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1、J IS JAPANESE INDUSTRIAL STANDARD Translated and Published by Japanese Standards Association Methods for determination of zirconium in aluminium alloys ICs 77.120.10 Reference number : JIS H 1363 : 2003 (E) PROTECTED BY COPYRIGHT H 1363 : 2003 Foreword This translation has been made based on the ori
2、ginal Japanese Industrial Standard revised by the Minister of Economy, Trade and Industry through deliberations at the Japanese Industrial Standards Committee, as the result of proposal for revision of Japanese Industrial Standard submitted by Japan Aluminium Association (JAA)/ Japanese Standards As
3、sociation (JSA) with the draft being attached, based on the provision of Article 12 Clause 1 of the Industrial Standardization Law applicable to the case of revision by the provision of Article 14. Consequently JIS H 1363 : 1971 is replaced with this Standard. Date of Establishment: 1971-12-01 Date
4、of Revision: 2003-10-20 Date of Public Notice in Official Gazette: 2003-10-20 Investigated by: Japanese Industrial Standards Committee Standards Board Technical Committee on Non-Ferrous Metals JIS H 1363 : 2003, First English edition published in 2004-02 Translated and published by: Japanese Standar
5、ds Association 4-1-24, Akasaka, Minato-ku, Tokyo, 107-8440 JAPAN In the event of any doubts arising as to the contents, the original JIS is to be the final authority. O JSA 2004 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or
6、by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. Printed in Japan PROTECTED BY COPYRIGHT H 1363 : 2003 1 2 3 4 5 5.1 5.2 5.3 5.4 6 6.1 6.2 6.3 6.4 7 Contents Page Scope Normative references General items . Classification
7、of quantitative determination methods . Zirconium diphosphate gravimetric method . Summary . Quantity of sample to be weighed out . Operation Xylenol orange absorptiometry . Summary . Quantity of sample to be weighed out . Operation Method for ICP emission spectrometric analysis Reagents Reagents 1
8、1 1 1 1 1 1 2 2 4 4 4 4 4 6 (i) PROTECTED BY COPYRIGHT JAPANESE INDUSTRIAL STANDARD JIS H 1363 : 2003 Methods for determination of zirconium in aluminium alloys 1 Scope tion of zirconium in aluminium alloys. This Japanese Industrial Standard specifies the methods for determina- 2 Normative reference
9、s The following standards contain provisions which, through reference in this Standard, constitute provisions of this Standard. The most recent editions of the standards (including amendments) indicated below shall be applied. JIS H 1307 Methods for inductively coupled plasma emission spectrometric
10、analysis of aluminium and aluminium alloys JIS H 1351 General rules for chemical analysis of aluminium and aluminium alloy 3 General items accordance with JIS H 1351. The general items common to analytical methods shall be in 4 Classification of quantitative determination methods The quantitative de
11、- termination of zirconium shall be in accordance with any one of the following: a) Zirconium diphosphate gravimetric method This method shall be applied to the sample of zirconium content in the range between not less than 0.05 % (m/m) and not more than 0.25 % (m/m). Xylenol orange absorptiometry T
12、his method shall be applied to the sample of zirconium content in the range between not less than 0.005 % (m/m) and not more than 0.25 % (m/m). Method of ICP emission spectrometric analysis T h i s method shall be applied to the sample of zirconium content in the range between not less than 0.01 % (
13、m/m) and not more than 0.5 % (m/m). b) c) 5 Zirconium diphosphate gravimetric method 5 . 1 Decompose the sample with sodium hydroxide solution, add warm water and separate precipitates of zirconium and the like by filtering. Decompose the precipitates with nitric acid and sulfuric acid, heat to evap
14、orate, allow to gener- ate the white fume of sulfuric acid and, after cooling it as it is, dissolve the salts by adding water. After adjusting the concentration of sulfuric acid in the solution, oxidize titanium with hydrogen peroxide, then add diammonium hydrogen phosphate to settle the precipitate
15、 of zirconium. Separate the precipitate by filtering, dry and ignite to make zirconium diphosphate, and weigh the mass. Summary 5.2 Reagents The reagents shall be as follows: a) Nitric acid b) Nitric acid (l+l) PROTECTED BY COPYRIGHT 2 H 1363 : 2003 Hydrofluoric acid Sulfuric acid Sulfuric acid (l+U
16、 Sodium hydroxide solution Dissolve 200 g of sodium hydroxide in 1 O00 ml of water. Preserve this solution in a bottle of polyethylene and use the superna- tant. Hydrogen peroxide (1+9) Ammonium nitrate solution Dissolve 50 g of ammonium nitrate in 1 O00 ml of water. Diammonium hydrogen phosphate so
17、lution drogen phosphate in 1 O00 ml of water. Dissolve 200 g of diammonium hy- Quantity of sample to be weighed out The quantity of sample to be weighed out shall be 3.00 g and weighed to the nearest 1 mg. 5 . 4 Operation 5 . 4 . 1 Preparation of sample solution The preparation of sample solution sh
