Professional Documents
Culture Documents
INDUSTRIAL
STANDARD
Translated and Published by
Japanese Standards Association
(JFA/JSA)
Method for chemical analysis of
silicomanganese - Part 1: Determination
of manganese content
ICS 77.100
Reference number: JIS G 1314-1 : 2011 (E)
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G 1314-1 : 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 1314-1 : 2011
Contents
Page
Introduction································································································· 1
1 Scope ...................................................... ···········································1
2 Normative references············································································ 1
3 General ...................................................... ········································1
4 Classification of determination method ....................................... ·············1
(i)
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G 1314-1 : 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Consequently JIS G 1314:1998 has been withdrawn and partially replaced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 1314-1 : 2011
Introduction
This Japanese Industrial Standard has been prepared based on the first edition of
ISO 4159 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 in which the con-
tents of the corresponding International Standard have been modified. A list of modifi-
cations with the explanations is given in Annex JA.
1 Scope
This Standard specifies the determination method of manganese content in silico-
manganese.
NOTE: The International Standard corresponding to this Standard and the sym-
bol of degree of correspondence are as follows.
ISO 4159 : 1978 Ferromanganese and ferrosilicomanganese - Deter-
mination ofmanganese content - Potentiometric 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.
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3 General
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c) Wash the lower surface of the cover with water, and remove it.
d) Add 10 ml of sulfuric acid (1 + 1), vaporize it by heating to generate vigorously
white fume of sulfuric acid for about 10 min, then, allow the solution as it is to cool.
When coloured insoluble residue exists at that time, add about 5 ml of hydro-
chloric acid (1 + 1), and generate again white fume of sulfuric acid by heating.
e) Add about 30 ml of water, and dissolve soluble salts by heating.
f) Filter the solution with filter paper (Class 5A), and wash it several times with
warm water. Receive the filtrate and washings in a beaker (300 m!), and store it as
the principal solution. Transfer the residue together with filter paper into a plati-
num crucible (No. 30), and ash the filter paper by ignition. After allowing it to cool,
add about 2 g of sodium disulfate, and fuse it by heating. After allowing it to cool,
put the melt together with the platinum crucible into the previously stored princi-
pal solution, and dissolve it by heating. Wash the platinum crucible with a small
amount of water, and take it out.
When insoluble residue is not observed, the operation of:tj is not carried out and
transfer the solution of e) to a beaker (300 m!) by using water.
5.4.2 Removal of iron, etc.
The removal of iron, etc. shall be carried out according to the following procedure.
a) Add water to the solution obtained in 5.4.1 :tj and make the liquid amount about
100 ml.
b) Add zinc oxide milk (5.2.6) gradually to neutralize, further add it a little exces-
sively, and heat to boiling.
c) Filter the precipitate together with excessive zinc oxide with filter paper (Class 5A),
wash it with warm water, and receive the filtrate and washings with an Erlen-
meyer flask (500 m!) 1).
Note 1) At this time, the opaque in filtrate and washings is permissible.
d) Add hot water to make the liquid amount to about 200 ml, and further add one or
two drops of zinc oxide milk (5.2.6) to make the solution opaque.
5.4.3 Titration
For the titration, boil the solution obtained in 5.4.2 d) by heating, immediately ti-
trate it with 0.02 mollL potassium permanganate solution (5.2.7), and take the point at
which faint pink colour of supernatant liquid does not disappear even though the solu-
tion is boiled for about 1 min after it has coloured to faint pink as the end point, and
obtain the amount of 0.02 mollL potassium permanganate solution used.
5.5 Blank test
A blank test is not carried out.
5.6 Calculation
The manganese content rate in the sample shall be calculated from the used amount
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G 1314-1 : 2011
of 0.02 mollL potassium permanganate solution obtained in 5.4.3 according to the fol-
lowing formula.
VI X J, x 0.001648
Mn = x100
ml
Table 1 Tolerances
Unit: % (mass fraction)
Manganese content rate I Wi thin -labora tory-reprod ucibility limit I Reproducibility limit
62.49 I 0.269 I 0.319
NOTE: The manganese content rate given in this table is the manganese content rate in the
sample used in the cooperative experiment for determining the tolerances based on
JIS Z 8402 : 1991.
