Professional Documents
Culture Documents
( Second Revision )
UDC 661.842.321
... .
@ Copytipht 1984
Gr 7
June 1984
IS:1314 - 1984
Indian Standard
SPEClFICATION FOR CALCIUM CHLORIDE
( Second Revision )
Acids, Alkalis and Halides Sectional Committee, CDC 56
Chairman Represenfing
Pno~ M. M. TAQ~JI KHAN Central Salt & Marine Chemicals Research Insti-
tute ( CSIR ), Bhavnagar
Members
DR G. D. BHAT (nlternate to
Prof M. M. Taqui Khan )
SHRI S. K. BASU Dirctorate General of Supplies & Disposals, New
Delhi
SHRI D. S. CHOWDHU~Y (Alternate )
SIIRI M. L. BHAMUANI National Test House, Calcutta
SHnI R. C. RHATTACHARYA Directorate General of Technical Dcvclopmcnt,
New Delhi
SHRI H. KHAPAKDE ( Affernafe)
SHRI M. V. DESAI The Atul Products Ltd, .Itul
DR J. M. TUREL ( Alternate )
SHHI P. N. HALDAR Bengal Chemicals & Pharmaceuticals Ltd,
Calcutta
San1 R. N. BANERJEE (Alternate)
SHRI P.S. ~~ARIHARAXRISllNAK The Travancore Rayons Ltd, Rayonpuram
DR H. V. R. IEN~.U II. I. D. Parry ( India ) Ltd, Madras
DID V. C. NAIR ( Alfernafe )
SHRI N. V. KA~IULE Saurashtra Chemicals, Porbandar
SHRI L. K. MALAVIYA ( Alternafe )
SHRI MA~HOHAN SINGH Indian Paper Mills Association, Calcutta
SHKI N. K. GUPTA (dkrnate)
DR B. S. NAO.UL Indian Dyestulf Industries Ltd, Uombay
SI~RI N. R. FADSIS ( Alfernafe )
DR V. N. N~oai\r Ministry of Defence ( DC1 )
SHRI K. B. DUTTA ( Alternafe )
SHRI M. PADMANABAN The Mettur Chemical & Industrial Corporation
. Ltd, Mettur Darn
Dn ANIL PA~DIT Deepak Nitrite Ltd, Vadodara
SHRI J. T. VORA ( rihmafe )
( Confinuedon page 2 )
0 Copyrighf 1981
BUREAU OF INDIAN STANDARDS
This publication is protected under the It~dia,r Cojyrighf .4cf ( XIV of 1957) and
reproduction in whole or in part by any means cxccpt with written permission of the
publisher shall be deemed to be an infringement of copyright under the said Act.
IS : 1314- 1984
( Contit;uedftom page1 )
Members Repeseuting
Susu P. RA~AKRISHNAN The Fertilizers & Chemicals Travancore Lto,
rJdyogamauda1
SHRI V. N. RAO Tata Chemicals Ltd, Bombay
SHIU K. H. PAREKH (Alternate )
SHRI B. REVENNA Salt Commissioner, Jaipur
SHRI N. K. SACHAH Gujarat Alkalies & Chemicals Ltd, Vadodara
SHRI J. B. SHARMA (Alternate )
SHRI C. R. SANTHANAKRISHNAN Travancore Chemical & Manufacturing Co Ltd,
Mettur Dam
SHRI K. V. MANI ( Alternate )
SHRI V. S. SAXENA Ballarpur Industries Ltd, New Delhi
SHRI J. S. TALWAR ( Alternate )
Da N. SEN Indian Soap & Toiletries Makers’ Association,
Bombay
SARI S. K. SUBBAROYAN Hindustan Lever Ltd, Bombay
DR A. N. BHAT ( Alternate )
SRRI B. K. VAHI Shriram Foods & Fertilizer Industries, New
Delhi
SARI S. S. BANSAL ( Alternate )
DR M. S. VAIDYA The Dharamsi Morarji Chemical Co Ltd, Bombay
DR A. S. VAWYANATKAN Standard Alkali ( Chemicals Division), Bombay
SI~XI T. P. VENKATRAMAN ( Alternate )
SHRI H. K. VENKA+ARAMAIAH Hindustan Organic Chemicals Ltd, Rasayani
DR K. M. VRI~~IA Projects & .Development India Ltd, Sindri
SEKI S. K. MATHUR, Director General, IS1 ( Ex-ofitio Member )
Director ( Chem )
Secretary
SHRI M. BAKSHI GUPTA
As&taut Director ( Chem ), IS1
Convener
DR N. N. SHARYA Tata Chemicals Ltd, Bombay
Members
SHRI K. H. PAREKH ( Alternate to
Dr N. N. Sharma )
SHRI T. N. BALAKRISIINAN The Mettur Chemical & Industrial Corporation
Ltd, Mettur Dam
SHRI D. S. CHADHA Central Committee for Food Standards, Directorate
General of Health Services, New Delhi
SMT DEBI MCKEE RJEE ( Alternate )
SHRI M. V. DESAI The Atul Products Ltd, Atul
Da J. M. TUREL ( Alternate )
DR K; GOPAKUMAR Central Institute of Fisheries Technology, Cochin
SH~I N. V. KAMBLE Saurashtra Chemicals, Porbandar
SI~RI L. K. MALAVIYA ( Alternate )
( Continued on page 25 )
2
1s : 1314- 1984
Indian Standard .
