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1、STD-JIS 6 L22L-ENGL 1798 E 4733b06 0553392 b73 E JIS b c. L JAPANESE I NDUSTRIAL STANDARD Translated and Published by Japanese Standards Association Iron and steel - Methods for deter- mination of vanadium content ICs 77.080.01 Descriptors : iron, transition metals, steels, ferrous metals, ferrous a
2、lloys, vanadium, determination of content, chemical analysis and testing Reference number : JIS G 1221 : 1998 (E) 17 S COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services STD-JIS G 1221-
3、ENGL 1998 = 4933bO 0553393 50T D G 1221 :1998 Foreword This translation has been made based on the original Japanese Industrial Standard revised by the Minister of International Trade and Industry through deliberations at Japanese Industrial Standards Committee in accordance with the Industrial Stan
4、dardization Law. Consequently JIS G 1221:1992 is replaced with JIS G 1221:1998. In this revision, Annex 2 and Annex 4 are prepared based on the corresponding IS0 Standards. Date of Establishment: 1954-03-29 Date of Revision: 1998-02-20 Date of Public Notice in Official Gazette: 1998-02-20 Investigat
5、ed by: Japanese Industrial Standards Committee Divisional Council on Iron and Steel JIS G 1221:1998, First English edition published in 1999-02 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 c
6、ontents, the original JIS is to be the final authority. b .1 O JSA 1999 All rights reserved. Unless otherwise specified, 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 writin
7、g from the publisher. Printed in Japan COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services JAPANESE INDUSTRIAL STANDARD JIS G 1221 : 1998 Iron and steel-Methods for determination of vana
8、dium content Introduction In this Japanese Industrial Standards, Annex 2 is prepared based on IS0 4947, Steel and cast iron-Determination of vanadium content-Potentiometric ti- tration method issued in 1986 and Annex 4 is prepared based on IS0 4942, Steel and iron-Determination of vanadium content-N
9、-BPHA spectrophotometric method issued in 1988, without changing original technical contents. Items not specified in the corre- sponding International Standards are added as Japanese Industrial Standard. The “informative reference“ underlined with dotted line in this Standard is the item which does
10、not exist in the original International Standard. 1 of vanadium in iron and steel. Scope This Japanese Industrial Standard specifies the methods for determination Remarks : The International Standards corresponding to this Standard are shown below. IS0 4947 Steel and cast iron-Determination of vanad
11、ium content-Potenti- ometric titration method Steel and iron-Determination of vanadium content-N-BPHA spectro- photometric method IS0 4942 2 Normative references The following standards contain provisions which, through reference in this Standard, constitute provisions of this Standard. The most rec
12、ent edi- tions of the standards indicated below shall be applied. JIS G 1201 JIS K 0557 JIS K 8001 JIS Z 8402 General rules for chemical analysis of iron and steel Water used for industrial water and wastewater analysis General rule for test methods of reagents General rules for permissible toleranc
13、e of chemical analyses and physi- cal tests 3 General matters given in JIS G 1201. General matters common to determination method shall be as However, JIS G 1201 is not applied to Annexes 2 and 4. 4 Classification of determination methods The method for determination of vanadi- um shall be any one o
14、f following methods: a) Potassium permanganate oxidation ammonium iron ( II ) sulfate titration method This method applied to the sample of 0.10 % (rn/rn) or over up to and incl. 6.0 % (rn/rn) and shall be as specified in Annex 1 (normative). COPYRIGHT Japanese Standards Association Licensed by Info
15、rmation Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services STD-JIS G 1221-ENGL 1778 Li933b08 0553375 382 2 G 1221 1 1998 Potassium permanganate oxidation ammonium iron ( II ) sulfate potentiometric ti- tration method (IS0 4947) This method applies to
16、 the sample of 0.04 % (rnlrn) or over up to and incl. 2 % (rn/rn) vanadium content, and shall be as specified in An- nex 2 (normative). N-benzoylphenylhydroxylamine extraction absorptiometry (1) This method ap- plies to the sample of 0.005 % (rn/rn) or over up to and incl. 0.50 % (rn/rn) vanadi- um
17、content, and shall be as specified in Annex 3 (normative). N-benzoylphenylhydroxylamine extraction absorptiometry (2) (IS0 4942) N- BPHA spectrophotometric method This method applies to the sample of 0.005 % (rn/rn) or over up to and incl. 0.50 % (rn/rn), and shall be as specified in Annex 4 (normat
