DETERMINATION OF ALUMINIUM OXIDE IN POLYALUMINIUM CHLORIDE(PAC)

A-1.2 Reagents A-1.3 Procedure

A-1.2.1 Nitric Acid ( 1 : 12 ) A-1.3.1 Weigh accurately, to the nearest 1 mg, for
A-1.2.2 M/100 EDTA — Dissolve about 3.722 g of powder about 2.5 g, for liquid about 7 g, of the test
ethylenediamine tetra acetic acid disodium salt sample in a weighing bottle. Transfer it quantitatively
dihydratc in distilled water, transfer to a 1000 ml to a 500 ml volumetric flask with aid of about 150 ml
volumetric flask and make up to the mark by distilled water dissolve by shaking and make up to mark.
water and shake well. A-1.3.2 Pipette out accurately 10 ml of this
A-1.2.3 Sodium Acetate Buffer Solution — Dissolve solution to a 250 ml conical flask add 2 ml of
272 g of sodium acetate trihydrate in water and dilute nitric acid, 1:12 (the pH value shall be between 1
to 1 litre. to 2), boil for 1 min, allow to cool and add 50 ml
of M / 100 EDTA solution exactly by pipette.
A-1.2.4 Xylenol Indicator Orange — (a) Solution, 0.1
percent (w/v) — Dissolve 0.1 g of xylenol orange A-1.3.3 Boil for about 2 min.
powder in about 70 ml water, shake and make up to A-1.3.4 Cool and add approximately 10 ml sodium
100 ml. Shake well. (b) Powder, xylenol orange acetate buffer solution (pH of mixture should be
mixture (1 percent w/w in potassium nitrate): Grind between 5 and 6) add 2 to 5 drops of xylenol orange
1.0 g of xylenol orange with 99 g of potassium nitrate solution (0.1 percent w/v) or add 30-50 mg 1 percent
in a mortar until a homogeneous material is obtained. w/w xylenol orange mixture in potassium nitrate.
A-1.3.5 Titrate the solution with M/100 zinc solution,
making the end point the time when the colour of the
solution turns from pink colour to pale red.
A-1.3.6 In parallel, pipette out 10 ml M/100
EDTA, add 2 ml of nitric acid (1:12) solution to a
250 ml conical flask, add about 20 ml distilled
water and proceed the blank test as described in A-
1.3.3 to
A-1.3.5.
Calculate for factor F1 as follows:
F1= 10 ml EDTA/ml ZnCl2

A-1.2.5 Hydrochloric Acid — AR grade (see IS 265). A-2 CALCULATION

A-1.2.6 M/100 Zinc Solution — Weigh accurately Aluminium oxide (A12O3), %
about 0.6539 g of AR grade zinc metal (A - BxF1) x 2.549
pellets/granule, transfer to a 250 ml beaker, add small = ----------------------
amount of water and 6-7 ml of concentrated Weight of Sample
hydrochloric acid AR, heat to dissolve zinc, evaporate
on a water bath nearly to dryness, dissolve the residue Where
in water, transfer the contents quantitatively to a 1000 A = EDTA solution, in ml;
ml volumetric flask and make up to the mark. B= Zinc solution, in ml

Molarity of zinc solution, M1 =

where
M1 = morality of zinc solution, and
m = mass of zinc metal taken for preparation of
solution.

