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Indian Standard
SODIUM BICARl3ONATE - SPECIFICATION
( Second Revision )
ICS 71.060.50
0 BIS 2000
FOREWORD
This Indian Standard (Second 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.
The specifications for pure and analytical reagent grade, and that for refined grade were first issued in 1954.
Subsequently, in the year 1962, these were revised with a view to upgrade the refined grade and amalgamate the
two standards.
In the first revision the requirements for heavy metals and arsenic content were modified for the refined grade,
and for the pure grade, the requirement for matter insoluble in water and dilute ammonium hydroxide were
deleted. Also the limits for copper content have been prescribed as per PFA rules for both the grades.
Further, the analytical reagent grade of the material was modified on the basis of the prevailing standards for
laboratory chemicals.
In the present revision, calorimetric mefhod for determination of chlorides, heavy metals, phosphates, copper,
silicates and nephlometric method for determination of sulphate has been incorporated as alternative methods,
while some other modifications have been made inother test methods also.
Sodium bicarbonate is used as baking powder, reagent in analytical chemistry; in the manufacture of effervescent
salts and beverages. It also finds use in artificial mineral waters, gold and platinum plating, tanning industry,
treating wool and silk, fire extinguishers and ceramics.
For particle size, sieves conforming to IS 460 is prescribed. Where IS sieves are not available, other equivalent
standard sieves as judged by aperture size, may be used.
A scheme for labelling environment friendly products to be known as EC0 Mark is being introduced at the
instance of the Ministry of Environment and Forests (MEF),Govemment of India. The EC0 Mark shall be
administered by the Bureau of Indian Standards (BIS) under the Bureau ofZ&ian Standards Act, 1986 as per
the Resolution No.71 dated 20 February 1991 as published in the Gazette of the Government of India vide
GSR No. 85 (E) dated 21 February 1991. For a product to be eligible for marking with EC0 Mark it shall
also carry the Standard Mark of BIS for quality besides meeting additional optional environment friendly (EF)
requirements. The EF requirements for Sodium Bicarbonate (refined grade) are based on Gazette
Notification No. 215 (E) dated 17 May 1996 for labelling Food Additives as environment friendly products,
published by the Ministry of Environment and Forests.
Composition of the Committee responsible for formulating of this standard is given in Annex T.
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 significant places retained in the
rounded off value should be the same as that of the specified value in this standard.
IS 2124 : 2000
Indian Standard
SODIUM BICARBONATE - SPECIFICATION
( Second Revision )
Suitable for aerated water and baking powder industry. 5.1 Packing
4.1.1 The pure grade material suitable for the b) Indication of the source of manufacture,
manufa;:t!u-e of effervescent powders shall have the c> Mass of the material in the packaging, and
1
L_.
IS 2124 : 2000
ANNEX A
[Clause 4.2 and Table 1, Sl No. (i)]
DETERMINATION OF TOTAL ALKALINITY
ANNEX B
[Clause 4.2 and Table 1, Sl No. (ii)]
DETERMINATION OF pH
Two methods have been prescribed for determination of Dissolve 0.1 g in 100 ml of rectified spirit conforming
to IS 323.
pH electrometricmethod (Method A) and indicatormethod
(Method B). However, in case of dispute, the electrometric B-3.2 Procedure
method shall be considered as the referee method. Weigh 1 g of the material and dissolve in 100 ml 6f
water: Take 10 ml of this solution in a hard glass test
B-2 METHOD A (ELECTROMETRIC METHOD) tube and add 0.5 ml of bromothymol blue indicator.
Compare the colour produced with a series of buffer
B-2.1 Procedure
solutions of knownpH in the range 8.0 to 9.0. Report
The determination shall be made on 1 percent (m/v) as pH, the pH of the buffer solution which gives the
solution by any pH meter with glass electrode. closest match with the colour produced with the
sample.
B-3 METHOD B (INDICATOR METHOD) NOTE-Standard calibrated glass discs may also be used for the
B-3.1 Reagents determination ofpH.
IS 2124 : 2000
ANNEX C
[Chuse 4.2 and Table 1, Sl No. (iii)]
DETERMINATION OF CHLORIDES
C-2.1 For Pure and Refined Grades C-2.2.2.1 Concentrated nitric acid
4
IS 2124 : 2000
C-3.2.2 Spectrophotometer or Photocolorimeter Allow to stand for 15 minutes, transfer to the cell of
spectrophotometer and measure absorbance~of 450 nm
C-3.2.3 Platinum Evaporating Dish
wave length with compensation solution in reference
60 ml capacity. cell.
