,,

JAPANESE
INDUSTRIAL
STANDAR·D
Translated and Published by
Japanese Standards Association

JIS G 2402= 2009

(JAA/JSA)

Aluminium dross for iron and steel mak-

ing

PRI TED
JAPANESE STANDARDS ASSOCIATION

ICS 77.120.10; 77.140.01

Reference number : . JIS G 2402 : 2009 (E)

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G 2402:2009

Date of Establishment: 2002-01-20

Data of Revision: 2009-04-20
Date of Public Notice in Official Gazette: 2009-04-20
Investigated by: Japanese Industrial Standards Committee
Standards Board
Technical Committee on Non-Ferrous Metals

JIS G 2402 : 2009, First English edition published in 2009-11

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.

© JSA 2009
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 2402:2009

Contents

Page

1 Scope ........•...................... ,; ...~............... ~.......~ ................... , .................. 1

2 Normative references .... ···· .... ··· .... · ... ·· .... ···· .. · ..·.... ·· ... ·· .. ····.~;~; ... ·· .. · .... ·: .. ·1
3 General matters ...·..... , ............~····.·:···· .. ··················"····.:,·:····:··················1
4 Classification and symbol · · · · · · · · · · ·: · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · 1
5 Quality · · .............................. ~, .... · · · · ... · .. ; ..... ·;. .... · · ..... · · ............ · · · · ..... · · · 2
6 Tests ................... ,; ........................................................................... 4
6.1 Quantitative determination method for metallic aluminium · · · · · · · · · · · · · · · · · · · · · · · 4
6.2 ~Quantitative determination method of nitrogen · · · · · · ·, · · ·' · · · · · · · · · · · · · · · · · · · · · · · · · · ·12
6.3 Quantitative determination method of chloride ion ··· ·· ·· ···· · · · ··· ·· ···· · ·· ···· ····17
6.4 ·Quantitative determination method of total silicon · · · · · · · · · · · · · · · ·: · · · · · · · · · · · · · · · · ·23
6.5 Quantitative determination method of aluminium oxide ·· · · · · · · · · · · · · · · · · · · · · · ·' · ·29
6.6 Quantitative determination method of carbon · · · · · ·'' · ·' · · · · · · · '· · · · · · · · · · · · · · · · · · · · · ·29
6.7 Determination method of water ............................................................29
6.8 Sampling arid preparation method ......................... , ..............................29
7 Inspection .. ·· .... ··· ...... :.· .. · .. · .. · ........ ···· .... ·· ........ · .... · .. ·· .... ·· .... ·· .... · .... · .. ·29
8 Marking · · · · · · · · · · · ··· · · · · · · · · · · · · · · · · · · · · · · · ·· · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · · ·29

(i)
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the content of metallic aluminium and further divided into 3 grades (Grade 11 to Grade
13) according to the content of aluminium oxide. In addition, it is subdivided into A to
D according to the permissible amount of impurities or composition of analysis control.

Table 1 Classification and symbol

Classification Subdivision Symbol Classification Subdivision Symbol
Aluminium dross A DR70A Aluminium dross A DR30A
Grade 1 B DR70B Grade 5 B DR30B
c DR70C Aluminium dross A DR20A
Aluminium dross A DR60A Grade 6 B DR20B
Grade 2 B DR60B Aluminium dross A DR lOA
c D~60C Grade7 B DR lOB
Aluminium dross A DR50A Aluminium dross A AOX65A
Grade 3 B DR5.0B Grade 11 B AOX65B
c DR50C Aluminium dross A AOX60A
D DR50D Grade 12 B AOX60B
Aluminium dross A DR40A Aluminium dross A AOX50A
Grade 4 B DR40B Grade 13 B AOX50B
c DR40C

5 Quality
The quality of aluminium dross shall be as follows.
a) The incorporation of foreign matters such as dust shall not be permitted. However,
the additives as effective composition such as metallic aluminium and aluminium
oxide shall be excepted from the rule.
b) In the case of adding metallic aluminium, such aluminium powder (dangerous
goods Class 2) Il that more than 50 % (mass fraction) of powder can pass through
the sieve of metal wire cloth with nominal aperture of 150 J.llil specified in JIS Z
8801-1 shall not be used.
Note Il It is based on Article 1 (iii) of General Provisions in Rules ori Control of
Dangerous Goods (the Ordinance of the Prime Minister's Office No. 55
of 1960).
c) The moisture content in aluminium dross shall not exceed 2 % excluding crystalli-
zation water.
d) Aluminium dross shall be tested in accordance with clause 6. The chemical compo-
sition of aluminium dross shall be as shown in tables 2 and 3.

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{ ; G 2402:2009
"--''
Table 2 Chemical components of Grade 1 to Grade 7 that are
composed mainly of metallic aluminium

Moisture

DR70A 70 min. 1 max. 0.5 max. 3 max. - -

DR70B 70 min. 2 max. 1 max. 5 max. - -
DR70C 70min. - - - - -
DR60A 60 or over to and excl. 70 1 max. 0.5 max. 3 max. - -
DR60B 60 or over to and excl. 70 2 max. 1 max. 5 max. - -
DR60C 60 or over to and excl. 70 - - - - -
DR50A 50 or over to and excl. 60 2 max. 2 max. 5 max. - -
DR50B 50 or over to and excl. 60 2 max. 2 max. 10 niax. - -
DR50C .50 or over to and excl. 60 3 max. 2 max. 10 max. -
DR50D 50 or over to and excl. 60 - - - - -
DR40A 40 or over to and excl. 50 2 max. 2 max. 10 max. 25 min. -
DR40B 40 or over to and excl. 50 3 max. 2 max. 10 max. 25 min. -
DR40C 40 or over to and excl. 50 - - - 25 min. -
DR30A 30 or over to and'exel. 40 3 max. 2 max. 15 niax. 25'miri. -
DR30B 30or over to and excl. 40 - - - 25 min. -
DR20A 20 or over to and excl. 30 3 max. 2 max. 20 max. 30 min. -
DR20B 20 or over to and excl. 30 - - - 30 min. -
DRlOA 10 or over to an:d excl. 20:. ' 5 max-. .3 max. .20 max.. .40-·min. -
DR10B 10 or over to and excl. 20 - 40 min. -
- Carbon shall be not JnOre than 5% (mass fraction). However, the analysis shall be carried
out only at the time of request from the purchaser.··
- For .the components not specified in table 2, the analysis shall be carried out only at the
time of request from the purchaser. ·
Notes al It is permitted to deal with it as the total amount of Al + Mg including the amount
of metallic magnesium. .
h) The analysis of other components shall be carried out only at the time of request
from the purchaser.
cl For obtaining the value of silicon oxide (SiOz), the value converted to SiOz from the
total amount of silicon in sample shall be used.

Table 3 Chemical components ofGrade.ll to Grade13 that are

composed mainly of aluminium oxide
Symbol Chemical component % (mass fraction)
of Grade Alumin- Nitrogen Chloride Metallic Others al
ium oxide ion alumin- Carbon Silicon Moisture
ium dioxide b)
AOX65A 65 min. 5 max. 3 max. 20 max. 5 max. 5 inax. -
AOX65B 65 min. 7 max. 3 max. 20 max. 5 max. 5 max. -
AOX60A 60 min. 5 max. 3 max. 15 max. 5 max. 10 max. -
AOX60B 60 min. 7 max. 3 max. 15 max. 5 max. 10 max. -
AOX50A 50 min. 5 .max. 3 max. 15 max. 5 max. 20 max. -
AOX50B 50 min. - - .15 max. 5 max; 20 max. -
For the components not specified in table 3, the analysis shall be carried out only at the time
of request from the purchaser.
Notes al The analysis of other components shall be carried out only at the time of request
from the purchaser.
bl For obtaining the value of silicon oxide (SiOz), the value converted to SiOz from the
total amount of silicon in sample shall be used.