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6.2.6 0.02 mollL potassium permanganate solution The preparation shall be in ac-
cordance with 5.2.7.
6.3 Apparatus and implements
The following apparatus and implements shall be generally used.
6.3.1 Potentiometer That capable of measuring the potential difference between
electrodes by connecting electrodes of 6.3.2. pH meter having m V display may be used.
6.3.2 Electrodes For electrodes, any of the combination of platinum - saturated
calomel, platinum - tungsten or platinum - platinum shall be used.
6.4 Amount of test portion
The test portion shall be 1.0 g weighed out to the digit of 0.1 mg.
6.5 Procedure
Warning: The vapour of perchloric acid has a risk of explosion under presence of
ammonia, nitrite vapour or organic matters. The vapour shall be treated
at a place equipped with an exhaust equipment which ensures safety
under use of perchloric acid.
6.5.1 Preparation of sample solution
The preparation of sample solution shall be carried out according to the following
procedure.
a) Weigh out the sample, transfer it to a platinum dish (No. 200) or a PTFE beaker
(300 mn, and place a platinum or PTFE cover.
b) Add 10 ml of hydrochloric acid and 15 ml of perchloric acid, then decompose it by
adding about 20 ml of hydrofluoric acid gradually.
c) Heat gently at first, then increase the heat until dense white fume of perchloric
acid is generated. Continue heating until a syrupy consistency is obtained and
manganese dioxide begins to precipitate.
d) After allowing it to cool, add 20 ml of hydrochloric acid (1 + 4), and dissolve soluble
salts by heating. Heat the solution gently until it becomes transparent.
The case where insoluble residue exists shall be in accordance with 5.4.1 t).
e) Add 50 ml of hot water and allow it to cool to the room temperature.
6.5.2 Titration
The titration shall be carried out according to the following procedure.
a) Transfer the sample solution obtained in 6.5.1 e) into the volumetric flask (250 mn
using water, allow it to cool to the ordinary temperature, and add water up to the
marked line.
b) Take 50 ml of the solution using the pipette, transfer it to a beaker (500 mn, and
dilute it to 100 ml by adding water, and add 250 ml of sodium diphosphate solution
(6.2.5) 2).
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Note 2) When using the automatic titration apparatus having the potential dif-
ference meter on the market, a beaker (200 m!) used for titration may
be used. In this case, the aliquot shall be 25 ml, the amount after addi-
tion of water shall be 50 ml, and the addition amount of sodium di-
phosphate solution shall be 100 ml.
c) Place a beaker on the magnetic stirrer, put a rotator, and start to stir.
d) Adjust pH of this solution to 6.5 to 7.0 with hydrochloric acid (1 + 2) by using a pH
meter.
e) Titrate the solution with 0.02 mollL potassium permanganate solution (6.2.6) by
using the potentiometer and read the amount used by taking the point at which the
deflection of potentiometer becomes largest as the end point.
6.6 Blank test
6.7 Calculation
The manganese content rate in the sample shall be calculated from the used amount
of 0.02 mollL potassium permanganate solution obtained in 6.5.2 according to the fol-
lowing formula.
V, Xf2 xO.004395
Mn = ~ xiOO
m 2 xB /250
Table 2 Tolerances
Unit: % (mass fraction)
Manganese content rate I Within-laboratory-reproducibility limit I Reproducibility limit
62.49 I 0.277 I 0.342
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b) Slide the cover a little, add 15 ml of nitric acid, and decompose it by dripping sev-
eral drops of hydrofluoric acid step by step. When the reaction becomes vigorous in
this procedure, cool the outside of the container with water.
c) Evaporate the solution to dry up by heating, further heat for about 10 min, then,
allow it to cool.
d) Wash the lower surface of the cover with a small amount of water and remove it,
add 10 ml of hydrochloric acid (1 + 1), and dissolve soluble salts by heating 3).
