in the Lunge- All.dimensiona.in.millimetres,
Rey pipette or weighing bottle, transfer the FIG. 1 LUNGE-REY PIPETTE

3
IS 265: 1993

ter,nperature, add 1 ml of concentrated sulphuric


acid and heat to dryness. Place the dish con-
taining the residue in an electric furnace at
800 ± SoC and keep at this temperature for
about IS minutes. Remove the dish from the
furnace, cool in a desiccator and weigh. Repeat
the heating, cooling and weighing to constant
mass.
B-3.3 Calculation
Residueon ignition,
percent by mass
where
M] = mass in g of the residue, and
M2 = mass in g of the sample taken for the
test.
B-4 DETERMINATION OF SULPHATES
B-4.0 Outline the Method
The sulphate in acid is precipitated as barium
sulphate, dried and weighed.
B-4.1 For Technical and Boiler Water Grades
FIG. 2 SPHERICAL GLASS AMPOULE B-4.1.1 Reagents
B-4.1.1.1 Sodium carbonate - analytical reagent
B-2.4 Calculation grade. .
Total acidity (as HCl ), v x Nx 3'646 B-4.1.1.2 Barium chloride solution - approxima-
percent by mass tely 10 percent ( m]» ).
M
where B-4.1.2 Procedure
V = volume in ml of standard sodium Weigh to the nearest 0'01 g about 10 g of the.
hydroxide solution used in titration, material (M]) in a porcelain dish; add 0'5 g of
sodium. carbonate and evaporate to dryness.
N = normality of standard sodium hydro- Moisten the residue with about 1'00 g of the
xide solution, and material accurately weighed (M2) , add 200 ml of
M = mass in g of the sample taken for the boiling water and filter, if necessary. Bring the
test. contents to boil over a low flame and add
slowly, with stirring, 5 ml of hot barium chlo-
B-3 DETERMINATION OF RESIDUE ON ride solution. Boil the contents for 2 minutes
IGNITION and allow the precipitate to settle for 4 hours.
Filter the supernatant liquid through a tared
B-3.0 Outline of the Method sintered glass crucible ('G No.4) or a tared
Gooch crucible and transfer the precipitate care-
A known mass of the acid is evoporated, dried, fully into the crucible. Wash thoroughly with
and the residue weighed. hot water till the washings are free from chloride.
B-3.1 Reagent Heat the crucible at 105 to 110°C to constant
mass.
B-3.1.1 Concentrated Sulphuric Acid - See
IS 266 : 1993. B4.1.3 Calculation
B-3.2 Procedure Sulphates ( as H 2S0 4 ),
percent by mass
In a platinum dish previously ignited at 800°C,
~ in a desiccator and weighed; weigh to the where
nearest 10 mg approximately lOGg of the test M = mass in g of the precipitate,
sample. Evaporate most of the acid (the final
volume should amount to about 5 to 10 ml ) by M 1 = mass in g of the sample taken for the
carefully heating the. dish containingthe test testinitially, and
portion (on a sand bath, for example) in a M 2 = mass in g of the sample added subs-
fuming cup board. Then allow to cool to room equently.

4
IS 265 : 1993

B-4.2 For Chemically Pure Grade B-5.1.2 Reagents


B-4.2.1 Reagents - as in B-4.1.1. B-5.1.2.1 Dilute hydrochloric acid - 1 N appro-
ximately.
B-4.2.2 Procedure
B_5.1.2.2 Hydroxy/ammonium chloride solution
Follow the procedure as given for technical
grade in B-4.1.2,' using about 50'0 g ?f the Dissolve' 10 g of hydroxylammonium chloride
material,' weighed to the nearest 0'01 g, Instead in water and dilute to 100 ml.
of 10 g.
Br 5.1.2.3 2, 2'-Bipyridyl solution
B-4.2.3 Calculation - calculate as in B-4.1.3.
B-4.3 For Analytical Reagent Grade Dissolve 1 gof 2, 2'-bipyridyl in 10 ml of dilute
hydrochloric acid ( 1 n) and dilute to 100 ml
B-4.3.1 Reagents with water.
B-4-3.1.1 Sodium carbonate - analytical reagent B-5.1.2.4 Standard iron solution A
grade. .
Dissolve 0·7022 g of ferrous ammonium sul-
B-4.3.1.2 Hydrochloric acid -.approximately IN, phate [ FeS04 (N H 4)2 S04.6H20] in water in a
sulphate-free. 1000-ml volumetric flask, add 4 ml of concen-
trated sulphuric acid and make up to the mark
B-4.3.1.3 Barium chloride solution - approxi- with water. One millilitre of this solution con-
mately 10 percent (m/v ). tains 0-1 mg of-iron (as Fe ).
B-4.3.1.4 Standard sulphate solution
B-5.1.2.5 Standard iron solution B
Dissolve 0·178 g of potassium sulphate in
water and make up the volume to 1000 mI. Take 100 ml of the standard iron solution A
Dilute 100mi of this. solution in a graduated ( see B-5.1.2.4) and dilute. to 1 000 J?l ~ith
flask to 1 000 ml. One rnillilitre of the diluted water in a 1 OOO-mi volumetric flask. This dilute
solution -- contains 0·01 rngvof' sulphate (as solution should be prepared fresh. One millilitre
H 2S0 4 ). of this solution contains 0'01 mg ofiron (as Fe).