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6 Tests
6.1 Quantitative determination method for metallic aluminium
6.1.1 Classification of quantitative determination method
The quantitative determination for metallic aluminium shall be in accordance with
any method among the followings.
Furthermore, the determination methods of c) and d) are specified as simple methods
and may be used for daily .control analysis.
a) Bromine . methanol decomposition inductively coupled plasma atomic emission
spectrometry This method shall be applied to the sample I;tot less than 1 % (mass
fraction) of metallic ahiminium content.
b) Bromine methanol decomposition chelate titration method This method .shall be
applied to the sample not less than 5% (mass fraction) of metallic aluminium con-
tent.
c) Volumetric method by gas dissolved in hydrochloric acid This method shall be
applied to the sample not less than 5 % (mass fraction) of metallic aluminium con-
tent.
d) Reaction solution temperature measuring method · This method is specified as a
simple determination method for metallic aluminium and shall be applied to the
sample not less than 15 % (mass fraction) of metallic aluminium content.
6.1.2 Bromine methanol decomposition inductively coupled plasma atomic emission
spectrometry
6.1.2.1 Summary
Metallic aluminium is dissolved by reacting the ~ample with mixed solution of bro-
mine and methanol. After the residue has been filtered to separate, the solution is
made to a definite volume and aluminium is determined by inductively coupled plasma
atomic emission spectrometry (hereafter referred to as "ICP atomic emission spec-
trometry'').
6.1.2 Reagents
6.1.2.2.1 Hydrochloric acid (1 + 1)
6.1.2.2.2 Hydrogen peroxide (30 %)
6.1.2.2.3 Bromine
6.1.2.2.4 Methanol
6.1.2.2.5 Reference solution of aluminium .(AI : 1 giL) Weigh out 1.000 g of alumin-
ium [not less than 99.9% (mass fraction) in purity], transfer it into a conical beaker (500
ml). Add 2o ml of hydrochloric acid (1 + 1) and 20 ml of nitric acid (1 + 1), heat it to de-
compose. After decomposed completely, boil it quietly for 2 min to 3 min. After cooled in
running water to room temperature, wash it with water totransfer in a 1 000-ml volu-
metric flask and dilute it to the marked line.

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6.1.2.3 Apparatus

Apparatus shall be inductively coupled plasma atomic emission spectrophotometer

(hereafter referred to as "ICP emission spectrophotometer").
6.1.2.4 Pretreatment of sample
Pulverize the sample by using an appropriate pulverizer such as vibrating mill so as
not to oxidize it to the utmost. Make that pulverized to 0.5 mm or finer the sample for
analysis. Preserve the pulverized sample in a desiccator or a polyethylene bag and the
like.
6.1.2.5 .Am:ount of sample weighed out
The amount of sample weighed out shall be 2.0 g and measured to the nearest 1 mg.
6.1.2.6 Operation
The operation shall be as follows.
a) Preparation of sample solution
I) Weigh out the sample and transfer it into a conical beaker (500 ml):
2) Add 200 ml of methanol, put a cylindrical thermometer (0 °C to 100 °C) and cover
it with a watch glass. Add 10 ml of bromine 1 ml by 1 ml at initial.and 2 ml by 2
ml after the reaction becomes gentle. Adjust, if necessary, by cooling it in running
water and the like so as to maintain the temperature of solution at the time of
reaction at 40 °C or lower 2l.
3) Mter the addition of bromine has been completed and the decomposition reaction
of metallic aluminium, etc. has' been almost completed, leave it as it is for ap-
proximately 1 h and decompose it completely.
4) Filter to separate the solution with using filter paper of class 5 C or membrane
filter of 1 Jlm in pore size and wash the filter paper (membrane filter) and residue
with using a little amount of methanol 4 or 5 times. In addition, the membrane
filter made of polytetrafluoroethylene or of poly-carbonate shall be used. Receive
the filtrate and the washings together in a 500-ml volumetric flask added previ-
ously with 40 m. of hydrochloric acid (1 + 1), dilute it approximately to 450 ml
with water, cool it to room temperature in running water and afterwards dilute it
to the marked line with water.
5) Take an aliquot of 50 ml of this solution in a conical beaker (300 mD. Mter 5 ml of
hydrochloric acid (1 + I) has been added, heat it on a hot plate and concentrate it
to approximately 5 ml by evaporation. After it has been put down from the hot
plate and cooled as it is, remove bromine by addi:qg 1 ml of hydrogen peroxide and
heating. Furthermore, continue to heat it and cor1c1:mtrate the solution to become
syrup like.
6) Add 10 ml of hydrochloric acid (1 + 1), dissolve the deposited salts, boil it gently
for 1 min to 2 min and afterwards cool it to room temperature in running water.
7) Wash to transfer it with water into a 100-ml volumetric flask and dilute it to the

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marked line. Take an aliquot of 10 ml of this solution into a 100-ml volumetric

flask and dilute it to the marked line with water.
Note 2l
When the temperature of solution exceeds 40 oc at the time of decom-
position, the aluminium compounds other than metallic aluminium
start to be dissolved.
b) Measurement
1) Set ICP emission spectrophotometer at the measurement condition, light piasma
and make it the condition capable of measuring stably.
2) Spray a portion of the solution prepared in 6.1.2.6 ·a) 7) into the plasma in ICP
emission spectrophotometer and measure the emission intensity at the emission
wave length of aluminium such as 309.271 nm, 309.284 nm, 396.152 nm, etc. For
the apparatus capable of measuring background simultaneously, measure the
background at the wavelength without affecting aluminium and other coexisting
elements in the neighbourhood of measuring wavelength selected and obtain the
real emission intensity of aluminium.
3) Obtain the amount of aluminuim from the working curve prepared simultane-
ously according to 6.1.2.8.
6.1.2. 7 Blank test
The blank test shall not be carried out.
6.1.2.8 Preparation of working curve
Add the reference solution of aluminium (6.1.2.2.5) of 0 mg, 0.5 mg, 1 mg, 3 mg, 5 mg,
10 mg, 15 mg and 20 mg as aluminium into eight 100-ml volumetric flasks, respec-
tively. Add 1 ml of hydrochloric acid (1 + 1) and then dilute it to the marked line with
water. Mea~ure these solutions according to 6.1.2.6 b), prepare the relation curve of
emission intensity to amount of added aluminium and make it the working curve.
6.1.2.9 Calculation
Calculate the content of metallic aluminium according to the following formula.
500 100
ax--x.--
Al= SO lO xlOO
w
where, AI content of metallic aluminium [% (mass fraction)]
a : amount of aluminium obtained from working curve (g)
w: amout of sample weighed out (g)
In addition, that may be measured by the atomic absorption-spectrometry using di-
nitrogen monoxide-acetylene flame in place of IPC atomic emission spectrometry. For
the details of measuring conditions, see JIS K 0121.
6.1.3 Bromine methanol decomposition chelate titration method
6.1.3.1 Summary

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Metallic aluminium is dissolved by reacting the sample with the mixed solution of
bromine and methanol. After the residue has been filtered to separate, the solution is
made to a definite volume and aluminium is determined by the back titration method
using the free ethylenediaminetetraacetate with zinc.
6.1.3.2 Reagents
Reagents shall be as follows.
a) Hydrochloric acid (1 + 1)
b) Hydrogen peroxide (30 %)
c) Aqueous ammonia (1 + 2)
d) Buffer solution (pH 5.8) Dissolve 100 g of ammonium acetate in 700 ml of water,
make it pH 5.8 by adding glacial acetic acid and afterwards dilute it to 1 L with
water.
e) Saturated solution of sodium fluoride The saturated solution in which sodium
fluoride is dissolved in water.
f) Bromine
g) Reference solution of zinc (0.1 mol!L) Weigh out 6.538 g of zinc from which the
surface oxide is removed [not less than 99.99 % (mass fraction) in: purity] accu-
rately to the nearest 1 mg and transfer it into a conical beaker (1 L). Add 100 ml of
hydrochloric acid (1 + 1) and heat to decompose it. Mter decomposed completely,
cool it to room temperature in running water. Make the amount of solution ap-
proximately 500 ml, make it alkaline by adding aqueous ammonia and afterwards
adjust the solution to pH 5 to pH 6 using acetic acid. Cool it to ordinary tempera~
ture in running water and then wash to transfer it by water into a 1 000-ml volu-
, metric flask and dilute it to the marked line. Stopper it hermetically and preserve.
h) Disodium dihydrogen ethylenediaminetetraacetate solution Dissolve 37.2 g of
disodium dihydrogen ethylenediaminetetraacetate in water and dilute it to 1 L.
Preserve it in a polyethylene bottle (hereafter this solution is referred to as "EDTA
solution").
i) Methanol
j) Xylenol orange solution Dissolve 0.1 g of xylenol orange (XO) in 100 ml of water.
Preserve it at cool and dark place.
6.1.3.3 Pretreatment of sample
In accordance with 6.1.2.4.
6.1.3.4 Amount of sample weighed out
The amount of sample weighed out shall be 2.0 g and measured to the nearest 1 mg.
6.1.3.5 Operation
The operation shall be as follows.

