1、INTERNATIONAL STANDARD INTERNATIONAL ORGANIZATION FOR STANDARDIZATION .rilti(i3,1,0,1HAII OPrAH113AUMR I10 AHAPTM3AMI.ORGANISATION INTERNATIONALE DE NORMALISATION Aluminium oxide primarily used for the production of aluminium - Determination of vanadium content - N-Benzoyl-N-phenylhydroxylamine phot
2、ometric method Oxyde dbluminium principalement utilisk pour la production de lbluminium - Dosage du vanadium - Methode pho tomCtriyue P la N-benzoyl-N-phnylhydroxylamine First edition - 1976-09-15 Y ,M : (, f : , ,. ,? ,i.,i ! ?:, I, 3i:, .I ?, J UDC 661.862.22 : 546.881 : 543.42 b Ref. No. IS0 1618
3、-1976 (E) ; Descriptors : aluminium oxide, chemical analysis, determination of content, vanadium, spectrophotometric analysis. ; ) , Price based on 4 pages Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permi
4、tted 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 Committees. Every Member Body intere
5、sted 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 by the Technical Committees are
6、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 being transformed into International
7、 Standards. As part of this process,Technical Committee ISO/TC47 has reviewed IS0 Recommendation R 1618 and found it technically suitable for transformation. International Standard IS0 1618 therefore replaces IS0 Recommendation R 1618-1970 to which it is technically identical. IS0 Recommendation R 1
8、618 was approved by the Member Bodies of the following countries : Australia Austria Belgium Brazil Canada Chile Czechoslovakia Egypt, Arab Rep. of France Germany Greece Hungary India Iran Israel Italy Korea, Rep. of Netherlands New Zealand Norway Peru Poland Portugal Romania South Africa, Rep. of S
9、pain Sweden Switzerland Thailand Turkey United Kingdom U.S.S.R. Yugoslavia No Member Body expressed disapproval of the Recommendation The Member Bodies of the following countries disapproved the transformation of ISO/R 1618 into an International Standard : Romania United Kingdom 0 International Orga
10、nization for Standardization, 1976 l Printed in Switzerland 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 1618-1976 (E) Aluminium oxide prima
11、rily used for the production of aluminium - Determination of vanadium content - N-Benzoyl-N-phenylhydroxylamine photometric method 1 SCOPE AND FIELD OF APPLICATION This International Standard specifies an/V-benzoyl-N-phenyl- hydroxylamine photometric method for the determination of the vanadium cont
12、ent of aluminium oxide primarily used for the production of aluminium. The method is applicable to products having a vanadium content, expr-essed as vzo5t between 0,000 3 and 0,016 % (m/m), provided that the G2D3 and the Ti02 contents do not exceed 0,002 and 0,006 % (m/m) respectively. 1.1 Special c
13、ases (under- study) Cr203 contents greater than 0,002 % (m/m) and TiOp contents greater than 0,006 % (m/m). 2 REFERENCES IS0 802, Aluminium oxide primarily used for the pro- duction of aluminium - Preparation and storage of test samples. IS0 804, Aluminium oxide primarily used for the pro- duction o
14、f aluminium - Preparation of solution for analysis - Method by alkaline fusion. IS0 2927, Aluminium oxide primarily used for the pro- due tion of aluminium - Sampling. 3 PRINCIPLE Preliminary oxidation of the vanadium present in a test portion to vanadium(V) using potassium permanganate in a 4,5 N s
15、ulphuric acid medium. Formation of the vanadium N-benzoyl-N-phenylhydroxyl- amine complex. Extraction of the (violet) coloured complex, by means of chloroform in a 3,5 N hydrochloric acid medium. Photometric measurement of the colout-ed complex at a wavelength of about 524 nm. 4 REAGENTS During the
16、analysis, use only reagents of recognized ana- lytical grade and only distilled water or water of equivalent purity. 4.2 Boric acid (HaBOa), or 4.2.1 Boron trioxide (B,O,). 4.3 Sodium sulphate, anhydrous. 4.4 Chloroform, free from ethanol Purify the chloroform, p approximately I,49 g/ml, by washing