B-4.3.2 Procedure B-5.1.2.6 Ammonium acetate solution


Add 20 mg of sodium carbonate to 20'00 g of Dissolve 30 g of ammonium acetate in water
thematerial and evaporate to dryness. Take up and dilute to 100 rol.
the residue with 5 ml of water and 0·5 ml of
hydrochloric acid. Filter, wash with water to B-5.1.3 Procedure
make up to 10 ml and add 1 ml of barium B-5.1.3.1 Weigh accurately about 50 g of the
chloride solution. Carry out a control test in the. sample in a platinum or silica dish (IOO-ml
same manner using 4 ml of standard sulphate capacity.), place on a boiling water bath and
solution in place of the material. Stir the two c~teft).lly evaporate to dryness. Cool, take up
solutions and compare the turbidity produced. witli 2 ml of dilute hydrochloric acid and 25 ml
B-4.3.3 The limit prescribed in Table I shall be of water, and heat to facilitate dissolution.
taken as not having been exceeded if the turbi- Transfer quantitatively to a 100-ml one-mark
dity produced with the material is not greater volumetric flask, dilute to the mark, mix and
than that produced in the control test. filter, if necessary. Transfer an aliq uot of the
sample solution containing, between 50 and
B-5 DETEMINAT{ON Of' IRON 500 fLg of iron to a lOO-mt one-mark volumetric
flask. Dilute to approximately 50 ml, if neces-
B-5.0 Two methods are prescribed. Method A sary, and then add successively 2 ml of dilute
shall be the referee method and Method B the hydrochloric acid solution, 2 ml of hydroxyl-
alternative method. ammonium chloride solution and, after 5 minu-
B-5.1 Method A ( Bipyridyl Method) tes, 5 ml of ammonium" acetate solution and
I m12, 2:-bipyridyl solution. Dilute to the mark,
B-5;1.0 Outline of the Method mix and wait for 10 minutes. Carry out the mea.
Iron is separated as coloured complex with 2,2'- surement on the spectrophotometer at a wave-
bipyridyl and estimated spectrophotometricallv, length of about 522 nm, adjusting the instrument
We Ae-f& eptieal density- using as I ere I encethe
B-5.1.1 Apparatus blank test.
B-5.1.1.1 Photometer B-5.1.3.2 Blank test
Any spectrophotometer suitable for measure- At the same time,carryout a blank test using:
ment at a wavelength of about 522 nm, or a the same procedure and quantities of all.
photoelectric absorptiometer. reagents employed in the test.

5
IS 265: 1993

B-5.1.3.3 Prepare a calibration curve by taking B-5.2.2 Reagents


the quan tities of standard iron solution indica-
ted below in a series of eleven 100-ml volumetric B-S.2.2.1 Ammonium persulphate
flasks:
B-5.2.2.2 Butanolic potassium thiocyanate solution
Volume of Standard Corresponding Mass
Iron Solution B of [ron ( Fe) Dissolve 10 g of potassium thiocyanate in 10 rnl
of water. Add sufficient n-butanol to make up
ml f-Gg to 100 ml and shake vigorously till the solution
o ( Compensation o is clear,
Solution)
R.5.2.2.3 Standard iron solution B
5'0 50
10'0 100 Take 100 ml of standard iron solution A
15'0 150 ( see B-5.1.~.4 ), add dilute potassium perrnanga.
n~te solution (0'2 percent, m/v) until a slight
20'0 200 pink colour persists after stirring and dilute to
75'0 250 the mark in a ) OOO-ml volumetric flask. This
30'0 350 dilute solution should be prepared afresh. One
millilitre of this solution contains 0'01 mg of
40'0 400 iron ( as Fe ).
45'0 450
B-5.2.3 Procedure
50'0 500
B-5.2.3.1 For technical and boiler water grades
Add to each volumetric flask an amount of
water sufficient to dilute to approximately 50 ml Dilute 1'00 g of the technical grade material
then 2 ml of dilute hydrochloric acid solution, ( 20'00 g in case of boiler water grade) to 100
2 ml of hydroxylammonium chloride solution ml with water. Transfer 10 ml of this solution to
and, after 5 minutes,S ml of ammonium acetate a Nessler cylinder, add about 30 mg of ammo-
solution and I rnl of 2,2'-bipyridyl solution. nium persulphate, boil for a few minutes, cool
Dilute to the mark, mix thoroughly and wait and add 15 ml of butanoIic potassium thiocya-
for 10 minutes. nate solution. Make up to 50 ml, shake
vigorously for about 30 seconds and allow the
B-5.1.3.4 Carry out the photometric measure- layers to separate. Carry out a control test in
ment as in B-S:l.3.1, adjusting the instrument another Nessler cylinder using the same reagents
to zero optical density using as reference the and maintaining the same total volume with 2 ml
compensation solution. Prepare a calibration dilute hydrochloric acid and 2 ml of the
curve having, for example, the iron content in standard iron solution B in place of the materiat.
micrograms per 100 ml of the standard matching Compare the intensity of the colour produced
solution as abscissa and the corresponding in the butanol layers in the two cylinders.
values of absorbance as ordinate.
B-S.1.4 Calculation B.5.2.3.2 For chemically pure grade