3
IS 15573 : 2005

ANNEX B
[Table 1, Sl No. (ii)]
DETERMINATION OF BASICITY

B-1 PRINCIPLE where

Sample solution is depolymerized by heating in acidic NA = normality of hydrochloric acid solution;
medium. Potassium fluoride is added to complex w = mass of sodium carbonate taken, in g; and
aluminium. Excess of acid is titrated with standard d = titre of N/2 hydrochloric acid solution,
alkali using phenolphthalein as an indicator. in ml.
B-1.1 Reagents B-1.1.8 Sodium Hydroxide Solution (N/2) — Add
B-1.1.1 Potassium Fluoride Solution (50 percent w/v) about 100 g of sodium hydroxide gradually in 250 ml
conical flask with about 100 ml of water, with care of
— Dissolve 250 g potassium fluoride anhydride in
generating heat, allow to dissolve with agitating by
water to 500 ml and filter through a filter paper. glass rod, prepare the saturated solution, allow to stand
B-1.1.2 Non-carbonic Water — Boil redistilled water, till over night with stopper, and dilute about 20 ml of
remove carbonic acid gas and volatile components and supernatant liquid with non-carbonic acid water to 1
allow to cool to ordinary temperature, preventing from 000 ml. Standardize this solution as follows.
the absorption of carbonic acid gas in the air. B-1.1.8.1 Standardization — Pipette out exactly
B-1.1.3 Ethyl Alcohol Solution of Methyl Red — 25 ml of hydrochloric acid (N/2) to a conical flask,
bromocresol green — Dissolve 0.02 g of methyl and after adding 2 to 3 drops of ethyl alcohol
red and 0.1 g of bromocresol green in 100 ml solution (0.5 percent w/v) of phenolphthalein,
ethyl alcohol (95 percent w/v). titrate it with sodium hydroxide solution, and
B-1.1.4 Ethyl Alcohol Solution of Phenolphthalein (0.5 making the end point to time when the colour of
percent w/v) — Dissolve 0.5 g of phenolphthalein in the solution turns to pink. Normality of sodium
100 ml of ethyl alcohol (50 percent v/v), add sodium
hydroxide solution is given as below:
hydroxide solution (N/50) drop by drop until the colour Calculation
of the solution turns slightly pink.
B-1.1.5 Sodium Carbonate (Anhydrous) — AR grade.
B-1.1.6 Sodium Hydroxide — AR grade.
where
B-1.1.7 Hydrochloric Acid Solution (N/2) — Transfer
40 to 45 ml conc hydrochloric acid (AR grade) to a NB = normality of sodium hydroxide solution;
1 000 ml volumetric flask and make upto the NA = normality of hydrochloric acid solution;
mark with distilled water, shake well and and
standardize this solution as follows. V = titre of N/2 sodium hydroxide solution,
B-1.1.7.1 Standardization — Sodium carbonate in ml.
(anhydrous) of 99.9 percent purity contains a little B-1.2 Procedure
moisture, which is to be dehydrated by heating at
260-270°C for half an hour and allow to cool in B-1.2.1 Weigh about 2 g of the liquid/solid sample in a
desiccators before use. Weigh out accurately from a beaker accurately to the nearest 1 mg and transfer with
weighing bottle about 0.5 to 0.7 g of sodium 20-30 ml of water to a 250 ml conical flask.
carbonate into a 250 ml conical flask. Dissolve it in B-1.2.2 Pipette out precisely 25 ml of hydrochloric
20 ml distilled water and add some drops of methyl acid solution (N/2) and add to the sample, cover with a
red — bromocresol green, titrate with hydrochloric watch glass, after heating for 10 min on a water bath,
acid making the end point the time when colour of cool to room temperature and add at once 25 ml of
solution turns from blue to purplish red. Calculate potassium fluoride solution (50 percent w/v).
normality of HC1 as follows:
B-1.2.3 Add about 5 drops of ethyl alcohol solution
(0.5 percent w/v) of phenolphthalein, and immediately
titrate with N/2 sodium hydroxide solution, making the

4
 IS 15573 : 2005

end point the time when the colour of the solution where
turns to pink.
B = basicity, percent by mass;
B-1.2.4 In parallel, pipette out 25 ml water to a 250
V1 = titre of N/2 sodium hydroxide solution
ml conical flask and proceed as given in B-1.2.2 and
consumed in sample in ml;
B-1.2.3.
V2 = titre of N/2 sodium hydroxide solution
B-1.3 Calculation consumed in blank (see B-1.2.4);
Relative basicity, B in terms of moles of OH per three NB = normality of sodium hydroxide solution
moles of aluminium in percent is given by following used;
17 = gram equivalent of hydroxy 1 group;
equation:
M = mass, of sample taken for test, in gram;
A = percent of aluminium oxide obtained in A-
2;
0.529 3 = conversion factor of aluminium in
aluminium oxide; and
= gram equivalent of aluminium.

ANNEX C
[Table 1, Sl No. (iii)]
DETERMINATION OF CHLORIDE

C-1 PRINCIPLE water acidified with 1 ml of concentrated nitric acid

(sp. gr. 1.42). Dilute the acidified mercuric nitrate
Acidified sample solution is titrated with standard
solution with distilled water to 1 litre.
mercuric nitrate solution using mixed
diphenylcarbazone and bromophenol blue indicator. C-1.1.5 Standardization of Mercuric Nitrate Solution
The end point is shown by the formation of the blue- (0.1 N) — Take 25 ml of standard 0.1 N sodium
violet mercury diphenylcarbazone complex. chloride solution in a 250 ml conical flask, dilute with
distilled water, add 5 to 10 drops of mixed indicator
C-1.1 Reagents solution, add 2 to 3 drops of dilute nitric acid (3 : 997)
and titrate it with 0.1 N mercuric nitrate solution till
C-1.1.1 Nitric Acid — Mix 3 volumes of
colour turns from yellow to blue violet.
concentrated, nitric acid (sp.gr. 1.42) with 997
volumes of distilled water.
Normality of mercuric nitrate solution, N =
C-1.1.2 Mixed Indicator Solution — Dissolve 0.5 g of
where
crystalline diphenylcarbazone and 0.5 g of
bromophenol, blue powder in 100 ml of methyl N = normality of mercuric nitrate solution;
alcohol (95 percent). Store in a brown bottle and n = normality of standard sodium chloride
replace after every 6 months. solution; and
C-1.1.3 Standard Sodium Chloride Solution (0.1 N) V = volume of mercuric nitrate solution, in ml.
— Weigh accurately about 5.844 g (w g) of sodium
chloride (previously dried at 105°C for 2 h and cooled C-1.2 Procedure
in desicator), transfer to 1 000 ml volumetric flask
with the help of distilled water and make up to the Weigh accurately about Mg (for liquid 5g, solid 1.7g)
mark with distilled water. of the sample in a 100 ml beaker and dissolve it in
approximately 30 ml of water, transfer it to a 500 ml
Normality of sodium chloride solution, n = volumetric flask, and dilute with water and make up
C-1.1.4 Mercuric Nitrate Solution (0.1 N) — Dissolve to the mark. Shake well. Pipette out 25 ml of this
17.130 g of mercuric nitrate monohydrate in 50 ml of solution in to a 300 ml Erlenmeyer flask and dilute

5
IS 15573 : 2005

with water to 50 ml. Add 5-10 drops of mixed indicator C-1.3 Calculation
solution and shake the flask. If a blue violet or red
colour develops, add nitric acid (3 : 997) drop-wise Chloride percent =
until the colour changes to yellow. Add 1 ml of excess
acid. Titrate the solution against standard 0.1 N where
mercuric nitrate solution, until the colour of solution V = volume (ml) of mercuric nitrate
turns to blue-violet. Record the volume (say V ml) of solution used in titration;
mercuric nitrate solution used in titration.
N = normality of mercuric nitrate solution; and
M = mass of the material taken for test, in g.

