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“The Right to Information, The Right to Live” “Step Out From the Old to the New”

IS 5305 (1969): Method for volumetric determination of

phosphorus [CHD 1: Inorganic Chemicals]

“!ान $ एक न' भारत का +नम-ण”

Satyanarayan Gangaram Pitroda
“Invent a New India Using Knowledge”

“!ान एक ऐसा खजाना > जो कभी च0राया नहB जा सकता ह”

है”
ह
Bhartṛhari—Nītiśatakam
“Knowledge is such a treasure which cannot be stolen”
 IS:5305-l!J@
( Reaffirmed 2003 )
fndian Standard ( Rmffirm* ‘983)

METHOD FOR VOLUMETRIC;

DETERMINATION OF PHOSPHORUS
( Second Reprint JUNE 1988 )

-.
UDC 543.?4:546.18

@I CoPyi& 1969

BUREAU OF INDIAN STANDARDS

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MAR0
NEW DELHI 110002

December 1969 .
 Is:5305-198)

Indian Standard
METHOD FOR VOLUMETRIC
DETERMINATION OF PHOSPHORUS
Chemical Standards Sectional Committee, CDC 1

Chainnan
DR K. L. Mouno~u
Morning Side, Camel’s Back Road, Mussoorie

Manbsrs &Pm-%
SIUU V. J_ BARRE Central Revenues Control Laboratory, New Delhi
SBRI K. S. SU~RAMANIAN( Al&mate )
SHRI V. M. BHUCHAR National Physical Laboratory ( CSIR ), New Delhi
SHRI S. K. BOSE National Test Nouse, Calcutta
Ca~snsr & METALLURGIST,CEN- Railway Board ( Ministry of Railways )
TRAL RAILWAY, PAREL, BOMBAY
ASSISTANTDIRECTOR(.MET ), RDSO, ’
CIWITARANJAN (Alternate)
DIRECTOR Central Agmark Laboratory, Nagpur
DRS. GHOSH IS1 Laboratory, New Delhi
DR N. JAYARAHAN Fssen & Co, Bangalore
SHRI M. R. G. SHARMA ( Al&mate )
DR S. M. KAJI Italah Pvt Ltd, Bombay
SHRI S. S. HONAVAR (Alternate)
DRN.M. KHANNA Central Drug Research Institute ( CSIR ), Lucknow
DR H. S. MAHAL Maharashtra State Forensic Laboratory, Bombay
SHRXS. N. hkTRA Central *Food Laboratory (Ministry of Health,
Fad~x;ta Planning & Urban Develepment ),

DR V. S. K. N~UR Bird & Co Pvt Ltd, Calcutta

SHR~S. BAGCHI ( Altcmati )
DR V. SADASIVAN Bombay Municipal Corporation, Bombay
DR B. R. SANT Regional Research Laboratory I CSIR ),
Bhubaneswar
DR T. P. PRA~AD ( Alfernate)
DR E. R. SAXENA Regional Research Laboratory ( CSIR ), Hyderabad
Da ZAFAR ZAMEEL ( Alternate )
SHR~M. L. SETH ,Institution
\ of Chemists ( India), Calcutta
SHRI SHYAMDAS BAGCHI( Altemarc )
( Continwd on page 2 )

BUREAU OF INDIAN STANDARDS r-

MANAK BHAVAN, 9 BAHADUR SHAH ZAFAR MARG 1
NEW DELHI 110002
18:x305-1969

( Continuedfrom page 1 )
Members R.+resenting

DR R.S. SRIVASTAVA Swasthya Scwa Nideshalaya, Lucknow

DR P. R. SWHARAMAN National Chemical Laboratory ( CSIR ), Poona
SHRXL. R. SUD Ministry of Defence ( DC1 )
SHRI S. G. KAJREKAR( Alternate )
DR J. N. TAYAL Central Indian Pharmacopoeia Laboratory,
Ghaziabad
DR R. T. THAMPY Shri Ram ‘Institute for Industrial Research, Delhi
SHRI D. DAS GUPTA, Director General, BIS ( Ex-o#cio Mrmbcr)
Director ( Chem )
Secretary
SHRI S. ARAVAYUDHAN
Assistant Director ( Chem ),BIS

2
 IS:5305-1969

Indian Standard
METHOD FOR VOLUMETRIC
DETERMINATION OF PHOSPHORUS

0. FOREWORD
0.1This Indian Standard was adopted by the Indian Standards Institution
on 18 September 1969, after the draft finalized by the Chemical Standards
Sectional Committee had been approved by the Chemical Division Council.

