《JIS-H-1364-2002-R2007-ENG.pdf》由会员分享，可在线阅读，更多相关《JIS-H-1364-2002-R2007-ENG.pdf（13页珍藏版）》请在三一文库上搜索。
1、JAPANESE I NDUSTRIAL STANDARD Translated and Published by Japanese Standards Association JIS H 1364:20*2 Methods for determination of bismuth in aluminium and aluminium alloys ICs 77.120.10 Reference number : JIS H 1364 : 2002 (E) PROTECTED BY COPYRIGHT 7s Copyright Japanese Standards Association Pr
2、ovided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:24 MDTNo reproduction or networking permitted without license from IHS -,-,- H 1364 : 2002 Foreword This translation has been made based on the original Japanese Industrial Stand
3、ard 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 the Japan Aluminium Association (JAA)/ the Japanese standards Association (JSA) with th
4、e draft being attached, based on the provision of Article 12 Clause 1 of the Industrial Standardization Law. Consequently JiS H 1364 : 1971 is revised, and the method for determination of bismuth in the former JIS H 1364 is replaced by this Standard. Though in JIS H 1364 : 1971, the method for deter
5、mination of lead and the method for determination of bismuth were specified together, as a result of the revision they are separately specified in the following individual standards. JIS H 1364 Methods for determination of bismuth in aluminium and aluminium alloys JIS H 1366 Methods for determinatio
6、n of lead in aluminium and aluminium alloys Date of Establishment: 1971-12-01 Date of Revision: 2002-01-20 Date of Public Notice in Official Gazette: 2002-01-21 Investigated by: Japanese Industrial Standards Committee Standards Board Technical Committee on Non-Ferrous Metals JIS H 1364 : 2002, First
7、 English edition published in 2002-10 Translated and published by: Japanese Standards 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 2002 All rights reserved. Unless otherwise s
8、pecified, no part of this publication may be reproduced or utilized in any form or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. Printed in Japan PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided
9、 by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:24 MDTNo reproduction or networking permitted without license from IHS -,-,- JAPANESE INDUSTRIAL STANDARD JIS H 1364 : 2002 Methods for determination of bismuth in aluminium and alumin
10、ium alloys 1 Scope This Japanese Industrial Standard specifies the methods for determina- tion of bismuth in aluminium and aluminium alloys. 2 Normative references The following standards contain provisions which, through reference in this Standard, constitute provisions of this Standard. The most r
11、ecent editions of the standards (including amendments) indicated below shall be applied. JIS H 1306 Methods for atomic absorption spectrometric analysis of aluminium and aluminium alloys JIS H 1307 Methods for inductively coupled plasma emission spectrometric analysis of aluminium and aluminium allo
12、ys JIS H 1351 General rules for chemical analysis of aluminium and aluminium alloy JIS P 3801 Filter paper (for chemical analysis) 3 General requirements General requirements common to the analysis shall con- form to JIS H 1351. 4 Classification of determination methods The methods for determination
13、 of bismuth shall conform to the appropriate one among those specified in the follow- ing: a) Electrolytic separation disodium ethylenediamine tetraacetate titrimetric method This method is applied to the sample of a bismuth content of 0.1 % (m/m) up to and including 1.0 % (m/m). b) Thiourea absorpt
14、iometry This method is applied to the sample of a bismuth content of 0.1 % (rn/m up to and including 1.0 % (m/m. Bromide and rnethyltrioctylammonium bromide extraction atomic ab- sorption spectrometry This method is applied to the sample of a bismuth content of 0.003 % (m/m) up to and including 0.1
15、% (m/m). Atomic absorption spectrometry This method is applied to the sample of a bismuth content of 0.1 % (m/m up to and including 1.0 % (m/m). c) d) e) Inductively coupled plasma emission spectrometric analysis This method is applied to the sample of a bismuth content of 0.01 % (m/m) up to and inc
16、lud- ing 1.0 % (m/m). 5 Electrolytic separation disodium ethylenediamine tetraacetate titrimet- ric method 5.1 Summary After decomposing a sample by a sodium hydroxide solution, make it acid by adding nitric acid. Carry out electrolysis by using a platinum electrode, and after decomposing bismuth, l
17、ead, copper and the like with nitric acid which are deposited on an anode and a cathode, adjust the concentration of acid of the solution. PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not fo