17、it five or six times with a volume of water equal to half the volume of the chloroform treated. Dry on anhydrous calcium chloride and distil, collecting the distillate in a dark glass container. Keep in a cool place (temperature below 25 “C) and away from the light. 4.5 Hydrochloric acid, p approxim
18、ately I,19 g/ml, about 38 % (m/m) solution. 4.6 Sulphuric acid, approximately 16 N solution. Carefully pour 450 ml of sulphuric acid solution, p approximately I,84 g/ml, about 96 % (m/m) solution, into 500 ml of water, cool, dilute to 1 000 ml and mix. 4.7 Sulphuric acid, approximately 8 N solution
19、Carefully pour 225 ml of sulphuric acid solution, p approxi- mately I,84 g/ml, about 96 % (m/m) solution, into approximately 500 ml of water, cool, dilute to 1 000 ml and mix. 4.8 Potassium permanganate, 0,6 g/l solution. 4.9 N-Benzoyl-N-phenylhydroxylamine, 1 g/l solution in chloroform. Dissolve 0,
20、l g of N-benzoyl-A-phenylhydroxylamine in 100 ml of purified chloroform (4.4). 4.10 Vanadium, standard solution corresponding to 1,000 g of V,05 per litre. Weigh, to the nearest 0,001 g, 1 g of V205, previously dried at 110 “C and cooled in a desiccator, transfer it to a beaker of suitable capacity
21、(for example 250 ml) and add 20 ml of a 5 % (m/m) sodium hydroxide solution. After dissolving, acidify with 12 ml of the sulphuric acid solution (4.6), transfer the solution quantitatively to a 1 000 ml one-mark volumetric flask, dilute to the mat k and mix. 1 ml of this standard solution contains I
22、,0 mg of V20s,. 4.1 Sodium carbonate, anhydrous. 1 Copyright International Organization for Standardization Provided by IHS under license with ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IS0 1618-1976 (E) 4.11 Vanadium, standard solution corresponding to 0.1
23、0 g of V205 per litre. Take 50,O ml of the standard solution (4.10), transfer to a 500 ml one-mark volumetric flask, dilute to the mark and mix. 1 ml of this standard solution contains 0,lO mg of VzOs. 4.12 Vanadium, standard solution corresponding to 0,010 g of VZOs per litre. Take 50,O ml of the s
24、tandard solution (4.1), transfer to a 500 ml one-mark volumetric flask, dilute to the mark and mix. 1 ml of this standard solution contains 0,010 mg of V,Os. 5 APPARATUS Ordinary laboratory apparatus and 5.1 Separating funnels, having a very short stem, and of capacity approximately 150 ml. 5.2 Spec
25、trophotometer, or 5.3 Photoelectric absorptiometer, fitted with filters ensuring a maximum transmission between 520 and 530 nm. 6 PROCEDURE 6.1 Aliquot portion of principal solution (test portion) Take 50,O ml of the principal solution P (prepared in accordance with 6.1, 6.2 and 6.3 of IS0 804, but
26、using the sulphuric acid solution (4.7) instead of nitric acid solution to take up the fused mass, and diluting to 250 or 500 ml, according to the V205 content). 6.2 Preparation of the calibration graph 6.2.1 Preparation of standard calorimetric solutions for photometric measurements with a cell of
27、optical path length equal to or greater than 3 cm Into a series of six separating funnels (5.1) which have been completely dried and the taps of which have previously been moistened with the chloroform (4.4), place the volumes of the standard vanadium solution (4.12) indicated in the following table
28、 : Standard vanadium solution (4.12) ml 0* 1 ,oo 2.00 4.00 6,00 8.00 * Compensation solution. 2 Corresponding mass of “2O5 w 0 0,010 0,020 0,040 0,060 0,080 Add to each funnel 20 ml of the sulphuric acid solution (4.6), dilute with water to approximately 70 ml, and cool. (The temperature must not ex
29、ceed 25 “C.) Then add a few (3 or 4) drops of the potassium permanganate solution (4.8) until the solution shows a faintly pink coloration. Stir gently and wait 5 min for complete oxidation of the vanadium to take place. 6.2.2 Colour development In order to avoid reduction of the vanadium, the addit
30、ion of the cooled hydrochloric acid solution to the standard calorimetric solutions must be carried out immediately before extraction of the complex. It is therefore necessary to prepare only one point of the calibration graph at a time. Add 10 ml of the A/-benzoyl-N-phenylhydroxylamine solution (4.