Note 3) When insoluble residue is not observed, the operation of e) need not be
carried out.
e) Filter the solution with filter paper (Class 5A), and wash it several times with
warm water. Receive the filtrate and washings in a beaker (300 m!), and store it as
the principal solution. Transfer the residue together with filter paper into a plati-
num crucible (No. 30), and ash the filter paper by ignition. After allowing it to cool,
moisten with several drops of sulfuric acid (1 + 1), add about 1 ml of hydrofluoric
acid, and heat to dry up. After allowing it to cool, add about 2 g of sodium disulfate,
and fuse it by heating. After allowing it to cool, put the melt together with the
platinum crucible into the previously stored principal solution, and dissolve it by
heating. Wash the platinum crucible with a small amount of water, and take it out.
7.4.2 Titration
The titration shall be carried out according to the following procedure.
a) Transfer the solution obtained in d) or e) of 7.4.1 into an Erlenmeyer flask (500 m!)
with water, add water to make the liquid amount about 150 ml, and allow it to cool
to the room temperature.
b) Add 5 ml of hydroxyl ammonium chloride solution (50 giL) and 20 ml of 2,2',2"-ni-
trotriethanol solution (1 + 4) while shaking the solution, and further gradually add
50 ml of ammonium buffer solution (7.2.7). Thereafter, add about 1 mlofpotassium
cyanide solution (10 giL).
c) Add 0.05 g to 0.08 g of thymolphthalein complexion indicator (7.2.11). After shak-
ing, immediately titrate with 0.05 mollL EDTA2Na solution (7.2.10), take the point
at which the solution turns from blue to yellow or colourless as the end point, and
obtain the amount of 0.05 mollL EDTA2Na solution used.
7.5 Blank test
A blank test is not carried out.
7.6 Calculation
The manganese content rate in the sample shall be calculated from the used amount
of 0.05 mollL EDTA2Na solution obtained in 7.4.2 according to the following formula.
Mn =
~
-
xh- x 0.002747 x 100
m3
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Table 3 Tolerances
Unit : % (mass fraction)
Manganese content rate I Within-laboratory-reproducibility limit I Reproducibility limit
62.59 I 0.314 I 0.546
NOTE: The manganese content rate given in this table is the manganese 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) ~
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3 General In accordance with JIS 1 Scope In accordance with Alteration Practically identical. -
G 130l. ISO 3713.
4 Classifi- Potassium permanga- 1 Scope Only potentiometric Addition In ISO Standard, only po- For determination meth-
cation of nate visual titration method is specified. tentiometric method is ods other than potenti-
determina- method, potassium specified. In JIS, two other ometric method, proposal
tion permanganate potenti- determination methods are to ISO will be studied.
method ometric method, and specified.
disodium ethylenedia-
minetetraacetate di-
hydrate titration
method
(n 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 de via tion
title of clause tion by
clause clause
5 Potas- Potassium permanga- - - Addition Potassium permanganate Added because this method
sium per- nate visual titration visual titration method is widely used in Japan.
manganate method which utilizes faint pink col-
visual ti- our is added.
tration
method
"'d
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o 6.1 Sum- Decompose sample 3 Prin- Identical with JIS. Identical - -
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t:rj mary with acid, adjust pH ciple
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t:rj
U ometric method
to
~ 6.2 Re- 0.02 mollL potassium 4Re- 0.1 N potassium per- Alteration In JIS, mollL which is of SI Proposal to ISO will be
o
o agents permanganate solution agents manganate solution units is used. studied.
~ 6.3 Appara- Potentiometer, elec- 5 Appa- Conical flask, reflux Deletion General instruments such There is no deviation prac-
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"""" tus and im- trodes ratus condenser, pH meter, as glass instruments quoted tically.
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~ plements potentiometer, etc. in JIS G 1301 are deleted.
are specified.
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national International Standard deviation between JIS and the Interna- technical deviation and
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Standard tional Standard by clause future measures o
~
number
No. and Content No. of Content Classifica - Detail of technical de via tion ~
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"""" - Identical: Identical in technical contents.
~
~ - Deletion: Deletes the specification item(s) or content(s) of International Standard.
- Addition: Adds the specification item(s) or content(s) which are not included in International Standard.
- Alteration: Alters the specification content(s) which are included in International Standard.
NOTE 2 Symbol in column of overall degree of correspondence between JIS and International Standard in the above table indicates as follows:
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