18、r Resale, 03/13/2007 08:22:24 MDTNo reproduction or networking permitted without license from IHS -,-,- 2 H 1364 : 2002 Partially take a specific amount of the solution and titrate it with disodium ethylenediamine tetraacetate (hereafter referred to as “EDTA2Na”) standard solu- tion by using Xylenol
19、 Orange (hereafter referred to as “XO”) as an indicator. 5.2 Reagents The reagents shall be as follows. a) Nitric acid b) Nitric acid (l+l) c) Sodium hydroxide solution Dissolve 200 g of sodium hydroxide in water, and make 1 O00 ml with water. Reserve the solution in a polyethylene bottle, and use t
20、he supernatant. d) Hydrogen peroxide (1+9) e) 0.01 mom EDTMNa standard solution Dissolve 3.72 g of disodium ethylene- diamine tetraacetate dihydrate in water, dilute accurately to 1 O00 ml with wa- ter, and reserve it in a polyethylene bottle. Obtain the bismuth equivalent amount of this solution ac
21、cording to the fol- lowing procedure. Weigh out 1.000 g of bismuth 99.9 % ( m h ) or higher, transfer it into a bea- ker (200 mi), cover it with a watch glass, add 30 ml of nitric acid (l+l), and decompose it by gently heating. After cooling to ordinary temperature, rinse the bottom surface of the w
22、atch glass and the inner wall of the beaker with water, remove the watch glass, transfer the solution to a one-mark volumetric flask of 500 ml by using water, and dilute to the mark with water. Accurately take 20 ml from this solution into a beaker (300 mi). After diluting to about 100 ml with water
23、, carry out hereafter the operation according to the procedure of 5.5.2, titrate it with 0.01 mol/L EDTA2Na standard solution, and obtain the bismuth equivalent amount according to the following formula. 0.04 .fi = 1 - 2 where, fBi : bismuth equivalent amount of 0.01 mol& EDTA2Na standard solution o
24、f 1 ml (g) 0.04 : bismuth amount in standard bismuth solution of Vi : used amount of 0.01 mom EDTA2Na standard so- lution (mi) Vz : used amount of 0.01 mol& EDTA2Na standard so- lution in blank test (mi) 20 ml (g f) XO solution with water. Dissolve 0.1 g of Xylenol Orange in water, and dilute it to
25、100 ml 5 . 3 a) Apparatus and device Cylindrical platinum electrode drical platinum electrode specified in Attached Fig. 1 shall be used. Semi-circular watch glass whose shape is similar to that given in Attached Fig. 2 shall be used. The apparatus and device shall be as follows. For both the anode
26、and cathode, the cylin- b) For the semi-circular watch glass, the watch glass PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:24 MDTNo reproduction or networkin
27、g permitted without license from IHS -,-,- 3 H 1364 : 2002 5.4 Weighing out amount of sample Weigh out a sample of 2.50 g to the near- est 1 mg. 5.5 Operation Carry out the operation according to the following procedure. 5.5.1 Preparation of sample solution Weigh out a sample, and transfer it into a
28、 beaker (300 mi. Cover it with a watch glass, decompose by adding 40 ml of sodium hydroxide solution 5.2 c), and when the reaction becomes gentle, wash the bottom sur- face of the watch glass and the inner wall of the beaker with water. Heat to decompose completely. Dilute to approximately 100 ml wi
29、th warm water, make it acid by adding 45 ml of nitric acid, and expel nitrogen oxide by heating gently. After cooling to room temperature, wash the bottom surface of the watch glass and the inner wall of the beaker with water. Thereafter, remove the watch glass, and dilute it to about 200 ml by addi
30、ng water. Insert two cylindrical platinum electrodes as the anode and cathode into the sample solution obtained in d). Cover the beaker with a semi-circular watch glass, and electrolyze for about 4 h by a current density of 0.04 to 0.05 kA/m2 at 15 “C to 30 “C liquid tempera- ture while gently stirr
31、ing with a magnetic stirrer. Wash the bottom surface of the semi-circular watch glass, the inner wall of the beaker and the part of the electrode exposed above the liquid surface with water, raise the liquid surface by approximately 5 mm with the washings, further con- tinue electrolysis for 30 min,
32、 and confirm that there is no deposit on the part newly immersed in the electrolyte of the cathode(1). Remove the semi-circular watch glass, and pull up the anode and the cathode while water-washing is carried out by using a washing bottle with a current is passed as it is. Wash quickly by dipping i
33、nto a beaker containing water of about 250 ml, and detach the anode and the cathode. Disconnect the power source. Transfer the anode and the cathode into another beaker (300 mi), and add 15 ml of nitric acid (l+l. After dissolving the bismuth, lead, copper and the like which are deposited on the ele
