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1、 STD*JIS G 131B-ENGL 1998 = Li733bOB 0553819 27T = J IS . b JAPANESE I NDUSTRIAL STANDARD Translated and Published by Ja pa n ese Sta nda rds Association Method for chemical analysis of ferrovan ad i um c b ICs 77.100 Descriptors : ferrovanadium, ferro-alloys, vanadium-containing alloys, chemical an
2、alysis and testing, testing, determination of content, vanadium, carbon, silicon, sulphur, phosphorus, aluminium Reference number : JIS G 1318 : 1998 (E) 18 S Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for R
3、esale, 03/13/2007 19:30:28 MDTNo reproduction or networking permitted without license from IHS -,-,- G 1318 : 1998 Foreword This translation has been based on the original Japanese Industrial Standard revised by the Minister of International Trade and Industry through deliberations at Japanese Indus
4、trial Standards Committee in accordance with the Industrial Standardization Law. Consequently, JIS G 1318:1982 has been replaced with JIS G 1318:1998. In this revision, the relevant provisions of IS0 Standard are described as Annex 2, and also the determination of each element is shown in the form o
5、f Annex, for the purpose of conformity with the corresponding 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
6、 G 1318 :1998, First English edition published in 1999-03 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. .i- , O JSA 1999 All rights re
7、served. 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 the publisher. Printed in Japan Copyright Japanese Standards Association Provi
8、ded by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:30:28 MDTNo reproduction or networking permitted without license from IHS -,-,- STD*JIS G 1338-ENGL 3778 4733b08 0553823 728 JAPANESE INDUSTRIAL STANDARD JIS G 1318 : 1998 Method for c
9、hemical analysis of ferrovanadium Introduction In the application of standard, normative references to the standard shall be simultaneously referred to. Since ferrovanadium has many chances to be used as the supplementary raw material in iron and steel making process, JIS G 1318 which specifies the
10、determination of vanadium as main element and other 5 elements including carbon which give rise to discussion in the iron and steel produc- tion, was established in 1953. Annex 2 is the Japanese Industrial Standard prepared based on IS0 6467, Ferrovanadium - Determination of vanadium content - Poten
11、tiometric method, pub- lished in 1980 as the first edition, without modifying its technical content and struc- ture. The Informative references underlined with dots in Annex 2 show the matters not given in the original International Standard. 1 Scope This Japanese Industrial Standard specifies deter
12、mination of vanadium, carbon, silicon, phosphorus, sulfur and aluminium in ferrovanadium. 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 standards indicated below sha
13、ll be applied. JIS G 1301 General rules for chemical analysis of ferroalloys JIS K 0121 General rules for atomic absorption spectrochemical analysis JIS K 8001 General rule for test methods of reagents JIS Z 2615 General rules for determinution of carbon in metallic materials JIS Z 2616 General rule
14、s for determination of sulfur in metallic materials 3 General matters General matters common to the methods for chemical analy- sis shall be in accordance with JIS G 1301 and JIS K 0121. However, these shall not be applied to Annex 2. 4 Classification for determination of each component The methods
15、for de- termination of each component in ferrovanadium shall be according to Table l. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:30:28 MDTNo reproduction or networking permitted wit
16、hout license from IHS -,-,- STD*JIS G LILB-ENGL 1778 4733bOB 0553822 BbY 2 G 1318 : 1998 Table 1 The methods for determination of each component in ferrovanadium Range of percentage of components % (mlm) Annex (normative) No. Component I Determination method Vanadium 30 or over up to and incl. 90 1
17、Potassium permanganate oxidation ferrous (II) ammonium sulfate visual titrimetric method Potassium permanganate oxidation ferrous (II) ammonium sulfate potentiometric titration method (IS0 6467) , not more than 85 2 Carbon Combustion-gas volumetric method 0.05 or over up to and incl. 0.30 3 0.001 or
18、 over up to and incl. 0.30 Combustion-infrared absorption method Silicon dioxide gravimetric method Silicon 0.1 or over up to and incl. 3.0 5 Iron and vanadium separation Phosphomolybdenum blue spectrophotometric method 0.01 or over up to and incl. 0.10 6 Phosphorus Sulfur Combustion-sodium hydroxid