Dissolve 49.02 g of Ferric Ammonium Sulphate Weigh suitable mass of sodium bicarbonate sample
Dodecahydrate [FeNH,(SO,),. 12H,O] in ~203 ml of containing 50 to 150 pg of chloride (as Cl) correct to
dilute nitric acid (about 1.5 mol/l) and dilute to 500 ml 1 mg and transfer into the platinum evaporating dish
with distilled water. wet this with 15 to 20 ml of distilled water and slowly
neutralize with sulphuric acid solution add a few drops
C-3.3.2 Mercury (II) Thiocyanate Solution
in excess. Evaporate to nearly dryness on hot water
Saturated solution in absolute alcohol. bath. Add 20 to 30 ml of distilled water and
quantitatively transfer into a 100 ml volumetric flask,
C-3.3.3 Standard Sodium Chloride Solution
cool and make upto the mark with distilled water and
Weigh accurately 0.165 0 g of previously dried (at mix well.
500°C) and cooled A.R. sodium chloride, dissolve in
Filter through Whatman No. 41 filter paper and
a beaker in distilled water and quantitatively transfer
discard a small volume of initial filtrate.
into a one-litre volumetric flask, dilute to mark and
mix well 1 ml of this solution = 100 pg of Cl. Transfer suitable volume (25 to 40 ml) into 50 ml
volumetric flask add 2 ml of ferric ammonium sulphate
C-3.3.3.1 Dilute Standard Sodium Chloride Solution
solution and 2 ml of mercury thiocyanate solution in
Transfer 50 ml of standard sodium chloride solution that order, dilute to mark with distilled water and mix
into a 500 ml volumetric flask, dilute with distilled well.
water to the mark and mix well. 1 ml of this solution
Allow to stand for 15 minutes, transfer to the cell of
= 10 /.Lgof Cl.
spectrophotometer and measure absorbance at 450 nm
C-3.3.4 Sufphtrric Acid Solution wave length with distilled water in the reference cell.
5
IS 2124 : 2000
ANNEX D
[Clause 4.2 and Tuble l,.SZ No. (iv)]
DETERMINATION OF INSOLUBLE MATTER
D-l PROCEDURE the crucible along with the residue to constant mass
at 105 to 110°C.
Weigh accurately about 10 g of the material, transfer
it to a 400 ml ~beaker, add about 200 ml of freshly D-2 CALCULATION
boiled water and boil the resulting solution for
15 minutes. Filter any undissolved residue through a Insoluble matter, percent by mass = 100 5
tared Gooch or a sintered glass crucible (G No.4) and M,
wash the residue free from soluble salts with where
water.Collect the filtrate and washings in a one-litre
M, = mass in g of the residue, and
graduated flask and dilute to mark. Preserve the
solution so obtained for the test under Annex L. Dry IV, = mass in g ‘of the material taken for the test.
ANNEX E
[Clause 4.2 and Table 1, Sl No. (v)]
DETERMINATION OF SULPHATES
residue in 20 ml of water and add a ~few drops of E-3.2.5.1 Standard sulphuric acid solution
concentrated hydrochloric acid and 2 ml of barium
0.100 g SO, per litre - Transfer 20.8 ml of 0.05 mol/l
chloride solution. Transfer to a Nessler cylinder and
standard sulphuric acid solution into a I-litre
dilute to mark. Carry out a control test in another
volumetric flask, dilute to mark with distilled water
Nessler cylinder using O-O.6ml of standard sulphate
and mix well. 1 ml of this solution = 0.100 mg SO,.
solution in place of the material and the same
quantities of other reagents in the same total volume E-3.3 Apparatus
of the reaction mixture.
E-3.3.1 Standard Laboratory Apparatus
The limit prescribed in Table 1 shall be taken as not
having been exceeded if the turbidity in the test with E-3.3.2 Platinum Evaporating Dish
the material is not greater than that in the control test.. 60 ml capacity.
7
IS 2124 : 2000
E-3.4.2 Determination NOTE - If the turbidity developed in the test portion is beyond
the limits of the calibration range, dilute an aliquot filtrate
E-3.4.2.1 Test portion (E-3.4.2.1) to 50 ml and use 25 ml of this diluted solution to
develop turbidity. In this case use the diluted solution in the
Weigh to the nearest 1 mg a-quantity of the test sample reference cell.
of sodium bicarbonate containing 1 to 4 mg of SO,,
E-3.4.2.4 Blank test
and transfer into a platinum evaporating dish. Wet
the sample with 10 to 20 ml of distilled water and At the same time, carryout a blank test following the
neutralize with hydrochloric acid solution (E-3.2.4) same procedure and using the same quantities of all
and add a few drops in excess. Heat the evaporating reagents used for determination, but by replacing the
dish on a water bath to almost dryness and add 5 ml test portion by 5 ml of standard sulphuric acid solution
of hydrochloric acid solution (E-3.2.3) and 20 to 30 ml corresponding to 0.5 mg of SO, to allow operation in
distilled water. Heat again on water bath for a few the linear part of the calibration curve.
