JAPANESE

INDUSTRIAL
STANDARD
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Translated and Published by

Japanese Standards Association

JIS K 0108 :2010

(JSAC/JSA)
Methods for determination of
hydrogen sulfide in flue gas

ICS 13.040.40 ; 71.040.40

Reference number: JIS K 0108: 2010 (E)

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K 0108 : 2010

Date of Establishment: 1967-09-01

Date of Revision: 2010-05-20
Date of Public Notice in Official Gazette: 2010-05-20
Investigated by: Japanese Industrial Standards Committee
Standards Board
Technical Committee on Environment and
Recycling Policy

JIS K 0108:2010, First English edition published in 2011-11

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 2011
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
NH/AT

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Contents

Page

1 Scope················································· ...................................................... ···················1

2 Normative references ...................................................... ········································1
3 Terms and definitions ............................................................................................. 2

4 General matters ...................................................... ·················································2

5 Types and summaries of analysis methods ...................................................... ···3
6 Method of sampling gas ...................................................... ····································4
6.1 Sampling position ...................................................... ··············································4
6.2 Sampling gas apparatus and instrument ...................................................... ······4
6.3 Constitution of gas sampling apparatus and sampling procedure ···················4
7 Sample gas sampling procedure and preparation of sample solutions
for analysis ............................................................................................................. 14
7.1 In the case of gas chromatography ...................................................... ···············14
7.2 In the case of methylene blue absorptiometry and ion selective
electrode method···································································································· 14
8 Gas chromatograph ...................................................... ·········································14
8.1 Summary··············································· ...................................................... ············14
8.2 Reagents and gas ................................................................................................... 14
8.3 Apparatus and instruments ................................................................................. 15
8.4 Introduction of sample gas for analysis into gas chromatography ················17
8.5 Operation conditions of gas chromatograph ...................................................... 17
8.6 Determination procedure ...................................................... ································19
8.7 Preparation of working curve··· ........................................................................... 19
8.8 Calculation of hydrogen sulfide concentration ··················································19
9 Methylene blue absorptiometry ...................................................... ·····················20
9.1 Reagents and preparation of reagent solutions ················································20
9.2 Apparatus and instrument ...................................................... ·····························23
9.3 Determination procedure ...................................................... ································23
9.4 Preparation of working curve ...................................................... ························23
9.5 Calculation of hydrogen sulfide concentration .................................................. 23
10 Ion selective electrode method ...................................................... ·······················24
10.1 Reagents and preparation of reagent solutions ················································24
10.2 Apparatus and instruments ...................................................... ···························25
10.3 Determination procedure ...................................................... ································25
lOA Preparation of working curve ...................................................... ························26
10.5 Calculation of hydrogen sulfide concentration .................................................. 26

(i)
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11 Record of analysis results ·...................... · .......................... ·.......................... ·······28

Annex A (informative) Silver nitrate potentiometric titration ................................ 29
Annex B (informative) Sulfur dioxide conversion ultraviolet ray fluorescent
method ...................................................... ·······························34
Annex C (informative) Detecting tube method .......................................................... 38

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(ii)

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Foreword
This translation has been made based on the original Japanese Industrial Standard
revised by the Minister of Economy, Trade and Industry through deliberations at
the Japanese Industrial Standards Committee as the result of proposal for revision
of Japanese Industrial Standard submitted by The Japan Society For Analytical
Chemistry (JSAC)/Japanese Standards Association (JSA) with the draft being attached,
based on the provision of Article 12 Clause 1 of the Industrial Standardization Law
applicable to the case of revision by the provision of Article 14.
Consequently JIS K 0108: 1983 is 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, utility model
right or application for registration of utility model after opening to the public which
have technical properties. 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, utility model right or application for registration of utility
model after opening to the public which have the said technical properties.
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(iii)

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JAPANESE INDUSTRIAL STANDARD JIS K 0108 : 2010

Methods for determination of hydrogen

sulfide in flue gas

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1 Scope
This Japanese Industrial Standard specifies the methods for determination of
hydrogen sulfide in flue gas which is generated by combustion or chemical reaction or
the like, and exhausted into flue, chimney, duct, etc.
Warning: Persons performing analysis based on this Standard should be famil-
iar with normal laboratory practice. This Standard does not purport
to address all of the safety problems, if any, associated with its use.
It is the responsibility of the user to establish appropriate safety and
health practices.

