ISO 900-1977 Aluminium oxide primarily used for the production of aluminium Determination of titanium content Diantipyrylmethane photometric method《主要用于铝生产的氧化铝 .pdf

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1、INTERNATIONAL INTERNATIONAL ORGANIZATION FOR STANDARDIZATION MEXUYHAPOAHAR OPI-AHHJAUWI n0 CTAHAAPTM3AUAW.ORGANISATION INTERNATIONALE DE NORMALISATION Aluminium oxide primarily used for the production of aluminium - Determination of titanium content - Diantipyrylmethane photometric method Oxyde dalu

2、minium principalement utilise pour la production de laluminium - Dosage du titane - Mkthode photometrique au diantipyrylmethane First edition - 1977-10-01 UDC 661.862.22 : 546.82 : 543.42 Ref. No. IS0 900-1977 (E) Descriptors : aluminium oxides, chemical analysis, determination of content, titanium,

3、 spectrophotometric analysis. Price based on 4 pages Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-FOREWORD IS0 (the International Organization for Standardization) is

4、a worldwide federation of national standards institutes (IS0 member bodies). The work of developing International Standards is carried out through IS0 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 th

5、at committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. Draft International Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the

6、IS0 Council. International Standard IS0 900 was developed by Technical Committee ISO/TC47, Chemistry, and was circulated to the member bodies in September 1975. It has been approved by the member bodies of the following countries : Austria Italy Belgium Mexico France Netherlands Germany Poland Hunga

7、ry Romania India South Africa, Rep. of Israel Spain Sweden Switzerland Thailand Turkey United Kingdom No member body expressed disapproval of the document. This International Standard has also been approved by the International Union of Pure and Applied Chemistry (IUPAC). It cancels and replaces IS0

8、 Recommendation R 900-1968, of which it constitutes a technical revision. 0 International Organization for Standardization, 1977 l Printed in Switzerland Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitt

9、ed without license from IHS-,-,-INTERNATIONAL STANDARD IS0 900-1977 (E) Aluminium oxide primarily used for the production of aluminium - Determination of titanium content - Diantipyrylmethane photometric method 1 SCOPE AND FIELD OF APPLICATION This International Standard specifies a diantipyrylmetha

10、ne photometric method for the determination of the titanium content of aluminium oxide primarily used for the production of aluminium. The method is applicable to products having a titanium content, expressed as titanium dioxide (TiO,), equal to or greater than 0,001 % (m/m). 2 REFERENCES IS0 802, A

11、luminium oxide primarily used for the production of aluminium - Preparation and storage of test samples. IS0 804, Aluminium oxide primarily used for the production of aluminium - Preparation of sample solution for analysis - Method by alkaline fusion. 3 PRINCIPLE Alkaline fusion of a test portion an

12、d extraction of the fused mass with sulphuric acid solution. Formation of the titanium-diantipyrylmethane complex in approximately 4,6 N sulphuric acid solution. Photometric measurement of the coloured complex at a wavelength of approximately 420 nm. 4 REAGENTS During the analysis, use only reagents

13、 of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Sodium carbonate, anhydrous. 4.2 Boric acid (HaBOa), or 4.2.1 Sodium tetraborate, anhydrous (Na,B,07). 4.3 Sulphuric acid, approximately 8 N solution. 4.4 Sulphuric acid, approximately 18 N solution 4.5 Ascor

14、bic acid, 30 g/l solution. Use a freshly prepared solution. 4.6 Copper sulphate pentahydrate (CuS0,.5H,O), 50 g/l solution. 4.7 Diantipyrylmethane, 50 g/l hydrochloric acid solution. Dissolve 5 g of 4,4-methylenediantipyrine (diantipyryl- methane) (C,H,N,O,) in 100 ml of approximately 1 N hydrochlor

15、ic acid solution. 4.8 Titanium, standard solution corresponding to 0,400 g of titanium dioxide (TiO,) per litre. Prepare the solution by either of the following two methods : 4.8.1 In a platinum dish of suitable capacity, weigh, to the nearest 0,000 1 g, 0,601 5 g of dipotassium hexafluoro- titanate

16、 (K,TiF,) previously dried at about 50 “C and cooled in a desiccator. Moisten the product with a few drops of water and then add 15 ml of sulphuric acid solution, p approximately I,84 g/ml. Evaporate carefully almost to dryness in a well-ventilated fume cupboard. Repeat the operation until the fluor

17、ine is completely expelled, using each time 5 to 6 ml of the same sulphuric acid solution. Finally, add 3 ml of the same sulphuric acid solution and heat until the residue is completely dissolved. Allow to cool, immerse the dish and its contents in a beaker containing 95 ml of water and 5 ml of the