minutes and transfer quantitatively into a 50 ml
volumetric flask. Cool, make upto the mark and mix E-3.5 Calculations
well. Filter through a Whatman No. 41 filter paper, The sulphate content is obtained by the following
discarding a small volume of the initial filtrate. formula:
E-3.4.2.2 Turbidimetric reaction Sulphate (as SO,), (M, -M*)x 1000
Transfer 25 ml filtrate (E-3.4.2.1) into a 100 ml beaker percent by mass =
M,xlO
containing 0.15 g of barium chloride stir by hand for where
1 minute at the rate of 2 revolutions per second. The
barium chloride should then be in complete solution. M, = mass of sulphate in milligrams
Leave undisturbed for 15 minutes at 27 f 2°C. corresponding to absorbance of the test
portion,
E-3,4.2.3 Turbidity measurement
M, = mass of sulphate in milligrams
Transfer a sufficient quantity of the test solution to a corresponding to the absorbance of the
cell of the spectrophotometer (same size as the one blank solution after deduction of 0.5 mg
used for calibration) and use to adjust optical zero of of SO, added (that is Graph value - 0.5)
the spectrophotometer. and
Stirr by hand the turbidity developed in the solution M,, = mass of the sodium bicarbonate in grams
(E-3.4.2.2). Transfer it into a cell (same sizes as the corresponding to aliquot used for turbidity
one used for calibration) and measure absorbance at development.
8
IS2124:ZOOO
ANNEX F
[Clause 4.2 and Table 1, Sl No. (vi)]
TEST FOR IRON
Dissolve 0.702 g of ferrous ammonium sulphate The limit prescribed in Table 1 shall be taken as not
[FeSO,.(NH& S0,6H20] in 10 ml of dilute sulphuric having been exceeded if the intensity of colour
acid (10 percent v/v) and dilute with water to produced in the test with the material is not greater
1 000 ml.Dilute 10 ml of this solution to 100 ml. than that produced in the control test.
ANNEX G
[Clauses 4.2 and S-5.1.2 and Table 1, Sl No. (vii)]
TEST FOR HEAVY METALS
Two methods have been prescribed for determination Dissolve 1.598 5 g of lead nitrate in water and make
of heavy metals as lead,namely,v~isual colour up the volume to 1 000 ml. Transfer exactly 10 ml of
comparison (Method A) and spectrophotometric the solution into a vo!umetric flask and dilute it against
method (Method B). In case of dispute Method A with water to 1 000 ml mark. One millilitre of this
shall be referee method. solution contains 0.01 mg of lead (as Pb). The solution
should be freshly prepared.
G-2 METHOD A (VISUAL COLOUR
COMPARISON) G-2.2.3 Acetic Acid
Approximately 1 N.
G-2.1 Apparatus
G-2.2.4 Hydrogen Sulphide Solution
G-2.1 .l Nessler Cylinders
Saturated.
50 ml capacity.
G-2.3 Procedure
G-2.2 Reagents
Weigh 4.000 g of the material and add 15 ml of
G-2.2.1 Corrcentrmed Hydrochloric Acid water.Add 6 ml of concentrated hydrochloric acid and
Conforming to IS 265. evaporate to dryness on a water-bath. Dissolve the
residue in water and transfer this solution into a
9
IS 2124 : 2000
Nessler cylinder. Dilute it with water to 30 ml and (CAUTION- Potassium cyanide is highly poisonous)
add 1 ml of acetic acid and 10 ml of hydrogen sulphide add 35 ml of concentrated ammonia and dilute to
solutionIn a’ second Nessler cylinder, carry out a 100 ml. Add 0.15 g of sodium sulphite and mix well.
control test using 2 ml of standard lead solution for
G-3.3.5 Dilute Hydrochloric Acid Solution
,pure grade, analytical reagent grade and refined grade
in place of the material, and the same quantities of Approximately 1 moY1.
other reagents. Dilute the contents of each tube to
G-3.3.6 Hydrochloric Acid Solution
50 ml and shake well. Compare the colour produced.
Approximately 6 mol/l.
The limit prescribed in Table 1 shall be taken as not
having been exceeded if the intensity of colour G-3.4 Procedure
produced with the material is not greater than that
G-3.4.1 Calibration
produced in the control test.
Transfer dilute standard lead solution to a series of
G-3 METHOD B (SPECTROPHOTOMETRIC six 250-ml separating funnels as given below:
METHOD)
Standard Lead Corresponding
G-3.1 Outline of the Method Solution, ml Lead Content, pg
0 (Compensation) 0
Lead reacts with dithizone (diphenylthio Carbazone)
to form a pink coloured complex in chloroform 2.0 20
solution. The complex is separated by extraction with 4.0 40
chloroform from an aqueous Ammonia-Cyanide- 6.0 60
Sulphite solution. The absorbance of the extracted 8.0 80
complex is measured using a spectrophotometer at 10.0 100
5 10 nm wavelength.
