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Jis G 1314-2-2011
Jis G 1314-2-2011
INDUSTRIAL
STANDARD
Translated and Published by
Japanese Standards Association
(JFA/JSA)
Method for chemical analysis of
silicomanganese - Part 2: Determination
of silicon content
ICS 77.100
Reference number: JIS G 1314-2 : 2011 (E)
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G 1314-2 : 2011
© J5A 2013
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 the publisher.
Printed in Japan HN
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G 1314-2 : 2011
Contents
Page
Introduction································································································· 1
1 Scope ...................................................... ···········································1
2 Normative references············································································ 1
3 General ...................................................... ········································1
4 Classification of determination method ....................................... ·············1
5 Silicon dioxide gravimetric method ......................................................... 2
5.1 Summary···························································································· 2
5.2 Reagents ...................................................... ······································2
5.3 Amount of test portion·········································································· 2
5.4 Procedure ...................................................... ·····································2
5.5 Blank test················ ...................................................... ·····················4
5.6 Calculation ........................................................................ ·················4
5.7 Tolerances ...................................................... ····································4
(i)
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G 1314-2 : 2011
Foreword
This translation has been made based on the original Japanese Indus-
trial Standard established by the Minister of Economy, Trade and In-
dustry through deliberations at the Japanese Industrial Standards
Committee according to the proposal for establishment of Japanese In-
dustrial Standard submitted by the Japan Ferroalloy Association (JFA)I
Japanese Standards Association (JSA) with the draft being attached,
based on the provision of Article 12 Clause 1 of the Industrial Stan-
dardization Law.
Consequently JIS G 1314:1998 has been withdrawn and partially replaced
with this Standard.
This JIS document is protected by the Copyright Law.
Attention is drawn to the possibility that some parts of this Standard
may conflict with a patent right, application for a patent after opening to
the public or utility model right. The relevant Minister and the Japanese
Industrial Standards Committee are not responsible for identifying the
patent right, application for a patent after opening to the public or utility
model right.
JIS G 1314 series consists of the following 6 parts under the general title
"Method for chemical analysis ofsilicomanganese":
Part 1: Determina tion ofmanganese con ten t
Part 2: Determination ofsilicon content
Part 3: Determination of carbon content
Part 4: Determina tion ofphosphorus con ten t
Part 5: Determination ofsulfur content
Part 6: Determina tion of boron con ten t
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JAPANESE INDUSTRIAL STANDARD JIS G 1314-2 : 2011
Introduction
This Japanese Industrial Standard has been prepared based on the first edition of
ISO 4158 published in 1978 with some modifications of the technical contents to corre-
spond to the progress in analysis technology.
The portions given sidelines or dotted underlines are the matters not given in the
corresponding International Standard. A list of modifications with the explanations is
given in Annex JA.
1 Scope
This Standard specifies the determination method of silicon content in silicomanga-
nese.
NOTE: The International Standard corresponding to this Standard and the sym-
bol of degree of correspondence are as follows.
ISO 4158 : 1978 Ferrosilicon) ferrosilicomanganese and ferrosilicochro-
mium - Determination ofsilicon content - Gravimetric method (MOD)
In addition, symbols which denote the degree of correspondence in the
contents between the relevant International Standard and JIS are IDT
(identical), MOD (modified), and NEQ (not equivalent) according to
ISOIIEC Guide 21-1.
2 Normative references
The following standards contain provisions which, through reference in this text,
constitute provisions of this Standard. The most recent editions of the standards (in-
cluding amendments) indicated below shall be applied.
JJS_J!__19J)l ___ }i}!!:J;:Q!!JlQy§_~_G?lJ.?XEJIXl!}?§fQ~[lh~!!!jf;!!l/!-lJ.!Jlx~i~
J1SJ(_8_QQl ____ G~IJ.?XEJIXlJl~fQJ;:j;~~t!!!_f!_~.hQd$._Qfr..?_EJgf!!Jt~
3 General
.G-_~_1l~x~1_m_~_tt~x~ __GQm}:p.9}~~_JQ_Jh~ __ ~h~mj._G~1_~n~J.Y~5o~__ m_~thQd __ ~J~~ll_b~ __ in_~~~_Qxd~nG~
wj,th .JJS_ -'1 _l3-')t~
4 Classification of determination method
The determination method of silicon content shall be according to either of the fol-
lowing.
a) Silicon dioxide gravimetric method This method is applicable to the sample of
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G 1314-2 : 2011
which the silicon content rate is 10 % (mass fraction) or over up to and including
35 % (mass fraction).