18、same sulphuric acid solution and heat on a boiling water bath until the solution is completely clear. Remove the platinum dish, wash it carefully with water, transfer the solution and the washings quantitatively to a 500 ml one-mark volumetric flask, dilute to the mark and mix. 1 ml of this standard

19、 solution contains the equivalent of 0,400 mg of TiO,. 4.8.2 Weigh, to the nearest 0,000 1 g , 0,886 5 g of dipotassium titanyl dioxalate dihydrate K,TiO(C,0,)2. 2H,O and place in a Kjeldahl flask of capacity about 100 ml. Add 0,80 g of ammonium sulphate and 10 ml of sulphuric acid solution, p appro

20、ximately I,84 g/ml. Heat carefully until the reaction subsides and then boil for 10 min. 1 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IS0 900-1977 (E) Cool and trans

21、fer the solution quantitatively to a beaker of suitable capacity containing 100 ml of water. Add, drop by drop, approximately 0,l N potassium permanganate solution until the colour of the solution is permanently pink. Transfer the solution quantitatively to a 500 ml one-mark volumetric flask, dilute

22、 to the mark and mix. 1 ml of this standard solution contains the equivalent of 0,400 mg of TiO,. NOTE - If dipotassium hexafluorotitanate or dipotassium titanyf dioxalate dihydrate is not available, the following alternative procedure may be adopted : In a platinum crucible of suitable capacity, we

23、igh, to the nearest 0,000 1 g, 0,200 0 g of titanium dioxide (TiOg) previously calcined at 1 200 “C and cooled in a desiccator. Add 4 g of potassium pryosulphate (K$ig07) and fuse carefully at about 1 2OOC. Allow to cool and place the crucible and contents in a beaker of suitable capacity. Add 100 m

24、l of the sulphuric acid solution (4.4) and heat gently to dissolve the melt. Remove the crucible and wash it with hot water, collecting the washings in the beaker. Transfer the solution and the washings quantitatively to a 500 ml one-mark volumetric flask, dilute to the mark and mix. 4.9 Titanium, s

25、tandard solution corresponding to 0,040 g of titanium dioxide (TiO,) per litre. Transfer 50,O ml of the standard titanium solution (4.8) to a 500 ml one-mark volumetric flask, dilute to the mark and mix. 1 ml of this standard solution contains the equivalent of 0,040 mg of TiO,. Prepare this solutio

26、n at the time of use. 4.10 Titanium, standard solution corresponding to 0,010 g of titanium dioxide (TiO,) per litre. Transfer 25.0 ml of the standard titanium solution (4.9) to a 100 ml one-mark volumetric flask, dilute to the mark and mix. 1 ml of this standard solution contains the equivalent of

27、0,010 mg of TiO,. Prepare this solution at the time of use. 5 APPARATUS Ordinary laboratory apparatus and 5.1 Burette, graduated in 0.05 ml, complying with the requirements of ISO/R 385. 5.2 Spectrophotometer, or 5.3 Photoelectric absorptiometer, fitted with suitable filters, having maximum absorpti

28、on at about 420 nm. 6 PROCEDURE 6.1 Preparation of the test solution (principal solution P) Proceed in accordance with sub-clauses 6.1, 6.2 and 6.3 of IS0 804, replacing the nitric acid solution (4.5 of IS0 804) by the sulphuric acid solution (4.3) and diluting the principal solutions to 250 ml. 6.2

29、 Test portion Place 50.0 ml of the test solution (6.11, containing 1,000 g of the dried sample (see sub-clause 3.3 of IS0 8021, in a 100 ml one-mark volumetric flask. NOTE - If the TiOg content is greater than 0.01 % (m/m), reduce the test portion proportionately and take this into account in the ca

30、lculation of the results. 6.3 Preparation of the calibration graph 6.3.1 Preparation of the standard colorime tric solutions, for photometric measurements using 4 cm cells Into a series of seven 100 ml one-mark volumetric flasks transfer, by means of the burette (5.1). the volumes of the standard ti

31、tanium solution (4.10) shown in the following table : T Standard titanium Corresponding solution mass of (4.101 TiOZ ml mg / iiii g * Compensation solution. Add 25 ml of the sulphuric acid solution (4.4) to each flask. Dilute with water to about 70 ml, add 3 ml of the ascorbic acid solution (4.5) an

32、d 3 drops of the copper sulphate solution (4.6) and mix. Allow to stand for 20 min, add 10 ml of the diantipyrylmethane solution (4.7), dilute to the mark and mix. 6.3.2 Photometric measurements After at least 40 min, carry out the photometric measure- ments using the spectrophotometer (5.2) at a wa