ANNEX D
[Table 1, Sl No. (iv)]
DETERMINATION OF SULPHATE

D-1 PRINCIPLE drop so that the addition is in slight excess and continue
boiling for 4 min to obtain a granular precipitate. Allow to
Sulphate in solution is determined gravimetrically by
stand for 4 h and filter through a weighed sintered glass
precipitation as barium sulphate in acidic medium. crucible G-4. Wash the precipitate repeatedly with hot
D-1.1 Reagents water (at 60-70°C) until the filtrate is chloride free on
testing with silver nitrate solution. Dry to constant mass at
D-1.1.1 Hydrochloric Acid Solution — 105-110°C and weigh.
Approximately 4N.
D-1.3 Calculation
D-1.1.2 Barium Chloride Solution — 10 percent,
w/v. D-1.2 Procedure
Percent sulphate (as SO4) =
Weigh accurately Mg (for liquid about 10 g, for solid
about 2.5 g) of the sample and transfer to a 250 ml where
beaker and dissolve in about 100 ml of water. Adjust M1 = mass of empty crucible, in g;
the pH to 2.0-2.5 by drop-wise addition of the
hydrochloric acid and heat to boil. Add to the boiling M2 = mass of crucible with BaSO4, in g;
solution 10-12 ml of barium chloride solution drop by and M = mass of sample taken, in g.

ANNEX E
[Table 1, Sl No. (v)]
DETERMINATION OF SPECIFIC GRAVITY

E-1 OUTLINE OF THE METHOD glass, having no distortion which may disturb the
reading of hydrometer and its size shall be such
Specific gravity at 25°C temperature by specific gravity
that when the hydrometer is floated in the
hydrometer. In case of dispute, specific gravity shall be cylinder, the distance between any part of the
determined by Pyknometer method as per IS 3506. hydrometer and the inner wall or the bottom
E-1.1 Apparatus surface of cylinder shall be not less than 1 cm.
E-1.1.3 Thermometer — Glass mercurial thermometer
E-1.1.1 Specific Gravity Hydrometer — The hydrometer shall be of scale range — 10 to 110°C. shall
be of scale range 1.1-1.3 (effective scale range
1.150 to 1.250). E-1.2 Procedure
E-1.1.2 Cylinder — The cylinder shall be made of Thoroughly cleaned hydrometer and cylinder before

6
 IS 15573 : 2005
use so as to show the clear meniscus. Proper amount of scale adopting upper edge of the meniscus. Repeat this
sample shall be transferred into the cylinder and kept at measurement 2 to 3 times and the average value of the
25°C. After mixing sample completely with an readings gives the specific gravity of the liquid.
agitating rod, pick up the upper end of the hydrometer,
NOTES
float it on the liquid gently so as it does not adhere any
1 Differences between the measured value of 2 to 3 times
bubbles. After standing quietly, push down and sink it and the average value shall not be more than the value
approximately 2 scale marks in the sample and release. which corresponds to one scale interval.
After the hydrometer has stopped perfectly, read the 2 Fans, etc, should be avoided in surrounding area of the
specific gravity determination.

ANNEX F
[Table 1, Sl No. (vii)]
BULK DENSITY

F-1 PRINCIPLE fingers of one hand, gently grasp the upper portion
of the cylinder and lift it as far as 50 mm height and
Measured amount of powder sample is weighed
let it drop on rubber base pad. Continue lifting and
and expressed weight per unit volume. dropping until 50 complete drops have been given
F-1.1 Apparatus to the cylinder. As soon as 50 drops are completed,
raise the cylinder to eye level and level the cylinder
F-1.1.1 Rubber Base Pad with the material without further knocking and read
F-1.1.2 Funnel — Glass funnel of 12.5 mm diameter. the volume of material.
F-1.1.3 Cylinder — 100 ml measuring glass F-1.3 Calculation
cylinder, with stopper.
F-1.2 Procedure Bulk density, g/ml =
Weigh accurately sufficient sample required to fill where
measuring cylinder up to 100 ml mark. Slip the weighed
M = mass of the material taken for the test, in
sample gently and smoothly through a funnel in
g; and
measuring cylinder (without knocking or squeezing).
Stopper the cylinder properly. With the thumb and V = volume of the material in cylinder after
50 taps, in ml.

ANNEX G
[Table 1, Sl No. (viii)]
DETERMINATION OF MERCURY

G-1 MERCURY ANALYZER METHOD As the cold vapour absorption technique of mercury is
based on absorption of UV radiation by mercury
G-1.0 Outline of the Method atoms, all substances which absorb UV radiation will
Mercury analyzer works on the principle of cold cause the positive error. Vapours of organic
vapour atomic absorption spectrometry technique. compounds like alcohols, ketones, esters and acids and
Mercury ions are reduced to elemental state by water also absorb UV radiation. These can be avoided
stannous chloride and the solution is stirred with suitable traps provided along with the instrument.
vigorously so that an equilibrium is achieved G-1.1 Apparatus
between the mercury in the solution and air phase.
The vapour is then purged into the absorption G-1.1.1 Mercury Analyzer — Based on cold
which is located in the light path of spectrometer. vapour atomic absorption spectrometry technique.