Add to each funnel 75 ml of ammonia-cyanide-sulphite
G-3.2 Apparatus reagent solution and cautiously adjust pH to 9.5 using
apH meter (equipped with a combined electrode). This
G-3.2.1 Standard Laboratory Apparatus operation must be carried out slowly because, if the
G-3.2.2 Separating Funnels pH of the solution falls below 9.5 even temporarily,
HCN gas may be liberated. Use of fume cupboard
250 ml capacity. during this operation is necessary. Then add 7.5 ml of
G-3.2.3 Spectrophotometer or Photocolorimeter dithizone reagent to each separating funnel. Maintain
time difference among each such that the time after
G-3.3 Reagents addition of dithizone reagent and final absorbance
G-3.3.1 Standard Lead Solution measurement is same for all. Then add 17.5 ml of
chloroform and shake for one minute to extract the
Dissolve 0.799 2 g of A.R. lead nitrate [Pb(NO,),] lead complex into the chloroform layer, allow the
in distilled water in a beaker, transfer quantitatively phases to separate. Transfer the chloroform layer
into a 500-ml one-mark volumetric flask, dilute to the (lower one) through a cotton plug (placed in the stem
mark and mix well. One ml of this solution contains of the separating funnel) into a 1 cm cell of the
1 mg lead. spectrophotometer. Immediately replace the lid of the
G-3.3.1.1 Dilute Standard Lead Solution cell. Measure absorbance (using chloroform extract
of compensation solution, in reference cell) at 5 10 nm
Transfer 10 ml of the above solution (G-3.3.1) into a wavelength.-
I-litre volumetric flask, dilute to mark~and mix well.
1 ml of this solution contains 10 pg of lead. Plot a graph using 20-25 ml of lead (in 25 ml of
chloroform) as abscissae and corresponding
G-3.3.2 Chloroform absorbance values as ordinates.
Reagent grade chloroform. G-3.4.2 Determination
G-3.3.3 Dithizone Reagent Weigh accurately correct to 1 mg about 10 g of Sodium
50 mgll solution in chloroform. Dissolve 5 mg of the bicarbonate sample (the quantity to be weighed,
reagent in 100 ml of chloroform. should be such that it contains 20 to 100 pg of lead)
and transfer to 50 ml beaker dissolve in about 20-25
G-3.3.4 Ammonia-Cyanide-Sulphite Reagent ml distilled water and transfer quantitatively into a
To 3 ml of 10 percent potassium cyanide solution 250 ml separating funnel and rinse the beaker twice
with 5 ml portions of distilled water. 75 ml of
10
IS 2124 : 2000
ANNEX H
[Clauses 4.2 and S-5.1.2 and Table 1, Sl No. (viii)]
TEST FOR ARSENIC
ANNEX J
[Clause 4.2 and Table 1, Sl No. (ix)]
TEST FOR AMMONIUM COMPOUNDS
11
IS 2124 : 2000
potassium hydroxide and, when it has dissolved, add The material shall be considered to have passed the
1 ml more of mercuric chloride solution and dilute to test if no ammonia is detected in the vapours on testing
200 -ml with ammonia-free water. Allow to settle with moistened litmus paper.
overnight, decant the clear solution and keep it in a
J-3.2 For Analytical Reagent Grade
bottle closed with a well-fitting rubber stopper.
Dissolve 2.0 g of the material in 45 ml of water and
J-2.4 Standard Ammonium Chloride Solution add 15 ml of sodium hydroxide solution. Filter through
a sintered glass crucible, previously washed with
Dissolve 0.296 g of ammonium chloride (NH,Cl) in
sodium hydroxide solution. Take 6 ml of the filtrate,
water and dilute to 100 ml. Dilute 10 ml ofthis solution
dilute with water to 50 ml and add 2 ml of Nessler
to 1 000 ml. One millilitre of this diluted solution is
solution. In a control test, having an equal volume of
equivalent to 0.01 mg of ammonium (as NH,).
the solution and containing 1 ml of standard
ammonium chloride solution and 1.5 ml of sodium
J-3 PROCEDURE
hydroxide solution, add 2 ml of Nessler solution.
J-3.1 For Pure Grade
The limit prescribed in Table 1 shall be taken as not
Dissolve 1.O g of the material in 10 ml of water, add having been exceeded if the intensity of colour
20 ml of sodium hydroxide solution and warm the produced in the test with the material is not greater
reaction mixture. than that produced in the control test.
ANNEX K
[Clause 4.2 and Table 1, Sl No. (x)]
TEST FOR PHOSPHATES
Two methods have been prescribed for determination Dissolve without heating 0.2 g of methyl-p-
of phosphates,namely,visual colour comparison aminophenol sulphate (metal) and 20 g of sodium
(Method A) and spectrophotometric method (Method metabisulphite in 100 ml of water.
B). In case of dispute Method A shall be referee method, K-2.2.4 Standard Phosphate Solution
12
IS 2124 : 2000
The limit -prescribed in Table 1 shall be taken as not K-3.3.4.1 Dilute Standard Phosphate Solution
having been exceeded if the intensity of colour
10 pg PO, per litre - Transfer 50 ml of standard
produced in the test with the material is not greater
phosphate solution into a 500 ml volumetric flask,
than that produced in the control test.
dilute to mark and mix well.