18、all be carried out according to the following procedure: Weigh out the sample and transfer it into a beaker (300 mi). Cover it with a watch glass and add 40 ml of sodium hydroxide solution 5.2 f) little by little. When the reaction falls, wash the under surface of watch glass and the inside wall of
19、beaker with water and heat to decompose(1) it. Add approximately 150 ml of warm water and heat, boil for 1 min to 2 min, then separate the precipitate by filtering with a filter paper (class 5 B), and wash the inside wall of beaker and the precipitate on filter paper with warm water twice. Put both
20、the precipitate and the filter paper in the former beaker, add 20 ml of nitric acid and 10 ml of sulfuric acid, cover it with a watch glass, and heat gen- tly to decompose it. Wash the under surface of watch glass with a small amount of water, remove the watch glass and furthermore continue to heat
21、to generate the white fume of sulfuric acid. In the case where organic matter is insuffi- ciently decomposed, and it looks black or brown, after cooling it as it is, add 5 ml of nitric acid, and repeat thermal decomposition. Heat to evaporate until the volume of the solution becomes to 7 ml to 8 ml,
22、 and allow to generate the white fume of sulfuric acid sufficiently. After cooling it as it is, wash the watch glass and the inside wall of beaker with water, make up the volume of solution to approximately 50 ml, and heat to dis- solve the soluble salts (2). After the addition of 50 ml of sulfuric
23、acid (1+1) and 1 ml of hydrogen peroxide (1+9) into the solution, add 15 ml of diammonium hydrogen phosphate solution 5.2 i) while stirring the solution, allow to precipitate zirconium and dilute it approximately to 200 ml with warm water. PROTECTED BY COPYRIGHT 3 H 1363 : 2003 g) After leaving it f
24、or 5 h to 6 h quietly at a warm place for aging of precipitates, separate by filtering with the filter paper (class 5 B) to which a small amount of ash-free pulp is added and wash it sufficiently with ammonium nitrate solu- tion 15.2 h)l. Notes (1) A small amount of undecomposed silicon, precipitate
25、d sponge copper and the like shall be ignored and the operation continued. (2) When insoluble residue is found, filter it with a filter paper (class 5 B), wash it with warm water and then put the filtrate and the washings together to make the main solution and preserve it. Transfer both the residue
26、and the filter paper into a platinum cru- cible (Type No. 30) and reduce the filter paper to ashes by heating them carefully with a burner. After cooling them as they are, add 5 ml of nitric acid (l+l) and decompose the residue by adding ap- proximately 3 ml of hydrofluoric acid little by little. Ad
27、d 2 ml of sulfuric acid (l+l) and heat to evaporate until the white fume of sulfuric acid generates. Furthermore, continue to heat until the generation of white fume of sulfuric acid has nearly finished, and remove hydrofluoric acid completely. After cooling them as they are, transfer a portion of t
28、he solution preserved as the main solution into the platinum cru- cible, dissolve the salts by heating, then transfer it into the beaker containing main solution by using water. Restart the normal proce- dure from 5.4.1 f). 5.4.2 Weighing of mass The weighing of mass shall be carried out according t
29、o the following procedure: a) After igniting a platinum crucible (Type No. 30) at approximately 1 O00 “C for approximately 30 min, cool it as it is in a desiccator to room temperature and weigh the mass. Transfer both the precipitate obtained in 5.4.1 g) and the filter paper into the platinum crucib
30、le of which the mass has been weighed in a). After heating to dry the filter paper, ignite it to reduce it to ashes. Raise the temperature gradually, and finally ignite it at approximately 1 O00 “C for approximately 30 min, then cool it as it is in a desiccator to room temperature and weigh the mass
31、. Repeat this operation until it reaches a constant weight. b) 5.4.3 Blank test The blank test shall not be carried out. 5.4.4 Calculation Calculate the content of zirconium in the sample according to the following formula: x 100 where, Zr : content of zirconium in sample % (mlm) (mz - mi) x 0.344 O
32、 m Zr = ml : mass of platinum crucible obtained in 5.4.2 a) (g) mz : mass obtained in 5.4.2 b) (g) m : quantity of sample weighed out (g) PROTECTED BY COPYRIGHT 4 H 1363 : 2003 6 Xylenol orange absorptiometry 6.1 Decompose the sample with hydrochloric acid and hydrogen per- oxide and take an aliquot
33、 of a portion of the solution. Add perchloric acid to adjust the acidity, add xylenol orange to colorate and measure the absorbance, Summary Reagents Hydrochloric acid (l+l) Nitric acid (l+l) Perchloric acid make it 500 ml with water. Hydrofluoric acid Sulfuric acid (l+l) Aluminium, of which the pur
34、ity is not less than 99.85 % (m/m and which does not contain zirconium. The reagents shall be as follows: Add 280 ml of perchloric acid to proper quantity of water and Hydrogen peroxide Xylenol orange solution Dissolve 0.1 g of xylenol orange in water and dilute it to 100 ml. Put this solution in a