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b~~~tl~Q:rg~ili~~W____ Thif?__ m~thQsljf?__~F..Rli~9.:Rl~_t_Q__tb~_~mmI>Jg__Qf_wJli~h_tbg_f?51i~_Qn_~_Qn~
t~nt_r9.:t~_i~_14_%_~l).)._~_I?~_fr:9.:~_ti~H1tQX_9.Y:~X_llP__tQ_9.:!HtjJJgJJJdinK3Q_%_(m9.:f?_I?_f:t;~~tjQn.t
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G 1314-2 : 2011
d) Raise its temperature, heat it at about 700°C (dark red colour state) for about 5
min by swirling the crucible until it completely fuses, then allow it to cool.
e) Place the crucible and the cover into a beaker (500 m!) in which 60 ml of hydro-
chloric acid (1 + 2) has been put, dissolve the melt, and remove the crucible and the
cover after being rinsed with water.
5.4.2 Dehydration of silicon dioxide
The dehydration of silicon dioxide shall be carried out according to the following pro-
cedure.
a) Add 60 ml ofperchloric acid into the solution obtained in 5.4.1 e).
b) Heat it on a hot plate for evaporation and for generation of the dense white fume of
perchloric acid, then cover it with a watch glass.
c) Continue heating for about 15 min under the condition where the perchloric acid
vapour is refluxed along the inside wall of the beaker, then allow it to cool.
d) Add 20 ml of hydrochloric acid (1 + 1) and heat, decompose precipitated manganese
oxides, etc., and add about 100 ml of warm water to dissolve soluble salts.
e) Immediately filter the solution through filter paper (Class 5A), and put the filtrate
into another beaker (500 m!).
f) Transfer the precipitate stuck on the inside wall of the beaker and the watch glass
by rubbing it with a rubber-tipped stirring rod onto the filter paper, wash it with
warm hydrochloric acid (1 + 10) five times, wash it with warm water until no iron
(III) ion can be detected 1), then put the washings together with the filtrate. Pre-
serve this precipitate and filter paper.
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.n9.t_t~king_gn_x~dQ.j_$h __Qx~rrg~ __ ~9.l9.1-!~ __wll&rr __ ~dQ.j_ng_'p'9.t~~~i~m___thjg~y-=
.~rr~ t~__$Qlll_tiQ!1_ {lQQ _g~L} JQ _jt~
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Table 1 Tolerances
Unit: % (mass fraction)
Silicon content rate Within -laboratory-reproducibility limit Reproducibility limit
17.21 0.120 0.526
16.18 0.140 0.554
NQrE__:___ r.b_~_~ili9_Qn~9D_t~_ntx~t~_giy~p.:.ip.:_thi~_t~Rl~.if?_tb&_~ili~9D__G9.P.:t~P.:t.K~_t~__in_th~_f?~n:ml~_
:tJ_~~<i.iP.:_tb~_~Q9.P_~K~tiY~_~~:R~:rj_I)J._~ntJQK_<i~_t~xminin.Kt.b.~_t.Ql~:r_~)J._G~_I?_h~~gg_QP.:_JJS_Z_
~~Q~_:_U)_~_L
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G 1314-2 : 2011
f= m6 x_A_
0.04855 x VI 100
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5) Transfer the solution by using warm water into a polyethylene beaker (300 mn in
which 50 ml of nitric acid (1 + 1) has been put.
6) Add 3 ml of hydrochloric acid into the crucible to dissolve the melt stuck on the
inside wall of the crucible, wash the crucible and the cover with water sufficiently,
then put this solution and washings together with the solution of 5).
7) Heat the solution on a water bath to completely dissolve the melt, and add water
to make the liquid amount about 80 ml.
8) Add 10 ml of hydrofluoric acid and 3 g of potassium nitrate, mix them, and heat it
for about 15 min on a water bath.
9) Add small amount of filter paper pulp, allow it to stand for about 30 min while
being cooled to 15°C or lower, and precipitate potassium hexafluorosilicate.
6.4.2 Filtration of precipitate
The filtration of precipitate shall be carried out according to the following procedure.
a) Filter the precipitate obtained in a) 4) or b) 9) of 6.4.1 while being cooled to 15°C or
lower by using a polyethylene funnel attached with a filter paper (Class 5A).
b) Wash sufficiently the precipitate and the filter paper with potassium nitrate solu-
tion (50 giL) (6.2.5) cooled to 15°C or lower until blue litmus paper gives no change
to red colour when the washings are dripped. Discard the filtrate and washings.
6.4.3 Titration
The titration shall be carried out acording to the following procedure.
a) Transfer the precipitate obtained in 6.4.2 b) together with filter paper into an Er-
lenmeyer flask (200 mn.
b) Add about 50 ml of warm water, sufficiently mix by shaking, and crush the filter
paper.
c) After boiling the solution by heating, add several drops of phenolphthalein solution
(6.2.9), and add 0.5 mollL sodium hydroxide solution (6.2.8) at once approximate to
the end point.
d) Add several drops of phenolphthalein solution (6.2.9), titrate again with 0.5 mollL
sodium hydroxide solution (6.2.8), and stop the titration for a while when the solu-
tion turns faint pink colour.
e) Stopper the Erlenmeyer flask, mix sufficiently the solution by shaking, continue
titration when the faint pink colour vanishes, take the point where the solution has
turned again to faint pink colour as the end point, and obtain the amount of 0.5
mollL sodium hydroxide solution (6.2.8) used.
