1、INTERNATIONAL STANDARD INTERNATIONAL ORGANIZATION FOR STANDARDIZATION .MEXjIYHAPOflHAR OPTAHM3AUMR IlO CTAHAPTM3AUBB.ORGANISATION INTERNATIONALE DE NORMALISATION Aluminium oxide primarily used for the production of aluminium - Determination of calcium content - Flame atomic absorption method Oxyde d
2、aluminium principalement utilise pour la production de Ialuminium - Dosage du calcium Methode par absorption atomique dans la flamme First edition - 1976-08-01 I 4 3, p i 1 i UDC 661.862.22 : 546.41 : 543.42 Ref. No. IS0 2069-1976 (E) Descriptors : aluminium oxide, chemical analysis, determination o
3、f content, calcium, atomic absorption method. 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 Stan
4、dardization) is 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 r
5、epresented on that 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
6、Standards by the IS0 Council. Prior to 1972, the results of the work of the Technical Committees were published as IS0 Recommendations; these documents are now in the process of being transformed into International Standards. As part of this process, Technical Committee lSO/TC 47 has reviewed IS0 Re
7、commendation R 2869 and found it technically suitable for transformation. International Standard IS0 2069 therefore replaces IS0 Recommendation R 2069-1971 to which it is technically identical. IS0 Recommendation R 2069 was approved by the Member Bodies of the following countries : Austria Belgium C
8、zechoslovakia Egypt, Arab Rep. of France Germany Greece Hungary India Iran Israel Italy Korea, Rep. of Netherlands Poland Portugal South Africa, Rep. of Spain Sweden Switzerland Thailand United Kingdom U.S.A. U.S.S.R. No Member Body expressed disapproval of the Recommendation. The Member Body of the
9、 following country disapproved the transformation of ISO/R 2069 into an Internationalstandard : United Kingdom 0 International Organization for Standardization, 1976 l Printed in Switzerland Copyright International Organization for Standardization Provided by IHS under license with ISONot for Resale
10、No reproduction or networking permitted without license from IHS-,-,-INTERNATIONAL STANDARD IS0 2069-1976 (E) Aluminium oxide primarily used for the production of aluminium - Determination of calcium content - Flame atomic absorption method 1 SCOPE AND FIELD OF APPLICATION This International Standar
11、d specifies a flame atomic absorption method for the determination of the calcium content of aluminium oxide primarily used for the production of aluminium. The method is applicable to products having a calcium content, expressed as CaO, equal to or greater than 0,003 % (m/m). 2 REFERENCES IS0 802,
12、Aluminium oxide primarily used for the pro- duction of aluminium - Preparation and storage of test samples. IS0 1617, Aluminium oxide primarily used for the pro- duction of aluminium - Determination ofsodium content - Flame emission spectrophotometric method. IS0 2073, Aluminium oxide primarily used
13、 for the pro- duction of aluminium - Preparation of solution for analysis - Method by hydrochloric acid attack under pressure. IS0 2927, Aluminium oxide primarily used for the pro- duction of aluminium - Sampling. 3 PRINCIPLE Dissolution of a test portion by attack with hydrochloric acid under press
14、ure. Addition of sodium ions to the solution to stabilize the promotion of the emission of calcium, and of lanthanum ions or triethanolamine to increase the sensitivity. Aspiration of the solution into an acetylene/dinitrogen monoxide flame, and determination of the calcium content by spectrophotome
15、tric measurement of the absorption of the 422.7 nm line emitted by a calcium hollow-cathode lamp. For the determination of relatively high CaD contents greater than approximately 0.03 % (m/m), an acetylene/air flame can be used. 4 REAGENTS During the analysis, use only reagents of recognized ana- ly