Iron content ( as Fe ), Weigh 50'0 g of the material and evaporate it


m X 100 x 100 almost to dryness. Dilute it to 30 ml, add about
percent by mass
V x M 30 mg of ammonium persulphate and 15 ml of
where butanolic potassium thiocyanate solution. Make
up to 50 ml, shake vigorously for about 30
m = mass in g of iron determined in the seconds and allow layers to separate. Carry out
aliquot of sample solution, a control test in another Nessler cylinder using
V = volume in ml of the sample taken for 5 ml of standard iron solution B. Compare the
colour reaction, and intensity of the colour produced in the butanol
layers in the two cylinders.
M = mass in g of the material taken for
test. B.5.2.3.3 For analytical reagent grade
B-S.2 Method B ( Thiocyanate Method ) Carry out the test as given for chemically pure
B-S.2.0 Outline of the Method grade in B.5.2.3.2, using 2 ml of the standard
iron solution B for the control test.
Iron is e.xuacfed with mnanoUG potassium
thiocyanate and estimated by comparing colori- B-5.2.4 The limit prescribed in Table 1 shall be
metrically. taken as not having been exceeded if the
B-5.2.1 ApplJr(ltu~
intensity of colour produced with the material
is not greater than tha.t produced in the control
B-5.2.1.1 Nessler cylinders - 50-ml capacity. test.

6
IS 265 : 1993

B-6 DETERMINATION OF F~EE CHLORINE Where


AND BROMINE
V = volume in ml of 0'1 sodium thiosulphate
,8-6;0 Qutline of the Meth()d solution used/ in titration (correct«d
for the/blank);
The material is shaken wirn potassium iodide
starch solution and estimated iodimetrically. m = mass iq. g of chlorine corresponding to
1 ml of 0'1 sodium thiosulphate solution
B-6.1 For Technical Grade (theoretical value, 1 ml = 0'003 55 g
B-6.1.1 Reagents
or ct j, and
M = mass in g of the test portion.
8-6.1.1.1 Potassium iodide - crystals.
B-6.2 For Boiler Water, Chemically Pure and
B-6.1.1.2 Starch solution Analytical:Reagent Grades
Make a paste of 0'5 g of starch with 2'5 ml of B·6.2.1 Apparatus
water. Pour the paste in small quantities into
200.ml of water. Boil for 15 minutes with stir- B-6.2.1.1 Microburette
ring. Preserve in small containers previously
sterilized in boiling water for 2 hours. B-6.2.2 Reagents

