SIST ISO 4293:2001

Manganese ores and concentrates -- Determination of phosphorus content -- Extraction-molybdovanadate photometric method

The method is applicable to products having phosphorus contents from 0,02 to 0,5 % (m/m). ISO 4293 should be read in conjunction with ISO 4297. Specifies principle, reagents, apparatus, sample, procedure and expression of results.

Minerais et concentrés de manganèse -- Dosage du phosphore -- Méthode photométrique au molybdovanadate avec extraction

Manganove rude in koncentrati - Določevanje fosforja - Ekstrakcijsko-fotometrijska metoda z molibdenovim vanadatom

General Information

• Status: Published
• Publication Date: 31-May-2001
• ICS: 73.060.20 - Manganese ores
• Technical Committee: IRUD - Mining
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Jun-2001
• Due Date: 01-Jun-2001
• Completion Date: 01-Jun-2001
• Ref Project: ISO 4293:1982 - Manganese ores and concentrates - Determination of phosphorus content - Extraction-molybdovanadate photometric method

Relations

• Revised: ISO/R 321:1963 - Methods of chemical analysis of manganese ores - Determination of phosphorus
• Effective Date: 12-May-2008

Overview

SIST ISO 4293:2001 specifies a photometric method using an extraction-molybdovanadate technique for determining phosphorus content in manganese ores and concentrates. This international standard applies to products with phosphorus levels ranging from 0.02% to 0.5% by mass. Designed for accuracy and reproducibility, the method outlines detailed procedures involving sample preparation, chemical reagents, apparatus, and measurement techniques to ensure precise analysis of phosphorus impurities.

Key Topics

• Scope and Applicability
  The method targets manganese ores and concentrates containing phosphorus within 0.02% to 0.5% mass range, essential for quality control in manganese processing. This standard must be used in conjunction with ISO 4297 for comprehensive chemical analysis instructions.

• Analytical Principle
  The determination involves dissolving a sample in hydrochloric and nitric acids, separating silica by evaporation, and removing insoluble residues. Phosphorus is then converted into a phosphovanadomolybdate complex, which is extracted using methyl isobutyl ketone. The complex’s concentration, correlating to phosphorus content, is measured photometrically at 425 nm.

• Required Reagents and Apparatus
  Key chemicals include sodium carbonate, hydrochloric acid (various dilutions), nitric acid, perchloric acid, sulfuric acid, hydrofluoric acid, ammonium vanadate, ammonium molybdate, citric acid, and methyl isobutyl ketone. Essential apparatus includes a spectrophotometer or photometer, platinum crucibles, filtration equipment, and laboratory glassware.

• Sample Preparation
  Samples must be finely ground (<100 µm) and dried under laboratory conditions. Proper sampling as per ISO 4296 (parts 1 and 2) is crucial to ensure representative material for analysis.

• Procedure Highlights

  1. Dissolution of the sample using acids and filtration of insoluble residues.
  2. Recovery and fusion of residues for complete phosphorus extraction.
  3. Chemical treatment to form phosphovanadomolybdate, followed by solvent extraction.
  4. Photometric measurement of the organic phase to quantify phosphorus.

• Calibration & Results Expression
  Phosphorus standards ranging from 0.05 mg to 0.5 mg are prepared to construct a calibration curve. The phosphorus content in samples is calculated using absorbance readings adjusted for blank measurements, with clearly defined tolerance limits to ensure analytical precision.

Applications

• Quality Control in Manganese Production
  Monitoring phosphorus content affects manganese ore quality, influencing downstream metallurgical processes and ensuring compliance with product specifications.

• Mining and Mineral Processing
  Identifying phosphorus levels aids in grade assessment, beneficiation decisions, and environmental management.

• Regulatory Compliance
  Accurate phosphorus measurement supports adherence to mining standards and export regulations, where impurity control is critical.

• Research and Development
  Facilitates material characterization and development of advanced refining methods in manganese metallurgy.

Related Standards

• ISO 4297 - General methods of chemical analysis for manganese ores and concentrates, providing procedural guidelines that complement ISO 4293.
• ISO 4296-1 and ISO 4296-2 - Cover sampling and sample preparation methods essential for reliable phosphorus analysis in manganese materials.
• ISO 4296-11 and ISO 4296-12 - Detail manganese ore sampling operations critical for representative analysis.

---

Keywords: ISO 4293, manganese ores, phosphorus determination, molybdovanadate photometric method, manganese concentrates analysis, phosphorus content testing, photometric analysis, mineral sampling standards, chemical assay manganese, phosphorus impurities measurement.