0.2 In the determination of phosphorus, it is generally required that the

phosphorus shall be present as orthophosphate. Phosphorus in minerals
is inuariably present as orthophosphate and so requires no special
treatment. In the case of organic phosphorus compounds, initial decom-
position may sometimes be accomplished by treatment with nitric and
perchloric acid or heating with nitric acid and potassium permanganate
If these fail, then more drastic treatment, such as heating with nitric acid
in sealed tubes or fusion with peroxide may be necessary. Use of sulphuric
acid for making solution of the sample shall be avoided.

0.3 When calcium, iron, vanadium, titanium, zirconium, tungsten,

talurium, silicon, selenium and arsenic are present, they interfere
and retard the precipitation of phosphomolybdate. Interference of
calcium and iron may be overcome by either precipitating phosphorus as
magnesium ammonium phosphate in <presence of much ammonium citrate
or separating phosphorus from these elements by precipitation as
ammonium phosphomolybdate in acid media, then the precipitate dissolved
in alkali and phosphate precipitated as magnesium ammonium phosphate.
Interference of elements like vanadium, titanium, zirconium, etc, may be
overcome by employing a large excess of molybdate reagent and allowing a
longer period for precipitation. Silica and arsenic may be eliminated by
using tartaric acid, suitably modifying the method.

0.4 The method of precipitation of phosphorus as ammonium phospho-

molybdate has been used for many years and is still used, especially in the
analysis of minerals, fertilizers and ferrous and non-ferrous metals, It is of
almost universal application.

0.5 Although gravimetric determination by precipitation of phosphorus as

magnesium ammonium phosphate, direct titration of orthophosphata
( phosphoric acid ), direct titration of pyrophosphates (pyrophosphoric acid)
and titration of the reduced acids of phosphorus are still in use for
routine analysis, the ammonium phosphomolybdate method and the

3
 P

ISr5505-1969

quinoline phosphomolybdate method are good for routine analysis so they

have been recommended and prescribed in this standard.
0.6 In reporting the result of a test or analysis made in accordance with
this standard, if the final value, observed or calculated, is to be rounded off,
it shall be done in accordance with IS : 2-1960*.

1. SCOPE
1.1 This standard prescribes the method for the volumetric determination
of phosphorus by using (a) ammonium molybdate, and (b) quinoline.
NOTE- The methodis intendedaa a generalanalyticalmethodand does not apply
to metal analysis whete limits for various interferingelementsand/or radicalsare
prescribed.

2. &UALITY OF REAGENTS
2.1 Unless specified otherwise, pure chemicals and distilled water
( see IS : 1070.1960t ) shall be used in tests.
NOTE- ‘ Pure chemicals’ shall mean chemicals that do not contain impurities
which affect the results of analysis.

3. METHOD A- AMMONIUM PHOSPKOMOLYBDATE METHOD

3.0 Outline of the Method - The solution of the sample is treated at
about 45°C with a large excess of ammonium molybdate solution in the
presence of nitric acid. The precipitated ammonium phosphomolybdate is
suitably washed with dilute potassium nitrate solution, dissolved in an
excess of standard sodium hydroxide and the solution of sodium hydroxide
is titrated with standard hydrochloric acid. The phosphorus is calculated
from the volume of sodium hydroxide solution that was required to react
with the ammonium phosphomo1ybdat.e.
3.1 Reagent8
3.1.1 Phenolphthalein Indicator-See Table 1 of IS : 2263-1962:.
3.1.2 Dilute’J\rric Acid- 10 percent ( v/vi> and 40 percent ( v/v ),
3.1.3 Ammonium N&ate - 10 percent ( w/v ).
3.1.4 Standard Sodium Hydroxide Solution - Carbonate-free, 0.1 N ( see
IS : 2316-1968s ).
3.1.5 Standard Hydrochloric Acid- 0.1 N ( see IS : 2316-1968s).
*Rules for roundingoffnumericalvalues( rsuised ) .
tSpecification for water, distilled quality ( mired ).
SMethods of preparation of indicator solution for volumetric analysis.
OMethods of preparation of standard solutions for calorimetric and volumetric analysis
( mired ).