( Second Revision)
0. FOREWORD
0.1 This Indian Standard ( Second Revision ) was adopted by the Indian
Standards Institution on 25 January 1984, after the draft finalized by the
Acids, Alkalis and Halides Sectional Committee had been approved by the
Chemical Division Council.
0.2 Calcium chloride, technical, hydrous and anhydrous were covered in
IS i 1334-1958* and IS : 1314-1958, respectively. The two standards were
amalgamated and revised in 1967 and consequently IS : 1334-1958” was
withdrawn. Analytical reagent grades for both were also added in the first
revision.
0.3 Calcium chloride, technical, is used by the refrigeration and ice manu-
facturing industries for making brine and in the chemical industry as a raw
material. It is also used for the purpose of spraying on road surfaces as an
accelerative for concrete and in curing of concrete. Magnesium compountls
are undesirable as refrigerating brines due to their sludge-forming proprr-
ties, hence in the first revisjon more stringent limits for magnesium had
been specified. Anhydrous calcium chloride, technical, is used as a
dehydrating agent in laboratory and a number of industries.
0.4 The standard has been revised once again in the light of the pro$rcss
made by the industry. In the second revision, with the addition 01 the
fused calcium chloride, three types of the material have been covered.
Three grades have been specified for the hydrous material. The two grades
which were prescribed for anhydrous material in the first revision have now
been merged into one.
0.5 This standard contains clauses 3.2 and 4.2 which permit the purchaser
to use his option for selection to suit his requirements.
0.6 For the purpose of deciding whether a particular rcquircment of this
standard is complied with, the final value, obsrrvetl or cnlculatcd, exprcs-
sing the result of a test br analysis, shall bc rounclcd off in accordance with
IS : 2-196tif. The number of significant plncc~s rctninrd in the rountl(sd OK
value should be the same as that of the spcscilictl valr~: in tllis standard.
3
IS:1314- 1984
1. SCOPE
1.1 This standard prescribes the requirements and the methods of sampl-
ing and test for calcium chloride.
2.2 Grades
2.2.1 Type A of the material, that is, hydrated calcium chloride shall
be of the following grades:
a) Grade 1 - Suitable as analytical reagent;
b) Grade 2 - Lye suitable for refrigeration and chemical industry;
und
c) Grade 3 - Suitable for use as refrigerant in ice manufacture and
as raw material in chemical industries also suitable for
use for road construction purposes, for acceleration
and curing of concrete.
3. ,REQJJIREMENTS
3.2 Size of Lumps - The size of lumps for Type B and Type C material
shall be as agreed to between the purchaser and the supplier.
3.3 The material shall als, comply with the requirements given in Table, 1
when tested in accordance with the methods prescribed in Appendix A.
References to the relevant clauses of Appendix A are given in co1 8 of
Table 1.
3.4 Rejection - The ntatcrial shall IX rcjcctcd if it becomes caked or
sticks tl) the cont:lil!c,r.c; b~f’orr* c,pc!~illc: c,ucept I;)r T>‘pc A, (;rade 3.
IS :1314 - 1984
5
IS: 1314 - 1984
4. PACKING
4.1 Type B and Type C of the material shall be packed in flakes or lumps
in moisture-proof bags or steel drums.
5.1.1 The packages may also be marked with the IS1 Certification
Mark.
NOTE - The use of the ISI Certification Mark is governed by the provisions of
the Indian Standards Institution ( Certification Marks ) Act and the Rules and
Regulations made thereunder. The IS1 Mark on products covered by an Indian
Standard conveys the assurance that they have been produced to comply with the
requirements of that standard under a well-defined system of inspection, testing and
quality control which is devised and supervised by IS1 and operated by the
producer. ISI marked products are also continuously checked by IS1 for conformity
to that standard as a further safeguard. Details of conditions under which a Iicence
for the use of the IS1 Certification Mark may be granted to manufacturers or
processors, may be obtained from the Indian Standards Institution.
