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1、STD*JIS G 1214-ENGL 1998 V933b08 0553597 T17 9 r JAPANESE INDUSTRIAL STANDARD J1S G 1214: 1998 Iron and steel -Methods for determination of phosphorus content February, 1999 ERRATA Page 19 The formula of log Ris changed as follows: Error log R= 0.860 3 log GpaI - 0.872 4 Correct log R= 0.860 3 log k
2、pa1 - 0.812 4 Remarks: This erratum is for correcting the first edition of this Standard. Japanese Standards Association COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services JIS JAPANESE
3、INDUSTRIAL STAN DARD Translated and Published by Japanese Standards Association Iron and steel-Methods for determination of phosphorus content IC$ 77.080.01 Descriptors : Iron, transition metals, steels, ferrous metals, ferrous alloys, phosphorus, Reference number : JI$ G 1214 : 1998 (E) determinati
4、on of content, chemical analysis and testing 17 S COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services G 1214 : 1998 Foreword This translation has been made based on the original Japanese
5、 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, JIS G 1214:1992 is replaced with JIS G 1214:1998. In this revision, IS0 10714 has bee
6、n employed in Annex 2 for conforming to International Standard. Date of Establishment: 1953-03-28 Date of Revision: 1998-02-20 Date of Public Notice in Official Gazette: 1998-02-20 Investigated by: Japanese Industrial Standards Committee Divisional Council on Iron and Steel JIS G 1214 :1998, First E
7、nglish edition published in 1999-01 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. . 8 JSA 1999 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 COPYRIGHT Japanese Standards Association Licensed by Information Handlin
9、g Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services JAPANESE INDUSTRIAL STANDARD JIS G 1214 : 1998 Iron and steel-Methods for determination of phosphorus content Introduction This Japanese Industrial Standard is prepared by citing the trans- lation of IS0 10
10、714, Steel and iron - Determination of phosphorus content - Phospho- vanadomolybdate spectrometric method issued in 1992 in Annex 2 without changing technical contents and the style. Items which are not specified in the corresponding International Standard are added as JIS. The underlined “informati
11、ve references in this Standard are items which do not exist in the original International Standard. 1 Scope This Japanese Industrial Standard specifies the methods for determina- tion of phosphorus in iron and steel. Remarks : The corresponding International Standard to this Standard is as follows :
12、 IS0 10714 Steel and iron - Determination of phosphorus content - Phosphovanadomolybdate spectrophotometric method 2 Normative references The following standards contain provisions which, through reference in this Standard, constitute provisions of this Standard. The most recent editions of the stan
13、dards indicated below shall be applied. JIS G 1201 General rules for chemical analysis of iron and steel JIS Z 8402 General rules for permissible tolerance of chemical analyses and physical tests 3 General matters General matters common to methods for determination shall be in accordance with JIS G
14、1201. However, JIS G 1201 shall not apply to Annex 2. 4 Classification of methods for determination The methods for determination of phosphorus in iron and steel shall be in accordance with any one of the following : Reduced molybdophosphate spectrophotometric method This method shall apply to the s
15、ample of 0,005 % (m/m) or over up to and including 0.50 % (m/m) phosphorus content as specified in Annex 1 (normative). Phosphovanadomolybdate spectrophotometric method (IS0 10714) This method shall apply to the sample of 0.001 O % (m/m) or over up to and includ- ing 1.0 % (m/m) phosphorus content,
16、as specified in Annex 2 (normative). Molybdophosphate extraction spectrophotometric method This method shall apply to the sample of 0.000 3 % (mlm) or over up to and including 0.010 % (m/rn as specified in Annex 3 (normative). However, it can not apply to the sample containing 0.1 % (rn/m) or over t
17、ungsten. Reduced molybdophosphate spectrophotometric method after extrac- tion of molybdophosphate This method shall apply to the sample of 0.000 3 % (m/rn) or over up to and including 0.010 % (m/m) phosphorus content as specified in Annex 4 (normative). However, it can not apply to the sample conta
18、ining 0.1 % (m/m) or over tungsten. COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services 2 G 1214 : 1998 Annex 1 (normative) Reduced molybdophosphate spectrophotometric method 1 Summary D