19、e titrimetric method I 0.005 or over up to and incl. 0.10 7 Combustion-infrared absorption I method 0.001 or over up to and incl. 0.10 8 Disodium dihydrogen ethylene-. diamine tetraacetate titrimetric method 0.1 or over up to and incl. 5.0 9 Aluminium Atomic absorption method 0.005 or over up to and
20、 incl. 1.0 10 .- Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:30:28 MDTNo reproduction or networking permitted without license from IHS -,-,- STDOJIS G 1318-ENGL 1998 m Li933b08 05538
21、23 7T0 = 3 G 1318 : 1998 Annex 1 (normative) Determination of vanadium - Potassium permanganate oxidation ferrous (II) ammonium sulfate visual titrimetric method 1 Summary Decompose a sample with nitric acid and hydrochloric acid. Add sulfuric acid and phosphoric acid, heat to generate white fumes f
22、or removing hydro- chloric acid and nitric acid. Oxidize vanadium with potassium permanganate, de- compose the excess amounts of permanganate with sodium nitrite and decompose the excess amounts of nitrous acid with urea. After suppressing the interferences of generated dichromic acid with arsenious
23、 acid, the sample solution is titrated with ferrous (II) ammonium sulfate standard solution by using diphenylamine as the in- dicator. 2 Reagents The reagents shall be as follows : a) Hydrochloric acid b) Nitric acid c) Mixed acid (3 parts of sulfuric acid, 13 parts of phosphoric acid, and 14 parts
24、of water) d) Sodium nitrite solution (30 g/Z) e) Potassium permanganate solution (3 gil) This solution shall be stored in the brown color bottle. f) Arsenious acid solution Dissolve 3 g of sodium carbonate in approx. 150 ml of water, dissolve 0.85 g of diarsenic trioxide and dilute to approx. 950 ml
25、 with water. After saturating the solution by passing carbon dioxide for approx. 3 min, dilute to 1 O00 ml with water. WARNING FOR SAFETY Because arsenious acid solution is a deadly poi- son, it is necessary to pay attention when its so- lution and a solution with arsenious acid added are treated. g
26、) Urea h) 0 . 1 mol/Z ferrous (II) ammonium sulfate standard solution The method of preparation and standardization of this solution shall be in accordance with 4.5 (27) in JIS K 8001. i) Diphenylamine solution Dissolve 1.0 g of diphenylamine in 100 ml of phos- phoric acid. 3 Test portion Weigh out
27、0.20 g of a sample, to the nearest 0.1 mg. 4 Operation Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:30:28 MDTNo reproduction or networking permitted without license from IHS -,-,- STD
28、*JIS G 13LB-ENGL 1998 4933b08 O553824 637 4 G 1318 : 1998 4.1 Preparation of sample solution Preparation of sample solution shall be according to the following procedures. a) Weigh out the sample, transfer it into an Erlenmeyer flask (500 ml) and insert a funnel into the inlet of the flask. b) Add 5
29、 ml of nitric acid and 15 ml of hydrochloric acid. Decompose the sample by gently heating at approx. 60 OC. c) Wash the inner and outer sides of leg of the funnel with water and remove it. d) Add 30 ml of mixed acid 2 c), heat it until white fumes start to be generated, and stand it to cool. e) Add
30、approx. 150 ml of water, dissolve the soluble salts by heating, and cool it. 4.2 Oxidation of vanadium following procedures. Oxidation of vanadium shall be according to the a) Drop potassium permanganate solution 2 e) while stirring the solution obtained in 4.1 e) and allow the pale red color of the
31、 solution to develop. Add further 0.5 ml of potassium permanganate solution in excess, mix them and allow to stand for approx. 10 min. b) Add 5 g of urea to this solution and dissolve it. Add drop by drop sodium nitrite solution, while stirring the solution, until the red color completely disappears
32、. c) After stirring the solution until the fine bubbles caused by the decomposition of nitrous acid disappears, add 5 mi of arsenious acid solution 2 f (I) and stir them for about 1 min. Note (1) When chromium does not coexist, arsenious acid solution may not be added. 4.3 Titration Titration shall
33、be according to the following procedures. a) Dilute the solution obtained in 4.2 c) to approx. 200 ml with water. b) Add 0.05 ml of diphenylamine solution 2 i) as the indicator and mix them by shaking. Thereafter, allow to stand for 2 min to 3 min to develop purple color. c) Titrate this purple solu