B-6.1.1.3 Potassium iodide solution - 10 percent. B-6.2.2.1 Cadmium iodide solution
8-6.1.1.4 Standard sodium' thiosulphate solution- Dissolve 9'2 g of cadmium' iodide in 1'00 ml of
o-i N. water.
B-6.1.2 Procedure B-6.2.2.2 Starch solution - See B-6.1.1.2.
B-6.1.2.1 Preliminary test B-6.2.2.3 Standard sodium thiosulphatesolutions :--
Place about 20 ml of the test sample in a 100-ml 0'05 Nand 0'005 N.
conical flask, add 50 ml of water, one crystal of B-6.2.3 Procedure
potassium iodide, 0'5 ml of starch solution and
stir. If a blue colour indicating iodine liberation Dilute 4 ml of the materialwith 20 ml of freshly
appears, follow the procedure prescribed boiled and cooled water. Add 1 ml of cadmium
in B-6.1.2.2 for determination of free chlorine iodide solution and 1 ml of starch solution, and
and bromine. If no colour appears, proceed for allow to stand in the dark for 10 minutes.
the determination of sulphites as in B-7. B-6.2.4 The limit prescribed in Table I shall be
B-6.1.2.2 Fill a ground grass stoppered weighing taken as not having been exceeded if any blue
bottle with test sample and take a portion of colour produced on treating the material as
approximately 50 g, weighing by difference to in B·6.2.3 is discharged by the addition of not
the nearest 10 mg. Transfer the test portion to more than 0'05 ml of 0'05 N sodium thiosulphate
.a conical flask fitted with ground glass stopper solution for chemically pure grade, not more
of capacity 500-ml containing 100 m1 .of water. than 0-125 ml of 0'005 N sodium thiosulphate
Stopper the flask and cool. Add to the conical solution in the case of boiler water grade and
flask, 10'0 ml of potassium iodide solution, not more than 0'05 nil of 0'005 N sodium thio-
stopper and flask and shake. Allow to stand for sulphate solution iJ,1 the case of analytical
2 minutes and then add 1 ml of starch solution. reagent grade.
Allow to stand for two minutes and then titrate B-7 DETERMINATION OF SULPHITES
'with standard sodium thiosulphate solution until
the blue colour disappears. B-7.0 Outline of the Method
B-6.1.2.3 Since iron may interfere in the deter- The material is shaken with standard iodine
mination, carry out a blank determination using solution and estimated iodimetrically.
100 ml of water, and adding to 'it a water-soluble
ferric iron salt equivalent to that contained in B-7.1 For Boiler Water, Technical and
50 g of the sample. Add other reagents as added Chemically ~ure Grades
to the sample. Subtract the volume 'of sodium B-7.1.1 Reagents
thiosulphate solution required for titration from
the volume required with sample ( B-6.1.2.2 )._ B-1.1.1.1 .Standard: iodine ,s()JlItt~- (}-l N.
freSh1ystandardlzed.
B-6.1.3 Calculation
B-7.1.1.2 Standard sodium thiosulphate solution-
Free chlorine and bromine 0'1 N, freshly standardized.
( as Cl ), percent by mass _ V x m x 100
M B-7.1.1.3 Starch solution - See B-6.1.1.2.

7
IS 265 : 1993

8_7.1.2 Procedure 8-8.2.4 Standard Iron Solution - See 8~5.1.2.4.

Introduce successively into a 500 ml glass stop- B-.8.2.5 Standard Lead Solution
pered conical flask 100 ml of freshly boiled- Dissolve 0'160 g of lead nitrate in water; add'
water and 10 ml of standard iodine solution. 1 ml of concentrated nitric acid and make up-
s
Add, while cooling, about 50 of the material the solution to 1000 ml. Pipette out 10 ml of
weighed to ± 0'01 g. Stopper the flask, mix and the solution and dilute again to 100 ml with
after 2 minutes titrate the excess iodine with water. One millilitre of this solution contains.
standard sodium thiosulphate solution, adding 0·0 I mg of lead (. as Pb ).
5 ml of starch solution towards the end of the
titration. B-8.2.6 Hydrogen Sulphide Gas
8-7.1.3 Calculation 8·8.3 Procedure
Sulphites ( as S02 ), 0'320 3 ( 10 - V ) Accurately weigh 2'5 g of the material in the
percent = M
case of boiler watergrade, 10 g in the case of
chemically pure grade and 50 g in the case of
where analytical reagent grade in a platinum or silica
V = volume in ml of standard sodium thio- crucible (IOO.ml capacity) and evaporate to
, sulphate solution used in titration, and dryness on a steam bath.' Dissol ve the residue
by heating to boiling ,with a mixture of 3 mt
M = mass in g of the material taken for the dilute hydrochloric acid and 10' ml of water.
test. Cool, dilute with 20 mlof water and transfer to
8-7.2 For Analytical Reagent Grade a Nessler cylinder. Add 10 mlof dilute ammo-
nia solution and.standard, iron solution equiva-
B·7.2.1 Reagents lent to the amount of iron present in 50 g of the
B-7.2.1.1 Potassium iodine solution - 10 percent sample as determined in accordance with B-5,
and make the volume to 50 ml with water. In
( m,v).
another Nessler cylinder, take 5 or 4 ml of
B-7.2.1.2 Standard iodine solution - 0'01 N. standard lead solution according as the material
is of boiler water grade, chemically pure grade
B-7.2.1.3 Starch solution - See 8-6.1.1.2. or analytical reagent grade, for control test.
B- 7.2.2 Procedure Add 3 ml of dilute acetic acid solution, the
same amount of standard iron solution as taken
To 400 ml of freshly boiled and cooled water, in the case of sample, and 10 ml of dilute,
add 1'5 ml of potassium iodide solution,S ml ammonia solution. Make the volume to 50 ml.
of hydrochloric acid and 2 ml of starch solution Pass hydrogen sulphide in both the Nessler
and titrate with 0'01 N iodine solution to a faint cylinders for a few seconds.
permanent blue colour. Add 100 g of the sample
and titrate with 0'01 N iodine solution to the B-8.4 The limit prescribed in Table 1 shallbe-
same end point. The liniit prescribed tin Table 1 taken as not having been exceeded if the
shall be taken as not having been exceeded if turbidity produced in the test with the sample-
not more than 0'25 ml of 0'01 N iodine is is not greater than that produced in the control
required for the titration. test.
B-8 DETERMINATION OF HEAVY METALS B-9 DETERMINATION OF ARSENIC
B-8.0 Outline of the Method B-9.0 Outline of the Method
The presence of heavy metals is indicated from Arsenic is extracted with silver diethyl dithio--
the turbidity formed when hydrogen sulphide is carbamate as a red complex and measured
passed through the material. spectrophotoroetrically.
B-8.1 Apparatus 8-9.1 Take a suitable quantity of the material
so that the test solution contains 1 to ro ",g of"
B-8.1.1 Nessler Cylinders - 50 ml capacity. arsenic in a final volume of 5'0 ± 0'5 ml, Deter-
mine arsenic by silver diethyl dithiocarbamate.
8-8.2 Reagents method as prescribed in IS 2088 : 1983. .
B-8.2.1 Dilute Hydrochloric Acid - 1 : 1 ( v]v ). 8-10 DETERMINATION OF AMMONIUM
B-1t.2.2 DttureAm1'fUYffti.l Solutton COMPOUNDS
Dilute 280 ml of strong ammonia solution to 8-10.0 Outline of the Method
1000 ml with water.
The material is made slightly alkaline and
B-8.2;3 Dilute Acetic Acid---'- Dilute 285ml of shaken well with Nessler's reagent and the
acetic acid to I 000 ml with water. colour developed is compared with a standard.

