ISO-553-1981.pdf
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1、International Standard 553 0 QigjjN INTERNATIONAL ORGANIZATION FOR S.TANDARDlZATlON.MEYHAPOAHAR OPrAHbl3AUMR ll0 CTAHAPT113AUHMRGANlSATlON INTERNATIONALE DE NORMALISATION Manganese ores - Determination of vanadium content - Titrimetric method and phosphotungstovanadate photometric method Minerais de
2、 mangankse - Dosage du vanadium - Mbthode titrimitrique et m - Method II : phosphotungstovanadate photometric method, which is applicable to manganese ores having vanadium contents less than 0,05 % (m/m). This International Standard should be read in conjunction with IS0 4297. 2 References IS0 42961
3、1, Manganese ores - Sampling - Part 1: Increment sampling. 1) IS0 429612, Manganese ores - Sampling - Part 2: Prepara- tion of samples. 1) IS0 4297, Manganese ores and concentrates - Methods of chemical analysis - General instructions. 3 Method I: Titrimetric method 3.1 Principle Oxidation of tetrav
4、alenf vanadium in sulphate solution by potassium permanganate to the pentavalent form. Titration of the pentavalent vanadium with standard volumetric ammonium iron(ll1 sulphate solution in the presence of phenylanthranilic acid or sodium diphenylamine sulphonate as indicator. 3.2 Reagents 3.2.1 Urea
5、. 3.2.2 Sodium carbonate, anhydrous. 3.2.3 Hydrochloric acid, Q I,19 g/ml. 3.2.4 Sulphuric acid, Q I,64 g/ml. 3.2.5 Sulphuric acid, diluted 1 + 1. 3.2.6 Sulphuric acid, diluted 1 + 20. 3.2.7 Phosphoric acid, Q 1,70 g/ml. 3.2.6 Hydrofluoric acid, 40 % (m/m) solution. 3.2.9 Potassium permanganate, 10
6、g/l solution. 3.2.10 Sodium nitrite, 50 g/l solution. 3.2.11 Sodium diphenylamine sulphonate, 0,8 g/l solution. 3.2.12 Ammonium iron(h) sulphate, standard volumetric solution, c(NHq)2Fe(S04)2.6H201 = 0,Ol moM.2) 3.2.12.1 Preparation of the solution Dissolve 4 g of ammonium iron sulphate hexahydrate
7、in the sulphuric acid (3.2.6) and dilute to 1 000 ml with the same acid. 1) At present at the stage of draft. 2) Hitherto expressed as “0,Ol N standard volumetric solution”. 1 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Stan
8、dards 1/9972545001 Not for Resale, 04/27/2007 23:15:16 MDTNo reproduction or networking permitted without license from IHS -,-,- IS0 553-1981 (El 3.2.12.2 Standardization of the solution Take three test portions from a standard sample of manganese ore having a known vanadium content approximately th
9、e same as that of the sample to be analysed and carry out all the stages of the analysis (see 35.2) on them. The titre of the ammonium iron sulphate solution is given by the formula T= Bxm vx 100 where T is the titre of the ammonium iron(ll1 sulphate solution, expressed as grams of vanadium correspo
10、nding to 1 ml of the solution; B is the vanadium content, expressed as a percentage by mass, of the standard sample of manganese ore; m is the mass, in grams, of the test portion from the stan- dard sample; V is the volume, in millilitres, of ammonium iron sulphate solution used. Take as the titre t
11、he average of the three results. 3.2.13 Phenylanthranilic acid, 2 g/l solution. 3.5.2 Determination 3.5.2.1 Dissolve the test portion (3.5.1) in the 300 ml beaker in 30 ml of the hydrochloric acid (3.2.3). Add 25 ml of the sulphuric acid solution (3.2.5) and evaporate until sulphuric acid vapours ap
12、pear. Cool, wash the walls of the beaker with water and evaporate again until sulphuric acid vapours appear. Dissolve the salts in 50 ml of water, filter the insoluble residue and wash six to eight times with the sulphuric acid solution (3.2.6). Place the filter with the residue into the platinum cr
13、uci- ble (3.3.1) and ignite at a temperature of 500 to 600 OC. Moisten the residue in the crucible with water, add 1 to 2 drops of the sulphuric acid (3.2.41, 5 to 7 ml of the hydrofluoric acid solution (3.2.8) and evaporate to dryness. Ignite the residue at a temperature of 500 to 600 OC. Cool, add
14、 2 to 3 g of the sodium carbonate (3.2.21, cover the crucible with a lid and fuse at a temperature of 800 to 900 OC. Extract the fusion in 40 to 50 ml of the sulphuric acid solution (3.2.61, wash the crucible and the lid with water and remove them; add the solution thus obtained to the main solution
15、. 3.5.2.2 Add 10 ml of the phosphoric acid (3.2.7) and several drops of the potassium permanganate solution (3.2.91 to the cool, combined solution until a pink colouration, stable for 1 to 2 min, is obtained. Reduce the excess of potassium per- manganate by adding, drop by drop, the sodium nitrite s
16、olution (3.2.10). Introduce 2 g of the urea (3.2.11, stir, allow to stand for 1 min and add 80 ml of the sulphuric acid solution (3.2.5). Cool the solution, add 6 drops of phenylanthranilic acid solu- tion (3.2.13) or 2 ml of the sodium diphenylamine sulphonate solution (3.2.111, stir for 0,5 to 1 m
17、in, and titrate with the stan- dard volumetric ammonium iron sulphate solution (3.2.12) until the crimson colouring of the solution changes to green. Dissolve while boiling 0,2 g of phenylanthranilic acid in 100 ml of water containing 0,2 g of the sodium carbonate (3.2.2). 3.6 Expression of results
18、3.3 Apparatus Ordinary laboratory apparatus and 3.3.1 Platinum crucible. 3.6.1 Calculation The vanadium (VI content, expressed as a percentage by mass on the dry basis, is given by the formula 3.4 Sample where nv, - v, x 100 XK MO For increment sampling of manganese ores, see IS0 4296/l. For the pre
19、paration of samples, see IS0 4296/2, Use a test sample which has been crushed to a size not ex- ceeding 100 pm (checked on a sieve of appropriate aperture size), and air-dried under laboratory conditions. 3.5 Procedure 3.5.1 Test portion Weigh 1 to 2 g of the test sample into a 300 ml beaker. T is t
20、he titre of the ammonium iron sulphate solution (see 3.2.12.2) ; V, is the volume, in millilitres, of the ammonium iron sulphate solution used in the blank test; V2 is the volume, in millilitres, of the ammonium iron(H) sulphate solution used in the determination; m. is the mass, in grams, of the te
21、st portion; K is the conversion factor for expression of the vanadium content on the dry basis. 2 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/27/2007 23:15:16 MDTNo reproduction or n
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