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a) Preparation of sample solution After preparing sample solution according to

6.1.2.6 a) 1) to 6.1.2.6 a) 5), precipitated salt is dissolved with 5 ml of hydrochloric
acid (1 + 1) and a small amount of water. Boil it for 1 min to 2 min, cool it in run-
ning water to room temperature, transfer it by water into a 100-ml volumetric flask
and dilute it to the marked line.
b) Coverage of coexisting ion
1) Take an aliquot of 20 ml of solution prepared in a) into a conical beaker (300 ml)
and add 20 ml of EDTA solution [6.1.3.2 h)]. After the sample has been adjusted to
pH 5 to pH 6 using aqueous ammonia (1 + 2), add 15 ml of buffer solution (pH 5.8)
[6.1.3.2 d)].
2) Mter heated and boiled approximately for 3 min, cool it to room temperature in
running water. Add 4 drops or 5 drops of xylenol orange solution [6.1.3.2 j)], ti-
trate it using reference solution of zinc [6.1.3.2 g)] and stop when the colour of so-
lution changes from yellow to reddish orange.
c) Titration
1) Immediately add 50 ml of saturated solution of sodiurn fluoride [6.1.3.2 e)], heat
again and boil for 3 min and afterwards cool it to room temperature in running
water.
2) Add 2 drops or 3 drops of xylenol orange solution [6.1.3.2 j)] and titrate the free
ethylenediaminetetraacetaate corresponding to the amout of aluminium using
reference solution of zinc [6.1.3.2 g)]. Make the point where the colour of solution
changes from yellow to reddish orange the end point and record the titration
value at that time.
6.1.3.6 Blank test
The blank test shall not be carried out.
6.1.3. 7 Calculation
Obtain the content of metallic aluminium according to the following formula.
500
a x0.002 698x x lOO
Al- SO 20 xlOO
w
where, At: content of metallic aluminium[% (mass fraction)]
a: titration value of reference solution of zinc recorded in
6.1.3.5 c) 2) (ml)
w: amount of sample weighed out (g)
0.002 698: amount of aluminium corresponding to 1 ml of titration
value (g)
6.1.4 Volumetric method by gas dissolved in hydrochloric acid
6.1.4.1 Summary
The sample is dissolved by hydrochloric acid to generate hydrogen gas and the

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amount of hydrogen gas measured by a gas meter is converted to the content of metal-
lic aluminium.
6.1.4.2 Reagents
6.1.4.2.1 Hydrochloric acid (1 + 1)
6.1.4.2.2 Reference powder of metallic aluminium [99. 9 % (mass fraction) in purity
125 f.tm in particle size]
6.1.4.3 Instrument and apparatus
For the instrument and apparatus, the following shall be prepared and assembled as
shown in figure 1.
6.1.4.3.1 Erlenmeyer flask for reaction Two Erlenmeyer flasks (500 ml) of borosili-
cate glass shall be used.
6.1.4.3.2 Gas meter Wet gas meter for experiment (5 mllh to 300 mllh, the maxi-
mum amount read out= 0.005 L).

Funnel with
stopcock

Erlenmeyer flask
for reaction

Sample and hy-

drochloric acid
Gas meter

Figure 1 Apparatus for volumetric method by gas dissolved

in hydrochloric acid

6.1.4.4 Pretreatment of sample

Pulverize the sample by using an appropriate pulverizer such as vibrating mill so as
not to oxidize it to the utmost. Make that pulverized to 0.1 mm or finer the sample for
analysis. Preserve the pulverized sample in a desiccator or a polyethylene bag and the
like.
6.1.4.5 Amount of sample weighed out
The amount of sample weighed out shall be 5.0 g and measured to the nearest 1 mg.
6.1.4.6 Operation
The operation shall be as follows.

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a) Measurement
1) Put the sample and 75 ml of pure water in an Erlenmeyer flask for reaction and
stopper with a rubber stopper.
2) Add IOO ml of hydrochloric acid (I + I) into the Erlenmeyer flask for reaction
(6.1.4.3.1) through a funnel with stopcock and close the stopcock immediately.
3) Dissolve them at ordinary temperature for 10 min.
4) Measure the amount of hydrogen gas by a gas meter (6.1.4.3.2).
b) Calculating experiment for correction factor of gas amount
Weigh out two or more of 1.000 g of powder of metallic aluminium [99.9% (mass
fraction) in purity] to the nearest 0.1 mg, putit i11 an .Erlenmeyer flask for reaction,
operate as similarly as in the operation of 6.1.4.6 a) and measure the amount of
hydrogen gas. Calculate correction factor from this amount of· hydrogen gas ac·
cording to the following formula and use the mean value of measured factors.
F.=l.246
I V,
I

where, Ft : correction factor

V1 : dissolved gas amount of powder of metallic aluminium
(L)
1.246: dissolved gas amount (L) of 1 g metallic aluminium un-
der the standard condition (O oc, 1 atm), which is ob-
tained as follows.
33,62 X P0 =1. 244
26.98 100
where, 33.62 gas amount corresponding to 3/2 H2
molecular weight (L)
26.98 atomic weight of aluminium
Po : purity of powder of metallic alumin-
ium [%(mass fraction)]
6.1.4.7 Calculation
a) Quantitative calculation for correction of gas amout
p-~ xF1 x26,98 xlOO
1
33.62xW
where, P1 : purity of sample according to correction of gas amount [%
(mass fraction)]
V1 : dissolved gas amount of aluminium (L)
F 1 : correction factor obtained in 6.1.4.6 b)
33.62 : gas amount corresponding to 3/2 Hz molecular weight (L)
26.98 : atomic weight of aluminium
W: amount of sample weighed out (g)

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b) Quantitative calculation of sample

Al=P1 x F2
where, AI: content of metallic aluminium [% (mass fraction)]
Pt : content of metallic aluminium of sample according to cor-
rection of gas amount[% (mass fraction)]
Fz: correction factor according to reference quantitative de-
termination method
For obtaining the correction factor according to reference quantitative determi-
nation method, carry out the analysis according to the method of 6.1.2 or 6.1.3 and
calculate the correction factor.
6.1.5 Reaction solution temperature measuring method

_....., 6.1.5.1 Summary

U The sample is thrown into the reaction solution of hydrochloric acid in a Dewar ves-
sel, the metallic aluminium in sample and hydrochloric acid are made to react and the
reaction solution is heated by the reaction heat generated by the reaction. The total
amount of reaction heat is proportional to the reacted amount of aluminium and equal
to the amount of heat accumulated in reaction solution and therefore it follows to be
proportional to the temperature difference of reaction solution temperatures before and
after reaction. Then the content of metallic aluminium is calculated from the tempera-
ture difference of reaction solution temperatures before and-after reaction.
6.1.5.2 Reagents
Reaction solution (hydrochloric acid 1, water 2 : volume ratio) Make the reaction
solution by adding hydrochloric acid 1 to water 2 gradually and preserve it.
6~1.5.3 Pretreatment of sample
Pulverize the sample by using an appropriate pulverizer such as vibrating mill so as
not to oxidize it to the utmost. Make that pulverized to 0.5 mm or finer the sample for
analysis. Preserve the pulverized sample in a desiccator or a polyethylene bag and the
like.
6.1.5.4 Amount of sample weighed out
The amount of sample weighed out shall be 2.0 g and measured to the nearest 1 mg.
6.1.5.5 Operation
The operation shall be as follows.
a) Take an aliquot of 300 ml reaction solution and regulate it within 30 oc ± 1 °C by
the method so as not to volatilize hydrochloric acid as possible.
b) Transfer the reaction solution of a) into a Dewar vessel and measure the tempera·
ture of reaction solution to the nearest 0.1 oc (.Tt oc)
c) Put the sample in the Dewar vessel and stopper with rubber stopper immediately.
d) Measure the temperature of reaction solution every 1 min and measure the highest

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temperature to the nearest 0.1 "C ('F!. oc).