6.5 Blank test
The same operation as the sample shall be carried out without using the sample in
parallel with the sample.
6.6 Calculation
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G 1314-2 : 2011
The silicon content rate in the sample shall be calculated from the used amounts (m!)
of 0.5 mollL sodium hydroxide solution for the sample and in the blank test according
to the following formula.
(V2 - V3 ) x F x 0.003 511
Si= x100
m7
Table 2 Tolerances
Unit: % (mass fraction)
Silicon content rate Wi thin -labora tory-reprod ucibility limit Reproducibility limit
17.14 0.280 0.669
16.14 0.244 0.596
NOTE: The silicon content rate given in this table is the silicon content rate in the sample
used in the cooperative experiment for determining the tolerances based on JIS Z
8402 : 1991.
Bibliography
JIS Z 8402 : 1991 General rules for permissible tolerance of chemical analyses and
physical tests
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Annex JA (informative)
Comparison table between JIS and corresponding International Standard
JIS G 1314-2 : 2011 Method foI' chemical analysis ofs11icomanganese - PaI't 2 : ISO 4158 : 1978 FeITosilicon, feI'I'osilicomanganese and fen'osili-
DeteI'mination ofsilicon content cochI'omium - DeteI'mination ofsilicon content- GI'avimetI'ic method
(I) Requirements in JIS (II) Inter- (III) Requirements in (IV) Classification and details of technical (V) Justification for the
national International Standard deviation between JIS and the Interna- technical deviation and
Standard tional Standard by clause future measures
number
No. and Content No. of Content Classifica - Detail of technical deviation
title of clause tion by
clause clause
1 Scope Determination method 1 Determina tion Addition In ISO Standard, only sili- Proposal of addition of the
"'d of silicon content in method of silicon con dioxide gravimetric sodium hydroxide titration
~
o silicomanganese is content of ferrosili- method is specified. In JIS, method after separation of
~
t:rj
specified. con, ferrosilicoman- sodium hydroxide titration precipitated potassium
o
~ ganese and ferrosili- method after separation of hexafluorosilicate to ISO
t:rj
U cochromium is precipitated potassium will be studied.
to
~ specified. hexafluorosilicate is added.
o
o 2 Norma-
~ tive refer-
o
"""" ences
~
~
3 General In accordance with JIS - - Addition Not specified in ISO Stan- Proposal to ISO will be
G 130l. dard. studied.
4 Classifi- Silicon dioxide gra- Silicon dioxide gra- Addition In ISO Standard, only sili- Proposal of addition of the
cation of vimetric method vimetric method con dioxide gravimetric sodium hydroxide titration
determina- Sodium hydroxide ti- method is specified. In JIS, method after separation of
tion tration method after sodium hydroxide titration precipitated potassium
method separation ofprecipi- method after separation of hexafluorosilicate to ISO 0
I--'
tated potassium precipitated potassium will be studied. CA:l
I--'
hexafl uorosilica te hexafluorosilicate is added. *:'"
t-.:l
t-.:l
0
I--'
1--'\.0
o~
o
~
CJJ
~
~
(I) Requirements in JIS (II) Inter- (III) Requirements in (IV) Classification and details of technical (V) J ustifica tion for the I
~
national International Standard deviation between JIS and the Interna- technical deviation and
~
Standard tional Standard by clause future measures o
~
number
No. and Content No. of Content Classifica - Detail of technical deviation ~
5.4 Proce- Procedure is specified. 7.3 Procedure is speci- Addition There is difference in con- Proposal to ISO will be
dure fied. firmation method of wash- studied.
ing.
5.5 Blank Method of blank test is 7.2 Identical with JIS. Identical - -
test specified.
6 Sodium Sodium hydroxide ti- - - Addition Sodium hydroxide titration Proposal of addition of so-
hydroxide tration method after method after separation of dium hydroxide titration
"'d titration separation ofprecipi- precipitated potassium method after separation of
~
o method af- tated potassium hexafluorosilicate is added. precipitated potassium
~
t:rj ter separa- hexafl uorosilica te hexafluorosilicate to ISO
o
~ tion of pre- will be studied.
t:rj
U cipitated
to potassium
~
o hexafluoro-
o
silicate
~
o
""""
~
~
Overall degree of correspondence between JIS and International Standard (ISO 4158 : 1978): MOD
NOTE 1 Symbols in sub-columns of classification by clause in the above table indicate as follows:
- Addition: Adds the specification item(s) or content(s) which are not included in International Standard.
0
I--'
- Alteration: Alters the specification content(s) which are included in International Standard. CA:l
I--'
NOTE 2 Symbol in column of overall degree of correspondence between JIS and International Standard in the above table indicates as follows: *:'"
t-.:l
- MOD: Modifies International Standard. t-.:l
0
I--' I--'
I--' I--'
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monthly by the Japanese Standards Association, and also provided to subscribers of JIS
(English edition) in Monthly Information.
Errata will be provided upon request, please contact:
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