18、ive). COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services STD=JIS G L22L-ENGL 1978 4933608 055339b 217 . I j 3 G 1221 : 1998 Annex 1 (normative) Potassium permanganate oxidation ammonium
19、 iron (It) sulfate titration method 1 Summary Decompose a sample with appropriate acid after reducing chromium, manganese, etc., with ammonium iron ( II ) sulfate, oxidize vanadium with potassium permanganate. After decomposing excess permanganic acid with urea and sodium ni- trite, titrate with amm
20、onium iron (li) sulfate standard solution by using diphenyl- amine as an indicator. 2 Reagents The reagents shall be as follows. Hydrochloric acid (l+i) Nitric acid Perchloric acid Phosphoric acid Aqua regia (3 volumes of hydrochloric acid and one volume of nitric acid) Mixed acid (3 volumes of sulf
21、uric acid, 13 volumes phosphoric acid, and 14 volumes of water) Sodium chloride Ammonium hydrogendifluoride Sodium fluoride Sodium nitrite solution (30 gll) Ammonium iron (II ) sulfate solution Dissolve 40 g of ammonium iron ( II ) sulfate hexahydrate by adding about 100 ml of water and 100 ml of su
22、lfuric acid (l+l), and dilute the solution with water to 1 O00 ml. Diarsenic trioxide solution Dissolve 0.85 g of diarsenic trioxide in 5 ml of sodium hydroxide solution (50 giz), and add 50 ml of water, neutralize it with sulfuric acid (1+5), dissolve by adding 3 g of sodium hydrogencarbonate, and
23、dilute the solution to 1 O00 ml with water. Potassium permanganate solution (3 g/ 1 ) Urea 1/30 moYZ Ammonium iron (II) sulfate standard solution Dissolve 13.1 g of am- monium iron ( II ) sulfate hexahydrate by adding about 100 ml of water and 100 ml of sulfuric acid (l+l). After cooling to ordinary
24、 temperature, transfer the solution to a 1 O00 ml one-mark volumetric flask with water, and dilute to the mark with water. Determine a factor of the standard solution for each service as follows; Ac- curately sample 100 ml of water, 10 ml of sulfuric acid (l+l), and 25 ml of 1/30 mol/Z ammonium iron
25、 (II ) sulfate standard solution into a conical beaker (300 mi). COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services STD-JIS G 1221-ENGL 1778 4933bO 0553397 155 or over up to and incl. 6
26、.0 4 G 1221 : 1998 0.50 After cooling to room temperature, titrate with 0.008 mol/Z potassium permanga- nate standard solution ( I ) , obtain the amount of potassium permanganate solution used for the titration by taking a point when the color of solution turns red purple as the end point, and calcu
27、late the factor according to the following formula: F2 xVxl.2 FI = 25 where, F, : factor of 1/30 mol/Z ammonium iron (II) sulfate standard solution F2 : factor of 0.008 mol/Z potassium permanganate standard solution V : amount of 0.008 mol/Z potassium permanganate standard solution used (mi) Note (l
28、) Dilute accurately 0.02 moll Z potassium permanganate standard solution, which is prepared and standardized according to (7) of 4.5 of JIS K 8001, 2.5 times with the water of grade A2 or upward stated in Table 1 of 3 of JIS K 0557. The factor of 0.02 mol/Z potassium permanganate standard solution i
29、s used. p) Diphenylamine phosphoric acid solution Dissolve 1 .O g of diphenylamine (C,H,),NH in 100 ml of phosphoric acid. 3 Test portion The test portion shall be as given in Annex 1 Table 1. Annex 1 Table 1 Test portion Vanadium content Test portion % (mlm) I 1.0 I I 0.10 or over to and excl. 3.0
30、4 Procedure Informative reference : WARNING The vapour of perchloric acid has a risk of ex- plosion under existence of ammonia, nitrous acid vapour, or organic matter. The treatment for vaporizing perchloric acid shall be carried out at a place equipped with an exhaust fa- cility which ensures safet
31、y even though perchloric acid is used. 4 . 1 one of the following procedures: Preparation of sample solution Prepare a sample solution in accordance with any a) Sample easily decomposed with mixed acid 1) Weigh the sample, transfer into a beaker (300 mi), cover with a watch-glass, add COPYRIGHT Japa
32、nese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services - STD*JIS G L22L-ENGL 1978 9 4733b08 0553378 07L I 5 G 1221 1998 30 ml of mixed acid and 20 ml of water, decompose by heating gently, further add 3
33、ml of nitric acid, and heat. Wash the bottom face of the watch glass, remove the watch glass, and generate white fume of sulfuric acid by heating successively. After standing to cool, add 30 ml of water, dissolve salts by sufficiently shaking, cover with a watch glass, and heat to boiling. Wash the
34、bottom face of the watch glass with a small amount of warm water, remove the water glass, filter the solu- tion with filter paper (class 5 A) (2), and wash the filter paper and insoluble resi- due several times with warm water. Mix the filtrate and washings together, transfer into a conical beaker (