7
IS 15573 : 2005

G-1.2 Reagents G-1.3.4 Blank Preparation

G-1.2.1 Nitric Acid — 10 percent, 5 percent and Transfer 8 ml of 10 percent nitric acid solution and
2 percent v/v. 2 ml of stannous chloride solution to the reaction
G-1.2.2 Concentrated Hydrochloric Acid vessel. Stir it for 5 min. Stop the stirring and take
the reading for the mercury content, if any in the
G-1.2.3 Stannous Chloride — 20 percent (w/v) in 10 blank, repeat the stirring of the blank solution until
percent hydrochloric acid (v/v). Take 20 g stannous no deflection/reading is observed. Take various
chloride in a clean beaker, add 10 ml of concentrated readings for the various known concentration of
hydrochloric acid and dissolve while warming it over a mercury in the aliquots and prepare the graph.
hot plate. Boil for one minute, cool and dilute with
distilled water to make 100 ml. Add 1-2 g of tin metal G-1.4 Procedure
(pellet) after the preparation of the solution. Weigh accurately about 5 g of the liquid sample (or
G-1.2.4 Potassium Permanganate — 4 percent 1.7 g of solid sample) in a 50 ml beaker, dissolve
(w/v) in 10 percent sulphuric acid — Dissolve 20 the sample in 25 ml distilled water and transfer to a
g of potassium permanganate in water and add 250 ml volumetric flask with the help of more
carefully 50 ml of concentrated sulphuric acid. distilled water. Add drop -wise potassium
Make up a volume 500 ml using water. permanganate 4 percent (w/v) till purple colour
G-1.2.5 Hydroxylamine Hydrochloride — 10 remains, shake well and add 2-3 drops of
concentrated nitric acid, mix thoroughly and keep it
percent (w/v).
for 5-10 min. Decolourize the solution by adding
G-1.2.6 Mercuric Chloride — AR grade. drop-wise hydroxylamine hydrochloride solution,
G-1.2.7 Potassium Dichromate — 1 percent (w/v). shake well and make up to the mark with distilled
water. Prepare a fresh blank (see G-1.3.4), stir it for
G-1.3 Preparation of Standard Graph 5 min, stop the stirring take reading for the mercury
content if any in the blank. Transfer 5 ml of the
G-1.3.1 Preparation of Stock Solution
sample solution to the reaction vessel containing
Dissolve 0.135 4 g of mercuric chloride AR grade blank and determine the concentration of the
in 25 ml of 2 percent nitric acid (v/v). Add 1 ml of mercury with the help of the standard graph (see G-
potassium dichromate solution of 1 percent (w/v) 1.3.3). Prepare a blank solution using all reagents in
and make up to 100 ml with 2 percent nitric acid same quantities except sample in a 250 ml
(v/v). 1 ml of this stock solution = 1 mg of Hg. volumetric flask, use distilled water in place of
sample. Make up to mark with distilled water and
G-1.3.2 Preparation of Standard Solution
shake well. Transfer 5 ml of this solution to reaction
Dilute 10 ml of the above stock solution (see G- vessel containing blank in the same way as sample
1.3.1) to 1 000 ml in a volumetric flask, 1 ml of this and calculate mercury content and subtract from
solution, B = 10 microgram of Hg. Further pipette 10 sample result, and take for calculation of mercury
ml of this solution B (1 ml = 10 microgram) to 1 000 content in sample.
ml, which will contain 1 ml = 0.1 microgram/100
nanogram of Hg, keeping 5 percent nitric acid (v/v) G-1.5 Calculation
and 0.10 percent potassium dichromate (w/v)
concentration. This standard solution is generally Mercury
stable for a period of at least a month. (as Hg), ppm =
G-1.3.3 Procedure for Standard Graph
By using the standard solution find out the optical
G-2 ALTERNATE METHOD
density/absorbance for 10, 20, 40, 60, 80, 100, 120, 140,
150, nanograms of mercury. By following the procedure Determine Mercury content by atomic absorption
described below, plot a standard curve indicating mercury spectrophotometer with suitable attachment of metal
in nanograms against optical density. hydride system as prescribed in IS 3025 (Part 48).

8
 IS 15573 : 2005

ANNEX H
[Table 1, Sl No. (viii)]
DETERMINATION OF ARSENIC

H-1 PRINCIPLE a stain obtained with 0.005 mg of arsenic (as As)

[0.009 8 mg of arsenic trioxide as As2O3].
Arsenic is determined by Gutzeit method or by atomic
absorption spectrophotometer, this being referee H-1.2 The limit prescribed in Table 1 shall be taken as
method. not having been exceeded, if the length and intensity
of the stain is not greater than that produced in the
H-1.1 Procedure control sample.
Dissolve 1 g of liquid material (0.33 g of solid material) H-2 REFEREE METHOD
in the minimum amount of water. Carry out test for
By Atomic Absorption Spectrophotometer (AAS),
arsenic as prescribed in IS 2088 using for comparison
follow the method as prescribed in IS 3025 (Part 37).