8
IS 26S: 1993

B-10.1 Reagents chloroform layer which is separated and discar-


ded. 500 ml of chloroform are added to the
B.10.1.1 Sodium Hydroxide Solution - 5 N, aqueous layer in the separating funnel and the
ammonia-free. solution is mixed with 6 ml of glacial acetic
B-I0.1.2 Standard Ammonium Solution acid and gradually 1 ; 1 sulphuric ,acid.is added
till the orange phase. loses its colour. The
Dissolve 2'97 g of ammonium chloride in water solution is shaken well. 'When precipitated dithi-
and dilute to I 000 mI. One millilitre of this zone dissolved in the chloroform layer, this is,
solution contains I mg of ammonium. Dilute I ml separated and filtered. The volume is made up
of this solution to 100 ml with water immedia- to 500 ml and the solution is stored in an amber
tely before use to get 0'01 mg of ammonium coloured bottle. Stability of the prepared
per mI. reagent is 10 days.
B-10.1.3 Nessler's Reagent B-11.1.1.2 Diluted dithizone
Dissolve 35 g of potassium iodide and 12'5 g of Dilute 2 ml of the concentrated dithizone
mercuric chloride in 800 ml of water and add a solution to 100 ml with chloroform (I ml <=I
saturated solution of mercuric chloride until a 1 microgram of Hg ).' Stability of this reagent is
slight permanent precipitate is produced. Then 1 day.
add 120 g of sodium hydroxide and dissolve.
Add a little more mercuric chloride solution B.11.1.1.3 EDTA ( 5 percent)
and sufficient water to make up to 1000 ml.
Shake the solution occasionally for several days; 'Dissolve 5 g of disodium salt of EDTA in 100 ml
Allow to settle and decant the clear liquid. of water.
B-I0.2 Procedure B-11.1.1.4 Potassium thiocyanate solution - 10
percent ( miv ).
Dilute 2·8 ml ( 3'3 g ) of the ma~erial to ab(;>Ut
20 m1 with water and add sodium hydroxide B-ll.1.1.5 Sodium acetate buffer ( pH 5)'
solution until alkaline to litmus paper ( about 7 Weigh 56 g of sodium acetate and dissolve in
ml is required). Dilute to 50 ml with water. water. Add 24 ml of glacial acetic acid. Make
Prepare a standard by diluting 1 ?11 of standard. up to 100 ml with water.
ammonium solution to SO ml with water. To
both solutions, add 2 ml of Nessler's reagents B-11.1.1.6 Sulphuric acid - 10 percent.
and compare after 1. minute. B-ll.1.1.7 Standard mercury solution (1 ml =
B-10.3 The limit prescribed in Table 1 shall be 1 microgram of mercury)
taken as not having been exceeded if the yellow Dissolve' 0'135 4 g of pure mercuric chloride in
colouration produced, if any, with the test water and make up to I 000 mi. 10 ml of this
material is not deeper than that of the standard. solution is further diluted to I 000 mI. I mlof
this solution contains 1 microgram of mercury.
B-11 DETERMINATION OF MERCURY
B-ll.1.1.8 Ammonia solution - 1 ; 4.
B-ll.0 Two methods have been specified, B-ll.1.1.9 Potassium permanganate solution
namely, dithizone method and mercury analyzer ( 4 percent ).
method. In case of dispute, the mercury analyzer
method shall be taken as the referee method. Dissolve 4 g of potassium permanganate in 100
ml of water.
B-l1.1 Dithizone Method 8-11.1.1,10 Hydroxylamine hydrochloride ( 2 per-
8-11.1.0 Outline of the Method cent)
Mercuric mercury forms a complex with dithi- Dissolve 2gof hydroxylamine hydrochloride in
zone in the form of orange/red colour depending' 100 ml Of water.
upon its concentration. "B;.11.1.1.1l Chloroform
B-ll.1.1 Reagents B-11.1.1.12 Glacial acetic acid
B-ll.1.1.1 Dithizone B-ll.1.2 Procedure
-Concentrated stock solution ( 25 to 30 mg) in Neutralize 10 ml of the sample with 1 ; 4 ammo-
500 ml of chloroform; 25 mg of dithizone is nia solution in a 250 ml beaker. Add 10/ml of
dissolved in 100 ml of chloroform and extracted' 10 percent sulphuric acid followed by lml of 4
with 250 ml of 2 N ammonia. Most of the dithi- percent potassium permanganate solution. Digest
zone will pass into the aqueous layer and, change the same for half an hour, cool and neutralize
colour from green to orange. The oxidation the excess potassium permanganate/with 2 per-
products and contaminants are retained in the cent hydroxylammonium chloride solution.

