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1、- STD-JIS G 1314-ENGL 1998 D 4933b08 0553777 Ab3 m J IS JAPANESE INDUSTRIAL STANDARD Translated and Published by Japanese Standards Association Method for chemical analysis of silicomanganese h L ICs 77.100 Descriptors : silicon-containing alloys, chemical analysis and testing, testing, determina- t
2、ion of content, silico-manganese, manganese, silicon, carbon, phosphorus, sulphur Reference number : JIS G 1314 : 1998 (E) 21 s Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 23:17:49 MDTN
3、o reproduction or networking permitted without license from IHS -,-,- G 1314 : 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 Industrial Standards Committee in ac
4、cordance with the Industrial Standardization Law. Consequently, JIS G 1314: 1987 has been replaced with JIS G 1314 : 1998. In this revision, corresponding IS0 Standard is adopted as Annex 2 for the purpose of conformity with International Standards, and the method for determination of each constitue
5、nt is expressed in Annexes. 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 T I S G 1314:1998, First English edition published in 1999-03
6、 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 1999 All rights reserved. Unless otherwise specified, no part of this publication
7、 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 Provided by IHS under license with JSALicensee=IHS Employees/1111111
8、001, User=Wing, Bernie Not for Resale, 03/12/2007 23:17:49 MDTNo reproduction or networking permitted without license from IHS -,-,- STD*JIS G L3LLI-ENGL JAPANESE INDUSTRIAL STANDARD JIS G 1314 : 1998 Method for chemical analysis of silicomanganese Introduction In the application of a Standard, the
9、normative references to the Standard shall be simultaneously referred to. Since silicomanganese is often used as auxiliary raw material, in addition to the methods for determination of manganese and silicon as principal components, the methods for determination of three components such as carbon and
10、 the like coming into problems in the manufacture of iron and steel are specified, and JIS G 1314 was established in 1953. Annex 2 is Japanese Industrial Standard prepared based on IS0 4159 Ferromanganese and ferrosilicomanganese - Determination of man- ganese content - Potentiometric method issued
11、as the first edition in 1978 without changing the technical contents. Further, “Informative references” with the dotted underline in Annex 2 are mat- ters which do not exist in the original International Standard. 1 Scope This Japanese Industrial Standard specifies methods for determination of manga
12、nese, silicon, carbon, phosphorus and sulfur in silicomanganese. 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 shall be applied. JIS G 1301
13、 General rules for chemical analysis of ferroalloys JIS K O121 General rules for atomic absorption spectrochemical analysis JIS K 8001 General rule for test methods of reagents JIS Z 2615 General rules for determination of carbon in metallic materials JIS Z 2616 General rules for determination of su
14、lfur in metallic materials 3 General matters General matters common to the determination shall be in accordance with JIS G 1301 and JIS K 0121. However, they are not applied to Annex 2. 4 Classification of methods for determination The methods for determina- tion of various kinds of components in si
15、licomanganese shall be as given in Table 1. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 23:17:49 MDTNo reproduction or networking permitted without license from IHS -,-,- 2 G 1314 : 199
16、8 Molybdophosphate blue absorptiometry Combustion-Sodium hydroxide titration Combustion-Infrared absorption method method Table 1 Methods for determination of various kinds of components in silicomanganese 0.01 or over up to and incl. 0.40 0.005 or over up to and incl. 0.10 0.005 or over up to and i
17、ncl. 0.10 8 9 10 Component 0.001 or over up to and incl. 0.05 Manganese 11 Silicon Carbon Phosphorus Sulfur Determination method Annex (normative) Applicable content range 8 (rnlrnf Potassium permanganate visual observation titration method -1 55 or over up to and incl. 80 1 Potassium permanganate p
18、otentiometric method (IS0 4169) I 55 or over up to and incl. 95 2 Dissodium ethylenediaminetetraacetate dihydrate titration method Silicon dioxide gravimetric method Potassium hexafluorosilicate precipitation separation sodium hydroxide titration method Combustion-Gas volumetric method 55 or over up