31、9) and, without stirring, 32 ml of the hydro- chloric acid solution (4.5), which has previously been cooled to approximately 10 C. Shake for 1 min and leave to stand until the two phases are completely separate. Draw off the chloroform phase and collect it in a perfectly dry 50 ml one-mark volumetri
32、c flask in which approxi- mately 1 g of the sodium sulphate (4.3) has already been placed. Wash the residual aqueous phase in the separating funnel once by shaking it with IO ml of the chloroform (4.4) in order to extract the last traces of vanadium. Draw off the chloroform phase and collect it in t
33、he same flask, Dilute to the mark with the chloroform, mix, and leave to stand for 10 min. 6.2.3 Photometric measurements Carry out the photometric measurements using either the spectrophotometer (5.2) at a wavelength of about 524 nm, or the photoelectric absorptiometer (5.3) with a suitable filter,
34、 after having adjusted the instrument to zero absorbance against the compensation solution. 6.2.4 Plotting of the calibration graph Plot a graph having, for example, the V20, contents in milligrams per 50 ml of standard calorimetric solution as abscissae and the corresponding values of absorbance as
35、 ordinates. 6.3 Determination 6.3.1 Preparation of the test solution Place the test portion (6.1) in a separating funnel (5.1). Add 20 ml of the sulphuric acid solution (4.6) and proceed as specified in 6.2.1, first paragraph after the table. 6.3.2 Colour development Carry out the colour development
36、 as specified in 6.2.2. 6.3.3 Photometric measurement Carry out the photometric measurement as specified in 6.2.3, after having adjusted the instrument to zero absorbance against the blank test solution (6.4.2). Copyright International Organization for Standardization Provided by IHS under license w
37、ith ISONot for ResaleNo reproduction or networking permitted without license from IHS-,-,-IS0 1618-1976 (E) 6.4 Blank test 6.4.1 Preparation of the solution Prepare the solution for the blank test, in the absence of extra-pure aluminium oxide, by directly dissolving 12 g of the sodium carbonate (4.1
38、) and 4 g of the boric acid (4.2) or 2,25 g of the boron trioxide (4.2.1) in approximately 150 ml of hot water and 30 ml of the sulphuric acid solution (4.7). Boil for 10 min to eliminate the carbon dioxide; allow to cool and transfer the solution quanti- tatively to a volumetric flask of a capacity
39、 equal to that used for the preparation of the principal solution P (see 6.1). Place 36,7 ml of the sulphuric acid solution in a platinum dish of diameter approximately 70 mm, and evaporate until almost dry. Add to the dish a little hot water and 3,3 ml of the sulphuric acid solution. Heat, if neces
40、sary, and after cooling transfer the solution quanti- tatively to the flask containing the solution for the blank test. Cool, dilute to the mark and mix. Take 50,O ml of the solution and proceed as specified in 6.3.1. 6.4.2 Colour development Carry out the colour development as specified in 6.3.2. 7
41、 EXPRESSION OF RESULTS By means of the calibration graph (see 6.2.4). determine the quantity of V,05 corresponding to the value of the photometric measurement of the test solution. The vanadium content, expressed as a percentage by mass of V,O, is given by the formula D m, x- 10 xm, where mO is the
42、mass, in grams, of the test portion taken for the preparation of the principal solution P; 4 is the mass, in milligrams, of V,05 found in the aliquot portion of the principal solution P; D is the ratio between the solution P and the volume of for the determination. 8 TEST REPORT volume of the princi
43、pal the aliquot portion taken 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 feature noted during the determination; d) all operations not included in this International Standard or in th
44、e 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 permitted without license from IHS-,-,-IS0 1618-1976 (E) ANNEX IS0 PUBLICATIONS
45、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 solution for analysis - Method by alkaline fusion. IS0 805 - Determination
46、 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 of absolute density - Pyknometer method. IS0 902 - Measurement of the
47、 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 spectrophotometric method. IS0 1618 - Determination of vanadium content - A/-Benz
48、oyl-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. IS0 2071 - Determination of zinc content - Flame atomic absorption meth
49、od. 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 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 29