9
IS 265: 1993

Transfer the solution in' a 500-ml separating d) Hydroxylamine hydrochloride ~ 10 percent


funnel. Dilute to' 100 ml. Now add 10 ml of ( mJv),
sodium acetate buffer, 10 ml of 5 percent EDTA e) Nitric acid - 5 percent ( mjv ) , and
solution and 2 ml of 10 percent potassium thio-
cyanate solution. The solution is now saturated f) Potassium dichromate solution ...:..- 1 percent
with 5 ml chloroform. Drain off the organic ( mJv ).
layer. Add 5ml of glacial acetic acid and mix B-11.2.1.3 Preparation of sample solution
the solution thoroughly. Now add diluted dithi-
zone solutiop. ( 1 ml = 1 microgram of Hg) in Take 50 ml of the sample in a 100 ml standard
small quantities and extract separately till the volumetric flask. Add potassium permanganate
dithizone solution remains green in colour. solution drop-wise till the purple colour
Collect the dithizone extract and not the volume. remains, add 2 to 3 drops of concentrated nitric
By known quantities of standard mercury solu- acid. Keep it for, 5 to 10 minutes after shaking
tion, running a, blank and following the same flask. Decolourize the solution by adding
method of extraction standardized the dithizone hydroxylamine hydrochloride solution drop-
solution. wise. Make up the volume to 100 ml with
mercury free water.
B-1l.1.3 Calculation
Similarly, make the blank solution (B. S. ) by
Mercury ( as Hg ), ppm = V x N using 50 ml mercury free water instead of
10 X d
hydrochloric acid and using the same quantity
where' of reagents.
V = volume in ml of dithizone solution, B-11.2.1.4 Preparation of Standard Graph
N = strength of dithizone solution in pog, a) Preparation of stock solution
and Dissolve 0,135 4 g of mercuric chloride AR
d = relative density of hydrochloric acid. or GR grade in 25 ml of 2 percent of nitric
acid ( vJv). Add 2 ml of 1 percent ( m v)
B-11.2 Mercury Analyzer Method potassium dichromate solution of and make
up to 100 ml with 5 percent nitric acid
B-11.2.0 Outline of the Method ( v/v ).
Mercury analyzer works on the principle of cold 1 ml of this stock solution = 1 mg of Hg.
vapour atomic absorp.ion spectrometry tech-
nique .. Mercury ions are reduced to elemental
I
b) Preparation of standard solution
stateby stannous chloride and the solution is By successive dilution of the above stock
stirred vigorously so that an equilibrium is solution, prepare the standard solution Off
achieved between the mercury in solution and 1 ml = 100 nanogram of Hg, keeping 5 per-
air phase. The vapour is then purged into the cent nitric acid (vJv) and 0'10 percent
absorption cell which is located in the light potassium dichromate ( mlv ) concentration.
path of the spectrometer.. This standard solution is generally stable for
As the cold vapour absorption technique of a period of at least one month. '
mercury is based on absorption of UV radiation c) Procedure
by mercury atoms, all substances which absorb
UV radiation will cause the positive error. Using the above standard solution, find out
Vapours of organic compounds like alcohols, the transmission for 10, 20, 4Q, 60, 80, 100,
ketones, esters, and acids and water also absorb 120, 140 and 150 nanogram of mercury. By
UV radiation. These can be avoided with suit- following the procedure prescribed
.
able trap provided along with the instrument.
'