Standards Content (Sample)

SLOVENSKI STANDARD
01-junij-2001
0DQJDQRYHUXGHLQNRQFHQWUDWL'RORþHYDQMHIRVIRUMD(NVWUDNFLMVNR
IRWRPHWULMVNDPHWRGD]PROLEGHQRYLPYDQDGDWRP
Manganese ores and concentrates -- Determination of phosphorus content -- Extraction-
molybdovanadate photometric method
Minerais et concentrés de manganèse -- Dosage du phosphore -- Méthode
photométrique au molybdovanadate avec extraction
Ta slovenski standard je istoveten z: ISO 4293:1982
ICS:
73.060.20 Manganove rude Manganese ores
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

International Standard
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION.ME)I(L1YHAPO~HAR OPl-AHM3AI.&lR I-IO CTAH~APTbl3AL(MM.ORGANISATION INTERNATIONALE DE NORMALISATION
Manganese ores and concentrates - Determination of
phosphorus content - Extraction-molybdovanadate
photometric method
Mthode photometrique au molybdovanadate avec extraction
Minerais et concentrks de manganese - Dosage du Phosphore -
First edition - 1982-08-15
Ref. No. ISO 4293-1982 (E)
UDC 553.32 + 553.461: 543.4: 546.18
spectrophotometric analysis.
Descriptors : magnese ores, tests, determination of content, phosphorus,
Price based on 3 pages
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of
national Standards institutes (ISO member bedies). The work of developing Inter-
national Standards is carried out through ISO technical committees. Every member
body interested in a subject for which a technical committee has been set up has the
right to be represented on that committee. International organizations, governmental
and non-governmental, in liaison with ISO, also take part in the work.
Braf? International Standards adopted by the technical committees are circulated to
the member bodies for approval before their acceptance as International Standards by
the ISO Council.
International Standard ISO 4293 was developed by Technical Committee ISO/TC 65,
Manganese and chromium ores, and was circulated to the member bodies in June
1981.
lt has been approved by the member bodies of the following countries :
Austria France Romania
Brazil India South Africa, Rep. of
China Spain
Italy
Czechoslovakia Philippines United Kingdom
Egypt, Arab Rep. of Poland USSR
The member body of the ng country exp ressed pproval of the documen t on
technical grounds
Germany, F. R.
0 International Organkation for Standardkation, 1982
Printed in Switzerland
ISO 42934982 (EI
INTERNATIONAL STANDARD
Manganese ores and concentrates - Determination of
phosphorus content - Extraction-molybdovanadate
photometric method
acid and combination of the Solution obtained with the main
1 Scope and field of application
Solution. Evaporation of the Solution to fumes of perchloric
This International Standard specifies an extractionmolyb- acid. Conversion of the phosphorus to phosphovanadomolyb-
date complex.
dovanadate photometric method for the determination of the
phosphorus content of manganese ores and concentrates.
Elimination of the interference by iron and arsenic by addition
of citric acid. Extraction of the phosphovanadomolybdate into
The method is applicable to products having phosphorus con-
tents from 0,02 to 0,5 % bnlm). isobutyl methyl ketone with citric acid present to complex
arsenic and iron.
This International Standard should be read in conjunction with
ISO 4297. Photometric measurement using a spectrophotometer or a
photoelectric absorptiometer.
2 References
4 Reagents
ISO 429611, Manganese ores - Sampling - Part I : lncre-
men t sampkng. 1)
4.1 Sodium carbonate, anhydrous.
ISO 429612, Manganese ores - Sampling - Part 2 : Prepara-
4.2 Hydrochlorit acid, ,Q 1,19 g/ml.
tion of samples. 1)
4.3 Hydrochlorit acid, diluted 1 + 1.
ISO 4297, Manganese ores and concentrates - Methods of
Chemical analysis - General instructions.
4.4 Hydrochlorit acid, diluted 1 + 50.
3 Principle
4.5 Nitrit acid, Q 1,40 g/ml.
Decomposition of a test Portion by treatment with hydrochloric
4.6 Perchlorit acid, Q 1,51 g/ml.
and nitric acids. Separation of Silicon by evaporation to fumes
of perchloric acid. Dissolution of the salts in water, Separation
of the insoluble residue by filtration, the filtrate being reserved
4.7 Sulphuric acid, diluted 1 + 1.
as the main Solution.
4.8 Hydrofluoric acid, Q 1,14 g/ml.
Ignition of the filter with the residue and treatment with
sulphuric and hydrofluoric acids. Fusion of the ignited residue
with sodium carbonate. Dissolution of the melt in hydrochloric 4.9 Ammonium vanadate (NH$O,), 230 g/l Solution.
1) At present at the Stage of draft.
ISO 4293=1982(E)
If the test material does not contain insoluble Phosphates,
4.10 Ammonium molybdate tetrahydrate
discard the filter with the residue obtained.
[(NH4)6M07024~4H20], 150 g/l solution.
4.11 Citric acid [C3H&0H)(COOH)3], 500 g/l Solution.
7.2 Treatment of residue
Transfer the filter and residue to the platinum crucible (5.2), ash
4.12 lsobutyl methyl ketone (CGHJ20).
and ignite at 500 to 600 OC. Allow the crucible to cool, moisten
the residue with 2 or 3 drops of water, add 2 or 3 drops of the
4.13 Phosphorus, Standard solution, corresponding
sulphuric acid Solution (4.7), 5 to 7 ml of the hydrofluoric acid
to 0,l g of P per Iitre.
(4.8) and evaporate to dryness. Ignite the dry residue at 500 to
600 OC, cool, add 1 or 2 g of the sodium carbonate (4.1) and
Place 0,439 4 g of potassium orthophosphate (KH2PO,) (high fuse the residue at 900
...