6. SAMPLING
6.1 The methods for drawing representative samples of the material and
for determination of their conformity with the requirements of this standard
shall be as given in Appendix B.
APPENDIX A
( Clause 3.3; and Table I )
7
IS : 1314 - 1984
Dry the crucible along with the residue to constant mass at a temperature
of 105 to 110°C. _.
A-2.2 Calculation ,
100 A4
Matter insoluble in water, percent by mass = y
a
where
hrl, - mass in g of the residue, and
Ads = mass in g of the material taken for the test.
A-3.1 Reagents
A-3.1.1 Standard Disodium Ethylenediaminetetraacetafe ( ED TA ) Solution -
Weigh 3.72 g of disodium erhylenediaminetetraacetatc dihydrate, dissolve
in water and dilute in a graduated flask to 1 litre. Starrdardize the solution
against the standard calcium chloride solution according to the procedure
given in A-3.2.
A-3.1.2 Standard Calcium Chloride Solution -- Dissolve I.0 g of calcium
carbonate, dried at 120°C to constant mass in the minimum quantity of
concentrated hydrochloric acid ( see IS : 265-1976* ) and then make up the
volume to 1 Iitre. One millilitre of this solution is equivalent to 0~000 4 g
of calcium:
A-3.1.3 Eriochrome Black T Indicator - Dissolve 0.1 g of the material in
20 ml of rectified spirit. This solution shall be prepared fresh every w,cc.k.
A-3.1.4 Calceirz Indicator - Mix 0.01 g of calcein thoroughly with 1 g ol‘
potassium chloride.
A-3.1.5 Bugler Solufion - Dissolve 67.5 g of ammonium chloride in a
mixture of 520 ml of ammonium hydroxide ( sp gr 0.90 ) and 250 ml of
water. Dissolve a mixture of 0.93 1 g of EDTA and 0.6 16 g of magnesium
sulphate heptahydrate ( MgS047HzO) in 50 ml of water, combine both
the solutions and make up to 1 litre. Five millilitres of buffer solution
added to 50 ml of water should not consume more than one drop of ED’f.4
solution to change to distinct blue with eriochrome black T inclicator.
A-3.1 .tj Standtrrd Sodiwn &dro.zidc Solution -- 2.5 N.
-
*Specification for hydrochloric acid ( seco,~!reoision ).
8
IS:1314-1984
A-3.5 Calculation
10 000 VIA,
Calcium ( as Ca ), percent by mass = -*?-
where
9
IS z 1314 - 1984
A-4.1 Reagents
A-4.1.1 B@r Solution - same as given in A-3.1.5.
A-4.1.2 Eriochrome Black T Indicator - same as given in A-3.1.3.
A-4.1.3 Standard Disodium Ethylenediaminetetraacetate ( EDTA ) Solution -
same as given in A-3.1.1.
A-4.2 Procedure - Pipette out 10 ml of the pre&ared sample solution
( see A-3.3 ) in a 250-ml conical flask and dilute with 35 ml of water. Add
5 ml of buffer solution and 5 drops of eriochrome black T indicator.
Titrate against standard EDTA solution till the wine-red colour of the
solution changes to blue. Note the reading of the burette.
A-4.3 Calculation
6 068 ( VzA, - V,A, )
Magnesium, percent by mass = -
i@
where
vz = volume in ml of standard EDTA solution used in A-4.2,
A, = mass in g of calcium equivalent to 1 ml of standard EDTA
solution as obtained in A-3.2(a),
v, = volume in ml of standard EDTA solution used in A-3.4,
‘Al = mass in g of calcium equivalent to 1 ml of standard
EDTA solution as obtained in A-3.2(b), and
M = mass in g of the material taken- in A-3.3.
A-5.1 Reagents
10
ISr1314- 1984
A-5.3 Calculation
3.705 VJV
Alkalinity [ as Ca ( OH )s ] percent by mass = M
where
V = volume in ml of the standard hydrochloric acid used for
the titration,
.N = normality of standard hydrochloric acid, and
M= mass in g of the material taken for the test.
A-6.1 Reagents
A-6.1.1 Dilute Nitric Acid - approximately 5 N.
11
IS : 1314 - 1984
A-6.3 Calculation
3.546 ( B,- V, ) .N
Chloride ( as Cl ), percent by mass =
M
where
V, = volume in, ml of standard ammonium or potassium
thiocyanate solution required for the blank,
gB = volume in ml of standard ammonium or potassium
thiocyanate solution required for the test with the material,
.N = normality of standard ammonium or potassium thiocyanate
solution, and
hl = rnass in g of the material in the aliquot.