B-11.2.1 Mercury in the Chemically Pure Grade


in B-11.2.1.5, prepare the standard graph
indicating Hg in ng against absorbance.
B-11.2.1.5 Procedure
B-11.2.1.1 Apparatus
Add 8 ml of 10 percent nitric acid and 2 ml of
Mercury analyzer BC MA/S 800 A or equivalent. stannous chloride solution to the reaction vessel
B-11.2.1.2 Reagents and stir the mixture for 5 minutes. Remove the
blank transmission. Add 5 ml of prepared solu-
a) Nitric acid - 10 percent ( vjv), tion ( B-11.2.1.3 ). Volume in the reaction vessel
b) Stannous chloride - 20 g in 10 percent should not be more than 15 ml in any case. Stir
hyhrochloric acid ( m!v ), for 5 minutes and find out the transmission. This
gives 'BaCk reading' ( BR). Take the transmis-
c) Potassium 'permanganate - 1 percent sion for 5 ml of blank solution following same
( m/v), procedure. This gives 'Blank reading' (BLR )~

10
IS 265 l 1993

Difference in the two readings (BR and BLR ) ( 5 ml for boiler water grade also) and follow
corresponds..to mercury content in the sample the procedure prescribed for the preparation of
which can be obtained by referring the chart of sample solution for pure grade acid as also for
absorbance vIs mercury in nanograms. the blank solution.
B-11.2.1.6 Calculation B-11.2.2.2 Procedure
Mercury. ( as Hg ), 0'0004 X X Take 1 ml of sample solution ( B-11.2.2.1 ) and
ppm by mass follow the procedure prescribed for pure grade
rd
acid ( B-11.2.1.4 ).
where
X = mercury in nanograms for transmission B-11.2.2.3 Calculation
from the graph ( BR - BLR ), and
Mercury (as Hg ), 0'02 x X
rd = relative density ( see Annex A ). ppm by mass
rd
B_11.2.2 Mercury in Technical and Boiler Water
-Grades where
B-11.2.2.1 Preparation oj sample solution X and rd have the same significance as indi-
Take 5 ml of technical grade of the material cate in B-11.2.1.6.

ANNEX C
( Clause 6.1 )
SAMPLING OF HYDROCHI,ORIC ACID

c-iGENERAL REQUIREMENTS ON batch of manufacture shall constitute a lot. If' a


SAMPLING consignment is declared to consist of different
batches of manufacture, the batches shall'be
e-1.0 In drawing, preparing and storing test marked separately and the groups of containers
samples, the following precautions and directions in each batch shall consitute separate lots.
shall be observed.
C-2.2 Samples shall be tested from each lot
e-l.l Samples shall not be taken out in an separately for judging the conformity of the
exposed place. material to the requirements of the specification.
For this purpose, five containers shall be selected
C-1.2 The sampling instrument shall be clean at random from each lot.
and dry.
NOTE - ]f the number of containers in a lot is eight
C-1.3 Precautions shall be taken to protect the or less. the number of containers to be selected and
samples, the material being sa.mpled, the samp- the criteria for conformity of the lot to the specifica-
ling instrument and the con tamers for samples tion requirements shall be as agreed to between the
purchaser and the supplier.
from adventitious contamination.
C-2.3 The containers shall be selected at
-C-1.4 To draw repr.esentative sample, the con- random and to ensure randomness of selection,
tents of each container selected for sampling random number tables shall be used (see
shall be mixed thoroughly by rolling, shaking or IS 4905 : 1968). In case random number tables
stirring by suitable means and with necessary are not available, the following procedure may
.caution. be used:
e-1.S The samples shall be placed in suitable Starting from any container in the lot,' count-
dry and airtight glass containers. them as 1, 2, ...... , up to r, and so on.wherer
is the integral part of N ( N being the number
C-l.6 Each sample container shall be sealed of containers in the lot ). Every rth container
airtight after filling and shall be marked with thus counted shall be withdrawn to constitute
full details of sampling, the data of sampling a sample till the required number of five con-
and the year of manufacture of the material. tainers is obtained.
C-2 SCALE OF SAMPLING C-3 PREPARATION OF TEST SAMPLES
C-2.l Lot C-3.1 Sampling Tube
All containers in a single consignment of the The sampling tube shall be made of glass and
material of the same grade drawn from a single shall be 20 to 40 mm in diameter and 350 to

