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1、J IS JAPANESE INDUSTRIAL STANDARD Translated and Published by Japanese Standards Association Iron and steel - Methods for determination of silicon content ICs 77.080.01 Descriptors : iron, transition metals, steels, ferrous metals, ferrous alloys, silicon, Reference number : JIS G 1212 : 1997 (E) me
2、talloids, determination of content, chemical analysis and testing 22 s COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services G 1212 : 1997 Foreword This translation has been made based on
3、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 Standardization Law. Consequently, this revision supersedes JIS G 1212:1981. In this revision, the
4、relevant IS0 Standards are laid down as Annexes 2, 4 and 5 in order to harmonize with International Standards. JIS G 1212:1997 contains Annexes as under; Annex 1 Gravimetric method as silicon dioxide (1) Annex 2 Gravimetric method as silicon dioxide (2) (IS0 439) Annex 3 Reduced molybdosilicate spec
5、trophotometric method (1) Annex 4 Reduced molybdosilicate spectrophotometric method (2) Annex 5 Reduced molybdosilicate spectrophotometric method (3) (IS0 4829-1) (IS0 4829-2) Date of Establishment: 1953-03-28 Date of Revision: 1997-04-20 Date of Public Notice in Oficial Gazette: 1997-04-21 Investig
6、ated by: Japanese Industrial Standards Committee Divisional Council on Iron and Steel JIS G 1212 :1997, First English edition published in 1997-11 Translated and published by: Japanese Standards Association 4-1-24, Akasaka, Minato-ku, Tokyo, 107 JAPAN In the event of any doubts arising as to the con
7、tents, the original JIS is to be the final authority. O JSA 1997 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 writing from
8、 the publisher. Printed in Japan COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services STD-JIS G 12L2-ENGL 1997 m Li933bO 0547500 111 JIS G 1212 : 1997 JAPANESE INDUSTRIAL STANDARD Iron an
9、d steel - Methods for determination of silicon content Introduction This Japanese Industrial Standard has been prepared on the basis of the second edition of IS0 439, Steel and iron-Determination of total silicon content-Gravimetric method published in 1994, IS0 4829-1, Steel and cast iron - Determi
10、nation of total silicon content-Reduced molybdosilicate spectrophotometric method-Part 1: Silicon contents between 0.05 and 1.0 % published in 1986 and IS0 4829-2, Steel and iron -Determination of total silicon content -Reduced molybdosilicate spectrophotometric method - Part 2 : Silicon contents be
11、tween 0.01 and 0.05% published in 1988 which are edited in Annexes 2, 4 and 5, respectively without any modification in technical content and style thereof, but some additional requirements not specified in the corresponding International Standards are given as a part of the Japanese Industrial Stan
12、dard. Further, in this Standard, the “Informative reference” underlined with dotted line are the matters not specified in the original International Standards. 1 of silicon content in iron and steel. Scope This Japanese Industrial Standard specifies the methods for determination 2 Normative referenc
13、es The following standards contain provisions which, through reference in this text, constitute provisions of this Standard. As to those normative references, the most recent editions thereof shall be applied. JIS G 1201 JIS Z 8402 General rules for chemical analysis of iron and steel General rules
14、for permissible tolerance of chemical analyses and physical tests Steel and iron-Determination of total silicon content-Gravimetric method Steel and cast iron-Determination of total silicon content-Reduced molybdosilicate spectrophotometric method-Part 1 : Silicon contents between 0.05 and 1.0 % Ste
15、el and iron-Determination of total sil icon content-Reduced molybdosilicate spectrophotometric method-Part 2 : Silicon contents between 0.01 and 0.05 % IS0 439 IS0 4829- 1 IS0 4829-2 3 General requirements General requirements common to methods for determination shall be in accordance with JIS G 120
16、1, provided that this dose not cover Annexes 2, 4 and 5. 4 content shall be in accordance with any one of the following: Division of determination methods The method for determination of silicon (1) Gravimetric method as silicon dioxide (1) This method is applicable to the sample of total silicon co
17、ntents between 0.1 % (m/m) and 8.0 % (m/m), and the method for determination shall be in accordance with Annex 1. COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services 2 G 1212 : 1997 (2)
18、Gravimetric method as silicon dioxide (2) (IS0 439) This method is applicable to the sample of total silicon contents between 0.10 % (rn/rn and 5.0 % (rn/rn, and the method for determination shall be in accordance with Annex 2. (3) Reduced molybdosilicate spectrophotometric method (i) This method is