A-7.1 Reagents
IS:131491984
13
F
IS : 1314 - 1984
A-8.3 The limit prescribed in Table 1 shall be taken as not having been
exceeded if the colour produced with the material is not darker than that
produced with the standard nitrate solution.
A-9.1 Reagents
A-9.1.1 Methyl Red Indicator Solution - same as in A-7.1.2.
A-9.1.2 Ammonium .Hydroxide SQlution -- free from carbonate.
A-9.1.3 Concentrated Hydrochloric Acid - ( see IS : 265-1976* ).
A-9.1.4 Barium Chloride Solution - Dissolve 120 g of barium chloride
( BaCls2HsO ) in water and dilute to 1 litre.
A-9.2 Procedure - Dissolve 10.0 g of the material in 100 ml of water
and heat to boiling. Add a few drops of methyl red indicator solution,
make alkaline with ammonium hydroxide solution and boil for 5 minutes.
Filter through a small filter paper, and wash with a little hot water.
Reject the residue. Neutralize the filtrate with hydrochloric acid and
add 1 ml in excess. Determine the sulphate content as prescribed
in IS : 2317-1975t ).
A-9.3 Calculation
A-11.1 Reagents
15
IS : 1314 - 1984
A-11.3 The limit prescribed in Table 1 shall be taken as not having been
exceeded if the turbidity produced with the material is not greater than
that produced in the control test.
A-12.1 Reagents
16
IS : 1314 - 1984
A-14.1 Reagents
17
IS : 1314 - 1984
A-14.3 The limit prescribed in Table 1 shall be taken as not having been
exceeded if the colour in cylinder B is not darker than that in cylinder C.
A-15.1.1 Apparatus
A-15.1.1.1 Flame photometer - with red-sensitive photo-tube.
A-15.2.1 Apparatus
A-15.2.1.1 Sintered glass crucible - C No. 4 or Gooch crucible.
A-15.2.1.2 Ice-bath
A-15.2.2 Reagents
A-16.1 Apparatus
A-16.1.1 Flame Photometer - same as in A-15.1.1.1.
19
‘.‘
-._.- _.
__
IS : 1314 - 1984
A-16.2 Reagents
A-17.2 Reagents
20
.
IS: 1314-1984
A-17.3 Procedure
A-17.3.1 Preparation oJ Svlutiom
A-17.3.1.1 Sample solution S - To n 5-ml aliquot of solution
A ( A-10.2 ), add 1 ml of hydrochloric acid and dilute to 100 ml with
water.
A-17.3.1.2 Control solution C - To another 5-ml aliquot of solution
A ( A-10.2 ), add 10 ml of standard strontium nitrate solution and 1 ml
of hydrochloric acid, and dilute to 100 ml with water.
A-18. DETERMINATION OF pH
A-18.1 Apparatus
A-18.1.1 pH Meter - Ariy suitable pH meter equipped with a standard
calomel electrode and glass electrode. The meter shall be accurate to
0.05 PH unit in the $H range of 4.01 to 9.18.
APPENDIX B
( Clause 6.1 )
21
IS : 1314 - 1984
B-2.3 These containers shall be selected at random from the lot and in
order to ensure the randomness of selection, random number tables shall
be used. In case such tables are not available, the following procedure
may be adopted:
Starting from any container, count them in-one order as 1, 2,
3, . . . . . up to r and so on, where r is the integral part of N/n ( J1’ and
n being the lot size and sample size, respectively ). Every rth container
thus counted shall bc withdrawn to constitute the sample.
22
._--
: __. _--. .--. ~-. - ~- --~~
L^______ _.__^ -
lS:1314-19114
B-3.3 The remaining portion of the material from each container shall be
divided into three equal parts, each forming an individual sample. One
set of individual samples representin g the containers sampled shall be
marked for the purchaser, another for the supplier and the third to be
used as referee sample.
B-3.4 All the individual samples and the composite sample shall be trans-
ferred to separate sampling containers. All the containers shall be sealed
and labelled with full identification particulars.
B-3.5 The referee test samples consisting of a composite sample and a set
of individual samples shall bear the seal of both the purchaser and the
supplier and’shall be kept at a place agreed to between the purchaser and
the supplier, to be used in case of any dispute between the two.
B-4.2 Tests for the determination of :iil other ( ll,:!Ynctcristics given ii1
Table 1 shall be perfurmcd OE the composi: , saniplt
23
IS : 1314 - 1984
B-5.2 For Composite Samples - The lot shall be deemed to have met
the requirements of the characteristics tested on the composite sample if
the test results satisfy the corresponding requirements given in Table 1.
24
-_. _~~_~_~~~.~~ -- --
IS : 1314 - 1984
25
i %a
,