ANNEX J
[Table 1, Sl No. (viii)]
DETERMINATION OF CADMIUM

J-1 Follow the method by AAS as prescribed in IS 3025 (Part 41).

ANNEX K
[Table 1, Sl No. (viii)]
DETERMINATION OF LEAD

K-1 DETERMINATION OF LEAD (As Pb) K-1.4 Procedure

K-1.1 Principle Weigh accurately 1 g of the liquid material (for powder

0.33 g) and dissolve it in 40 ml of water and transfer to
Lead is determined by comparing the colour produced a 100 ml Nessler cylinder. Add 5 ml of acetic acid. Pass
by the material with hydrogen sulphide against that hydrogen sulphide gas into the solution till colour
produced by a standard lead solution. Alternatively develops. Continue the passing of hydrogen sulphide gas
Lead to be determined by Atomic Absorption till further no more colour is developed. In the second
Spectrophotometer (Referee method). Nessler cylinder, carry out a control test using 3 ml of
K-1.2 Apparatus — Nessler cylinder, 100 ml standard lead solution in place of the sample and same
quantities of the other reagents. Dilute the content of
capacity. K-1.3 Reagents each cylinder to 100 ml and shake well. Compare the
colour produced in the two cylinders.
K-1.3.1 Standard Lead Solution — Dissolve 1.6 g
lead nitrate in water and make up the volume to 1 000 K-1.5 The limit prescribed in Table 1 shall be taken
ml. Transfer exactly 10 ml of the solution to as not having been exceeded if the intensity of colour
volumetric flask and dilute it again with distilled produced with the material is not greater than that
water to 1 000 ml mark. One millilitre of this solution produced in the control test
contains 0.01 mg of lead (as Pb). The dilute solution
K-2 REFEREE METHOD
shall be freshly prepared.
K-1.3.2 Acetic Acid — 1 N (approximately). Determine Lead content by Atomic Absorption
Spectrophotometer as per method given in IS 3025
K-1.3.3 Hydrogen Sulphide Gas (Part 47).

9
IS 15573 : 2005

ANNEX L
[Table 1, Sl No. (viii)]
DETERMINATION OF IRON

L-1 PRINCIPLE L-1.1.5 Dilute Sulphuric Acid — 1 : 5.

Iron reacts with thiocyanate to give a series of L-1.2 Procedure
internally red coloured compounds, which remain
in true solution. Strong acids (hydrochloric acid) Weigh accurately to the nearest Mg (about 10 g of
should be present to compress the hydrolysis. liquid sample and 3.5 g of solid PAC) in a 100 ml
Alternatively Iron may be determined by Atomic beaker, add 5 ml concentrated hydrochloric acid, warm
Absorption Spectrophotometer (Referee method). it and then cool it to room temperature. Transfer it into
100 ml Nessler cylinder. Take distilled water in another
L-1.1 Reagents Nessler cylinder as a blank. Add 5 ml of conc.
hydrochloric acid and 3-4 ml of potassium
L-1.1.1 Concentrated Hydrochloric Acid — (35-
permanganate solution, followed by addition of 10 ml
37 percent). ammonium thiocyanate to both the cylinders and shake.
L-1.1.2 Potassium Permanganate Solution — Dissolve Add distilled water up to the mark. Shake well. Using
2 g of potassium permanganate solution in 1 000 ml a micro pipette, add standard iron solution (1 ml =
of distilled water. 0.1 mg Fe) to the blank till colour matches with that of
L-1.1.3 Ammonium Thiocyanate Solution — Dissolve sample Nessler cylinder.
10 g of ammonium thiocyanate in 100 ml distilled water. L-1.3 Calculation
L-1.1.4 Standard Iron Solution — ( 1 ml = 0.1 mg Iron )
— Standard Iron solution prepared with ferrous Soluble iron compounds as Fe, ppm =
ammonium sulphate hexahydrate [FeSO4 (NH4)2
SO4.6H2O; Molecular weight 392.14 g]. where
Dissolve 0.702 2 g of AR grade ferrous ammonium V = volume of standard iron solution, in ml; and
sulphate hexahydrate in 100 ml of water, add 5 ml of M = mass of sample taken for the test, in g.
dilute sulphuric acid and run in continuously a dilute
solution of potassium permanganate (2 g/l) until a slight L-2 REFEREE METHOD
pink colour remains after stirring well. Dilute it up to Determine Iron content by Atomic Absorption
1 litre and mix thoroughly. Spetrophotometer method as given in IS 3025 (Part 53).

ANNEX M
[Table 1, Sl No. (viii)]
DETERMINATION OF MANGANESE

M-1 PRINCIPLE M-1.2.2 Dilute Phosphoric Acid — 1 : 1 (v/v).