6.1.5.6 Preparation of Dewar vessel working curve
a) Sample for preparation of working curve For the sample for preparation of work-
ing curve, 3 or more samples (in stages) of which the content of metallic aluminium
measured by the method of 6.1.2 or 6.1.3 have been known, shall be prepared.
b) Amount of sample weighed out The amount of sample weighed out shall be 2.0 g
and measured to the nearest 1 mg.
c) Operation The operation shall be carried out according to 6.1.5.5.
d) Calculation of Dewar vessel working curve Based on the measurement results of
3 or more samples measured in c), calculate f and a of conversion factors of Dewar
vessel working curve in the following formula by the method of least square.
20
AI= [(T,-T.1 ) x f +a] x ·
- w
where, At: content of metallic aluminium[% (mass fraction)]
T1 : temperature of reaction solution before reaction (°C)
T2 : the highest temperature of reaction solution after reac·
tion (°C)
w: amount of sample weighed out (g)
f, a: conversion factor of Dewar vessel working curve
6.1.5.7 Calculation
The content of metallic aluminium shall be calculated by the following formula.
20
AI=[(T,-T.,)xf+a] x ·
- w
where, At: content of metallic aluminium [%(mass fraction)]
T1 : temperature of reaction solution before reaction (°C)
T2 : the highest temperature of reaction solution after reac-
tion (°C)
w: amount of sample weighed out (g)
f, a: conversion factor of Dewar vessel working curve
6.2 Quantitative determination method of nitrogen
6.2.1 Quantitative determination method
The quantitative determination method of nitrogen shall be in accordance with the
distillation separation neutralization titration method. This method shall be applied to
the sample of 0.2 % (mass fraction) or over up to and including 7 % (mass fraction) in
nitrogen content.
6.2.2 Summary
The sample is decomposed with hydrochloric acid and hydrogen peroxide. The uncle-
composed residue and solution are transferred to a distillation flask and alkalized with

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sodium hydroxide. Ammonium ion is distilled by steam distillation in a receiver in

which a definite amount of reference solution of sulphuric acid has been previously put.
Ammonium ion is determined by titrating the remaining sulphuric acid by using ref-
erence solution of sodium hydroxide and the content of nitrogen is calculated.
6 ..2.3 Reagents
The reagents shall be as follows.
a) Hydrochloric acid (1 + 1)
b) Reference solution of 0.5 mol/L sulphuric acid After adding 28 ml of sulphuric
acid little by little in approximately 900 ml of water, dilute it to 1 L with water and
preserve it in a polyethylene bottle with stopper. The standardization shall be car-
ried out as follows.
Take an aliquot of 10 ml of this solution in an Erlenmeyer flask (300 ml) and add
approximately 100 ml of water. Titrate it using the reference solution of 0.2 mol/L
sodium hydroxide [6.2.3 d)] and bromothimol blue as an indicator and make the
point where the colour of solution changes to green the end point. Calculate the
factor of the reference solution of 0.5 mol/L sulphuric acid according to the follow-
ing formula.
a X 0.2 X fNaOH
fa,so,
10
where, Jr H,so, ·· factor of reference solution of0.5 mol/L sulphuric acid
I 0 : aliquot am out of reference solution of 0. 5 mol/L sulphuric
acid (ml)
a : titration amount of reference solution of 0.2 mol/L so-
dium hydroxide (ml)
fNaOH : factor of reference solution of0.2 mol/L sodium hydroxide
The reference solution of 0.5 mol/L sulphuric acid standardized for volumetric
analysis on the market may be used.
c) Sodium hydroxide solution (500 giL) Preserve it with stopper in polyethylene bot-
tle.
d) Reference solution of 0.2 mol/L sodium hydroxide Take 16 ml of supernatant so-
lution of sodium hydroxide solution (500 g/L) with elapse of 4 days to 5 days after
preparation in an airtight container (1 L) of polyethylene and make it 1 L by add-
ing water without containing carbonic acid. After mixing preserve it as intercepting
carbon dioxide.
1) Leave to dry amido sulphuric acid (HOS02NH2 reference material for volumetric
analysis) in a desiccator under 2 kPa or lower approximately for 48 h as it is.
Weigh out approximately 4 gof that to the nearest 1 mg, dissolve it in water,
transfer it into a volumetric flask (200 ml) and add water to the marked line.
Take an aliquot of 20 ml of that in an Erlenmeyer flask (300 mD and make it ap-
proximately 100 ml with water. Add 2 drops or 3 drops of bromothimol blue solu-

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tion as an indicator, titrate using this solution of 0.2 mol/L sodium hydroxide and
make it the time when the colour of solution changes to green the end point. Cal-
culate the factor of reference solution of 0.2 mol/L sodium hydroxide according to
the following formula.

where, fNaoH : factor of reference solution of 0.2 mol/L sodium hydroxide

a : amount of amido sulphuric acid weighed out (g)
b : purity of amido sulphuric acid [% (mass fraction)]
c : amount of 0.2 mol/L sodium hydroxide solution required
for titration (ml)
0.019 42 corresponding amount of amido sulphuric acid to 1 ml of
0.2 mol/L sodium hydroxide solution (g)
2) The preparation, standardization and storage shall be in accordance with JA.5.2
r) 2) of JIS K 8001.
The following procedure may be carried out ; take an aliquot of 20 ml solution
prepared so that the standardized reference solution of 0.5 mol/L sulphuric acid
on the market is correctly diluted on one fifth and standardize by titrating using
0.2 mol/L sodium hydroxide solution and bromothimol blue as an indicator. In
such a case, calculate the factor of reference solution of 0.2 mol/L sodium hydrox-
ide according to the following formula.
jH 2SO4 X OJ X 2 X a
fNaOH= b

where, factor of reference solution of 0.2 mol/L sodium hydroxide

Jr H,so, factor of reference solution of 0.5 mol/L sulphuric acid

a : aliquot amount of solution diluted to one fifth of refer-
ence solution. of 0.5 mol/L sulphuric acid (ml)
b : titration amount of reference solution of 0.2 mol/L so·
dium hydroxide (ml)
e) Hydrogen peroxide (1 + 9)
f) Bromothimol blue indicator Heat to dissolve 0.1 g of bromothimol blue in 20 ml of
ethanol and afterwards make it 100 ml by adding water.
6.2.4 Distillation apparatus An example is shown in figure 2. Glassware and the
like shall be washed well before use.

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Unit: mm

60 sphere

Condenser tube

Distillation
flask 300 ml in
capacity

2 OOO·ml
steam-generating
flask 300-ml flask

Figure 2 Example of apparatus for steam distillation

6.2.5 Amount of sample weighed out

..,.....,..__,
The amount of sample weighed out shall be 2.0 g and measured to the nearest 1 mg.
U 6.2.6 Operation
The operation shall be as follows.
a) Preparation of sample solution
1) Weigh out the sample and transfer it into a beaker (500 ml).
2) Cover it with a watch glass and add 30 ml of hydrochloric acid (I + I) little by lit-
tle. If necessary, heat to decompose metallic aluminium and the like. After reac·
tion has settled down, add 10 ml of hydrogen peroxide (I + 9) by dividing into
several times and decompose the soluble portion completely by heating. Cool it to
room temperature in running water.
b) Distillation separation of ammonium ion
1) Assemble a set of distillation apparatus and generate steam for 15 min or longer
by heating the water in a steam-generating flask prior to starting of distillation.

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Moreover pass cooling water through condenser tube beforehand.