2 Norma ti ve references
The following standards contain provisions which, through reference in this text,
constitute provisions of this Standard. For standards with the year indication, only
the editions of the indicated year shall be applied and the revisions (including amend-
ments) made thereafter shall not be applied. For those without the indication of the
year, the most recent edition (including amendments) shall be applied.
JIS K 0050: 2005 General rules for chemical analysis
JIS K 0095 Methods for sampling of flue gas
JIS K 0114 General rules for gas chromatographic analysis
JIS K 0115 General rules for molecular absorptiometric analysis
JIS K 0122 General rules for ion selective electrode method
JIS K 0211 Technical terms for analytical chemistry (General part)
JIS K 0212 Technical terms for analytical chemistry (optical part)
JIS K 0213 Technical terms for analytical chemistry (Electrochemistry part)
JIS K 0214 Technical terms for analytical chemistry (Chromatography part)
JIS K 0215 Technical terms for analytical chemistry (Analytical instrument part)
JIS K 0512 Hydrogen
JIS K 0557 Water used for industrial water and wastewater analysis
JIS K 1101 Oxygen
JIS K 1105 Argon
JIS K 1107 Nitrogen
JIS K 8005 Reference materials for volumetric analysis
JIS K 8107 Disodium dihydrogen ethylenediamine tetraacetate dihydrate (Reagent)
JIS K 8142 Iron (III) chloride hexahydrate (Reagent)
JIS K 8180 Hydrochloric acid (Reagent)

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JIS K 8193 N,N-Dimethyl-para-phenylenediammonium dichloride (Reagent)

JIS K 8295 Glycerin (Reagent)
JIS K 8576 Sodium hydroxide (Reagent)
JIS K 8625 Sodium carbonate (Reagent)
JIS K 8637 Sodium thiosulfate pentahydrate (Reagent)
JIS K 8659 Starch, soluble (Reagent)
JIS K 8913 Potassium iodide (Reagent)
JIS K 8920 Iodine (Reagent)
JIS K 8949 Sodium sulfide nonahydrate (Reagent)
JIS K 8951 Sulfuric acid (Reagent)
JIS K 8953 Zinc sulfate heptahydrate (Reagent)
JIS K 8960 Ammonium sulfate (Reagent)
JIS K 9005 Phosphoric acid (Reagent)
JIS K 9502 L(+)-Ascorbic acid (Reagent)
JIS Z 8401 Guide to the rounding of numbers
JIS Z 8808 Methods of measuring dust concentration in fZue gas

3 Terms and definitions

For the purpose of this Standard, the terms and definitions given in JIS K 0211,
JIS K 0212, JIS K 0213, JIS K 0214 and JIS K 0215 apply.

4 General matters
The general matters shall be as follows.
a) General matters of chemical analysis shall be in accordance with JIS K 0050: 2005.
b) General matters of flue gas sampling shall be in accordance with JIS K 0095.
c) General matters of gas chromatograph shall be in accordance with JIS K 0114.
d) General matters of absorptiometry shall be in accordance with JIS K 0115.
e) General matters of ion selective electrode method shall be in accordance with JIS
K 0122.
D Water to be used in analysis shall be of A3 or A4 among the classification and
qualities as specified in clause 4 of JIS K 0557 or Annex 1 of JIS K 0050: 2005,
or any water equivalent to these.
g) Reagents to be used shall be of the highest grade or of an appropriate quality as
specified in a relevant Japanese Industrial Standard, if applicable. If the reagent
does not have a relevant specification in Japanese Industrial Standard, that of a
quality adequate for the analysis shall be used.
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h) Apparatus and instrument to be used shall be provided with the specified func-
tions.

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i) When disposing flue gas, or absorbing solution of the flue gas used for the analy-
sis of hydrogen sulfide, it shall be done with utmost care.