34、tion with 0.1 molZ ferrous (II) ammonium sulfate stan- dard solution 2 h), and allow the point where the purple color disappears to be the end point. Obtain the titration amount of 0.1 mol/Z ferrous (II) ammonium sulfate standard solution used. , 5 Blank Test Blank tests shall not be carried out. 6
35、Calculation The vanadium content in the sample shall be calculated with the following formula. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:30:28 MDTNo reproduction or networking perm
36、itted without license from IHS -,-,- STD-JIS G L3L8-ENGL 1998 9933bUA 0553825 573 5 G 1318 : 1998 AxFx0.005 094 xloo V = m where, V : vanadium contents in the sample % (mlm) A : F : amount of 0.1 mol/Z ferrous (II) ammonium sulfate standard solution used in 4.3 c) (ml) factor of 0.1 mol/Z ferrous (I
37、I) ammonium sulfate standard solution test portion of the sample (g) m : Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:30:28 MDTNo reproduction or networking permitted without license
38、from IHS -,-,- 6 G 1318 : 1998 Annex 2 (normative) Determination of vanadium - Potassium permanganate oxidation ferrous (II) ammonium sulfate potentiometric method (IS0 6467) 1 Scope ferrovanadium. not more than 85 % (rn/m). This Annex 2 specifies a potentiometric method for determination of vanadiu
39、m in This method shall be applicable to ferrovanadium having a vanadium contents 3 Principle Decompose a sample with nitric and sulfuric acids. In the cold solution, oxidize vanadium (IV) into vanadium (VI with slight excess of potassium permanganate. Decompose the excess of potassium permanganate b
40、y potassium nitrite and decom- pose the excess of potassium nitrite by urea. Reduce vanadium (V) into vanadium (IV) with iron (II) and obtain vanadium contents with the potentiometric titration. 4 Reagents During the analysis, use only reagents of recognized analytical grade, and only distilled wate
41、r or water of equivalent purity, except where otherwise speci- fied. 4:l Urea 4.2 Nitric acid p1.38 g/ml to 1.42 g/ml 4.3 Phosphoric acid 4.4 Sulfuric acid 50 % (V/v solution, rendered inert to potassium permanga- nate by adding a slight excess of this reagent. To 400 ml of water, add cautiously 500
42、 ml of sulfuric acid (p approximately 1.84 g/mi); mix, cool, dilute to 1 O00 ml and mix. 4.5 Potassium nitrite solution (10 gll) Dissolve 10 g of potassium nitrite in water and dilute the volume to 1 O00 ml. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS
43、Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 19:30:28 MDTNo reproduction or networking permitted without license from IHS -,-,- STD*JIS G 1318-ENGL 1778 Li933b08 0553827 34b 7 G 1318 : 1998 4.7 Potassium dichromate standard solution c(K2Cr207) = 0.2 moV1 Weigh to the nearest 0.
44、000 5 g, exactly 9.806 4 g of potassium dichromate dried at 105 “C previously, dissolve it in water, transfer the solution to a volumetric flask of 1 O00 ml and dilute the volume to the mark with water. 4.8 Ammonium iron (II) sulfate standard solution cFSO,(NH,)SO, = 0.2 mol4 4.8.1 Preparation Disso
45、lve 78.4 g of ammonium iron (II) sulfate FeS04(NH4)2S04-6H201 into 500 ml of warm water and transfer it into a volumetric flask of 1 O00 ml. After dissolving it thoroughly, add 100 ml of sulfuric acid (4.41, cool, and dilute to the mark with water. 4.8.2 Standardization Put 280 ml of water into a be
46、aker (600 ml), add 10 ml of sulfuric acid (4.4) and 10 ml of phosphoric acid (4.3). Introduce 40 ml of potassium dichromate solution (4.7). Titrate the solution potentiometrically with ammonium iron (II) sulfate solution. The end of the reaction is obtained when the maximum fall in potential of at T
47、he correction factor C is given by the following expression : least 100 mV is observed. This is taken as the end point of the titration. where, VI : amounts of ammonium iron (II) sulfate solution used (ml) The concentration of this ammonium iron (II) sulfate solution varies, and it shall be verified
48、 for each series of determinations. 5 Apparatus and equipments ments in general use at laboratory. The following equipments shall be also used as well as the apparatus and equip- 5.1 Beaker (400 ml) 5.2 Precision potentiometer 5.2.1 Electrode Indicator electrode : platinum Reference electrode : Hg/Hg2S04/K2S04 (saturated) 5.2.2 Checking of measuring system the saturated potassium sulfate solution. solution. When the apparatus is not used, the reference electrode should be Immersed in The platinum electrode should be