19、 applicable to the sample of silicon contents between 0.01 % (rn/rn) and 1.0 % (rn/rn), and the method for determination shall be in accordance with Annex 3. Reduced molybdosilicate spectrophotometric method (2) (IS0 4829-1) This method is applicable to the sample of total silicon contents between 0
20、.05 % (rn/rn) and 1.0 % (rn/rn), and the method for determination shall be in accordance with Annex 4. Reduced molybdosilicate spectrophotometric method (3) (IS0 4829-2) This method is applicable to the sample of total silicon contents between 0.01 % (rn/rn and 0.05 % (rn/rn), and the method for det
21、ermination shall be in accordance with Annex 5. (4) (5) COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services ”. Silicon content I % (mim) STD-JIS G 1212-ENGL 1977 4933b08 0547502 T94 = We
22、igh-out mass of test portion g 3 G 1212 : 1997 1.0 and over, up to and incl. 8.0 Annex 1 Gravimetric method as silicon dioxide (i) 1.0 1 Decompose the test portion with appropriate acids, heat to vaporize with addition of perchloric acid or sulfuric acid, and convert silicon to insoluble silicic aci
23、d. After separation of the precipitate by filtration, ignite it to make silicon dioxide, and measure the mass. Further, add sulfuric acid and hydrofluoric acid, heat to volatilize silicon dioxide, then measure the mass. Purport 2 Reagents The reagents shall be as follows: (1) Hydrochloric acid (2) H
24、ydrochloric acid (2+1, 1+4, 1+10) (3) Nitric acid (4) Nitric acid (l+l) (5) Perchloric acid (6) Hydrofluoric acid * (7) Sulfuric acid (8) Sulfuric acid (l+l, 1+3) (91, Aqua regia (hydrochloric acid 3, nitric acid i) (10) Hydrogen peroxide (1 i) Sodium carbonate (12) Ammonium thiocyanate solution (sa
25、turated) 3 Weigh-out mass of test portion shall be as given in Annex 1 Table 1. The mass of test portion to be weighed out Annex 1 Table 1 Weigh-out mass of test portion I 0.10 and over, to and excl. 1.0 I 3.0 I 4 Procedure Informative reference: Warning -Perchloric acid vapour may cause ex- plosion
26、s in the presence of ammonia, nitrous fumes or organic material. All vaporations of perchloric acid must be carried out in fume cupboards suitable for use with perchloric acid. COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association
27、 Licensed by Information Handling Services STD=JIS G L212-ENGL I997 D 4933b08 05Li7503 920 = 4 G 1212 : 1997 4.1 Decomposition of test portion and dehydrating treatment of silicic acid The decomposition of the test portion and the dehydrating treatment of silicic acid shall be carried out in accorda
28、nce with any one of the following procedures: (1) Sample easy for decomposition with perchloric acid and nitric acid (a) Transfer the test portion weighed out to a beaker (300 mi) and cover it with a watch glass. (b) Add 20 ml of perchloric acid for the weigh-out test portion of 1.0 g, or 40 ml for
29、3.0 g thereof. Further, add 15 ml to 20 ml of nitric acid (1+1) for every 1.0 g of weigh-out test portion, and heat gently to decompose. Ignite successively, and continue heating for 15 min to 20 min after attaining the condition where incurred vapour of perchloric acid refluxes on the inner wall of
30、 the beaker. Sample difficult for decomposition with perchloric acid and nitric acid or sample containing niobium or tantalum (a) Transfer the test portion weighed out to a beaker (300 mi), and cover it with a watch glass. (b) Add 20 ml to 30 ml of aqua regia, and heat gently to decompose. 4 I (c) (
31、2) (c) (d) Sample containing chromium or tungsten (a) (b) (cl (d) Add 20 ml of perchloric acid for the weigh-out test portion of 1.0 g, or 40 ml for 3.0 g thereof. Carry out the operation in accordance with (l)(c). (3) Transfer the test portion weighed out to a beaker (300 mi), and cover it with a w
32、atch glass. Add 20 ml of hydrochloric acid (2+1) little by little for the weighed-out test portion of 1.0 g, or 40 ml for 3.0 g thereof, and heat it gently to decompose. Add 20 ml of perchloric acid for the weighed-out test portion of 1.0 g, or 40 ml for 3.0 g thereof. Ignite successively, and conti
33、nue heating for 15 min to 20 min after attaining the condition where chromium is oxidized whereby it is converted to red dichromic acid and the vapour of perchloric acid refluxes on the inner wall of the beaker. (4) Sample of high nickel, chromium, tungsten, cobalt, etc. content (a) (b) Transfer the
34、 test portion(l1 weighed out to a beaker (300 mi), and cover it with a watch glass. Add 50 ml of water and 10 ml of hydrochloric acid, and add 30 ml of hydrogen peroxide little by little, then heat it gently to decompose after the completion of violent reaction. Add 20 ml of perchloric acid. Carry o