2) Wash to transfer the sample solution prepared in a) and undecomposed residue
together into a distillation flask of distillation apparatus using a small amount of
water.
3) Set a distillation flask to distillation apparatus. Next, set an Erlenmeyer flask
(300 ml), in whiGh 10.00 ml of reference solution of 0.5 mol/L sulphuric acid [6.2.3
b)], 10 ml of water and 3 drops or 4 drops of bromothimol blue indicator [6.2.3 f)]
have been added beforehand, so that the outlet of distillate of condenser tube is
immersed in the solution in the flask.
4) Mter 50 ml of sodium hydroxide solution (500 giL) has been added through the
funnel connected to the upper part of distillation flask, wash the funnel part us-
ing a small amount of water. Close the cock of funnel part and introduce the
steam generated in the steam-generating flask into the distillation flask.
5) Continue to distill until the amount of distilled solution reaches approximately
150 ml 3>.
6) When the amount of distilled solution reaches approximately 150 ml, separate the
outlet of distillate of condens~r tube from the distilled solution and open the cock
of upper part of distillation flask.
7) Take off the condenser tube, wash the inside wall of inside tube using a small
amount of water and put it into distilled solution together.
Note 3> When the colour of indicator changes to green in the middle of distilla-
tion, the content of nitrogen is not less than 7% (rnassfraction).
c) Titration Titrate the sulphuric acid remaining in distilled solution with the ref-
erence solution of 0.2 mol/L sodium hydroxide [6.2.3 d)l. Make the point where the
colour of solution changes to green the end point.
6.2.7 Blank test
For blank test, operate according to 6.2.6 a) to 6.2.6 c) without using the sample.
6.2.8 Calculation
Calculate the content of nitrogen in the sample from the titration amount obtained
in 6.2.6 c) and 6.2. 7 according to the following formula.

N= [(fs x0.5 x2 x a-JN x 0.2 x b)-(fs x 0.5 x2 x a-JN x 0.2 x BT)] x 14.01 x IOO
W xi 000
where, N : content of nitrogen[% (mass fraction)]
f, : factor of reference solution of 0.5 mol/L sulphuric acid
a : added amount of reference solution of 0.5 mol/L sul-
phuric acid (ml)
Usually 10.00 ml
/N : factor of reference solution of 0.2 mol/L sodium hydroxide

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b : titration amount of reference solution of 0.2 mol/L so-

dium hydroxide (ml)
BT: titration value of reference solution of 0.2 mol/L sodium
hydroxide in blank test (ml)
w: amount of sample weighed out (g)
14.01: atomic weight of nitrogen
6.3 Quantitative determination method of chloride ion
6.3.1 Classification of quantitative determination methods
The quantitative determination of chloride ion shall be in accordance with either
method of the following.
a) Ion chromatography This method shall be applied to the sample of chloride ion
content of 0.05 % (mass fraction) or over up to and including 3 % (mass fraction).
b) Silver nitrate titration method This method shall be applied to the sample of
chloride ion content of 0.2 % (mass fraction) or over up to ~nd including 3 % (mass
fraction).
6.3.2 Ion chromatography
6.3.2.1 Summary
The sample is boiled approximately for 1 h by adding water and the chloride ion
compound is eluted. After the residue has been filtered to separate, it is made a defi-
nite volume and chloride ion is determined by ion chromatography.
6.3.2.2 Reagents
6.3.2.2.1 Eluent Eiuent is different depending on the type of apparatus and the type
of anion exchanger filled in separation column and therefore confirm the separation of
chloride ion and nitrite ion beforehand by the operation of6.3.2.3 a).
NOTE : ·An example of preparation method of eluent is shown as follows.
a) Example in the case of using suppressor
1) Sodium hydrogen carbonate solution (1. 7 mmol/L)/sodium carbonate solution (1.8
mmoiiL) Take 0.143 g of sodium hydrogen carbonate and 0.286 g of sodium car-
bonate and make them 1 L by dissolving in water.
2) Sodium hydrogen carbonate solution (0.3 mmol/L)/sodium carbonate solution (2. 7
mmol/L) Take 0.025 g of sodium hydrogen carbonate and 0.286 g of sodium car-
bonate and make them 1 L by dissolving in water.
3) Sodium carbonate solution (3 mmol/L) Take 0.318 g of sodium carbonate and
make it 1 L by dissolv-ing in water.
b) Example in case of not using suppressor
1) Potassium gluconate solution (1.3 mmol/L)/sodium tetraborate solution (1.3
mmol/L)/boric acid solution (30 mmol/L)/acetonitrile solution (100 g/L)/glycerin
solution (5 giL) Dissolve 0.31 g of potassium gluconate, 0.50 g sodium tetrabo-

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rate decahydrate, 1.86 g of boric acid, 100 g (128 ml) of acetonitrile and 5 g (4 ml)
of glycerin in water and make it 1 L;
2) Phthalic acid solution (2.5 mmol/L)/2-aDlino~2-hydroxylmethyH,3-propanediol
solution (2.4 mmol/L) Dissolve 0.415 g of phthalic acid and 0.291 g of 2-ammo-2-
hydroxymethyl-1, 3-propanediol [tris (hydroxymethyl) amihomethane] in water
and make it 1 L.
6.3.2.2.2 Regener~t Regenerant is used in the case of using suppressor, however, it
is different depending on the type of apparatus and the type of suppressor. Combine it
with separation column beforehand and confirm the performance of regenerant by car·
rying out the operation of 6.3.2.3 a).
NOTE : Apexample of preparation method ofregenerant is shown as follows.
Sulphuric acid (12.5 mDlol/L) Dissolve 25 ml of sulphuric acid (0.5
mol/L) in water and make it 1 L
6.3.2.2.3 Reference solution of chloride ion (1 mgCl-/inl) Dry sodium chloride (ref-
erence material for volumetric analysis) at 600 oc approximately for 1 h beforehand
and cool it in a desiccator as it is. Take 1.684 g of that to 100 % NaCl and dissolve it in
a small amount of water. Wash to transfer it using water into a 1 OOO·rril volumetric
flask and dilute it to the marked line.
6.3.2.2.4 Reference solution of chloride ion (0.1mgCl-/ml) Take an aliquot of 10 ml
of reference solution of chloride ion: (1 mgC1 ~/ml) ,prepared in 6.3.2.2.3 in a 100-ml
volumetric flask and dilute it to the marked line with water.
6.3.2.3 Ion chromatograph For ion chromatograph, although either the combination
system of separation column with suppressor or the system of single separation column
is permitted, it sh~ll satisfy the following conditions and be able to separate to deter·
mine chloride ion, nitrite ion, bromine ion, nitrate ion, sulphate ion and so on,
The suppressor in whic]l the cation in eluent is converted to hydrogen ion and the
cation exchanging membrane (membrane type and electrodialysis) having sufficient
exchanging capacity to the concentra~ion cation in eluent or the cation exchanger hav-
ing the similar performance is filled. It shall be combined with regenerant for use.
However, in the case of electrodialysis type, the distilled solution from detector (the
solution exhausted from detector) shall be used as regenerant.
a) Separation column Stainless steel made or synthetic resin made 4>in which strong
basic anion exchanger (surface layer covered type, whole porous silica type, etc.) is
filled.
Pour the eluent at a definite flow rate (for example, 1 ml/min to 2 mllmin), inject
a definite amount of reference solution of mixed anions [10 JlgCr, 10 JlgN02-, 10
JlgBr·, 10 JlgNOs", 10 JlgS04 2-)/ml] into ion chromatograph, obtain a chromatogram
and use that capable of separating (resolution: not less than 1.3) respective anions.
It is recommended to confirm periodically the performance of separation column.
The reference solution of mixed anions [(10 JlgCl", 10 JlgNOz", 10 JlgBr·, 10

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'-"
flgNo~-. 10 flg804 2-)/ml] shall be prepared as follows. Take respectively every 5 ml ,
of reference solution of chloride ion (1 mgC1-ml), that of nitrite ion (1 mg N02 ·/ml),
that of bromide ion (1 mgBr-/ml), that of nitrate ion (1 mg N0 3 -/ml) and that of
sulphate ion (1 mg SOF/ml) in a 500-ml volumetric flask and dilute them to the
marked line with water.
Note 4> For instance, that of ethylenetetrafluoride resin made, polyether ketone
made and so on are available.
b) Detector Conductivity detector
c) Recording part Recording part shall be a data processing equipment or a recorder.
6.3.2.4 Amount of sample weighed out
The amount of sample weighed out shall be l.O.g and measured to the nearest 1 mg.
6.3.2.5 Operation
The operation shall be as follows,
a) Preparation of sample solution
1) Weigh out the sample and transfer to put it in a beaker (300 ml).
2) Cover it with a watch glass and add approximately 150 ml of water.
3) Heat it on a hot plate and boil it gently approximately for 1 h. During this period,
if necessary, add water appropriately so as to maintain the amount of solution to
150 ml.
4) Cool it to ordinary temperature in running water.
5) Filter to separate the solution with a filter paper of class 5 C or a membrane filter
of 1 11m in pore size and wash the filter paper (membrane filter) and the residue
with a small amount of water 4 times or 5 times. Receive the filtrate and the
washings together in a volumetric flask (200 ml) and dilute it to the marked line
with water.
6) Take an aliquot of the solution obtained from 5) in a volumetric flask (200 ml) ac·
cording to table 4 depending on the content of chloride ion in the sample and di-
lute it to the marked line with water to make it the sample solution.

