1、INTERNATIONAL STANDARD 805 INTERNATIONAL ORGANlZATlON FOR STANDARDlLATlON .,r.X;, HAPO;IHAR OPI AHI13AUMII nO CTAH;IAPTM3AUMM .OAGANISATION INTERNATIONALE DE NORMALISATON Aluminium oxide primarily used for the production of aluminium - Determination of iron content - I,1 0-Phenanthroline photometric
2、 method Oxyde dbluminium principalement utilisti pour la production de ILluminium - Dosage du fer - MCthode photometrique ij la phPnan throline- 1,lO First edition - 1976-09-15 Y 1, ( : .: , *Q / ,f i v;:I; r3 .L, ,$, 8 -4 :,-: 1 ), .1 , ,L. y 1 1 I,;:,$ j, b ( i; ,3 :A( : ; ( 3; . . ” s 1 , *a UDC
3、661.862.22 : 546.72 : 543.42 Ref. No. IS0 805-1976 (E) Descriptors : aluminium oxide, chemical analysis, determination of content, iron, spectrophotometric analysis. Price based on 4 pages Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo
4、 reproduction or networking permitted without license from IHS-,-,-FOREWORD IS0 (the international Organization for Standardization) is a worldwide federation of national standards institutes (IS0 Member Bodies). The work of developing International Standards is carried out through IS0 Technical Com
5、mittees. 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. Draft International Standards adopted
6、 by the Technical Committees are circulated to the Member Bodies for approval before their acceptance as International 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 bei
7、ng transformed into International Standards. As part of this process, Technical Committee ISO/TC 47 has reviewed IS0 Recommendation R 805 and fount it technically suitable for transformation. International Standard IS0 805 therefore replaces IS0 Recommendation R 805-1968 to which it is technically i
8、dentical. IS0 Recommendation R 805 was approved by the Member Bodies of the following countries : Austria Belgium Brazil Bulgaria Canada Chile Czechoslovakia Egypt, Arab Rep. of France Germany Hungary Korea, Rep. of India Ireland Israel Italy Japan Netherlands Norway Poland Romania South Africa, Rep
9、. of Spain Sweden Switzerland Turkey United Kingdom U.S.A. U.S.S.R. Yugoslavia No Member Body expressed disapproval of the Recommendation. No Member Body disapproved the transformation of ISO/R 805 into an International Standard. 0 International Organization for Standardization, 1976 l Printed in Sw
10、itzerland Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-INTERNATIONAL STANDARD IS0 805-1976 (E) Aluminium oxide primarily used for the production of aluminium - Determi
11、nation of iron content - 1 ,I 0-Phenanthroline photometric method 1 SCOPE AND FIELD OF APPLICATION This International Standard specifies a 1 ,lO-phenanthroline photometric method for the determination of the iron content of aluminium oxide primarily used fat- the production of aluminium. The method
12、is applicable to products having an iron content, expressed as iron( Ill) oxide, equal to or greatel than 0,005 % (m/m). 2 REFERENCES IS0 802, Aluminium oxide primarily used for the production of aluminium - Preparation and storage of test samples. IS0 804, Aluminium oxide primarily used for the pro
13、duction of aluminium - Preparation of solution for analysis - Method by alkaline fusion. IS0 2927, Aluminium oxide primarily used for the production of aluminium - Sampling. 3 PRINCIPLE Preliminary reduction of iron(lll) by means of hydroxyl- ammonium chloride. Formation of the iron( I I)-1 ,lO-phen
14、anthroline complex in a buffered medium (pH value between 3,5 and 4,2). Photometric measurement of the coloured complex at a wavelength of about 510 nm. NOTE Aluminium, elements usually present in aluminium oxide (impurities) and flux do not cause interference. 4 REAGENTS During the analysis, use on
15、ly treagents of recognized analytical grade and only distilled water or water of equivalent purity. 4.1 Hydroxylammonium chloride (NH,OH.HCI), 10 g/l solution. 4.2 l,lO-Phenanthroline hydrochloride monohydrate (C, ,H,N,.HCI.H,O), 2.5 g/l solution. This reagent may be replaced by a 2,5 g/l solution o