35、brown bottle and preserve at a cool and dark place. Zirconium standard solution (10 pgZr/mi) Dissolve 0.353 g of zirconyl chloride octahydrate (ZrClzO 8Hz0) in 100 ml of hydrochloric acid (l+l), then make it 1 O00 ml accurately with water and make it the stock solution. The concentra- tion of zircon
36、ium in this solution is approximately 100 pg/ml, however, the ac- curate concentration shall be determined by means of gravimetric method. Whenever this stock solution is used, dilute only the required quantity 10 times with water accurately and make it the zirconium standard solution. Quantity of s
37、ample to be weighed out The quantity of sample to be weighed out shall be 0.50 g to the nearest 1 mg. 6.4 Operation 6.4.1 Preparation of sample solution The preparation of sample solution shall be carried out according to the following procedure: a) b) Weigh out the sample and transfer it into a bea
38、ker (300 mi). Cover it with a watch glass, add 25 ml of hydrochloric acid (l+l) and heat it. After the decomposition of the most part of it, add 2 ml of hydrogen peroxide, decompose excess hydrogen peroxide by boilingP), then cool it in running water to room temperature. When insoluble residue is fo
39、und, filter it with a filter paper (class 5 B), wash it with warm water and put the filtrate and the washings together and preserve it as the main solution. c) PROTECTED BY COPYRIGHT 5 H 1363 : 2003 Zirconium content % (mlrn) d) Transfer both the insoluble residue and the filter paper into a platinu
40、m cru- cible (Type No. 301, heat it carefully by a burner to reduce the filter paper to ashes completely. After cooling it as it is, add 5 ml of nitric acid (l+l), add approximately 3 ml of hydrofluoric acid little by little to decompose the residue completely. Add 1 ml of sulfuric acid (l+l) and he
41、at to evaporate it until the white fume generates. Furthermore, continue to heat until the generation of white fume is almost finished, and remove the hydrofluoric acid completely. After cooling it as it is, add approximately 1 ml of hydrochloric acid (l+l) and heat to dissolve the salts, and then t
42、ransfer it into the beaker containing the main so- lution. Aliquot quantity ml e) After cooling it to room temperature, transfer it into a 100 ml volumetric flask and dilute it with water until it reaches the marked line. Note (3) After the decomposition of the sample, take care so as not to heat it
43、 beyond necessity to evaporate acid and not to make large difference in acidity between the sample and the solution for working curve. If hydrofluoric acid remains even slightly in the operation of 6.4.1 d), a negative error will be caused by it. Information : 0.1 or over up to and incl. 0.25 6.4.2
44、Coloration The coloration shall be carried out according to the following procedure: a) Take an aliquot of the solution obtained in 6.4.1 e) into a 50 ml volumetric flask depending on the zirconium content and according to Table 1. 5 10 I I 0.005 or over to and excl. 0.1 I b) Add 10 ml(4) of perchlo
45、ric acid 6.2 c) and dilute the solution to a quantity of approximately 40 ml with water. After adding 5 ml of xylenol orange solution 6.2 h), dilute it with water until it reaches the marked line and leave it for 30 min as it is(5). Notes (4) The concentration of perchloric acid shall be 0.9 mol/L t
46、o 1 molL at the time of colorating. (5) After leaving it for 30 min as it is, measure it within one and a half hours. 6.4.3 Measurement of absorbance Take a portion of the coloration solution ob- tained in 6.4.2 b) into an absorption cell (10 mm) of photometer and measure the absorbance in the neigh
47、borhood of 535 nm in wavelength referring to the reference solution. 6.4.4 Reference solution The solution without addition of zirconium in working curve shall be the reference solution. Prepare it according to 6.4.6. PROTECTED BY COPYRIGHT 6. H 1363 : 2003 6.4.5 Blank test The blank test shall not
48、be carried out. 6.4.6 Preparation of working curve Weigh out 0.50 g of aluminium 6.2 f) and operate according to the procedures from 6.4.1 b) to 6.4.1 e). Take an aliquot of 10 ml or 5 ml of the sample according to the aliquot quantity into several 50 ml volu- metric flasks, add increased amounts fr
49、om O ml to 7 ml (O pg to 70 pg as zirconium) of the zirconium standard solution L6.2 ill in respective flasks, then operate accord- ing to the procedures from 6.4.2 b) to 6.4.3, prepare the relation curve of the ob- tained absorbance to the quantity of zirconium, and make it the working curve. Prepare the working curve and the sample at the same time. 6.4.7 Calculation Obtain the quantity of zirconium from the absorbance obtained in 6.4.3 and the working curve prepared in 6.4.6, and calculate the zirconium con- tent in the sample according to the following formula: A x100 B
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