4
 l!s:5385-1969

3.1.6 Ammonia - sp gr O-90.

3.1.7 Potassium N&ate Solution - 1 percent ( w/v ).
3.1.8 Ammonium Molybdate Solution - Add solution A ( 3.1.8.1) slowly and
with constant stirring to solution B ( 3.1.8.2 ) kept cool in a cold waterbath.
Add 10 ml of ammonium phosphate solut;on ( one gram per litre ) and
keep the solution at least for 24 hours. Filter the solution through What-
man filter paper No. 1 before use.
3.1.8.1 Solution A - Dissolve 100 g of molybdid acid ( MOO,,
85 percent ) or 118 g of ammonium mo!ybdate in a mixture of 145 ml of
concentrated ammonium hydroxide and 270 ml of water. Cool the solution.
3.1.8.2 Solution % -Add 490 ml of concentrated nitric acid to
1 150 ml of water and cool.
3.2 Procedure -Take in an Erlenmeyer flask a clear solution of the
material, prepared as prescribed in the relevant material specification
containing 5 to 10 mg of phosphorus present as orthophosphate in about
100 ml of the solution. Add 10 ml of 10 percent nitric acid and 10 ml of
10 percent ammonium nitrate. Dilute to about 200 ml and heat to 45°C.
Add ammonium molybdate reagent in small quantities with stirring to
precipitate all hosphate present. After the precipitate formed on addition
of the reagent hpas settied, test for completion of precipitation and then add
further 10 ml of reagent ( generally 20 to 30 ml will be sufficient ),
Stopper the flask, shake vigorously for 5 to 10 minutes and allow to stand
for 30 minutes. Filter through a Whatman No. 40 filter paper or paper
pulp. Wash the flask and the precipitate a few times with 1 : 50 nitric acid
and then with 1 percent potassium nitrate solution until a portion of the
filtrate does not decolourise 1 ml of water containing 1 drop of 0.1 N
sodium hydroxide and 1 drop of phenolphthalein. Transfer the paper and
precipitate in the original flask. Add a slight excess of 0.1 N carbonate-
free sodium hydroxide ( say 50 ml ). Disintegrate the filter paper. or pulp
by means of a glass rod. Stopper the flask and shake, if all the precipitate
does not dissolve, a further quantity of standard alkali solution shall be
added. Dilute to approximately 150 ml, add 5 drops of phenolphthalein
indicator, and titrate with standard 0.1 N hydrochloric acid until the pink
colour is completely discharged.
3.2.1 Carry out a blank determination using all reagents but without
the sample in the same manner and simultaneously.

3.3 Calculation
0.134 9 x ( VI - v;I) Jv
Phosphates ( as P ), percent by weight = ----
CY
0.308 8 x ( V, - 16,‘) JV ,
Phosphates ( as P,O, ) =
W- -
IS : 5305 - 1969

where
Vr = volume in ml of 0.1 N hydrochloric acid consumed for the
blank determination,
V, = volume in ml of 0.1 N hvdrochloric acid consumed by
the excess sodium hydroxide solution,
.N= normality of standard hydrochloric acid, aud
W = weight in g of the material contained in the solution
taken for the precipitation.

4. METHOD B - QUINOLINE PHOSPHOMOLYBDATE METHOD

4.0 Outline of the Method- This method involves the formation of
phosphomolybdic acid in a solution free from ammonium salts, followed
by its precipitation as the salt of quinoline. Finally the quinoline
phosphomlybdate is titrated with sodium hydroxide.
4.0.1 General -This method has some advantages over the ammonium
phosphomolybdate method, namely, the precipitate is less soluble than
ammonium phosphomolybdate, of constant composition, free from absorbed
or occluded impurities and free from cations which interfere in the
subsequent titration of the precipitate.
The method is applicable in the presence of calcium, magnesium,
iron, aluminium, alkali salts, citric acid and citrates. Chromium present
up to 18 times the phosphorus content and titanium up to 3.5 times have
no effect on the method. The vanadium shall not exceed one-fifth of the
phosphorus content. Nitric acid may be substituted for hydrochloric acid.
Sulphuric and hydrofluoric acids are deleterious, but the effect of
hydrofluoric acid may be avoided by the addition of boric acid. The
interference of soluble silicates is avoided by the addition of citric acid with
which molybdic acid forms a complex of such stability that its reaction
with silicic acid is prevented, whereas the reaction with phosphoric acid
proceeds normally. The interference of ammonia is avoided in the same
manner.

4.1 Reagents
4.1.X Quinoline Hydrochloride Solution - Add 20 mi of purified quinoline
to 500 ml of hot distilled water acidified with 25 ml of concentrated
hydrochloric acid conforming to IS : 265-1962*. Cool and dilute to one
litre.
4.1.1.1 The quinoline used shall be purified and distilled as follows: s
Dissolve the technical grade quinoline in concentrated hydrochloric
acid and add excess zinc chloride solution. This precipitates i
*Specification for hydrochloric acid ( revisedj .
r

.-
 IS: 5305- 1969

quinoline as a complex salt [ ( C,H,N )z.ZnC1,] and in well-deEned

crystals. Separate and wash the crysta!s with cold di!ute
hydrochloric acid. Regenerate the pure quinoline bv sodium
hydroxide solution. Dry and distil to yield pure and distilled
quinoline.