K-3 METHOD B (SPECTROPHOTOMETR-IC K-3.3.5 Hydrochloric Acid Solution
METHOD)
Approximately 6 mol/l - Add slowly 535 ml of
K-3.1 Outline of the Method concentrated hydrochloric acid (sp gr 1.18) into
465 ml of disti1Ied water and mix.
Silica is eliminated by precipitation and filtration.
Formation of phosphomolybdic acid complex in acidic K-3.4 Procedure
solution and reduction of yellow complex to
molybdenum blue complex. Measurement of the K-3.4.1 Calibration
intensity of the blue colour (which is proportional to Into a series of six lOO-ml volumetric flasks, transfer
phosphate concentration) using a spectrophotometer dilute standard phosphate solution as given below:
or photocolorimeter at 580 nm wavelength.
Standard Phosphate Corresponding Mass of
K-3.2 Apparatu Solution, ml Phosphate as PO,, pg
0 (Compensation) 0
K-3.2.1 Standard Laboratory Apparatus
2 20
K-3.2.2 Spectrophotometer or Photoelectric 4 40
Colorimeter 60
6 .
K-3.2.3 Platinum Evaporating Dish 8 80
.lO 100
Approximately 60 ml capacity.
Add to each flask 2 ml of perchloric acid, 20 ml of
K-3.3 Reagents distilled water, 10 ml of ammonium molybdate
K-3.3.1 Perchloric Acid solution and finally 5 ml of reducing solution. Make
upto the mark and mix well. Place flasks in boiling
6@ to 70 percent solution (m/m). water-bath for 15 minutes,cool in running water
K-3.3.2_Ammonium Molybdate Solution and measure absorbance using 2 cm cell in a
spectrophotometer (or photocolorimeter) at 620 nm
Dissolve 10 g of ammonium molybdate tetra hydrate wavelength using compensation solution in the
(NH,),Mo,02,.4H,0 in 100 ml of water. Add slowly reference cell.
220 ml of sulphuric acid (1:l solution) and 70 ml
distilled water. Mix and allow to cool. Plot a graph with pg of PO, as abscissae and
corresponding absorbance values as ordinates.
K-3.3.3 Reducing Solution
K-3.4.2 Determination
Dissolve 0.25 g of l-amino 2-naphthol 4-sulphonic
Weigh about 1 g of sodium bicarbonate accurately to
acid and 0.5 g of anhydrous, sodium sulphite (Na,SO,)
1 mg (the quantity to be weighed should be such that it
in about 70 ml distilled water. Dissolve separately
contains 20 to 100 pg of phosphate) and transfer into a
24 g of anhydrous sodium bisulphite (Na,S,O,) in
60 ml platinum evaporating dish, wet it with some
about 100 ml distilled water. Mix both solutions and
~distilled water and neutralize with hydrochloric acid
dilute to 200 ml with distilled water, filter, if necessary
solution and add a few drops in excess. Evaporate to
and store in a cool dark place. nearly dryness and add 2 ml of perchloric acid and again
K-3.3.4 Standard Phosphate Solution evaporate to nearly dryness. Add a few drops of
hydrochloric acid solution and about 20 ml of distilled
Weigh accurately 1.433 g of finely powdered and dried water and transfer quantitatively into a 100 ml
A.R. potassium dihydrogen phosphate (KH,PO,) volumetric flask. Cool and dilute to mark and mix well.
dissolve in 100 to 150 ml distilled water in a 250 ml
Filter through a Whatman No. 4 1 filter paper, discard
beaker, transfer quantitatively to 1 000 ml volumetric
a small volume of initial filtrate and then transfer
flask, dilute :o mark and mix well. Transfer 50 ml of
50 ml of filtrate into 100 ml volumetric flask and
this solution to a 500 ml volumetric flask, dilute to
develop colour as described under calibration
mark and mix well. One millilitre ml of this solution
(K-3.4.1).
contains 100 pg of phosphate (as PO,).
Measure absorbance at 620 nm wavelength using same
13
IS 2124 : 2000
ANNEX L
[Chse 4.2 and Table 1, SZ No. (xi)]
DETERMINATION OF CALCIUM AND MAGNESIUM
14
IS 2124 : 2000
ANNEX M
[Clause 4.2 and Table 1, Sl No. (xii)]
TEST FOR COPPER
Two methods have been prescribed for determination Dissolve 0.392 g of copper sulphate pentahydrate
of copper,visual colour comparison (Method A) and in copper-free water and make up the volume to
spectrophotometric method (Method B). In case of 1 000 ml. Take 100 ml of this solution and dilute again
dispute Method A shall be referee method. to 1 000 ml. One millilitre of the diluted solution
contains 0.01 mg of copper (as Cu).
M-2 METHOD A (VISUAL COLOUR
M-2.2.7 Chloroform
COMPARISON)
M-2.3 Procedure
M-2.1 Apparatus
Weigh 1 .OOOg of the material and dissolve it in about
M-2.1.1 Nessler Cylinders 50 ml of water. Neutralize with concentrated
50 ml capacity. hydrochloric acid and add 4 to 5 drops of concentrated
nitric acid. Boil and cool. Add 1 g of citric acid and
M-2.2 Reagents adjustpH to 9 by adding dilute ammonium hydroxide.