International Standard
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION.ME)I(L1YHAPO~HAR OPl-AHM3AI.&lR I-IO CTAH~APTbl3AL(MM.ORGANISATION INTERNATIONALE DE NORMALISATION
Manganese ores and concentrates - Determination of
phosphorus content - Extraction-molybdovanadate
photometric method
Mthode photometrique au molybdovanadate avec extraction
Minerais et concentrks de manganese - Dosage du Phosphore -
First edition - 1982-08-15
Ref. No. ISO 4293-1982 (E)
UDC 553.32 + 553.461: 543.4: 546.18
spectrophotometric analysis.
Descriptors : magnese ores, tests, determination of content, phosphorus,
Price based on 3 pages
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of
national Standards institutes (ISO member bedies). The work of developing Inter-
national Standards is carried out through ISO technical committees. Every member
body interested in a subject for which a technical committee has been set up has the
right to be represented on that committee. International organizations, governmental
and non-governmental, in liaison with ISO, also take part in the work.
Braf? International Standards adopted by the technical committees are circulated to
the member bodies for approval before their acceptance as International Standards by
the ISO Council.
International Standard ISO 4293 was developed by Technical Committee ISO/TC 65,
Manganese and chromium ores, and was circulated to the member bodies in June
1981.
lt has been approved by the member bodies of the following countries :
Austria France Romania
Brazil India South Africa, Rep. of
China Spain
Italy
Czechoslovakia Philippines United Kingdom
Egypt, Arab Rep. of Poland USSR
The member body of the ng country exp ressed pproval of the documen t on
technical grounds
Germany, F. R.
0 International Organkation for Standardkation, 1982
Printed in Switzerland
ISO 42934982 (EI
INTERNATIONAL STANDARD
Manganese ores and concentrates - Determination of
phosphorus content - Extraction-molybdovanadate
photometric method
acid and combination of the Solution obtained with the main
1 Scope and field of application
Solution. Evaporation of the Solution to fumes of perchloric
This International Standard specifies an extractionmolyb- acid. Conversion of the phosphorus to phosphovanadomolyb-
date complex.
dovanadate photometric method for the determination of the
phosphorus content of manganese ores and concentrates.
Elimination of the interference by iron and arsenic by addition
of citric acid. Extraction of the phosphovanadomolybdate into
The method is applicable to products having phosphorus con-
tents from 0,02 to 0,5 % bnlm). isobutyl methyl ketone with citric acid present to complex
arsenic and iron.
This International Standard should be read in conjunction with
ISO 4297. Photometric measurement using a spectrophotometer or a
photoelectric absorptiometer.
2 References
4 Reagents
ISO 429611, Manganese ores - Sampling - Part I : lncre-
men t sampkng. 1)
4.1 Sodium carbonate, anhydrous.
ISO 429612, Manganese ores - Sampling - Part 2 : Prepara-
4.2 Hydrochlorit acid, ,Q 1,19 g/ml.
tion of samples. 1)
4.3 Hydrochlorit acid, diluted 1 + 1.
ISO 4297, Manganese ores and concentrates - Methods of
Chemical analysis - General instructions.
4.4 Hydrochlorit acid, diluted 1 + 50.
3 Principle
4.5 Nitrit acid, Q 1,40 g/ml.
Decomposition of a test Portion by treatment with hydrochloric
4.6 Perchlorit acid, Q 1,51 g/ml.
and nitric acids. Separation of Silicon by evaporation to fumes
of perchloric acid. Dissolution of the salts in water, Separation
of the insoluble residue by filtration, the filtrate being reserved
4.7 Sulphuric acid, diluted 1 + 1.
as the main Solution.
4.8 Hydrofluoric acid, Q 1,14 g/ml.
Ignition of the filter with the residue and treatment with
sulphuric and hydrofluoric acids. Fusion of the ignited residue
with sodium carbonate. Dissolution of the melt in hydrochloric 4.9 Ammonium vanadate (NH$O,), 230 g/l Solution.
1) At present at the Stage of draft.
ISO 4293=1982(E)
If the test material does not contain insoluble Phosphates,
4.10 Ammonium molybdate tetrahydrate
discard the filter with the residue obtained.
[(NH4)6M07024~4H20], 150 g/l solution.
4.11 Citric acid [C3H&0H)(COOH)3], 500 g/l Solution.
7.2 Treatment of residue
Transfer the filter and residue to the platinum crucible (5.2), ash
4.12 lsobutyl methyl ketone (CGHJ20).
and ignite at 500 to 600 OC. Allow the crucible to cool, moisten
the residue with 2 or 3 drops of water, add 2 or 3 drops of the
4.13 Phosphorus, Standard solution, corresponding
sulphuric acid Solution (4.7), 5 to 7 ml of the hydrofluoric acid
to 0,l g of P per Iitre.
(4.8) and evaporate to dryness. Ignite the dry residue at 500 to
600 OC, cool, add 1 or 2 g of the sodium carbonate (4.1) and
Place 0,439 4 g of potassium orthophosphate (KH2PO,) (high fuse the residue at 900 to 1 000 OC for 15 to 20 min. Place the
purity) previously dried at 105 OC for 1 to 2 h into a 1 000 ml crucible with the melt in a 100 ml beaker, add 20 ml of the
one-mark volumetric flask, dissolve in 100 ml of water, dilute to
hydrochloric acid Solution (4.3), and heat to dissolve the melt
the mark and mix. completely. Remove the crucible from the beaker and rinse it
with water. Boil the Solution obtained and combine it with the
1 ml of this Standard Solution contains 0,l mg of P.
main Solution (see 7.1).
4.14 Phosphorus, Standard Solution
...