11
]S 265: 1993

750 nun in length (see Fig. 3 ).. . The upper and shall be divided into three equal parts, one for
lower ends are conical and reach 6 to 12 nun the purchaser, another for the supplier and the
diameter at the narrow ends. For drawing the third to be use as a referee sample.
samples, the apparatus is first closed at the top
with a thumb or a stopper and lowered till a C-3•.4 The remaining portion of the material.
desired depth is reached. It is then opened for from each container shall be divided into three
a short time to admit the material and is finally equal parts, each forming an individual sample.
closed and withdrawn. One set of individual samples representing the
five containers sampled. shall be marked for the
purchaser, another for the supplier and the
third to be used as a referee sample.
C-3.S All individual composite sample shall be
transferred to separate bottles. The bottles shall
be sealed and labelled with full identification
particulars.
C-3.6 The referee samples consisting of compo-
site sample and a set of five individual samples
shall bear the seals of the purchaser and the
supplier. They shall be kept at a place agreed to
between the purchaser and the supplier, to be
350
used in the case of a dispute between the two.
TO
750 C-4 NUMBER OF TEST
C-4.1 Total acidity shall be tested on each of
the five individual samples.
C-4.2 Test for determination of remaining
characteristics listed in Table 1 shall be perform-
ed on the composite sample.

U
C-S CRITERIA FOR CONFPRMITY
C-5.1 For Individual Sample~

For th~ five test results for total acidity, the


---U-- ~S TO 12
mean X and range R shall be computed ( range
being defined as difference between the maximum
All dimensions in millimetres. and minimum values of test results ).
FIG. 3 SAMPLING TUBB The lot shall be declared as conforming to the
requirement of total acidity if the value of the
C-3.1.1 For small containers, the size of the expression }{ - 0·6 R is greater than or equal
sampling tube may be' altered suitably. to the relevant value specified in Table 1. .
C-3.2 For each of the containers selected C-5.2 For Composite Sample
according to C-2.•3 a small representative por-
tion of the material, about 200 ml, shall be taken For declaring the conformity of the lot to the
out with the help of the sampling tube after requirements of all other characteristics tested'
thoroughly stirring the acid with the help of a on the composite sample, the test result for
glass rod; each of the characteristics shall satisfy the
relevant value specified in Table 1.
C-3.3 Out of these portions, a small but equal
quantity of the material shall be taken out and C-S.3 A lot shall be declared as conforming to
thoroughly mixed to form a composite sample, the requirements of this specification if C-5.1
not less than 600 ml. The composite .sample and C-S.2 are satisfied.

12
Bureau of Indian Standards

BIS is a statutory institution established under the Bureau of Indian Standards Act, 1986 to promote
harmonious development of the activities of standardization, marking and quality certification of goods
and attending to connected matters in the country.
Copyright

BIS has the copyright of all its publications. No part of these publications may be reproduced in any form
without the prior permission in writing of BIS. This does not preclude the free use, in the course of
implementing the standard, of necessary details, such as symbols and sizes, type or grade designations.
Enquiries relating to copyright be addressed to the Director (Publications), BIS.
Review of Indian Standards

Amendments are issued to standards as the need arises on the basis of comments. Standards are also
reviewed periodically; a standard along with amendments is reaffirmed when such review indicates that
no changes are needed; if the review indicates that changes are needed, it is taken up for revision. Users
of Indian Standards should ascertain that they are in possession of the latest amendments or edition by
referring to the latest issue of 'BIS Handbook' and 'Standards: Monthly Additions'. .

This Indian Standard has been developed from Doc: No. CHD 002 ( 0107

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

BUREAU OF INDIAN STANDARDS

Headquarters:

Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 110002 Telegrams: Manaksanstha
Telephones: 323 01 31, 323 33 75, 323 9402 (Common to all offices)

Regional Offices: Telephone

Central : Manak Bhavan, 9 Bahadur Shah Zafar Marg 3237617


NEW DELHI 110002 { 3233841

Eastern : 1/14 C. LT. Scheme VII M, V. L P. Road, Maniktola 337 8499, 337 85 61
CALCUTTA 700054 { 3378626,3379120

Northern: SCO 335-336, Sector 34-A, CHANDIGARH 160022 603843


{ 602025

Southern: C. L T. Campus, IV Cross Road, CHENNAI 600113 2350216,2350442


{ 235 15 19, 235 23 15

Western: Manakalaya, E9 MIDC, Marol,Andheri (East) 832 92 95.' 832 78 58


MUMBAI400093 { 8327891,8327892

Branches: AHMADABAD. BANGALORE. BHOPAL. BHUBANESHWAR. COIMBATORE.


FARIDABAD. GHAZIABAD. GUWAHATL HYDERABAD. JAIPUR. KANPUR.
LUCKNOW. NAGPUR. PATNA PUNE. THIRUVANANTHAPURAM.

Printed at Printograph, New Delhi (INDIA).

You might also like