Add 10 ml of sodium diethyldithiocarbamate solution
M-2.2.1 Concentrated Hydrochloric Acid and extract the yellow colour produced four times with
Conforming to IS 265. 2.5 ml portions of chloroform. Collect the chloroform
extracts and filter through a dry filter into a Nessler
M-2.2.2 Concentrated Nitric Acid cylinder. Carry out a control test using3 ml of standard
copper solution in place of the material.
Conforming to IS 264.
The material shall be considere$ pg$ to have exceeded
M-2.2.3 Citric Acid
the limit prescribed in Table ! :if.:he intensity of the
M-2.2.4 Dilute Ammonium Hydroxide colour produced with the mater.@::is not greater than
that produced in the control test. ” ^
Approximately 5 N.
M-3 METHOD B (SPECTROPHOTOMETRIC
M-2.2.5 Sodium Diethyldithiocarbamate Solution
METHOD)
Dissolve 1.0 g of sodium diethyldithiocarbamate in
1 000 ml of copper-free water. Filter and keep in M-3.1 Outline ofthe Test Method
an amber bottle and protect from strong light. The material is neutralized with hydrochloric acid.
15
IS 2124 : 2000
The copper in the soluble form is treated with diethyl- M-3.3.9 Hydrochloric Acid So&ion
dithiocarbamate solution toproduce a coloured copper
Approximately 1 mol/l.
complex. This is extracted with carbon tetrachloride.
The absorbance of the Ccl, extracts measured at 440 ntn M-3.4 Procedure
using a spectrophotometer or a photocolorimeter.
M-3.4.1 Calibration
M-3.2 Apparatus
Into a series of six 250-ml separatory funnels, transfer
M-3.2.1 Spectrophotometer or a Photocolorimeter standard dilute copper solution as given below:
Suitable for measuring absorbance at 440 nm. Standard Copper Corresponding Mass
Approximately 6 mol/l -Dilute 500 ml cone HCl Add to each 20 ml hydrochloric acid solution,10 ml
(sp gr 1.19) with 500 ml distilled water. EDTA solution and then 5 drops of phenolphthalein
solution and mix well. Neutralize each with concen-
M-3.3.3 EDTA Solution trated ammonium hydroxide solution to a faint pink
colour and cool to room temperature. Add distilled
5 percent solution - Dissolve 50 g Ethylene diamine
water to each to a final volume of 45 ml.
tetra-acetic acid, disodium salt (C,,H,,O,Na,. 2H,O)
in distilled water, dilute to 1 000 ml and keep the Then add to each 5 ml DEDTC solution mix well
solution in a polyethylene bottle. and add 20 ml carbon tetrachloride.Shake the
funnel vigorously for at least 3 minutes and allow the
M-3.3.4 Sodium Diethyldithiocarbamate Solution
phases to separate.
(DEDTC)
Filter Ccl, phase (the lower phase) through a cotton
Dissolve 0.1 g of DEDTC [(C,H,),N.CS,Na.3H,O] in plug inserted in the outlet stem of the separatory funnel
100 ml of distilled water and keep the solution in a into photometer cells. Apply the lid of the cell and
dark bottle. measure absorbance at 440 nm with extract ofcopper
M-3.3.5 Standard Copper Solution free solution (compensation solution) as reference.
Dissolve 0.100 g pure copper metal in the smallest Plot copper content (yg/20 ml) as abscissae ‘vs
possible quantity nitric acid in a 1 000 ml volumetric corresponding absorbance values as ordinates.
flask, cool and dilute to mark. One millilitre of this M-3.4.2 Determination
solution contains 100 pg copper.
Weigh accurately correct to 1 mg an amount of sodium
Transfer 10 ml aliquot of this solution (M-3.3.5) in to
bicarbonate sample containing 200 to 1 000 pg of
100 ml volumetric flask, dilute to mark and mix. One
copper and transfer into a platinum dish.Wet it with
millilitre of this solution is equivalent to 10 pg of
minimum amount of distilled water and neutralize
copper.
with 6 mol/l hydrochloric acid solution and add a few
M-3.3.6 Ammonium Hydroxide Solution drops in excess. Evaporate to dryness on a water-bath.
Concentrated. Wet it with a few drops of dilute hydrochloric acid
solution and then dissolve in 20 to 30 ml of distilled
M-3.3.7 Carbon Tetrachloride
water and quantitatively transfer into a 100 ml one
Reagent grade Ccl,. mark volumetric flask, cool, make upto the mark and
mix well. If the solution is turbid, filter through a
M-3.3.8 Phenolphthalein Solution
Whatman No. 54 1 filter paper discarding 10 to 15 ml
Dissolve 0.5 g phenolphthalein powder in 500 ml of of initiate filtrate.