19、ecompose a sample with appropriate acid, add perchloric acid, and generate white fumes of perchloric acid by heating. After reducing iron or the like by adding sodium hydrogensulfite, generate molybdophosphate blue by adding hexa- ammonium heptamolybdate and hydrazinium sulfate, and measure the abso
20、rbance of the generated molybdophosphate blue with a photometer. 2 Reagents The reagents shall be as follows. a) Hydrochloric acid b) Nitric acid c) Nitric acid (l+l) d) Perchloric acid e) Hydrofluoric acid (1+4) f) Boric acid g) Mixed acid (1 part hydrochloric acid and 1 part nitric acid) h) Aqueou
21、s ammonia i) Iron It is the iron having as high purity as possible, which contains no phos- phorus or of which the phosphorus content is as low as possible and known. j) Beryllium sulfate solution After dissolving 19.7 g beryllium sulfate tetra- hydrate in 20 ml of sulfuric acid (1 + i), dilute the
22、solution with water to make up the volume to 1 O00 ml. k) Sodium hydrogensulfite solution (100 g/Z) 1) Hydrazinium sulfate sulfuric acid solution Add 15 ml of sulfuric acid (7 + 5) and 75 ml of water to 10 ml of hydrazinium sulfate solution (1.5 g/Z), and mix by shaking. m) Disodium ethylenediaminet
23、etraacetate dihydrate (hereafter referred to as EDTAZNa) n) EDTA2Na solution After dissolving 3.0 g of EDTA2Na and 3.0 g of ammo- nium nitrate in 6 ml of aqueous ammonia, dilute the solution with water to make up the volume to 500 ml. o) Color reagent solution After mixing 25 ml of hexaammonium hept
24、amolydate solution and 10 ml of hydrazinium sulfate solution (1.5 g/Z), dilute the solution with water to make up the volume to 100 ml, and mix sufficiently by shaking. Prepare this solution at each service. COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT
25、 Japanese Standards Association Licensed by Information Handling Services 3 G 1214 : 1998 Phosphorus content % mlm) 0.005 or over to and excl. 0.040 Prepare the hexaammonium heptamolybdate solution as follows. Dissolve 20g of hexaammonium heptamolybdate tetrahydrate in 600 ml of water, add 350 ml of
26、 sulfuric acid by stirring while the solution is cooled in running water, cool it to room temperature, and dilute the solution with water to make up the solution to 1 O00 ml. Test portion g 1 . 0 p) Standard phosphorus solution (40 pgP/ml) Weigh 0.8787 g potassium dihydrogenphosphate which was previ
27、ously made at 110 “C to constant mass and allowed to cool to ordinary temperature in a desiccator, transfer into a beaker (300 ml), dissolve by adding about 1 O00 ml of water, transfer the solu- tion into a 1 O00 ml one mark volumetric flask by using water, and dilute to the mark with water to make
28、stock solution (200 pgP/ml). Dilute only a necessary amount of this stock solution accurately five times with water at each service to make standard phosphorus solution. 3 Test portion The test portion of a sample shall be as given in Annex 1 Table 1. Annex 1 Table 1 Weighing amount of sample -1 0.5
29、0 I Gor over to and excl. 0.15 I I 0.15 or over up to and incl. 0.50 0.15 J 4 Operation Informative reference : WARNING The vapour of perchloric acid has a risk of explosion under existence of ammonia, nitrous acid vapour or organic matter. The treat- ment of perchloric acid vapour shall be carried
30、out at a place equipped with an exhaust facility which ensures safety even though perchloric acid is used. 4.1 Preparation of sample solution Prepare a sample solution in accordance with any one of the following procedures. a) Sample easily decomposed with nitric acid 1) Weigh a sample, transfer to
31、a beaker (200 mi). 2) Cover with a watch glass, add 10 ml of nitric acid (l+l), decompose by heating, add 5 ml of perchloric acid for 0.15 g of the weighed sample, 10 ml for 0.50 g and 15 ml for 1.0 g, continue to heat, and keep such state for 5 min to 10 min, that the inside of the beaker becomes t
32、ransparent and the vapour of perchloric acid is refluxed along the inner wall of the beaker (l). Note (l) When the concentration of perchloric acid in coloration exceeds 0.9 mol/Z, the coloration of phosphorus is remarkably disturbed. Therefore, treatment for generating white fumes shall be thor- ou
33、ghly performed. COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services 4 G 1214 : 1998 3) After allowing to cool, wash the bottom surface of a watch glass with a small amount of water, remo
34、ve the watch glass, add about 40 ml of water, dissolve salts by shaking, filter the solution into a one mark volumetric flask by use of filter paper (class 5A), wash several times with warm water, and combine the washings into filtrate. After cooling the solution to ordi- nary temperature, dilute to