Norme internationale
INTERNATIONAL ORGANlZATlON FOR STANDARDIZATIONWlE~YHAPOJJHAR OPTAHM3AW’lR l-l0 CTAH~APTbl3A~WWORGANISATION INTERNATIONALE DE NORMALISATION
Minerais et concentrés de manganèse - Dosage du
phosphore - Méthode photométrique au
molybdovanadate avec extraction
Manganese ores and concentrates - Determination of phosphorus content - Extraction-molybdovanadate photometric method
Première édition - 1982-08-15
CDU 553.32 + 553.461: 543.4: 546.18
Réf. no : ISO 4293-1982 (FI
Descripteurs : minerai de magnésium, essai, dosage, phosphore, méthode spectrophotométrique.
Prix basé sur 3 pages
Page blanche
ISO 42934982 (F)
NORME INTERNATIONALE
Minerais et concentrés de manganèse T Dosage du
Méthode p-hotométrique au
phosphore -
molybdovanadate avec extraction
1 Objet et domaine d’application 4 Réactifs
La présente Norme internationale spécifie une méthode photo-
4.1 Carbonate de sodium, anhydre.
métrique au molybdovanadate avec extraction, pour le dosage
du phosphore dans les minerais et concentrés de manganèse.
4.2 Acide chlorhydrique, Q 1,19 g/ml.
La méthode est applicable aux produits dont la teneur en phos-
phore est comprise entre 0,OZ et 0,5 % (mlm).
4.3 Acide chlorhydrique, dilué 1 + 1.
La présente Norme internationale devra être lue conjointement
avec I’ISO 4297.
4.4 Acide chlorhydrique, dilué 1 + 50.
2 Réfhences
4.5 Acide nitrique, Q 1,40 g/ml.
ISO 429611, Minerais de manganèse - Échantillonnage -
4.6 Acide perchlorique, Q 1,51 g/ml.
Partie 7 : Échantillonnage par prélèvements. 1)
ISO 429612, Minerais de manganèse - Échantillonnage -
4.7 Acide sulfurique, dilué 1 + 1.
Partie 2 : Préparation des Gchan tillons. 1)
ISO 4297, Minerais et concentrtb de manganèse - Méthodes
4.8 Acide fluorhydrique, ,Q 1,14 g/ml.
Instructions générales.
d’analyse chimique -
4.9 Vanadate d’ammonium (NH4V03), solution
3 Principe à 230 g/l.
Mise en solution d’une prise d’essai par attaque avec les acides
4.10 Molybdate d’ammonium tétrahydraté
chlorhydrique et nitrique. Séparation de la silice par évapora-
[(NH&M070~~.4H201, solution à 150 g/l.
tion jusqu’à l’apparition de vapeurs d’acide perchlorique. Disso-
lution des sels dans l’eau, séparation du résidu insoluble par fil-
tration, le filtrat etant à conserver comme solution principale.
4.11 Acide citrique [C3H,(OH)(COOH)31, solution à
500 g/l.
Incinération du filtre contenant le résidu, calcination et attaque
avec les acides sulfurique et fluorhydrique. Fusion du résidu
calciné avec du carbonate de sodium. Dissolution du culot de 4.12 Méthylisobutylc6tone (CGH120).
fusion par l’acide chlorhydrique et réunion de la solution obte-
nue a la solution principale. Évaporation de la solution jusqu’à
4.13 Phosphore, solution étalon correspondant à 0,l g de P
l’apparition de vapeurs d’acide perchlorique. Transformation
par litre.
du phosphore en un complexe phosphovanadomolybdate.
Introduire, dans une fiole jaugée de 1 000 ml, 0,439 4 g
Élimination de l’influence du fer et de l’arsenic par addition
d’orthophosphate de potassium (KH,PO,) (de haute pureté), .
d’acide citrique. Extraction du complexe phosphovanado-
préalablement séché à 105 OC durant 1 à 2 h, dissoudre dans
molybdate par la méthylisobutylcétone.
100 ml d’eau, compléter au volume et homogénéiser.
Mesurage photométrique au moyen d’un spectrophotomètre
. .
1 ml de cette solution étalon contient 0,l mg de P.
ou d’un photométre.
1) Actuellement au stade de projet.