33、velength of about 420 nm or the photoelectric absorptiometer (5.3) fitted with suitable filters, after having adjusted the in- strument to zero absorbance against the compensation solution. NOTE - The absorbance of the solution is stable for about 24 h. 6.3.3 Plotting of the calibration graph Plot a

34、 graph having, for example, the values of the masses, in milligrams, of titanium dioxide (TiO,) contained in 100 ml of standard calorimetric solution, as abscissae and the corresponding values of absorbance as ordinates. 6.4 Determination 6.4.1 Colour development To the test portion (6.2) placed in

35、the 100 ml one-mark volumetric flask, add 20 ml of the sulphuric acid solution (4.4). 3 ml of the ascorbic acid solution (4.5) and 3 drops 2 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without li

36、cense from IHS-,-,-IS0 900-1977 (E) of the copper sulphate solution (4.6) and mix. Allow to stand for 20 min, add 10 ml of the diantipyrylmethane solution (4.7), dilute to the mark and mix. 6.4.2 Photometric measurement After at least 40 min, carry out the photometric measure- ment following the pro

37、cedure specified in 6.3.2, after having adjusted the instrument to zero absorbance against water. 6.5 Blank test 6.5.1 Preparation of the blank test solution Proceed in accordance with sub-clause 6.4.2 of IS0 804, replacing the nitric acid solution (4.5 of IS0 804) by the sulphuric acid solution (4.

38、3) and diluting the solution to 250 ml. 6.5.2 Colour development Proceed as specified in 6.4.1. 6.5.3 Photometric measurement After at least 40 min, carry out the photometric measure- ment following the procedure specified in 6.3.2, after having adjusted the instrument to zero absorbance against wat

39、er. 7 EXPRESSION OF RESULTS From the calibration graph (see 6.3.3). determine the masses of titanium dioxide (TiO,) corresponding to the absorbance of the test solution and to that of the blank test solution. The titanium content, expressed as a percentage by mass of titanium dioxide (TiO,), is give

40、n by the formula ml -m2 250 100 1000 “%irXm, ml -m2 = zmo where m, is the mass, in grams, of the test portion used for the preparation of the test solution (6.1); m, is the mass, in milligrams, of titanium dioxide found in the aliquot portion of the test solution (6.1); m2 is the mass, in milligrams

41、, of titanium dioxide found in a corresponding aliquot portion of the blank test solution. 8 TEST REPORT The test report shall include the following particulars : a) the reference of the method used; b) the results and the method of expression used; c) any unusual features noted during the determina

42、tion; d) any operation not included in this International Standard or in the International Standards to which reference is made, or regarded as optional. 3 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permi

43、tted without license from IHS-,-,-ISO900-1977(E) ANNEX IS0 PUBLICATIONS RELATING TO ALUMINIUM OXIDE PRIMARILY USED FOR THE PRODUCTION OF ALUMINIUM IS0 802 - Preparation and storage of test samples. IS0 803 - Determination of loss of mass at 300 C (conventional moisture). IS0 804 - Preparation of sol

44、ution for analysis - Method by alkaline fusion. IS0 805 - Determination of iron content - l,lO-Phenanthroline photometric method. IS0 806 - Determination of loss of mass at 1 000 and 1 200 C. IS0 900 - Determination of titanium content - Diantipyrylmethane photometric method. IS0 901 - Determination

45、 of absolute density - Pyknometer method. IS0 902 - Measurement of the angle of repose. IS0 903 - Determination of untamped density. IS0 1232 - Determination of silica content - Reduced molybdosilicate spectrophotometric method. IS0 1617 - Determination of sodium content - Flame emission spectrophot

46、ometric method. IS0 1618 - Determination of vanadium content - A/-Benzoyl-N-phenylhydroxylamine photometric method. IS0 2069 - Determination of calcium content - Flame atomic absorption method. ISO/R 2070 - Determination of calcium content - Spectrophotometric method using naphthalhydroxamic acid. I

47、S0 2071 - Determination of zinc content - Flame atomic absorption method. ISO/R 2072 - Determination of zinc content - PAN photometric method. IS0 2073 - Preparation of solution for analysis - Method by hydrochloric acid attack under pressure. IS0 2828 - Determination of fluorine content - Alizarin

48、complexone and lanthanum chloride spectrophotometric method. IS0 2829 - Determination of phosphorus content - Reduced phosphomolybdate spectrophotometric method. IS0 2865 - Determination of boron content - Curcumin spectrophotometric method. IS0 2926 - Particle size analysis - Sieving method. IS0 29

49、27 - Sampling. IS0 2961 - Determination of an adsorption index. IS0 3390 - Determination of manganese content - Flame atomic absorption method. 4 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-