Table 4 Amount of aliquot

Content of chloride ion in sample Amount of aliquot
%(mass fraction) ml
0.05 or over to and excl. 0.2 No aliquot
0.2 or over to and excl. 2.0 20
2.0 or over up to and incl. 3.0 10

b) Measurement
1) Set a chromatograph at a definite condition for measurement to make it the state

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capable of operating and pour the eluent (6.3.2.2.1) in separation column and the
like by a definite rate of flow (for instance, 1 ml/min to 2 mllmin). For the appara-
tus requiring suppressor, pour the regenerant (6.3.2.2.2) by a definite rate of flow.
2) Use a syringe applied with cartridge filter of0.2 rm in pore size, pour a definite
amount of sample solution obtained in 6.3.2.5 a) 6) into the sampling part of ap~
paratus.
3) Operate the sample introduction part Of apparatus, pour the sample solution (50
111 to 200 rl of a definite amount) in sampling part into column part and record a
chromatogram.
4) Read out an indicated value on the peak corresponding. to chloride ion on the
chromatogram.
In addition, the indicated value shall be the peak height or peak area.
6.3.2.6 Blank test
Add 150 ml of water in a beaker (300 ml) and cover it with watch cover and read out
the indicated values of blank test by operating according to 6.3.2.5 a) 3) to 6) and b).
However, the amount of aliquot and the amount to be poured shall be the same as the
sample solution.
6.3.2. 7 Preparation of working curve
Take 0 mg to 2 mg as chloride ion in reference solution of chloride ion (6.3.2.2.3 and
6.3.2.2.4) step by step in several volumetric flasks (200 mD, dilute it to the marked line
with water. Carry out to measure on this solution according to 6.3.2.5 b), prepare the
relation line of indicated value to chloride ion amount and translate it in parallel so as
to pass through the origin and make it the working curve.
6.3.2.8 Calculation
Calculate the content of chloride ion in the sample from the indicated values ob-
tained in 6.3.2.5 and 6.3.2.6 and the working curve in 6.3.2. 7 according to the following
formula.

cz- a-b xlOO

Wx-c-
200
where, a : amount of chloride ion in 200 ml of sample solution ob-
tained from working curve (g)
b blank test value (g)
c : amount of aliquot (ml)
(In the case of not taking of an aliquot, c shall be 200.)
W : amount of sample weighed out (g)
6.3.3 Silver nitrate titration method
6.3.3.1 Summary
The sample is boiled with water and chloride ion is eluted, that is alkalized with so-

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~ium hydroxide and reductive material is oxidized by adding hydrogen peroxide. That
IS neutralized with nitric acid and the deposited hydroxide and the like are filtered to
separate. The filtrate is titrated by silver nitrate with sodium fluorescein as an indica- .
tor and chloride ion is determined.
6.3.3.2 Reagents
6.3.3.2.1 Potassium dichromate solution
6.3.3.2.2 Sulphuric acid
6.3.3.2.3 Nitric acid (1 + 1)
6.3.3.2.4 Hydroxylammonium sulfate
6.3.3.2.5 Hydroxylammonium chloride
6.3.3.2.6 Sodium hydroxide solution (20 g/100 ml)
6.3.3.2. 7 Hydrogen peroxide (1 + 9)
6.3.3.2.8 Dextrin solution Dissolve 2 g of dextrin hydrate in water and dilute it to
100 ml. Prepare it at every time of use.
6.3.3.2.9 Sodium fluorescein solution Dissolve 0.2 g of uranin (sodium fluorescein)
in water and dilute to 100 ml.
6.3.3.2.10 Reference solution of 40 mmolJL silver nitrate Dissolve 6.8 g of silver ni·
trate in water, dilute it to 1 L and preserve in a coloured glass bottle. Standardization
shall be carried out according to the following.
Heat sodium chloride(reference material for volumetric analysis of NaCl) at 600 oc
for approximately 1 h beforehand and cool it in a desiccator. Take 0.467 5 g of that, di-
lute it in a small amount of water, ·wash to transfer it in a volumetric flask (200 mD
and dilute it to the marked line. Take an aliquot of 20 ml of this solution in a beaker
and make the .amount of solution approximately 50 ml with water. Add 5 ml dextrin
solution and 1 drop or 2 drops of sodium fluorescein solution in it and titrate it with 40
mmol/L silver nitrate solution as stirring to mix it gently. Make the time when yellow-
ish green fluorescence turns to slightly red the end point. Calculate the factor of refer·
ence solution of 40 mmol/L silver nitrate according to the following formula.
b 20 1
/AgNOJ =a X 100 X 200 XC X 0.002 337 7

where, factor of reference solution of 40 mmol/L silver nitrate

a : amount of sodium chloride _weighed out (g)
b purity of sodium chloride [% (mass fraction)]
c : amount of titration with reference solution of 40. mmol/L
0.002 337 7 : corresponding amount of sodium chloride to 1 ml of 40
mmol/L silver nitrate solution (g)
6.3.3.2.11 pH test paper That colour changes from red to purple via yellow and
green in colour within the range of pH 2 to pH 10 and that shows green around pH 7.

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6.3.3.3 Amount of sample weighed out

The sample shall be measured to the nearest 1 mg according to table 5 depending on
the content of chloride ion.

Table 5 Amount of sample weighed out

Content of chloride ion in sample Amount of sample weighed out
%(mass fraction) g
0.2 or over to and excl. 1.0 2.0
1.0 or over up to and incl. 3.0 1.0

6.3.3.4 Operation
The operation shall be as follows.
a) Preparation of sample solution
1) Weigh out the sample and transfer it into a beaker (300 ml).
2) Cover it with a watch glass and add 80 ml of water. After heating and boiling the
solution gently approximately for 1 h, cool it to room temperature in running wa-
ter.
3) Filter to separate it using class 5 B of filter paper and wash the filter paper and
the residue with a small amount of water 4 times or 5 times. Put the filtrate and
the washings together and receive them in a beaker (300 ml).
4) Add 1 ml of sodium hydroxide solution (20 g/100 ml) and heat until it starts to
boil. Add 5 ml hydrogen peroxide (1 + 9) little by little and then boil it for ap-
proximately 10 min.
5) After cooling it to room temperature in running water, add nitric acid (1 + 1) and
neutralize it to around pH 7. Confirm with a pH test paper that the pH of the so-
lution is around 7.
6) . When the precipitate such as hydroxide is found, filter the solution using class 5 A
filter paper and wash the filter paper and the precipitate with a small amount of
water several times. Put the filtrate and the washings together and receive it in a
beaker. When the amount of solution exceeds 100 ml, heat to evaporate it and
make·it approximately 100 ml.
In addition, it is permitted that the suction filtration is carried out using the
membrane filter of 0.4 J.Lm to 1 Jlm in pore size in place of filter paper.
b) Titration of chloride ion
1) Add 5 ml of dextrin solution (6.3.3.2.8) and 2 drops or 3 drops of sodium fluo-
rescein indicator (6.3.3.2.9) in the sample solution obtained in 6.3.3.4 a) 6).
2) Titrate it with reference solution of 40 mmol/L silver nitrate (6.3.3.2.10) as stir-
ring to mix the solution gently. Make the time when yellowish green fluorescence
of solution turns to slightly red the end point.