ISO 42934982 (FI
4.14 Phosphore, solution étalon correspondant à 0,05 g de 7 ml d’acide fluorhydrique (4.8) et évaporer jusqu’à siccité. Cal-
P par litre. ciner le résidu sec entre 500 et 600 OC, refroidir, ajouter 1 à 2 g
de carbonate de sodium (4.1) et fondre le résidu entre 900 et
1 000 OC durant 15 à 20 min. Introduire le creuset contenant le
Introduire 50 ml de la solution étalon de phosphore (4.13) dans
une fiole jaugée de 100 ml, compléter au volume avec de l’eau culot de fusion dans un bécher de 100 ml, ajouter 20 ml de la
solution d’acide chlorhydrique (4.3) et chauffer pour dissoudre
et homogénéiser.
complétement le culot de fusion. Retirer le creuset du bécher et
1 ml de cette solution étalon contient O,O5 mg de P. le rincer avec de l’eau. Faire bouillir la solution obtenue et
l’ajouter à la solution principale (voir 7.1).
7.3 Extracti on du complexe phosp hovanado-
5 Appareillage
molybdate
Matériel courant de laboratoire, et
Évaporer la solution réunie jusqu’à l’apparition d’abondantes
vapeurs blanches d’acide perchlorique au-dessus de la fiole
conique, refroidir, ajouter 25 ml d’eau et 5 ml d’acide nitrique
51 . Spectrophotomètre, ou photomètre.
(4.51, et faire bouillir durant 5 min.
5.2 Creuset en platine.
Dans le cas de teneurs en phosphore supérieures à
0,08 % (mlm), transvaser la solution réunie dans une fiole jau-
gée de 200 ml, compléter au volume avec de l’eau et homogé-
néiser. Transférer une partie aliquote de 20 ml dans une fiole
conique de 125 ml, ajouter 9 ml d’acide perchlorique (4.6) et
6 Échantillon
évaporer jusqu’à l’apparition d’abondantes vapeurs d’acide
perchlorique. Après refroidissement de la solution, ajouter
Pour l’échantillonnage des minerais de manganèse, voir
25 ml d’eau, 5 ml d’acide nitrique (4.5) et faire bouillir durant
ISO 4296/1. Pour la préparation des é
...