35、 the mark with water. Discard the residue. b) Pig iron and sample not easily decomposed with nitric acid 1) Weigh a sample, transfer to a beaker (200 mi). 2) Cover with a watch glass, add 15 ml of mixed acid, decompose by heating, add 5 ml of perchloric acid for 0.15 g of the weighed sample, 10 ml f
36、or 0.50 g and 15 ml for 1.0 g, continue to heat, and keep such state for 5 min to 10 min that the inside of the beaker becomes transparent and the vapour of perchloric acid is refluxed along the inner wall of the beaker (l). 3) Carry out the operation stated in a) 3 ) . c) Sample containing 5 % (rn/
37、rn) or over chromium 1) Weigh a sample, transfer to a beaker (200 ml). 2) Cover with a watch glass, add 15 ml of mixed acid, decompose by heating, add 10 ml of perchloric acid for 0.15 g of the weighed sample, 15 ml for 0.50 g and 20 ml for 1.0 g, and continue to heat. After oxidizing chromium to di
38、chromate to the extent that the inside of the beaker becomes transparent and the vapour of perchloric acid is refluxed along the inner wall of the beaker, drip hydro- chloric acid several times little by little to volatilize most of chromium as dioxidechromium dichloride. After repeating the drippin
39、g of hydrochloric acid until brown fume is not generated, successively heat to generate white fume of perchloric acid (l) until residual chromium oxidizes to dichromate. 3) Carry out the operation stated in a) 3) d) Sample containing 0.1 % (mh) or over tungsten 1) Weigh a sample, and transfer into a
40、 beaker (200 mi). 2) Carry out the operation stated in b) 2). 3) After allowing to cool for a while, add about 70 ml of water, and shake to mix the salts to be dissolved. Add 2 g of EDTA2Na for 0.15 g of the weighed sample, 5 g for 0.50 g and 10 g for 1.0 g, and boil for 2 min to 3 min by heating. A
41、fter cooling to room temperature, add 5 ml of beryllium sulfate solution 2 j. 4) Adjust pH of the solution to 9.5 to 10.5 with aqueous ammonia by use of a pH meter. After boiling for 2 min to 3 min by heating, cool to room tem- perature. Wash the bottom surface of the watch glass with a small amount
42、 of water, remove the watch glass, filter the precipitate by use of filter paper (class 5B) to which a small amount of filter paper pulp is added, and wash 5 times to 7 times with EDTA2Na solution 2 n). Discard the filtrate and COPYRIGHT Japanese Standards Association Licensed by Information Handlin
43、g Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services 5 G 1214 : 1998 washings. Transfer the precipitate together with the filter paper into the original beaker, cover it with a watch glass, add 10 ml of nitric acid and 10 ml of perchloric acid, decompose by h
44、eating, further continue to heat, and keep such state until the amount of residual solution becomes 5 ml or under (l) that the vapour of perchloric acid is refluxed along the inner wall of the beaker. After allowing to cool for a while, wash the bottom surface of the watch glass with a small amount
45、of water, remove the watch glass, add about 40 ml of water, warm, and dissolve salts by shaking (2). Note (2) When the precipitate of tungstic acid is observed, add about 30 ml of water and 1 g of EDTAZNa, then repeat the procedure of 4) again. 5) After cooling to room temperature, filter the soluti
46、on into a 100 ml one mark volumetric flask by use of filter paper (class 5B), wash several times with warm water, and confine washings into the filtrate. After cooling the solution to ordinary temperature, dilute to the mark with water, discard the residue. e) Sample containing at least 0.5 % (m/m)
47、zirconium or at least 0.1 % (m/rn) niobium Weigh a sample, and transfer to a quartz beaker (200 mi). Informative reference : Instead of a quartz beaker, a polytetrafluoroethylene beaker with graphite base or a perfluoroalkoxy bea- ker can be used. Cover with a quartz watch glass, add 15 ml of mixed
48、acid, decompose by heating, add 5 ml of perchloric acid for 0.15 g of the weighed sample, 10 ml for 0.50 g and 15 ml for 1.0 g, continue to heat, and keep such a state for 5 min to 10 min that the inside of the beaker becomes transparent and the vapour of perchloric acid is refluxed along the inner
49、wall of the beaker P). After allowing to cool for a while, add approx. 40 ml of water, and shake to mix the salts to be dissolved. Add 25 ml of hydrofluoric acid (1 + 4), mix by shaking, dissolve niobic acid or the like which was deposited by heating gently, and immediately add 3.0 g of boric acid to mask excess hydrofluoric acid. After cooling to ordinary temperature, wash the bottom surface of the watch glass with a small amount of water, remove the watch glass, transfer to a 100 ml one mark quartz volumetric flask by using water, and dilute to the mark with water. 4.2 Colo