Manganese in sample is oxidized to permanganate, M-1.2.3 Potassium Periodate — AR grade powder.
violet colour of which is compared with standard
M-1.2.4 Concentrated Sulphuric Acid — AR grade.
solution of Manganese visually. Alternatively Mn is
determined by Atomic Absorption M-1.2.5 Standard Manganese Solution —
Spectrophotometer (Referee method). Dissolve 0.307 6 g of manganese sulphate
monohydrate (MnSO4.H2O) in water, add 1 ml of
M-1.1 Apparatus
concentrated sulphuric acid, AR grade, and make
M-1.1.1 Nessler Cylinder, 100 ml capacity. up the volume to 1 000 ml in a volumetric flask.
Dilute 10 ml of this solution to 1 000 ml. One
M-1.2 Reagent millilitre of this solution is equivalent to 0.001
M-1.2.1 Dilute Nitric Acid — 1 : 1 (v/v). mg of manganese (as Mn).
10
 IS 15573 : 2005

M-1.3 Procedure comparison. When V ml of sample solution

Weigh accurately 1 g of sample and dissolve in 100 ml obtained in M-1.3 diluted to 100 ml matches with
beaker, add 30 ml of water and 5 ml of dilute nitric control test solutions obtained in M-1.3.1
acid, heat to boil. Add 10 ml of dilute phosphoric acid Mangenese content is given by following equation:
and 0.6 to 0.8 g of potassium periodate. Again heat the
solution to boiling and then boil for 10 min. Cool the Mn (ppm) =
solution to room temperature. Transfer the solution
complete to a Nessler cylinder, make up the volume to M-1.3.4 If colour intensity of sample solution
100 ml mark. (see M-1.3) is less than control test solution (see
M-1.3.1 Separately carry out a control test using 5 ml
M-1.3.1), dilute suitable quantity (Y ml) of
control test solution to 100 ml so that it matches
of standard manganese solution in place of the sample
the colour intensity of sample solution obtained
and follow the procedure as mentioned above. in M-1.3. Mangenese content in sample is given
M-1.3.2 Compare the intensity of colour produced in the following formula:
with sample (see M-1.3) with that of produced in
the control test (see M-1.3.1). Same intensity of
colour in both solutions indicates Manganese Mn (ppm) =
content in sample as 5 ppm.
M-2 REFEREE METHOD
M-1.3.3 If colour intensity in the sample solution is
higher than the control test Manganese content is Determine Manganese content by Atomic Absorption
estimated by diluting suitable quantity of sample Spetrophotometer as per method given in IS 3025.
solution (see M-1.3) with water to 100 ml for

ANNEX N
[Table 1, Sl No. (viii)]
DETERMINATION OF CHROMIUM

N-1 PRINCIPLE N-1.1.6 Sodium Hydroxide Solution — 30 percent

Chromium hexavalent is reduced to Chromium trivalent (w/v). N-1.1.7 Neutral Sodium Sulphite Solution
by boiling with potassium iodide and sodium sulphite and
co-precipitated with aluminium hydroxide. The
N-1.1.8 Potassium Bichromate — AR grade.
aluminium hydroxide is dissolved in 1:1 sulphuric acid, N-1.1.9 Concentrate Hydrochloric Acid — AR grade.
and chrominium is oxidized to hexavalent form by
N-1.1.10 Aluminium Solution — Dissolve 1 g of
bromine water. Chromium is determined colorimetrically
aluminium metal in a little quantity of AR grade
by reacting with diphenyl carbazide reagent, which gives
hydrochloric acid and dilute, transfer to 1 000 ml
a purple colour with chromium. Alternatively Chromium
volumetric flask and make to the mark with
is determined by Atomic Absorption Spectrophotometer
distilled water. Shake well.
(Referee method).
N-1.2 Procedure
N-1.1 Reagents
N-1.2.1 Weigh accurately about 1 g of the liquid
N-1.1.1 Sulphuric Acid — 1 : 1 (v/v) and 1 : 9 (v/v).
(for solid about 0.33 g) sample in 100 ml beaker,
N-1.1.2 Phosphoric Acid — 1 : 5 (v/v). dissolve in water and transfer in 500 mi volumetric
N-1.1.3 Dephenyl Carbazide Reagent — flask, make up to the mark with water.
Dissolve 0.25 g of diphenyl carbazide and 0.4 g Pipette out 100 ml of sample and transfer it in a 1 000
of phthalic anhydride in 100 ml ethanol. The ml beaker, add 20 ml of potassium iodide and 20 ml
solution is stable for one month. of sulphuric acid and 100 ml of water. Boil for about
10 min. Add sodium sulphite in small portion, to
N-1.1.4 Bromine Water
decolourize the sample. In case the solution turns
N-1.1.5 Potassium Iodide Solution — 16 percent (w/v). brown on further boiling, continue adding sodium