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In addition, the titration operation shall be in accordance with either of the fol- .
lowing.

2.1) When the content of .chloride ion in solution is under 1 % (mass fraction), carry
out the titration using microburette (10 ml).
2.2) When the content of chloride ion is less than 10 mg at titration, the judgement of
end point requires a high level of skill. When it is unable to judge the end point
by all means, it is permitted that titration is carried out using 1 ml of potassium
dichromate solution (5 g/100 ml) in place of fluorescein indicator (the dextrin
solution of protective colloid is not added). In such a case, the point, where the
colour of solution changes from yellow to slight reddish brown, shall be the end
point.

Furthermore, the solution after completion of this titration contains hexava·

lent chrome ion and therefore the chrome shall be reduced to trivalent by add-
ing a small amount of sulphuric acid and hydroxylammonium sulphate or hy-
droxylammonium chloride and thus waste treatment shall be carried out.
6.3.3.5 Blank test
Take 80 ml of water in a beaker, operate as similarly as in the case of sample on and
after the operations of boiling of 6.3.3.4 a) 2) and obtain the titration value of blank
test.
6.3.3.6 Calculation
Calculate the content of chloride ion in sample according to the following formula.
/AgNO X (a-b) X 1.418
CI- 3
xlOO
WxiOOO
where, Cl content of chloride ion[% (mass fraction)]
/AgNo
3
: factor of reference solution of 40 mmol/L silver nitrate

~;·--·\
a : titration value of sample (ml)
\._,) b titration value of blank test (ml)
1.418 amount of chloride ion corresponding to 1 ml of reference
solution of 40 mmol!L silver nitrate (mg)
6.4 Quantitative determination method of total silicon
6.4.1 Classification of quantitative determination method
The quantitative determination method of total silicon shall be in accordance with
either of the following.
a) Molybdo silicic acid absorption spectrophotometry This method shall be applied
to the sample of 0.5 % (mass fraction) or over up to and including 20 % (mass frac·
tion) in the content of total silicon (expressed as Si02).
b) Silicon dioxide gravimetric method This method shall be applied to the sample of
0.5 % (mass fraction) or over up to and including 20 % (mass fraction) in the con·
tent of total silicon (expressed as SiOz).

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6.4.2 Molybdo silicic acid absorption spectrophotometry

6.4.2.1 Summary
After the sample has been decomposed with the mixed acid of hydrochloric acid and
nitric acid, the undecomposed residue is filtered to separate and ashed by igniting in a
platinum crucible. Mter the residue has been molten with sodium carbonate and boric
acid and dissolved in water, it is put with the filtrate together. Take an aliquot of a
portion and the solution is adjusted to pH 0.8. Molybdo silicic acid is produced by add-
ing ammonium molybdate and the absorbance is measured using photometer. The
analytical results are expressed as Si02.
6.4.2.2 Reagents
6.4.2.2.1 Mixed acid (hydrochloric acid 1, nitric acid 1, water 2: volume ratio)
6.4.2.2.2 Melting mixture agent (boric acid 3, sodium carbonate 5 : mass ratio)
6.4.2.2.3 Sodium nitrite
6.4.2.2.4 Ammonium molybdate solution Mter dissolving 10 g of hexaammonium
heptamolybdate tetrahydrate in water and make it 100 mi. Preserve it in a polyethyl-
ene bottle.
6.4.2.2.5 Reference solution of silicon (500 Jlglml) Reference solution of silicon shall
be as follows.
a) Weigh out 0.535 0 g of silicon dioxide [not less than 99.95% (mass fraction)], which
has been ignited at 1 000 °C in temperature beforehand and left in a desiccator to
room temperature as it is, in a platinum crucible (No. 30 or No. 40), mix 4.0 g of
sodium carbonate (anhydride) and melt it by heating.
b) Mter cooled, immerse the platinum crucible in a beaker (300 mD of ethylene tetra-
fluoride made containing 100 ml warm water, dissolve the molten matters, wash
the platinum crucible with water and take out the content. Mter cooled to room
temperature, filter the solution using the filter paper (class 5 B) containing a small
amount of filter paper pulp and wash the filter paper with sodium carbonate solu-
tion (10 giL). Wash to transfer the filter paper and the washings in a volumetric
flask (500 ml) with water and dilute it to the marked line. Preserve it in a polyeth-
ylene bottle.
c) Take an aliquot of 50 ml of this solution in a beaker (500 ml) contained with 30 ml
of perchloric acid, 5 ml of nitric acid (1 + 1) and 20 ml of water beforehand, carry
out the operation according to the generation operation of white fumes of perchloric
acid [6.4.3.4 a) 3)] to 6.4.3.4 c) 4) and obtain the concentration of silica. The factor
to convert mass of silicon dioxide to mass of silicon shall be 0.467 4.
6.4.2.3 Amount of sample weighed out
The amount of sample weighed out shall be 1.0 g and measured to the nearest 1 mg.
6.4.2.4 Operation The operation shall be as follows.
a) Preparation of sample solution

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I) Weigh out the sample and transfer it into a beaker (500 ml).
2) Add 30 rill of mixed acid little by little, cover it with a watch glass and decompose
metallic aluminium and the like by heating. Mter the decomposition reaction has
been completed, cool it to room temperature in running water without heating
beyond necessary temperature.
3) Filter to separate the solution using filter paper class 5 Band wash the filter pa-
per and the undecomposed residue with a small amount of water several times.
Receive the filtrate and the washings in a beaker (500 ml) and preserve it.
4) Transfer the undecomposed residue and the filter paper into a platinum crucible
(No. 30 or No. 40), dry the filter paper by heating and afterwards ash them by ig-
niting. Continue to ignite them until metallic silicon and the like are completely
oxidized and the residue becomes almost white.
5) Mter cooled, add 6 g of melting mixture in the crucil:lle and mix it with platinum
stick. Add 2 g of melting mixture agent so as to cover the mixture.
6) Mter removing moisture completely by heating gently, melt the residue by heat-
ing strongly step by step. Continue to ighite it for approximately 20 min from the
time when the melting mixture agent has molten down and becomes the st~te
without adhered matters on the inside wall of crucible.
7) Mter stopping heating and cooling it .as it is, transfer the crucible and the ll10lten
matters together in a beaker (300 ml) of ethylenetetrafluoride, add approximately
100 m1 of water and dissolve the molten matters by heating.
8) Mter the molten matters have been dissolved and the adhered matters have dis-
+
appeared, add 30 ml of nitric acid (1 1) and dissolve the precipitate such as hy-
droxide by heating. Mter the crucible has been washed with water and the con-
tent has been taken out, cool it to room temperature in running water. Wash to
transfer this solution, the filtrate and the washings preserved in 6.4.2.4 a) ·3) into
a volumetric flask (500 ml) with water and put them together. Dilute it to the

0 marked line with water.

In addition, when manganese oxide is found, add several drdps of sodium ni-
trite solution (1 g/100 mD.
b) Coloration
1) Take an aliquot of the sample solution obtained in 6.4.2.4 a) 8) in a beaker ac·
cording to table 6, depending on the content of total silicon.
2} Make the amount of solution 150 ml to 200 ml with water and adjust the solution
to pH 0.7 to pH 0.9 with nitric acid (1 +I) using a pH meter.
3) Transfer to wash the solution into a volumetric flask (250 ml) with a small
amount of water and regulate the temperature of solution to 20 oc to 30 oc. Add
15 ml of ammonium molybdate solution (6.4.2.2.4), dilute it to the marked line
with water, mix it sufficiently and leave it approximately for 10 min as it is.

