HCL Testing Procedure PDF
HCL Testing Procedure PDF
HCL Testing Procedure PDF
REAFFIRMED
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Indian Standard
HYDROCHLORIC ACID-SPECIFICATION
( Fourth Revision)
Third Reprint MAY 2002
( Incorporating Amendment No.1)
UDe 561·419
C BIS 1997
(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."
(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
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
4
IS 265 : 1993
5
IS 265: 1993
6
IS 265 : 1993
7
IS 265 : 1993
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
9
IS 265: 1993
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
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~
12
Bureau of Indian Standards
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Enquiries relating to copyright be addressed to the Director (Publications), BIS.
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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
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This Indian Standard has been developed from Doc: No. CHD 002 ( 0107
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