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IS0
I N T E R N AT I O NA L O R G A N I ZAl I O N FOR STAND AR D I2 Al I O N
IS0 R E CO M M EN DATl O N
'i
R 315
METHODS OF CHEMICAL ANALYSIS OF MANGANESE ORES
DETERMINATION OF NICKEL
1st EDITION
July 1963
COPYRIGHT RESERVED
The copyright of IS0 Recommendations and IS0 Standards
belongs to IS0 Member Bodies. Reproduction of these
documents, in any country, may be authorized therefore only
by the national standards organization of that country, being
a member of BO.
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 31 5, Methods of Chemical Analysis of Manganese Ores-
Determination of Nickel, 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.
Work on this question by the Technical Committee began in 1954 and led, in 1957,
to the adoption of a Draft IS0 Recommendation.
In October 1958, this Draft IS0 Recommendation (No. 248) was circulated to all the
IS0 Member Bodies for enquiry. It was approved by the following Member Bodies:
Austria Hungary Republic of
Bulgaria Ireland South Africa
Burma Italy Romania
Chile Japan Spain
Czechoslovakia Netherlands United Kingdom
France Poland U.S.S.R.
Germ an y Portugal
One Member Body opposed the approval of the Draft: India.
The Draft IS0 Recommendation was then submitted by correspondence to the IS0
Council, which decided, in July 1963, to accept it as an IS0 RECOMMENDATION.
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[SO/ R 315 - 1963 (E)
IS0 Recommendation R 315 July 1963
METHODS OF CHEMICAL ANALYSIS OF MANGANESE ORES
DETERMINATION OF NICKEL
(Atomic mass Ni: 58.69; molecular mass NiO: 74.69)
This IS0 Recommendation contains three parts :
I. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . section 1,
i
II. Gravimetric method, for nickel content exceeding 0.1 per cent . . . . . sections 2 to 5,
III. Colorimetric method, for nickel content below 0.1 per cent . . . . . . sections 6 to 9.
I. INTRODUCTION
1. GENERAL INSTRUCTIONS
1.1 In the following analysis, use a sample for chemical analysis of air-dried manganese ore,
which has been crushed to a size not exceeding 0.10 mm and checked on a sieve of appro-
priate size.
Simultaneously with the collection of samples for the determination of nickel, take three
more test samples for the determination of hygroscopic moisture.
Calculate the content of nickel in ore which is absolutely dry by multiplying the numerical
results of the determination of nickel by the conversion factor K, as found from the following
formula :
100
K=-
100-A
where
A = hygroscopic moisture content, per cent.
1.2 The determination of nickel 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 nickel content.
The arithmetical mean of the three results is accepted as the final result.
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ISO/ R 315 - 1963 (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 nickel content), shown in the tables under clauses 5.2 and 9.2,
" Accuracy of method ".
The average result of the simultaneous check analysis of the standard sample of manganese
ore for nickel content should not differ from the result shown in the certificate by more
than the f value of the permissible tolerance (for the corresponding interval of nickel
content), shown in the tables under clauses 5.2 and 9.2, " 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 and the residues should be weighed to an accuracy of -& 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 :
d
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 : 1, 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
of the solvent.
the corresponding volume
1.7 The following symbols and abbreviations are used:
d relative density
3 gramme
dl grammes per litre
ml millilitre
Illfn millimetre
nm nanometre
PFA pure for analysis
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lSO/ R 315 - 1963 (E)
II. GRAVIMETRIC METHOD
FOR NICKEL CONTENT EXCEEDING 0.1 PER CENT
The method is based on the precipitation of nickel with dimethyl-glyoxime. Iron, manganese
and other elements are converted beforehand into tartrate or citrate complexes.
The precipitate of nickel glyoxime is dried and weighed.
3. REAGENTS REQUIRED
i
3.1 Ammonium hydroxide, PFA (d 0.91).
3.2 Dimethyl-glyoxime, PFA, alcohol solution (10 g/l).
3.3 Hydrochloric acid, PFA (d 1.19).
3.4 Hydrochloric acid, PFA, diluted 1 : 1.
3.5 Hydrochloric acid, PFA, diluted 1 : 5.
3.6 Hydrochloric acid, PFA, diluted 1 : 20.
3.7 Tartaric (citric) acid, PFA, solution (250 g/l).
3.8 Hydrofluoric acid, PFA (40 per cent).
3.9 Sulphuric acid, PFA (d 1.84).
3.10 Sodium carbonate, PFA, anhydrous.
4. PROCEDURE
4.1 Weigh 2 g of manganese ore into a 300 ml beaker and dissolve while heating in 25 ml of
hydrochloric acid (d 1.19). Evaporate the solution until dry, add 10 to 15 ml of hydrochloric
acid (d 1.19) to the dry residue, and evaporate again to dryness.
4.2 Add 10 to 15 ml of hydrochloric acid (d 1.19) to the dry residue, dilute with hot water to
30 to 40 mi, boil until salts are dissolved and then filter off the insoluble residue.
4.3 Wash the filter and residue 5 or 6 times with hot hydrochloric acid, diluted 1 : 20, and 2 or
3 times with hot water. Place in a platinum crucible, and ignite at a temperature of 500 to
600 OC.
4.4 Moisten the residue in the crucible with water, add 1 or 2 drops of sulphuric acid (d 1.84) and
5 to 10 ml of hydrofluoric acid (40 per cent), and evaporate until dry. Heat the residue to a
temperature of 500 to 600 "Cy cool, add 1 to 2 g of anhydrous sodium carbonate, and fuse the
mixture at a temperature of 900 to 1000 OC. Extract the fusion with hydrochloric acid,
diluted 1 : 5.
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lSO/ R 315 - 1963 (E)
4.5 Remove the crucible from the beaker, rinsing
...