16、tical grade and only water doubly distilled in borosilicate glass apparatus with ground glass joints, or water of equivalent purity. Avoid the use of lead glass. 4.1 Lanthanum chloride heptahydrate (LaCl,.7H,O), or 4.1 .I Triethanolamine (CH,0HCH2)aN,p approximately 1,130 g/ml. 4.2 Aluminium oxide,
17、of purity greater than 99,95 %, containing less than 0,000 5 % (m/m) of CaO. 4.3 Hydrochloric acid, p approximately 1 ,I9 g/ml, about 38 % (m/m) solution. 4.4 Aluminium, acid solution (main solution). Pickle 11 g of extra pure aluminium (99,999 % purity), in the form of shavings obtained by milling
18、or drilling, in a little nitric acid, p approximately I,40 g/ml, about 68 % (m/m) solution. Wash the pickled shavings with water and then dry them by washing with acetone. Weigh, to the nearest 0,001 g, 10,588 g of these dried shavings, place them in a beaker of suitable capacity (for example 500 ml
19、) and add 144 ml of the hydrochloric acid solution (4.3). Add 1 drop of extra-pure mercury to aid the attack. Wait until the reaction subsides, then place the beaker on a sand bath and maintain a gentle heat until all thealuminium is dissolved. Allow to cool, transfer the solution quanti- tatively t
20、o a 500 ml one-mark volumetric flask, dilute to the mark and mix. 4.5 Calcium, standard solution, corresponding to 1,000 g of CaO per litre. Weigh, to the nearest 0,000 1 g, 1,784 7 g of extra-pure calcium carbonate, previously dried at 250 “C for 2 h and cooled in a desiccator. Place this in a beak
21、er of suitable capacity (for example 600 ml), and dissolve carefully in 10 ml of the hydrochloric acid solution (4.3) and 15 ml of water. Dilute the solution and transfer it quantitatively to a 1 000 ml one-mark volumetric flask. Dilute to the mark and mix. 1 ml of this standard solution contains 1,
22、000 mg of CaO. Store this solution in a bottle of material free from calcium. 1 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-Is0 2069-1976 (El 4.6 Calcium, standard so
23、lution, corresponding to 0,100 g of CaO per litre. Take 100,O ml of the standard calcium solution (4.5), place in a 1 000 ml one-mark volumetric flask, dilute to the mark and mix. 1 ml of this standard solution contains 0,100 mg of CaO. Store this solution in a bottle of material free from calcium.
24、4.7 Calcium, standard solution corresponding to 0,020 g of CaO per litre. Take 100,O ml of the standard calcium solution (4.6), place in a 500 ml one-mark volumetric flask, dilute to the mark and mix. 1 ml of this standard solution contains 0,020 mg of CaO. Prepare this solution just before use. 4.8
25、 Sodium, solution corresponding to 8 g of Nap0 per litre. Weigh, to the nearest 0,000 1 g, 3,770 g of sodium chloride previously dried at 110 “C for 2 h and cooled in a desic- cator. Dissolve in about 200 ml of water and transfer the solution quantitatively to a 250 ml one-mark volumetric flask. Dil
26、ute to the mark and mix. 1 ml of this solution contains 8 mg of Na20. Store this solution in a bottle of material free from calcium and sodium. 5 APPARATUS Ordinary laboratory apparatus of material free from calcium, and 5.1 Apparatus as specified in IS0 2073. 5.2 Burette, graduated in 0.05 ml, conf
27、orming to ISO/R 385. 5.3 Spectrophotometer, atomic absorption type, fitted with an aspirator burner fed with acetylene and dinitrogen monoxide or with acetylene and air (see clause 3). 5.4 .Calcium hollow-cathode lamp. 6 PROCEDURE 6.1 Test portion Weigh, to the nearest 0,001 g, 2 g of the sample dri
28、ed at 300 C (see 3.3 of IS0 802). 6.2 Preparation of the calibration graph Prepare a calibration graph each time a set of samples is analysed. 6.2.1 Preparation of the standard matching solutions Into each of a series of six 100 ml one-mark volumetric flasks, place 50 ml of the acid solution of alum
