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Ref. No.: lSO/ R 553 - 1966 (E)
IS0
I NT ERN AT10 NA L O RG A N IZAT I O N FOR STANDARDIZATION
IS0 RECOMMENDATION
R 553
METHODS OF CHEMICAL ANALYSIS OF MANGANESE ORES
DETERMINATION OF VANADIUM CONTENT
1st EDITION
December 1966
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The copyright of IS0 Recommendations and IS0 Standards
belongs to IS0 Member Bodies. Reproduction of these
documents, in any country, may be authorized $herefore only
by the national standards organization of that country, being
a member of ISO.
For each individual country the only valid standard is the national standard of that country.
Printed in Switzerland
Also issued in French and Russian. Copies to be obtained through the national standards organizations.
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BRIEF HISTORY
The IS0 Recommendation R 553, Methods of Chemical Analysis of Manganese Ores-
Determination of Vanadium Content, was drawn up by Technical Committee ISO/TC 65,
Manganese Ores, the Secretariat of which is held by the Komitet Standartov, Mer i Izmeritel’
nyh Priborov pri Sovete Ministrov SSSR (GOST).
Work on this question by the Technical Committee began in 1957 and led, in 1959,
to the adoption of a Draft IS0 Recommendation.
In November 1962, this Draft IS0 Recommendation (No. 542) was circulated to all
L
the IS0 Member Bodies for enquiry. It was approved, subject to a few modifications of an
editorial nature, by the following Member Bodies :
Australia Hungary Romania
Austria India Spain
Burma Iran U.A.R.
United Kingdom
Chile Ireland
Czechoslovakia Italy U.S.S.R.
France Japan Yugoslavia
Germany Poland
No Member Body opposed the approval of the Draft.
The Draft IS0 Recommendation was then submitted by correspondence to the IS0
Council which decided, in December 1966, to accept it as an IS0 RECOMMENDATION.
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iSO/ R 553 - 1966 (E)
IS0 Recommendation R 553 Decem ber 1966
METHODS OF CHEMICAL ANALYSIS OF MANGANESE ORES
DETERMINATION OF VANADIUM CONTENT
(Atomic mass V : 50.95; molecular mass V,O,: 181.90)
This IS0 Recommendation contains three parts :
I. Introduction . section 1
II. Volumetric method of determination of vanadium content . sections 2 to 6
III. Photometric method of determination of vanadium content in the form
of phosphotungstovanadate complex . sections 7 to 10
I. INTRODUCTION
1. GENERAL INSTRUCTIONS
1.1 In the following analyses, use a sample for chemical analysis of air-dried manganese ore,
which has been crushed to a size not exceeding O. 10 mm and checked on a sieve of appropriate
size.
Simultaneously with the collection of the samples for the determination of vanadium, take
three more test samples for the determination of hygroscopic moisture.
Calculate the content of vanadium in ore which is absolutely dry by multiplying the numerical
results of the determination of vanadium by the conversion factor K, as found from the
following formula:
1 O0
K=
100 - A
where A = hygroscopic moisture content, per cent.
1.2 The determination of vanadium in manganese ore is carried out by simultaneously analysing
three samples of ore with two blank determinations to enable a corresponding correction in
the result of the determination to be made.
Simultaneously and under the same conditions, carry out a check analysis of a standard
sample of manganese ore, for vanadium content.
The arithmetical mean of the three results is accepted as the final result.
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IS0 / R 553 - 1966 (E)
The following conditions should be observed :
The maximum difference between the highest and the lowest results should not exceed
double the absolute value of the permissible tolerance on the result of the analysis (for the
corresponding interval of vanadium content), shown in the tables under clauses 6.2 and
10.2, " Accuracy of method ".
The average result of the simultaneous check analysis of the standard sample of manganese
ore for vanadium content should not differ from the result shown in the certificate by more
than the If value of the permissible tolerance (for the corresponding interval of vanadium
content), shown in the tables under clauses 6.2 and 10.2, " Accuracy of method ".
For the analysis take a standard sample of the type of ore to which the sample being analysed
belongs.
1.3 The test samples should be weighed to an accuracy of f 0.0002 g.
1.4 Distilled water should be used during the procedure and for the preparation of solutions.
1.5 Meanings of the following expressions :
hot water (or solution) implies a temperature of the liquid of 60 to 70 OC;
warm water (or solution) implies a temperature of the liquid of 40 to 50 OC;
diluted (1 : l), (1 : 2), (1 : 5), etc. means that
the first figure gives the number of parts by volume of
concentrated acid or some other solution, and
the second figure gives the number of parts by volume of
water.
1.6 Indications as to the concentration of solutions show the quantity of solute (in grammes) in
the corresponding volume of the solvent.
1.7 The following symbols and abbreviations are used:
CP chemically pure
d relative density
g gramme
g/l grammes per litre
1 litre
ml millilitre
N standard solution of normal concentration
nm nanometer
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lSO/ R 553 - 1966 (E)
II. VOLUMETRIC METHOD OF DETERMINATION OF VANADIUM CONTENT
(Vanadium content exceeds 0.05 %)
2. PRINCIPLE OF METHOD
Oxidize tetravalent vanadium in sulphate solution by potassium permanganate to the pentavalent
form. Titrate pentavalent vanadium with double ammonium ferrous sulphate solution in the
presence of the indicator. phenylantranilic acid.
3. REAGENTS REQUIRED
3.1 Urea, CP.
3.2 Sodium carbonate, anhydrous, CP.
3.3 Hydrochloric ocid, CP (d 1.19).
3.4 Sulphuric acid, CP (d 1.84).
3.5 Sulphuric acid, CP, diluted (1 : 1).
3.6 Sulphuric acid, CP, diluted (I : 20).
3.7 Phosphoric acid, CP (d 1.70).
3.8 HydroJEuoric acid, CP (40%).
3.9 Phenylantranilic acid, CP, solution (2 g/l):
0.2 g of the acid is dissolved while boiling in 100 ml of water,
containing 0.2 g of sodium carbonate.
3.10 Potassium permanganate, CP, Solution (10 g/i).
3.11 Sodium nitrite (NaNOJ CP, solution (50 g/l),
3.12 Sodium dyphenylamine sulphonate, CP, solution (0.8 g/l).
3.13 Standard solution 0.01 N of ammonium ferrous sulphate
Fe (”& (SO,), . 6H,O: 4 g of ammonium ferrous sulphate, CP,
are dissolved in one litre of sulphuric acid, diluted (1 : 20).
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IS0 / R 553 - 1966 (E
4. DETER-G THE TITRE OF DOUBLE AMMONIUM FERROUS SULPHATE SOLUTION
OF ORE
AGAINST THE STANDARD SAMPLE
4.1 To determine the titre of ammonium ferrous sulphate solution, take three weighed quantities
of standard sample of manganese ore, the vanadium content of which is close to that of the
analysed sample, and pass them through all the stages of the analysis.
4.2 The titre of ammonium ferrous sulphate solution expressed in grammes of vanadium (T)
is calculated from the following formula:
AG
T=
vx 100
where A = vanadium content in the standard sample of ore, in per cent;
G = mass of the standard sample of ore, in grammes;
V = volume of ammonium ferrous sulphate solution, used for titration of vanadium,
expressed in millilitres.
5. PROCEDURE
5.1 Place 1 to 2 g of manganese ore into a 300 ml beaker and dissolve in 30 ml of hydrochloric
acid (d 1.19). After dissolving add 25 ml of sulphuric acid, diluted (1 : 1), evaporate until
sulphuric acid vapour appears, cool, wash the walls of the flask with water an
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