11
IS 15573 : 2005

sulphite solution till the decolourization is stable and is equivalent to 1 microgram of chromium. Take
brown colour of iodine does not appear on boiling. Add various volumes of the standard solution so as to give
sodium hydroxide drop-wise, stir the solution well and 5, 10, 15, 20 and 25 microgram of chromium. Add 15
adjust the pH to 6.0 to 6.5. Allow to settle the complete ml aluminium solution to each dilute to about 50 ml
precipitation. Siphon out the clear solution and collect and add 30 ml 1 : 1 sulphuric acid and 2 ml bromine
the aluminium precipitate in a small beaker. Filter water. Further, add 30 percent sodium hydroxide drop-
through a sintered glass crucible and wash once with wise till the colour disappear and add 2 drops in excess.
water. Dissolve the precipitate by pouring 20 ml of Boil for 5 min and cautiously add 1 : 1 sulphuric acid
boiling sulphuric acid (1 : 9) into the crucible, apply till the bromine colour reappears and add 0.5 ml acid in
suction after 2 to 3 min and again wash with hot water. excess. Again boil for about 20 min until bromine
Collect the filtrate in 250 ml beaker. Add 4 ml bromine colour disappears. Check for bromine, cool and add 1
water and stir well. Decolourize the yellow colour with ml diphenyl carbazide solution and make up the
a few drops of sodium hydroxide solution and add 1 ml volume to 100 ml. Let stand for 15 min and then take
excess. Boil for 5 min and add 1 : 1 sulphuric acid until the reading using 460 nm filter. Find out corresponding
the brownish colour appears. Add 2 ml of the acid in optical density. For adjusting 100 percent transmittance
excess and boil again till brownish colour disappears. use 50 ml water in place of standard solution and
Cool and add 1 ml phosphoric acid. Add 1 ml diphenyl proceed in same manner as above. Plot the optical
carbazide solution and make up the solution to 100 ml densities against the corresponding chromium
shake well. Wait for 10 to 15 min for full colour to concentrations.
develop and then find out the percentage transmittance
on a spectrophotometer using 460 nm green filter and N-1.3 Calculation
calculate the corresponding optical density. From the
standard graph find out the concentration of chromium.
Chromium (as Cr), ppm =
N-1.2.2 Preparation of Standard Graph
Weigh 0.283 g of dried potassium dichromate, dissolve
N-2 REFEREE METHOD
in a little distilled water and dilute to 1 litre. One
millilitre of this solution is equivalent to 0.1 mg of Determine Chromium content by Atomic
chromium (as Cr). Further dilute 10 ml of the above Absorption Spectrophotometer as per method
solution to 1 litre. One millilitre of the diluted solution given in IS 3025 (Part 52).

ANNEX P
[Table 1, Sl No. (ix)]
DETERMINATION OF INSOLUBLE MATTER

P-1 OUTLINE OF THE METHOD the residue free from soluble salts with water.
Dry the crucible along with the residue to
Insoluble matter is determined by dissolving the
constant mass at 105-110°C.
material in water and filtration through tared
Gooch or sintered glass crucible G-4. P-1.2 Calculation
P-1.1 Procedure
Weigh accurately about 10 g of the material, transfer Insoluble matter, percent by mass =
into a 400 ml beaker, add about 200 ml of freshly where
boiled distilled water, and boil the resulting solution
for 15 min. Filter any undissolved residue through a M1 = mass of the residue, in g; and
tared Gooch or sintered glass crucible G-4 and wash M2 = mass of the material taken for the test, in g.

12
 IS 15573 : 2005

ANNEX Q
[Table 1, Sl No. (x)]
DETERMINATION OF pH

Q-1 OUTLINE OF THE METHOD Q-1.1 Procedure

Determination of pH of the solution by means of Q-1.1.1 Take 5 g of the material and dissolve in 100
a suitable pH meter. ml of freshly boiled and cooled distilled water.
Determine thepH of solution by means of a suitable
pre-calibrated pH meter, using glass electrode.

ANNEX R
(Clause 6)
SAMPLING OF POLYALUMINIUM CHLORIDE

R-1 GENERAL REQUIREMENTS OF SAMPLING R-2.3 The container/packages shall be drawn at random
R-1.1 While drawing samples, the following from the lot, and to ensure randomness of sampling
random number table (see IS 4905) may be used, if it is
precautions and directions shall be observed.
not available then following procedure may be adopted.
R-1.2 Sample shall not be taken in an exposed place.
Arrange all the containers in the lot in a systematic
R-1.3 The sampling instrument shall be clean and dry. manner, and starting from any one, count them as
R-1.4 Precaution shall be taken to protect the 1, 2 , up to n where n is the integral part of
material being sampled, the sampling instrument N/n. Every nth container thus counted shall
be included in the sample till the required
and the container for samples from adventitious
number of containers specified in col 2 of
contamination, particularly from absorption of Table 2 is taken out.
water (that is moisture from atmosphere).
R-1.5 To draw a representative sample, the Table 2 Number of Containers to be
content of each container selected from sampling Selected for Sampling
(Clause R-2.2)
shall be mixed thoroughly by suitable means.
R-1.6 The sample container shall be of such a size that Sl Lot Size Number of Containers
No. N to be Selected
these are almost completely filled by the sample. n
R-1.7 The sample shall be placed in clean, dry (1) (2) (3)
and air tight glass, PVC or polythene containers. i) Up to 25 3
R-1.8 Each sample container shall be sealed air-tight ii) 26 to 50 4
iii) 51 to 100 5
after filling, and marked with full details of sampling,
iv) 101 and above 7
the date of sampling and batch number, if any.
R-2 SCALE OF R-3 TEST SAMPLE AND REFERENCE SAMPLE

SAMPLING R-2.1 Lot R-3.1 Polyaluminium Chloride — Powder

Scrap off 50 mm of the material from the top centre and
All the containers in a single consignment of the
then take a sample. The quantity of the material so drawn
material drawn from a single batch of manufacture
shall be not less than 200 g and the mass of total material
shall constitute a lot. If a consignment is declared to
taken out shall not exceed 1 kg. Mix rapidly all the
consist of different batches of manufacture, the
sampled material to constitute the composite sample.
batches shall be marked separately and the groups of
Divide this composite sample into three parts. One of
containers in each batch shall constitute separate lot.
these three sets shall be marked for purchaser, another for
R-2.2 Samples shall be tested from each lot separately the supplier and third for the refree. All these three
for judging the conformity of the material to the samples should have proper label for easy identification.
specific requirements. The number of containers (n) to
R-3.2 Polyaluminium Chloride —
be selected at random from lots at different sizes (N)
shall be in accordance with Table 2. Liquid From tank cars or tank wagons.
13
IS 15573 : 2005