16、f l,lO-phenanthroline monohydrate (C12HaN2.H,0). 4.3 Buffer solution, of pH 4,90. Dissolve 272 g of sodium acetate trihydrate (CH,COONa.3H20) in approximately 500 ml of water-. Add 240 ml of glacial acetic acid, p approximately I,05 g/ml, about 17,4 N. Dilute to 1 000 ml and mix. 4.4 Sodium acetate
17、trihydrate (CH,COONa,3H,O), 500 g/l solution. 4.5 Acetic acid solution. Dilute 500 ml of glacial acetic acid, p approximately I,05 g/ml, about 17,4 N, with water to 1 000 ml. 4.6 Iron, standard solution corresponding to 0,200 g of iron( I I I) oxide pet- Iitre. Pt-epat-e this solution by either- of
18、the following two methods : 4.6.1 Weigh, to the nearest 0,001 g, 0,982 g of ammonium iron sulphate hexahydrate (NH,),Fe(S04),.6H,0. Place in a beaker of suitable capacity (for example 100 ml) and dissolve in water. Add 20 ml of a solution of sulphuric acid, p approximately I,84 g/ml, allow to cool,
19、transfer the solution quantitatively to a 1 000 ml one-mark volumetric flask, dilute to the mark and mix. 1 ml of this standard solution contains 0,200 mg of Fe203. 4.6.2 Weigh, to the nearest 0,001 g, 0,200 g of iron(lll) oxide previously ignited at 600 “C and allowed to cool in a desiccator. Place
20、 it in a beaker of suitable capacity (fat example 100 ml), add 10 ml of a hydrochloric acid solution, p appl-oximately 1.19 g/ml, and heat gently until it IS completely dissolved. Allow to cool, transfer the solution quantitatively to a 1 000 ml one-mark volumett-lc flask, dilute to the mark and mix
21、. 1 ml of this standard solution contains 0,200 mg of Fe,O,. 4.7 Iron, standard solution corresponding to 0,010 g of iron(lll) oxide pet- litre. Transfer 50.0 ml of the standard iron solution (4.6) to a 1 000 ml one-mark volumetric flask, dilute to the malk and mix. 1 ml of this standard solution co
22、ntains 0,010 mg of Fe,O,. Prepat-e this solution just before use. 1 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IS0 805-1976 (El 4.8 pH paper, covering the pH range 3
23、,5 to 4.2 at intervals of 0.2 unit. 5 APPARATUS Ordinary laboratory apparatus and 5.1 pH meter. 5.2 Spectrophotometer, or 5.3 Photoelectric absorptiometer, fitted with filters ensuring a maximum transmission between 500 and 520 nm. 6 PROCEDURE 6.1 Aliquot portion of principal solution (test portion)
24、 Depending on the iron content to be determined, place two aliquot portions of the principal solution P (see 6.3 of IS0 804) in a beaker of suitable capacity and in a 100 ml one-mark volumetric flask respectively, according to table 1. TABLE 1 Aliquot portions to be taken Fe203 Principal Correspondi
25、ng content solution P Volume mass of test portion % (m/m) ml ml 9 0,005 to 0.01 250 50.0 1 0.01 to 0,04 500 50,o 0.50 higher than 0.04 500 25.0 0,25 6.2 Blank test Carry out at the same time as the determination and following the same procedure, a blank test using the same quantities of all reagents
26、 as used for the determination. Use the blank test solution free from extra-pure aluminium oxide for taking the aliquot portions (see 6.4.2 of IS0 804). 6.3 Preparation of calibration graph 6.3.1 Preparation of the standard calorimetric solutions, for photometric measurements with a cell of optical
27、path length 1 cm Into each of a series of seven 100 ml one-mark volumetric flasks, place respectively the volumes of standard iron solution (4.7) shown in table 2. TABLE 2 Standard iron solution (4.7) Corresponding mass of Fe,03 ml mg 0” 0 2,5 0,025 5.0 0,050 10.0 0,100 15.0 0.150 20.0 0.200 25,0 0,
28、250 * Compensation solution. Add to each volumetric flask an amount of water sufficient to dilute to approximately 50 ml, then add 5 ml of the hydroxylammonium chloride solution (4.1), 5 ml of the l,lO-phenanthroline solution (4.2) and 25 ml of the buffer solution (4.3). Dilute to the mark and mix.