50-70 percent ethanol or methanol. Neutralize the
solution by adding 0.1 mol/l NaOH until a faint pink Transfer 10.0 ml of the aliquot volume (or the filtrate
colour appears and then remove this colour with a if filtered) into a 250-ml separatory funnel, and
drop or two of 0.1 mol/l hydrochloric acid. proceed further exactly as described under calibration.
16
IS 2124 : 2000
ANNEX N
[Clause 4.2 and Table 1, SZ No. (xiii)]
TEST FOR NITRATES
17
IS 2124 : 2000
ANNEX P
[Clause 4.2 and Table 1, Sl No. (xiv)]
TEST FOR SILICATES
18
IS 2124 : 2000
distilled water in a beaker of material free from silica silica solution (P-3.2.10) to 1 000 ml in a 1 OOO-ml
of suitable capacity and after cooling dilute to 100 ml. volumetric flask. Prepare this solution at the time of
Store, if necessary, in a bottle of material free from use. 1 ml of this solution = 2.0 ug SiO,.
silica and filter, if necessary, before use.
P-3.3 Apparatus
P-3.2.5 Oxalic Acid I
P-3.3.1 Standard Laboratory Apparatus
100 g/l Solution-Dissolve 10 g of oxalic acid dihydrate
(COOH.COOH.2HrO) in 100 ml distilled water. P-3.3.2 pH Meter
25 g/l Solution - Dissolve 2.5 g of ascorbic acid in P-3.3.4 Platinum Crucible with Lid of Suitable Size
water and dilute to 100 ml. Store the solution in a P-3.4 Procedure
bottle of material free from silica and protect from
light. P-3.4.1 Preparation of the Calibration Graph
Prepare this solution at the time of use or as an P-3.4.1 .l Preliminary Testfor Control and Correction
alternative, prepare reduction solution. of_pH
P-3.2.9 Boric Acid Solution In to a series of six 50-ml beakers, transfer standard
silica solution as given below:
Saturated solution at ambient temperature.
Standard Silica Corresponding Mass of
P-3.2.10 Standard Silica Solution Solution Silica
0.200 g SiO, per litre - Weigh to the nearest 1 mg ml pg
0.200 g SiO, obtained by heating pure silicic acid 0 (Compensation) 0.0
(H,SiO,) at 1 000°C until constant mass (consecutive 2.0 4.0
weighings should not differ by more than 1 mg) and 4.0 8.0
cooling in a desiccator into a platinum crucible of 6.0 12.0
convenient capacity. Add 2 g of anhydrous Na, CO, 16.0
8.0
to the crucible, mix well preferably with a platinum
10.0 20.0
spatula and carefully fuse the mixture. Add warm
water directly to the crucible, heat gently until the Add to each beaker distilled water to make up volume
contents are completely dissolved and transfer to 15.0 ml. Then add the volume of sulphuric acid
quantitatively to a beaker of material free from silica solution as calculated above (P-3.4.1.1) for pH
of suitable capacity. correction, mix well. Add 1 ml of sodium fluoride
Cool, dilute the solution to about 500 ml, transfer solution, mix and allow to stand for 5 min.
quantitatively to a 1 000 ml volumetric flask, dilute P-3.4.1.3 Colour Development
to mark and mix well. Transfer the solution
immediately to a bottle of material free from silica. Add to each beaker 5 ml of boric acid solution and
1 ml of this solution = 0.2 mg SiO,. 5 ml of sodium molybdate solution, mix and allow to
stand for 10 minutes. Add 5 ml of oxalic acid solution
P-3.2.10.1 Standard Silica Solution
and 8 ml of sulphuric acid solution (P-3.2.3) Allow to
2.0 mg SiO, per litre - Dilute 20.0 ml of standard stand for 2 minutes, add 2 ml of ascorbic acid solution
19
IS 2124 : 2000
ANNEX Q
[Clause 4.2 and Table 1, Sl No. (xv)]
DETERMINATION OF POTASSIUM
Q-1 APPAR 4TUS solution and dilute to 100 ml with distilled water in
different measuring flasks Each flask now contains
Q-l. 1 Flame Photometer 0.01, 0.02, 0.04, 0.06 and 0.08 g KC1 per 100 ml.
Equipped with interference filter. Use these dilute solutions to obtain a corresponding
galvanometer reading as given in Q-3.2.1 and plot
Q-2 REAGENTS the concentration against galvanometer reading in a
rectangular co-ordination graph. Draw a smooth curve
Q-2.X Standard Potassium Solution over the points which gives a calibration graph in the
Weigh exactly 1 g of potassium chloride, dissolve in range 0.01 to 0.1 percent KCl.
distilled water and dilute to one litre with distilled
Q-3.2 Sample Solution
water in a measuring flask. This solution contains
0.1 g KC1 per 100 ml. Dissolve approximately 10 g of the sample in
minimum quantity of distilled water and dilute to
Q-3 PROCEDURE 100 ml in measuring flask with distilled water.