34、ctrode surface by heating(9, sufficiently wash the elec- trode by water and remove it. Evaporate water content to drying up by heating the solution. After allowing to cool down to ordinary temperature, decompose salts by adding 5 ml of nitric acid (l+l), transfer it to a one-mark volumetric flask of
35、 250 ml by using water, and dilute to the mark with water. Notes (1) Though deposition of copper on the cathode is sometimes observed in this case, lead and bismuth are completely deposited. (2) The beaker is slanted and the electrode is rotated to dissolve the de- posit s. In case of the deposits b
36、eing difficult to be dissolved, add several drops of hydrogen peroxide (1+9). PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:24 MDTNo reproduction or networkin
37、g permitted without license from IHS -,-,- 4 H 1364 : 2002 5.5.2 Titration Partially take accurately 100 ml of the solution obtained in 5.5.1 j) into a conical beaker (300 ml(3), add 0.5 ml of XO solution 5.2 f), shake, titrate with 0.01 mol/L EDTA2Na standard solution L5.2 e) and deem a point at wh
38、ich the color of the solution is changed from red purple to yellow as the end point. Note (3) The concentration of acid in the titration is 0.5 ml to 4.0 ml of nitric acid (i+l) (pH 1.5 to pH 0.7) in the solution of 100 ml. 5.6 Blank test the sample according to the procedure of 5.5 wherein the samp
39、le is not used. Carry out the same operation as that for the sample parallel to 5.7 Calculation following formula. Calculate the content of bismuth in a sample according to the where, B i : vi : v z : fBi : m : bismuth content % (mim) in the sample used amount of 0.01 mol/L EDTA2Na standard solution
40、 used in titration of aliquot sample solu- tion (ml) used amount of 0.01 mol/L EDTA2Na standard solution used in titration of aliquot blank test solution (mi) bismuth equivalent amount of 1 ml of 0.01 molL EDTA2Na standard solution (g) weighed out amount of sample (g) 6 Thiourea absorptiometry 6.1 S
41、ummary Decompose a sample with sodium hydroxide solution. After add- ing potassium cyanide, precipitate sulfides of bismuth and the like by adding so- dium sulfide. After separating the precipitate by filtering, decompose the residue with nitric acid. Partially take the solution, adjust the concentr
42、ation of acid, color it by adding thiourea and measure the absorbance by using a photometer. Reagents Nitric acid (l+l, 1+2) Sodium hydroxide As described in 5.2 c). Hydrogen peroxide (1 +9 Potassium cyanide (20 g/lOO mi) Sodium sulfide solution Dissolve 25 g of sodium hydroxide and 25 g of so- dium
43、 sulfide in water, and dilute the solution to 500 ml with water. Put the solution into a polyethylene bottle, and reserve it in a cold dark place. Thiourea solution (10 g/lOO mi) The reagents shall be as follows. PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under l
44、icense with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:24 MDTNo reproduction or networking permitted without license from IHS -,-,- 5 H 1364 : 2002 g) Standard bismuth solution (50 pgBi/ml) Weigh out 0.500 g of bismuth 99.9 % (m/m or higher, transfer it
45、into a beaker (200 mi), cover it with a watch glass, add 15 ml of nitric acid (l+l), and decompose by gently heating. After cooling to ordinary temperature, wash the bottom surface of the watch glass and the inner wall of the beaker with water, remove the watch glass, transfer the solution into a on
46、e-mark volumetric flask of 500 ml by using water, dilute to the mark with water, to make stock solution (1.00 mgBi/ml). Dilute accu- rately only a necessary amount of this stock solution 20 times for every use to make standard bismuth solution. 6 . 3 est 1 mg. Weighing out amount of sample Weigh out
47、 a sample of 1.00 g to the near- 6.4 Operation Carry out the operation according to the following procedure. 6 . 4 . 1 Preparation of sample solution Weigh out a sample, and transfer it into a conical beaker (300 mi). Cover it with a watch glass, and decompose by adding little by little 20 ml of sod
48、ium hydroxide solution 16.2 b). After the reaction becomes gentle, wash the bottom surface of the watch glass and the inner wall of the beaker with water, and decompose completely by heating. Dilute to 200 ml with warm water, and add 20 ml of potassium cyanide. Pre- cipitate sulfide by dropping 5 ml
49、 of sodium sulfide solution 6.2 e) while the solution is stirred. After boiling for 2 to 3 min by heating, settle the deposits by standing still. Wash the bottom surface of the watch glass with water, and remove the watch glass. Filter the deposits by using filter paper (class 5B) specified in JIS P 3801. After sufficiently wash