ANNEX S
(Foreword)
COMMITTTEE COMPOSITION
Water Quality Sectional Committee, CHD 13

Organization Representative(s)

Bhabha Atomic Research Centre, Mumbai DR M. SUDERSANAN (Chairman)

All India Institute of Hygiene and Public Health, Kolkata DR P. H. ANANTHANARAYANAN
PROF ARUNABHA MAJUMDER (Alternate)

Bharat Heavy Electricals Ltd, Tiruchirapalli DR R. PATTABHIRAMAN

Central Food & Technological Research Institute, Mysore DIRECTOR

Central Ground Water Board, Faridabad SHRI M. M. GAUMAT

DR B. C. MEHTA (Alternate)

Central Leather Research Institute, Chennai DR GANGA RADHAKRISHNAN

Central Pollution Control Board, Delhi DR S. D. MAKHIJANI

DR R. C. TRIVEDI (Alternate)

Central Pulp and Paper Research Institute, Saharanpur DR A. G. KULKARNI

DR S. PANWAR (Alternate)

Central Salt and Marine Chemical Research Institute, Bhavnagar DR P. S. ANAND

DR S. K. THAMPY (Alternate)

Chembond Drewtreat Ltd, New Delhi DR P. SANYAL

Chemical Consultants, Chennai SHRI S. MAHADEVAN

SHRI M. RAVI KRISHNAN (Alternate)

Consumer Education and Research Centre, Ahmedabad SHRI S. YELLORE

SHRI J. SHISHOO (Alternate)

Department of Public Health & Preventive Medicine, Chennai SHRIMATI A. INDIRANI

Department of Industrial Policy and Promotion, New Delhi Director SHRI V. K. GOEL

General of Health Service (PFA), New Delhi Engineers India Ltd, DIRECTOR

New Delhi DR G. SAHA

SHRI G. V. SWAMY (Alternate)

Grasim Industries Ltd, Nagda SHRI ANAND BHANDARI

SHRI J. K. JAIN (Alternate)

Hindustan Dorr-Oliver Ltd, New Delhi SHRI B. P. MISRA

SHRI R. K. VERMA (Alternate)

Hindustan Lever Ltd, Mumbai DR NIMISH SHAH

DR G. RAMAN (Alternate)
Indian Council of Medical Research (ICMR), New Delhi DR RAKESH MITTAL
DR H. N. SAIYED (Alternate)

Indian Fanners Fertiliser Cooperative Ltd, Allahabad SHRI K. S. S. MOORTHY

SHRI GORAKH SINGH (Alternate)

Indian Institute of Safety and Environment, Bangalore DR R. VENKATESAN

DR S. R. DEVADASAN (Alternate)
Ion Exchange (I) Ltd, Mumbai REPRESENTATIVE

Maharashtra State Electricity Board, Durgapur SHRI TULSHIRAM JAGOBAJI GAIDHA

SHRI M . C . JOSHI (Alternate)

Ministry of Rural Development, Department of Drinking Water ADDITIONAL ADVISER (PHE)

Supply, New Delhi SHRI R. M. DESHPANDE (Alternate)

Ministry of Urban Development & Poverty Alleviation, SHRI SUKANTA KAR

New Delhi
Mohan Meakin Limited, Ghaziabad DR E. K. JAYANARAYANAN
SHRI JITENDRA MOHAN (Alternate)

National Environmental Engineering Research Institute, Nagpur DR M. V. NANOTI

DR S. P. ANDEY (Alternate)

14
 IS 15573 : 2005

Organization Representative(s)

National Thermal Power Corporation Ltd, New Delhi SHRI S. K. GUPTA

ONDEO-Nalco India Ltd, Kolkata DR ASHIS KUMAR SAMADDAR

SHRI R. S. CHAKRABARTI (Alternate)

Padarsh Pharmaccticals Pvt Ltd, Navl Mumbai SHRI MUNEESH CHADDA

SHRI S. Y. PANDIT (Alternate)

Projects & Development India Ltd, Dhanbad SHRI V. P. CHOUDHURY

SHRI R. K. VASHISHT (Alternate)

Shriram Institute for Industrial Research, Delhi DR V. K. VERMA

SHRIMATI MANJEET AGGARWAL (Alternate)

The Fertilizer Association of India, New Delhi DR (MS) B. SWAMINATHAN

Water and Steam Chemistry Lab, Kalpakkam DIRECTOR

Water Technology Mission, New Delhi REPRESENTATIVE

BIS Directorate General DR U. C. SRIVASTAVA, Director & Head (CHD)

[Representing Director General (Ex-officio)]

Member Secretary
DR (SHRIMATI) KANCHAN ANAND
Director (CHD), BIS

15
Bureau of Indian Standards

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harmonious development of the activities of standardization, marking and quality certification of goods
and attending to connected matters in the country.

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reviewed periodically; a standard along with amendments is reaffirmed when such review indicates that
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referring to the latest issue of 'BIS Catalogue' and 'Standards : Monthly Additions'.

This Indian Standard has been developed from Doc : No. CHD 13 (1037).

Amendments Issued Since Publication

Amend No. Date of Issue Text Affected

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