29、6.3.2 Photometric measurements After 10 min, carry out the photometric measurements using either the spectrophotometer (5.2) adjusted to a wavelength of about 510 nm or the photoelectric absorptiometer (5.3) fitted with suitable filters, after having adjusted the instrument to zero absorbance agains
30、t the compensation solution. 6.3.3 Preparation of calibration graph Plot a graph having, for example, the iron( Ill) oxide content, in milligrams per 100 ml of standard calorimetric solution, as abscissae and the corresponding values of absorbance as ordinates. 6.4 Determination 6.4.1 Preliminary te
31、st for control and adjustment of pH To the aliquot portion of the principal solution placed in the beaker (see 6.1), add an amount of water sufficient to dilute to approximately 60 ml. Then add 5 ml of the hydroxylammonium chloride solution (4.1), 5 ml of the l,lO-phenanthroline solution (4.2) and 2
32、5 ml of the buffer solution (4.3). Check the pH value by means of the pH paper (4.8) or the pH meter (5.1). The value should be between 3.5 and 4,2; if necessary, adjust the pH value by adding slowly, stirring after each addition, the necessary amount either of the sodium acetate solution (4.4) or o
33、f the acetic acid solution (4.5). Note the quantity of reagent added for the pH adjustment and discard the solution. 6.4.2 Colour developmeni To the other aliquot portion of the principal solution placed in the 100 ml one-mark volumetric flask (see 6.1), add the same quantities of all reagents as us
34、ed for the preliminary test (6.4.1). Dilute to the mark and mix. 6.4.3 Photometric measurements After 10 min, carry out the photometric measurements of the test solution (6.4.2) and the blank test solution (6.2) following the procedure specified in 6.3.2, after having adjusted the instrument to zero
35、 absorbance against water (see note in clause 7). 7 EXPRESSION OF RESULTS By reference to the calibration graph (see 6.3.3), read the iron contents corresponding to the values of the photo- metric readings of the principal solution P, and the corresponding blank test solution. 2 Copyright Internatio
36、nal Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IS0 805-1976 (E) The iron content, expressed as a percentage by mass of iron( I I I) oxide, is given by the formula (ml D -m,) x- 10 xm, where
37、 m. is the mass, in grams, of the test portion taken for the preparation of the principal solution P; ml is the mass, in milligrams, of iron(lll) oxide deter- mined in the aliquot portion of the principal solution P taken for the determination; m2 is the mass, in milligrams, of iron(lll) oxide deter
38、- mined in the aliquot portion corresponding to the blank test solution; D is the ratio of the volume of the principal solution P to the volume of the aliquot portion taken for the determination. NOTE - The aliquot portion of the blank test solution after preparation for the photometric determinatio
39、n generally shows a slight coloration. In thiscase, it is advisable to use it as compensation solution. The formula for expression of results then becomes D m, x- 10Xmo where the symbols have the same meaning as in the preceding formula. 8 TEST REPORT The test report shall include the following part
40、iculars : 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 regarded as optional.
41、 3 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IS0 805-1976 (El ANNEX IS0 PUBLICATIONS RELATING TO ALUMINIUM OXIDE PRIMARILY USED FOR THE PRODUCTION OF ALUMINIUM IS0
42、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 - 1.10.Phenanthroline photometric method. IS0 806 - Determinati
43、on 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. IS0 1232 - Determi
44、nation 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-A-phenylhydroxylamine photometric method. IS0 2069 - Determination of calcium
45、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 method. IS0 2073
46、- 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 spectrophotometric m
47、ethod. 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. Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-