20
IS 2124 : 2000
burner, optical selective device consisting of the indicate that the instrument has been made ready for
reflectors, lenses and diaphragms; and measuring measurement.
instrument consisting of photocell, amplifier and
Without altering the earlier adjustment of the
sensitive galvanometer. The galvanometer scale ranges
instrument spray various diluted solutions prepared
from 0 to 100 divisions which measures the intensity
in Q-3.1 and obtain a calibration graph in the range
of the radiation transmitted by the element.
0.0 1 to 0.1 percent KC 1. After washing with distilled
Insert the potassium filter Forresponding to wavelength water, spray the sample solution and obtain the
767 nm, light the Burner fed by illuminating gas galvanometer reading. From the graph, read out the
(laboratory gas), adjust the specified air pressure corresponding concentration of KC1 in the solution
between 0.5 to 0.6 kg/cm* and maintain the above air (say A).
pressure constant, such that flame is non-luminous
by turning the control knob. First spray distilled water Q-4 CALCULATION
and adjust the pointer to zero in galvanometer scale Potassium (as K), percent by mass = 52.35$
by zero adjustment knob. Then spray the KC1 standard
solution and adjust the deflection to maximum 100 by where
using sensitivity control knob. Again spray water to A = concentration of KC1 in the sample
see that the pointer comes to zero; then spray a solution, and
standard solution reads 100 with same adjustment M= mass of dried sample taken for the test.
during both the operations. A reading zero by water
and with the sameadjustment 100 by standard solution
ANNEXR
[Clause 4.2 and Table 1, Sl No. (xvi)]
TEST FOR SUBSTANCES REDUCING IODINE
21
IS 2124 : 2000
ANNEX S
(Clause 6)
SAMPLING OF SODIUM BICARBONATE
22
IS 2124 : 2000
and the supplier and shall be used in case of dispute Range (R) = The difference between the
between the two. maximum and the minimum
values of the test results.
S-4 NUMBER OF TESTS
and the value of expression (X - 0.6 R) shall be
S-4.1 Tests for the determination of total alkalinity calculated. If the value of this expression is equal to
shall be conducted on each of the individual samples or greater than the limit specified for the relevant grade
for all the three grades. For refined grade, tests for in Table 1, the lot shall be declared to have satisfied
heavy metals and arsenic also shall be conducted on the requirements for this characteristic.
each of the individual samples.
S-5.1.2 For Heavy Metal and Arsenic
S-4.2 Test for the remaining characteristics shall be
The lot shall be declared as conforming to the
conducted on the composite sample.
requirements for these characteristics if each of the
samples satisfies the test laid down in Annexes G
S-5 CRITERION FOR CONFORMITY
and H.
S-5.1 For Individual Samples
S-5.2 For Composite Sample
S-5.1.1 For Total Alkalinity
The test results on the composite sample shall
The test results for total alkalinity shall be recorded meet the corresponding requirements specified in
and the mean and the range for these test results shall Table 1.
be calculated as follows:
S-5.3 A lot shall be declared as conforming to the
Mean (x) = Sum of the test results divided by specification if it satisfies the requirements for each
the number of test results. of the characteristics listed in Table 1.
23
IS 2124 : 2000
ANNEXT
(FCJ7-eWO~d)
COMMITTEE COMPOSITION
24
IS2124:2000
Convener Representing
Members
SHRI H. G. NAIK (Alternate to
Shri J. B. Sharma)
SHRI V. K. BhhTH Ballarpur Industries Ltd, Karwar
SHRIV. V. S~v~w(Alremate)
DR R. N. VW.A Central Salt and Marine Chemicals Research lnstitute (CSIR), Bhavnagar
SHRI M. R. On (Alternate)
SHRI M. R. SOMAYAJI Chemplast Sanmar Ltd, Mettur Dam
(Alfemale)
SHKISIVASUBRAMAKIUM
SHRI B. H. PATEL Deepak Nitrite Ltd, Vadodara
SHRI B. S. METHA (Alternate)
SHRIJASBIRSIWII Deptartment of Chemicals and Petrochemicals, Ministry of Chemicals and Fertilizers,
SHRI R. C. SHARMA(Alternate) New Delhi
SHRIC. T. D.AIThIREYh Indian Paper Mills Association, Calcutta
SHRI P. L. BWMAN (Altemafe)
SHRIG S (;I\HLOT Modi Alkalis and Chemicals Ltd, Alwar
DR P. C. GWTA (Allemale)
SWI S. K. SAHA National Test House, Calcutta
SHRI B K. BISWAS(AllenWe)
SHRI S. C. TANDON Punjab Alkalies&Chemicals Ltd, Nayanangal
SHRI H. S. DAS (Alfernate)
DR B. R. SINCHVI Saurashtm Chemicals, Porbandar
DR V. S. VAIDYA (Alfemafe)
SHRI V. K. KAPOOR Standard Alkali, Thane
SHKI A. S. KULKARXI(Alfemate)
SHRIM. HARIHAILSWAMY Tata Chemicals Ltd, Mumbai
SHRI H. U. DOSHI (Alremate)
25
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