29、inium (4.4), 5 ml of the sodium solution (4.8), 45.6 g of the lanthanum chloride (4.1) or 10 ml of triethanolamine (4.1 .I) followed respectively by the volumes of the standard calcium solution (4.7) indicated in the following table, measured with the aid of the burette (5.2) : Standard calcium solu
30、tion (4.7) Corresponding mass of CaO w 0” 0 5.0 0.10 12.5 0.25 20.0 0,40 27.5 35.0 0.55 0.70 * Blank test on reagents for preparation of the calibration graph. Dilute to the mark and mix. 6.2.2 Spectrophotometric measurements 6.2.2.1 ADJUSTMENT OF THE INSTRUMENT, FITTED WITH CALCIUM HOLLOW-CATHODE L
31、AMP (5.4) Switch on the current to the instrument (5.3) a sufficient time in advance to ensure stabilization. Adjust the wavelength to about 422.7 nm and also the sensitivity and the aperture of the slit according to the characteristics of the instrument. Adjust the pressure of the acetylene and of
32、the dinitrogen monoxide according to the characteristics of the aspirator burner. 6.2.2.2 SPECTROPHOTOMETRIC MEASUREMENTS Aspirate the series of standard matching solutions (6.2.1) in the flame and for each measure the absorbance. Take care to keep the aspiration rate constant throughout the prepara
33、tion of the calibration graph. Aspirate water through the burner after each measurement. 6.2.3 Plotting the calibration graph Plot a graph having, for example, as abscissae the numbers of milligrams of CaO contained in 100 ml of standard matching solution, and as ordinates, the corresponding values
34、of the absorbances, reduced by the value for the zero term of the standard matching solutions (blank test on reagents for the preparation of the calibration graph). 2 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or netwo
35、rking permitted without license from IHS-,-,-IS0 2069-1976 (El 6.3 Determination 6.3.1 Preparation of the test sol ml is the mass, in milligrams, of calcium oxide found in the blank test solution (6.3.2). Express the result to three places of decimals. 8 TEST REPORT The test report shall include the
36、 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 determination; d) any operation not included in this International Standard or in the International Standards to which reference is made, or regard
37、ed as optional. 3 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-ISO2069-1976 (El ANNEX IS0 PUBLICATIONS RELATING TO ALUMINIUM OXIDE PRIMARILY USED FOR THE PRODUCTION OF
38、 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 solution for analysis - Method by alkaline fusion. IS0 805 - Determination of iron content - l,lO-Phenanthroline photometric method. IS0 80
39、6 - Determination of loss of mass at 1 000 and 1 200 “C. IS0 900 - Determination of titanium content - Diantipyrylmethane photometric method. IS0 901 - Determination of absolute density - Pyknometer method. IS0 902 - Measurement of the angle of repose. IS0 903 - Determination of untamped density. IS
40、0 1232 - Determination of silica content - Reduced molybdosilicate spectrophotometric method. IS0 1617 - Determination of sodium content - Flame emission spectrophotometric method. IS0 1618 - Determination of vanadium content - N-Benzoyl-N-phenylhydroxylamine photometric method. IS0 2069 - Determina
41、tion of calcium content - Flame atomic absorption method. ISO/R 2070 - Determination of calcium content - Spectrophotometric method using naphthalhydroxamic acid. IS0 2071 - Determination of zinc content - Flame atomic absorption method. ISO/R 2072 - Determination of zinc content - PAN photometric m
42、ethod. IS0 2073 - Preparation of solution for analysis - Method by hydrochloric acid attack under pressure. IS0 2828 - Determination of fluorine content - Alizarin complexone and lanthanum chloride spectrophotometric method. IS0 2829 - Determination of phosphorus content - Reduced phosphomolybdate s
43、pectrophotometric method. IS0 2865 - Determination of boron content - Curcumin spectrophotometric method. IS0 2926 - Particle size analysis - Sieving method. IS0 2927 - 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-,-,-