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Table 6 Amount of aliquot

Content of total silicon in sample (expressed as Si02) Amount of aliquot
% (massfraction) ml
0.5 or over to and excl. 2 100
2 br ovier to and. e:kcl. fd 50
10 or over up to and incl. 20 25

c) Measurement of absorbance Take a portion of the coloration solution obtained in

6.4.2.4 b) S) in an absorption cell of photometer and measure the absorbance in the
neighbourhood of 420 nm in wavelength .by making water as reference solution
within 15 min from the t~me of aqding ammonium molybdate solution. When the
sample solution obtained in 6.4.2.4 a) 8) is coloured, take an aliquot of the solution
in a beaker by the same amount as that for coloration and use the solution, ob-
tained by operating as similarly as in the sample without adding ammonium mo·
lybdate solution, as the reference solution.
6.4.2.5 Blank test
Use the same amount of reagents as in the case of sample, operate similarly to ob-
tain the absorbance.
6.4.2.6 Preparation of working curve
Take 8' g of melting mixture agent in several beakers of ethylene tetrafluoride, add
approximately 200 m:l of water and heat to dissolve it. Mter adding reference solution
of silicon (6.4.2.2.5) of 0 nig to 25 mg as silicon step by step, heat the solution and boil
it for 3 min to 4 min. Mter cooled to room temperature, make it acidic solution by add-
ing 30 ml of nitric acid (1 + 1), wash to transfer it in a volumetric flask (500 ml) with
water and dilute it to the marked line. Take an aliquot of 100 ml of this solution in a
beaker. Next, operate according to the procedures of 6.4.2.4 b) 2), 3) and 6.4.2.4 c) and
measure the absorl:lance. Prepare .the relation line of the obtained absorbance to the
amount of silicon contained in 50 ml solution taken as an aliquot, translate the relation
line in parallel as passing through the origin and make it the working curve.
6.4.2. 7 Calculation
Obtain the amount of silicon from the absorbance obtained by subtracting the ab·
sorbance obtained in 6.4,2.5 from the absorbance obtained in 6.4.2.4 c) and the working
curve prepared in 6.4.2.6 and calculate the content of total silicon in sample (expressed
as Si02) according to the following f<)rmula.
SiO ax 2.139 3 x 100
2
Wxb/500
where, Si02 content of total silicon in sample (marked with Si02) [%
:

(mass fraction)]
a : detected amount of silicon obtained from working curve
(g)
b : amount of aliquot (ml)
w: amount of sample weighed out (g)

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G 2402:2009

2.139 3 : conversion factor from Si to Si02

6.4.3 Silicon dioxide gravimetric method
6.4.3.1 Summary

After the sample has been decomposed with the mixed acid of hydrochloric acid and
nitric acid, the undecomposed residue is filtered to separate and ashed by igniting in a
platinum crucible. The residue is dissolved with sodium carbonate and boric acid and
after dissolved in water, it is put together with filtrate. Silicon is made to insoluble
silicon dioxide by adding perchloric acid, heating it and generating white fumes. After
soluble salts have been dissolved with warm"water, the precipitate is filtered to sepa·
rate and aft.er igniting it, the mass is measured. Next, sulphuric acid and hydrofluoric
acid are added, silicon dioxide is volatiled as silicon fluoride by heating and the mass is
measured after ignited. The content of total silicon (expressed as Si02) is obtained by
regarding the difference of mass as silicon dioxide.
Q 6.4.3.2 Reagents
6.4.3.2.1 Hydrochloric acid (1 + 100)
6.4.3.2.2 Sulphuric acid (1 + 1)
6.4.3.2.3 Hydrofluoric acid (40 %)
6.4.3.2.4 Perchloric acid
6.4.3.2.5 Mixed acid (hydrochloric acid 1, nitric acid 1, water 2 : volume :ratio)
6.4.3.2.6 Melting mixture agent (boric acid 3, anhydrous sodium carbonate 5 :mass
ratio)
6.4.3.3 Amount of sample weighed out
The amount of sample weighed out shall be 1.0 g and measured to the nearest 1 mg.
6.4.3.4 Operation
The operation shall,be as follows.
0 a) Decomposition of sample and dehydration treatment of silicon dioxide
1) Carry out according to 6.4.2.4 a) 1) to 6.4.2.4 a) 7).
2) When the molten matters are dissolved and the adhered matters disappear in
crucible, add 30 ml of nitric acid (1 + 1) and dissolve the precipitate such as hy·
droxide by heating. After the crucible has been washed by water and the content
has been taken out, wash to transfer the solution in the beaker (pQO II.J.l) contained
with the filtrate preserved in 6.4.2.4 a) 3) with a small amount of water and put
them together.
When manganese oxide is found, add several drops of sodium nitrite solution
(1 g/100 mD.
3) Add 50 ml of perchloric acid and generate the white fumes of perchloric acid by
heating. Cover it with a watch glass and make such condition that the fumes of
perchloric acid flow downwards along the inside wall of beaker by igniting on hot

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G 2402: 2009

plate and furthermore continue to heat it for 15 min to 20 min from such time.
After cooling as it is, take off the watch glass after washing the lower surface with
a small amount of water.
b) Filtrate and washing
1) Add warm water in the beaker (500 ml) containing of the salts obtained in 6.4.3.4
a) 3) to make the amount of solution approximately 300 ml and dissolve the salts
by stirring with a glass stick.
2) After the precipitate has settled by placing quietly, filter to separate the precipi-
tate quickly using the filter paper of class 5 B, scrape down the silicon dioxide
adhered to the inside wall of beaker using a. glass stick with rubber tube and
wash to transfer it on a filter paper with a small amount of warm hydrQGhloric
acid (1 + 100).
3) Wash the filter paper and the precipitate sufficiently with warm hydrochloric acid
(1 + 100) 5 times to 6 times and next with warm water until chloride ion has var
nished in the washings. Take a small amount of washings and add 4 drops to 5
drops of silver nitrate solution (1 g/100 mD. It is acceptable that the filtrate has
not become cloudy.
c) Weighing
1) Transfer to put the precipitate of silicon dioxide obtained in 6.4.3.4 b) 3) and the
filter paper together in a platinum crucible (No. 30), dry the filter paper by heat-
ing and afterwards ash them by igniting.
2) After it has been ignited at 1 100 °C to 1 150 oc approximately for 1 hand then
cooled in a desiccator as it is, weigh the mass. Repeat these operations until the
mass becomes constant within 0.3 mg.
3) Add 0.5 ml of sulphuric acid (1 + 1) and approximately 5 ml of hydrofluoric acid in
the platinum crucible, volatile silicon dioxide by heating gently and continue to
heat it until the white fumes of sulphuric acid has not been generated.
4) Mter it has been ignited at 1 100 oc to. 1 150 °G for approximately 30 min and
then cooled to room temperature in a desiccator as it is, weigh the mass. Repeat
these operations until the mass becomes constant within 0.3 mg.
6.4.3.5 Blank test
The blank test shall not be carried out.
6.4.3.6 Calculation
Calculate the content of total silicon (expressed as SiOz) in sample according to the
following formula.
SiO _m 1-m 2 xlOO
2 w
where, Si02 : content of total silicon in sample (expressed as SiOJ
[%(mass fraction)]

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 29.
G 2402:2009

mass obtained in 6.4.3.4 c) 2) (g)

mass obtained in 6.4.3.4 c) 4) (g)
W: amount of sample weighed out (g)
6.5 Quantitative determination method of aluminium oxide
The quantitative determination method of aluminium oxide shall be agreed between
the purchaser and the manufacturer.
6.6 Quantitative determination method of carbon
The quantitative determination method of carbon shall be agreed between the pur-
chaser and the manufacturer.
6. 7 Determination method of water
The determination method of water shall be in accordance with JIS G 2403.
6.8 Sampling and preparation method
The sampling and preparation method of the sample use for the analysis of compo-
nent and the measurement of_ water shall be in accordance with JIS G 2403.

7 Inspection
Aluminium dross shall be tested according to clause 6 and satisfy the requirements
in clause 5.

8 Marking
The following items shall be marked by an appropriate method on either package or
invoice of aluminium dross,
a) Number of this Standard
b) Classification and symbol.
c) Serial number
d) Name of the manufacturer or its abbreviation

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Errata for JIS (English edition) are printed in Standardization Journal, published monthly by
the Japanese Standards Association, and also provided to subscribers of JIS (English edition) in
11-fonth.l.v Information.
Errata will b~ provided upon request, please contact:
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2012-05-17 Printed by JSA