35、500 mi), and cool to room temperature. Thereafter, dilute the solution to about 200 ml with water. Discard the residue. 2) Note (2) In the case where insoluble residue is not observed, omit the filtrating operation. b) Sample not easily decomposed with mixed acid 1) Weigh the sample, transfer into a
36、 beaker (300 ml), cover with a watch glass, add 20 ml of aqua regia, decompose by heating gently, further add 30 ml of mixed acid, and heat. Wash the bottom face of the watch glass with water, remove the watch glass, and generate white fume of sulfuric acid by heating successively. Carry out the ope
37、ration of a)2). 2) c) Sample containing cast iron and a great amount of silicon 1) Weigh the sample, transfer into a beaker (300 mi), cover with a watch glass, add 0.5 g to 1 g of ammonium hydrogen fluoride and 50 ml of aqua regia, decompose by heating gently, further add 30 ml of mixed acid, and he
38、at. Wash the bottom face of the watch glass with water, remove the watch glass, and generate white fume of sulfuric acid by heating successively. Carry out the operation of a)2). 2) d) Sample containing tungsten, niobium or tantalum 1) Carry out the operation of a)l). After standing to cool, add 30
39、ml of water, 3 g of ammonium hydrogen fluoride or 2 g of sodium fluoride, dissolve salts by shaking sufficiently, cover with a watch glass, and heat until boiling. Wash the bottom face of the watch glass with a small amount of warm water, remove the watch glass, filter the solution with fil- ter pap
40、er (class 5A) (), and wash the insoluble residue several times with warm water. Mix the filtrate and washings together, transfer into a conical beaker (500 mi) and cool to room temperature. Thereafter, dilute the solution to about 200 ml with water, and discard the residue. e) Sample into which vana
41、dium carbide or the like may be undecomposable because of high carbon content 1) Carry out the operation of a)l). 2) After standing to cool for a short time, add 5 ml of nitric acid ,and generate white fume of sulfuric acid by heating. COPYRIGHT Japanese Standards Association Licensed by Information
42、 Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services 6 G 1221 1998 3) Repeat the operation of 2) two or three times, and decompose the carbide of va- nadium or the like. 4) Carry out the operation of a)2). f) Sample containing 10 % (m lm ) chromium 1)
43、 Weigh the sample, transfer into a beaker (300 mi), cover with a watch glass, add 30 ml of hydrochloric acid (l+l), and decompose most of the sample by heating gently. Add 5 ml of nitric acid and 30 ml of perchloric acid, generate white fume of perchloric acid by heating, and oxidize chromium to dic
44、hromic acid. Thereaf- ter, shift the watch glass, add little by little 1 g to 2 g of sodium chloride heating, and repeat the addition of sodium chloride until brown fume is not generated. After standing to cool for a short time, wash the bottom face of the watch glass with water, remove the watch gl
45、ass, and reduce the residual amount of perchloric acid to about 5 ml by heating successively. After standing to cool, add 50 ml of water, dissolve solts by shaking sufficiently, filter the solution with filter paper (class 5A) (), and wash the filter paper and insoluble residue several times with wa
46、rm water. Mix the filtrate and washings together, transfer into a conical beaker (500 mi), add 20 ml of phosphoric acid, and cool to room temperature. Thereafter dilute the solution to about 200 ml with water. Discard the residue. 2) 4.2 Reduce dichromic acid by dripping ammonium iron ( II ) sulfate
47、 solution 2 k) to the solution obtained in a) 2), b) 2), c) 2), d) 2), e) 4) or f) 2) of 4.1, and further add 2 ml per 1 % (mm) of manganese content. After the solution turns slightly red purple by dripping potassium permanganate solution while mixing by shaking, add further 0.5 ml to 1.0 ml, and al
48、low to stand for several min. Add about 5 g of urea, after dissolving by shaking, add drop by drop sodium nitrite solution while mixing the solution by shaking, and make red purple of permanganic acid disappear. Add 5 ml of diarsenic trioxide 2 i), mix by shaking sufficiently, and allow to stand for
49、 3 min. Oxidization of vanadium 4.3 Titration Add accurately 0.05 ml of diphenylamine phosphoric acid solution 2 p) as an indicator to the solution obtained in 4.2, mix by shaking. After the color of the solution turns purple, titrate with 1/30 mol/Z ammonium iron (II) sulfate standard solution 2 o) while mixing by shaking the solution (). Take the point when the purple disappears by the last one drop as the end point ( 4 ) , and obtain the used amount of am- monium iron ( II ) sulfate standard solution. Notes (3) In the case where the vanadium content in the sample