19、 to and incl. 80 I 3 8.0 or over up to and incl. 40 14 or over up to and incl. 40 0.05 or over up to and incl. 5.0 Combustion-Infrared absorption method I 0.001 or over up to and incl. 5.0 I 7 Hydrogen sulfide vaporizing separation methylene blue absorptiometry Copyright Japanese Standards Associati
20、on Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 23:17:49 MDTNo reproduction or networking permitted without license from IHS -,-,- , 3 G 1314 : 1998 Annex 1 (normative) Method for determination of manganese - Potassium permanga
21、nate visual observation titration method 1 Summary Decompose a sample with nitric acid and hydrofluoric acid, add sul- furic acid, generate white fume of sulfuric acid by heating, and remove nitric acid. Neutralize with zinc oxide, remove iron or the like, and titrate with potassium per- manganate s
22、tandard solution. Reagents The reagents shall be as follows : Hydrochloric acid (l+l) Nitric acid Hydrofluoric acid Sulfuric acid (1+1) Sodium disulfate Zinc oxide milk Add water to zinc oxide to make milky state. 0.02 mol/Z potassium permanganate standard solution The preparation and standardizatio
23、n method shall be in accordance with 4.5 (7) of JIS K 8001. Test portion The test portion shall be 0.10 g and read to the nearest 0.1 mg. Operation 4.1 Preparation of sample solution The preparation of sample solution shall be carried out according to the following procedures. a) Weigh a sample, tra
24、nsfer to a platinum dish (No. 100) or a polytetrafluoroethylene beaker (100 ml), and cover with a suitable cover. b) Slide the cover a little, add 15 ml of nitric acid, and decompose by dripping sev- eral drops of hydrofluoric acid step by step. When the reaction becomes violent in this procedure, c
25、ool the outside of the container with water. c) Wash the under surface of the cover with water, and remove it. d) Add 10 ml of sulfuric acid (l+l), vaporize by heating, and generate vigorously white fume of sulfuric acid for about 10 min, then, leave the solution to cool down (l). e) Add about 30 ml
26、 of water, and dissolve soluble salts by heating (2). fl Filter the solution with filter paper (class 5A), and wash several times with warm water. Receive the filtrate and washings in a beaker (300 ml), and reserve it as principal solution. Transfer the residue together with filter paper into a plat
27、inum Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 23:17:49 MDTNo reproduction or networking permitted without license from IHS -,-,- 4 G 1314 : 1998 crucible (No. 30), and incinerate. Af
28、ter allowing to cool, add about 2 g of sodium disulfate, and fuse by heating. After allowing to cool, put the solution together with the platinum crucible into the previously reserved principal solution, and dissolve the melt by heating. Wash the platinum crucible with a small amount of water, and t
29、ake it out. Notes (l) When colored insoluble matter exists at that time, add about 5 ml of hydrochloric acid (l+l), and generate again white fume of sulfuric acid by heating. (2) When undecomposed residue is not observed, the following (0 opera- tion is not carried out. 4.2 Removal of iron or the li
30、ke Carry out the removal of iron or the like ac- cording to the following procedures. Add water to the solution obtained in 4.1 e) or f) to dilute the solution to about 100 ml. Add little by little zinc oxide milk 2 f), neutralize, further add it a little exces- sively, and heat to boiling. Filter t
31、he precipitate together with excessive zinc oxide with filter paper (class 5A), wash sufficiently with warm water, and receive the filtrate and washings with an Erlenmeyer flask (500 ml) (3). Dilute the solution to about 200 ml by adding hot water, and further add one or two drops of zinc oxide milk
32、 2 f) to make the solution opaque. Note (3) At that time, the filtrate and washings may be opaque. 4.3 Titration For the titration, boil the solution obtained in 4.2 d) by heating, immediately titrate it with 0.02 mol/Z potassium permanganate standard solution 2 g), and take the point of time at whi
33、ch faint pink color of supernatant liquid does not disappear even though the solution is boiled for about 1 min after it has colored to faint pink as the end point, and obtain the amount of 0.02 mol/Z potas- sium permanganate standard solution used. 5 Blank Test A blank test is not carried out. 6 Ca