35、ut the operation in accordance with (3)(d). (c) (d) Note (l) For the sample of high nickel, chromium, tungsten, cobalt, etc. content, the mass of test portion to be weighed out shall be 1:O g, irrespective of the silicon contents. COPYRIGHT Japanese Standards Association Licensed by Information Hand
36、ling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services STD*JIS G 1212-ENGL L977 = 4933b08 U547504 8b7 5 G 1212 : 1997 (5) Sample containing molybdenum or titanium (a (b) (c) (d) Transfer the test portion() weighed out to a beaker (300 mi), and cover it with
37、a watch glass. Add 40 ml of sulfuric acid (1+3) for the weigh-out test portion of 1.0 g, or 60 ml for 3.0 g thereof, and heat to decompose. Add 5 ml of nitric acid for every 1.0 g of weigh-out test portion, and boil it. Add 5 ml to 10 ml of hydrochloric acid, remove the watch glass after washing its
38、 underneath surface with water, and continue heating on a sand bath to generate dense white fume of sulfuric acid for 15 min to 20 min. In the case of using sulfuric acid for dehydration of silicic acid in the sample which is easy for decomposition with nitric acid and hydrochloric acid (a) Transfer
39、 the test portion(l1 weighed out to a beaker (300 mi), and cover it with a watch glass. (b) Add 15 ml to 20 ml of nitric acid (l+l) little by little for every 1.0 g of weigh-out test portion, and heat it gently to decompose. (c) Add 5 ml to 10 ml of hydrochloric acid. (d) Add 20 ml of sulfuric acid
40、(l+l) for the weigh-out test portion of 1.0 g, or 30 ml for 3.0 g thereof. (e) Remove the watch glass after washing its underneath surface with water, continue heating on a sand bath to generate dense white fume of sulfuric acid for 15 min to 20 min. (6) 4.2 accordance with either of the following p
41、rocedures: Filtration and washing The filtration and washing shall be carried out in (i) In the case of dehydration with perchloric acid (a) (b) (c) Let to cool the salts obtained in (l)(c), (2)(d), (3)(d), or (4)(d) of 4.1 to approximate room temperature. Remove the watch glass after washing its un
42、derneath surface with water, add approximately 120 ml of warm water, and stir to dissolve the salts. Immediately, separate the precipitation by filtration with a filter paper (Class 5B), remove the silicic acid adhered to the inner wall of the beaker with a policeman (rubber-tipped glass rod), and t
43、ransfer it to the filter paper. At the beginning, wash it about 5 times alternately with warm water and with hydrochloric acid (1+10) heated at between 40 “C and 60 “C and at last wash it with warm water until the ferric (iron III) ion vanishes in the filtrate(2) (3) (4. Store the precipitate and di
44、scard the filtrate and the washings(5). (d) Notes (2) In the case where small quantity of the washing is taken and ammonium thiocyanate solution (saturated) is added, wash it sufficiently until the coloration of (orange) red vanishes. COPYRIGHT Japanese Standards Association Licensed by Information
45、Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services 6 G 1212 : 1997 (3) At the time of incineration according to 4 . 3 ( l ) ( b ) , insufficient washing may cause popping, that is dangerous, and may incur loss of residue. (4) In the case where undeco
46、mposed residue of the test portion is appreciated in the precipitate after washing by filtration, transfer the precipitate together with the residue and the filter paper to a platinum crucible (No.30), dry, incinerate, add approximately 6 times quantity of sodium carbonate, and heat to fuse. After l
47、etting to cool, transfer the fusion products together with the platinum crucible to a beaker (300 mi), and 100 ml of warm water to extract the fusion products, and take out the platinum crucible after washing with water. Cover it with a watch glass, and add hydrochloric acid little by little until i
48、t is acidified to dissolve the salts. Further, add 30 ml of perchloric acid, then carry out the operations in accordance with 4 . 1 (l)(c) and 4 . 2 (1). (5) In the case of the sample of silicon contents of 1 % (rn/rn) or more, it is necessary to recover silicon from the filtrate and washings in acc
49、ordance with the following procedure. Collect the filtrate and washings into a beaker (500 mi), cover with a watch glass, add 20 ml of perchloric acid, heat it, continue heating for 15 min to 20 min after attaining the condition where the vapour of perchloric acid being vaporized refluxes on the inner wall of the beaker, and let to cool to the room temperature. Thereafter, recover the silicon by the operation in accordance with (b) to (d), and incorporate with the precipitate having been stored. Discard the filtrate and washings. (2) In the case of dehydration with sulfuric acid (a) (b) (