4.1.2 Citro-MoEybdateReagent - prepared as follows:

a) Dissolve 150 g of sodium molybdate ( Na,Mo0,.2H,O ) in 400 ml
of water
b) Dissolve 250 g of citric acid in 250 to 300 ml of water and 280 ml
of concentrated hydroch!oric acid ( conforming to IS ; 2651962* ).
Pour with stirring solution (a) to solution (b), cool and filter
through a filter pad. A slight greenish colour is obtained on
mixing which may deepen when exposed to sunlight. Add in
drops, a O-5 percent ( w/v) solution of potassium bromate to
discharge the colour. Store the solution in coloured, air-tight,
stoppered glass bottles in the dark.
4.1.3 Mixed Indicator Solution-Mix 3 volumes of alcoholic phenol-
phthalein solution and 1 volume of alcoholic thymol blue solution
( s<e Table 3 of IS : 2263-1962t)
4.1.4 Standard Sodium Hydroxide Solutions- carbonate-free, 0.5 N and
O-1 N ( see IS : 2316-1968$ ).
4.1.5 Standard HydrochloricAcids - 0.5 N and 0.1.N (see IS : 2316-1968$ ).
4.1.6 Dilute HydrochloricAcid - 10 percent, dilute 100 ml of hydrochloric
acid ( conforming to IS ~265-1962” ) to 1 litre with water.
4.2 Procedure -I-Take in a 250-ml conical flask an aliquot of the clear
solution of the material, prepared as prescribed in the relevant material
specification containing about 50 mg of phosphorus pentaoxide ( 30 mg of
P ) present as orthophosphate in about 100 ml ( see Note 1 ). Add 50 ml
of citro-molybdate reagent and bring to boil. Add 5 drops of quinoline
hydrochloride solution, stirring during the addition. Again heat to
boiling and add quinoline hydrochloride solution drop by drop with
constant stirring until 2 ml have been added. To the gently boiling
solution add the quinoline hydrochloride solution few milliiitres at a time
with constant stirring until a total of 60 ml has been added. In this
manner, a coarsely crystalline precipitate is produced. Allow to stand on
the hot-plate for 15 minutes and then cool to room temperature. Filter
through a filter paper or pulp pa.d employing suction and wash the flask,
*Specificationfor hydrochloricacid ( revised ) . ( Since revised).
tMethods of preparationof indicatorsolutionfor volumetricanalysis.
SMethodsof preparationof standard solutionsfor calorimetricand volumetric analysis
\ revised ) .

7
IS : 5305 - 1969

precipitate and filter with cold water until they are free from acid. Transfer
the filter pad and the precipitate to the original flask and rinse the funnel
with water into the flask. If necessary, wipe the funnel with a small piece
of damp filter paper to ensure complete removal of the precipitate and place
the paper in the flask. Dilute to about 100 ml with water. Stopper the flask
and shake it vigorously until the pulp and the precipitate are completely
disintegrated. Remove the stopper and wash it with water, returning the
washings to the flask. From 2 burette add 50 ml of O-5 N standard sodium
hydroxide solution, shaking the !?ask during the addition. Shake vigorously
until all the precipitstc dissolves ( see Note 2 ). Add 1 ml of mixed indicator
solution and titrate the excess of sodium hydroxide solution with 0.5 N
hydrochioric acid until the indicator changes from violet to green-blue and
then very sharply to yellow.
4.2.1 Carry out a blank determination using all reagents, witliout the
sample and using exactly 0.1 N standard sodium hydroxide solution and
O-1 N standard hydrochloric acid instead of 0.5 N acid and 0.5 N alkali.
NOTE 1 ---Thr volume should not exceed 100 ml, as any rrduction in the
concentratkitn of hydrochloric acid may lead to the formation cf a cream coloured
precipitate cf the wrong composition. To avoid such rontaminaticm m the presence of
sulohatec, a higher concentration of hydrccilloric acid is necessary.

KOTF. :’ - Examine the disintegrated paper pulp carcfclly for sprcli~ of undissolved
precipitate which sometimes dissolve 5:in excess cf sodium hydroxidrr with difliculty.

4.3 Calculation
( L-:,- ;’
Phosphates ( as --5---
P ), percent =; 0.059
--__ 65 L- p-t- 1::-__
- cv,
--. 1
by weight
6$’

Phosphates ( as P,O, ), percent

by weight =_._- 1
L_-__-.-.---_.----
0.136 5 rl;l -

w
r2 _ i v, ;- v4 !

where
t; = volume in m! of Cl.5 N sodium hydroxide solution used
with the sample,
V, - volume in ml of 0.5 N hydrochloric acid used with the
sample,
P, = volume in ml of 0.1 N sodium hydroxide used jn the
blank,
V, = volume in ml of 0.1 N hydrochloric acid used in the
blank, and
W = weight in g of the material contained in t!re solution
taken for the precipitation.

8
 (_,

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