34、lculation Calculate the content of manganese in the sample according to the following formula : V x F x 0.001 648 Mn = m where, Mn : content of manganese in sample % (mlm) V : F : rn : test portion (g) amount of 0.02 mol/Z potassium permanganate stan- dard solution used which is obtained in 4.3 (mi)
35、 factor of 0.02 mol/Z potassium permanganate stan- dard solution used in 4.3 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 23:17:49 MDTNo reproduction or networking permitted without lice
36、nse from IHS -,-,- STD-JIS G L314-ENGL 1778 = 4933b08 0553785 Ob7 W Manganese content % mlm) 62.49 5 G 1314 : 1998 Within-laboratory reproducibility Reproducibility % mlm) % mlm) 0.269 0.319 7 Precision The precision shall be as given in Annex 1 Table 1. Annex 1 Table 1 Precision Informative referen
37、ce : The content of manganese given in the table is the manganese content in the sample used in the co-tests for determining the precision based on JIS Z 8402 (General rules for permissible tolerance of chemical analyses and physical tests). Copyright Japanese Standards Association Provided by IHS u
38、nder license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 23:17:49 MDTNo reproduction or networking permitted without license from IHS -,-,- 6 G 1314 : 1998 Annex 2 (normative) Manganese determination method - Potassium permanganate potentiometric method (I
39、S0 4159) 1 Scope and field of application This Annex 2 specifies a potentiometric method for the determination of the man- ganese content of silicomanganese. The method is applicable to alloys containing from 55 % (m/m to 95 % ( m / m ) of _ Informative reference : Though _-_-_-_ “of ferromanganese
40、_-_ and ferrosilicomanganese” - is stated in the original _ _ _ _ _ _ paper,the-ferroma-nganese- is- elimir- _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ nated since it is specified in JIS G 1311 and the silico- _ _ _ _ _ _ manganese _-_-_ is specified _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ - -
41、- - - - - - - - - - - - - - - - - z - - - - - - - in this Annex. Further the ferrosilicomanganese stated in the original paper is changed to “silicomanganese” according to the name of JIS prod- manganese. _-_- _ _ _ _ _ _ _ _ _ _ _ - - _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ . . . . . . . . . . . . . .
42、. . . . . . . _ - uct standard: 2 Reference IS0 3713 _._- Informative reference : Though _-_- in the original _- gaper, -:at -present-at the- stage- of Ferroalloys - Sampling and preparation of samples - General rules. l) braft”I .i% state4 as the -foot -not!? -9,- this heat without exceeding, even
43、locally, the tempera- ture of 60 O C , until the salt is completely dissolved. Cool. Prepare this solution at the time of use. 4.7 Potassium permanganate, recrystallized Place 50 g of pure analytical grade potassium permanganate in the conical flask (5.1), and dissolve it in 200 ml of warm distilled
44、 water (70 “C to 80 O C ) . Fit the reflux condenser (5.2) to the flask and boil the solution for 20 min. Filter the warm solution quickly under vacuum through a sintered glass funnel (5.3). Cool the filtrate in iced water, stirring vigorously, and allow the fine, crystalline precipitate to settle f
45、or 10 min. Decant the solution ; then, using a glass spatula, transfer the crystalline mass into a funnel with a filter plate, porosity 4, and place under suction for a few min- utes to remove most of the mother liquor. Dissolve the crystalline mass in 160 ml of distilled water (deionized water is n
46、ot permitted for this phase), and repeat the recrystallization. After filtering and placing under suction for approximately 5 min, transfer the crystalline mass onto a 150 mm diameter watch glass using a glass spatula, and dry it in air, protected from light and dust. When the crystalline mass no lo
47、nger ag- glomerates when crushed with the spatula, dry it at 110 “C for 2 h, then transfer it to a weighing bottle fitted with a ground glass stopper. Store in the dark. This salt contains 34.76 % (rn/rn) of Mn. Informative reference : When 0.02 mol/Z potassium permanganate standard so- 4.5 (7) of JIS K 8001, recrystallization is not required. _- -_-_ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ _ - lution (3.161 g _ _ _ _ _ _ _ _ _ _ KMno,!l)_ Mn = where, Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Emplo