5 Types and summaries of analysis methods

The types and summaries of analysis methods are as shown in table 1.
Table 1 Type and summary of analysis methods a)
Analysis Summary of analysis method
method
Outline Sampling Determina tion Sampling of sample gas
range b)
Gas chroma- Flue gas is introduced The syringe In the case of (Gas sampler)
tography into gas chromato- method, gas sample introduc- In the case of analyzing
(see clause 8) graph and separated sampling bag tion amount immediately after sampling:
by packed column or method, gas 100 f-tl: a gas sampling syringe made
capillary column, then collecting bottle Thermal conduc- of hard glass, 1 ml to 5 ml in
hydrogen sulfide is method or gas tivity detector: capacity, or a gas sample
determined from the collecting can 200 vol ppm to introducing apparatus
chromatogram method. 20 vol % attached to the apparatus,
obtained by the Sampling etc. is used.
detector. Flame photo-
amount of metric detector: In the case of transferring to
sample gas: 0.2 vol ppm to analysis room after sampling:
about 1 ml to 50 vol ppm a gas sampling bag 1 L or
1L over in capacity or a gas
Atomic emission
collecting bottle 1 L or over
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detector:
in capacity is used.
0.05 vol ppm to
50 vol ppm
Methylene After flue gas is Absorbing 1. 7 vol ppm to (Absorbing bottle of sample
blue absorp- allowed to be absorbed bottle method 6.9 vol ppm gas)
tiometry in the absorbing solu- Absorbing (volume concen- In the case of sampling
(see clause 9) tion, the absorbance of solutions: tration) amount of sample gas 1 L or
the methylene blue in accordance over: two absorbing bottles as
generated by N,N- with 6.3.2.3 a) shown in figure 4 are used.
dimethyl-p-phenylene-
diammonium and iron Sampling In the case of sampling
(III) is measured and amount of amount of sample gas less
hydrogen sulfide is sample gas: than 1 L: one absorbing
determined. 1 L to 20 L bottle as shown in figure 6 is
used.
Ion selective After flue gas is Absorbing 0.01 vol ppm to (Gas sampler)
electrode allowed to be absorbed bottle method 1000 vol ppm In the case of sampling
method in the absorbing solu- Absorbing amount of sample gas 1 L or
(see clause 10) tion, potential differ- solution: over: two absorbing bottles as
ence is measured by in accordance shown in figure 4 are used.
means of an ion selec- with 6.3.2.3 b)
tive electrode and In the case of sampling
hydrogen sulfide is Sampling amount of sample gas less
determined. amount of than 1 L: one absorbing
sample gas: bottle as shown in figure 6 is
1 L to 20 L used.
Notes a) In addition to the methods in this table, there are the silver nitrate potentiometry (Annex A),
sulfuric dioxide conversion ultraviolet ray fluorescent method (Annex B) and detecting tube
method (Annex C).
b)
For the purpose of knowing the approximate concentration of hydrogen sulfide, a detecting
tube type hydrogen sulfide measuring apparatus (Length of stain type) or detecting tube type
and hydrogen sulfide densitometer may be used.

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6 Method of sampling gas

6.1 Sampling position

The sampling position of sample gas shall be as follows.
a) For the point to sample representative gas, select a position with minimum ingress
of air or sediment of dust, where the flow of flue gas is generally uniformly recti-
fied, and avoid any curves in the flow path or positions where sectional shape sud-
denly changes.
b) Select a place where the sampling work can be safely and easily performed and if
necessary, provide a scaffold of appropriate area and height around the sampling
position.
c) At the sampling position, provide a sampling opening into which a gas sampling
tube can be inserted approximately at right angles to the flow direction of the flue
gas.
d) The sampling opening shall be of a material and construction such that it has
enough strength to hold the inserted gas sampling tube and thermal resistance
to endure heat up to about 120°C.
e) The sampling opening shall be provided with a cover so that whenever the gas
sampling tube is not being inserted, incidents such as spouting of flue gas (posi-
tive pressure) or ingress of air (negative pressure) can be avoided. Further, when
opening the cover of the sampling opening, sufficient care shall be taken for the
burn and the danger due to spouting of flue gas.
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6.2 Sampling gas apparatus and instrument

The sampling apparatus and instrument for sample gas shall be provided with the
following function and condition.
a) The tube used for the gas sampling tube and tubings connecting between instru-
ments shall be made of a material which is resistant to corrosion by hydrogen
sulfide in flue gas, e.g. borosilicate tube, silica glass tube or fluoroethylene resin
tube.
b) In order to prevent dust from mixing into sample gas, plug the end of the sam-
pling tube or other suitable place with filter medium (e.g. silica wool, sintered glass
filter, etc.)
c) Tubings shall be as short as possible in order to avoid condensation of moisture,
and shall be heated to 120°C. However, where there is no possibility of conden-
sation of moisture, heating may be omitted.
d) The washing bottle (E) as shown in figure 1 shall be used.
e) Set up the gas sampling apparatus and instruments at a site free from direct
sunlight.

6.3 Constitution of gas sampling apparatus and sampling procedure

The constitution of gas sampling apparatus and sampling procedure for respective
analysis methods shall be as follows.

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6.3.1 Gas chromatography

6.3.1.1 Gas sampling apparatus and instruments

An example of the gas sampling apparatus to be used in gas chromatography is
shown in figure 1.

A: Gas sampling tube

B: Filtering material
C: Three-way cock
D: Conduit tube
E: Washing bottle [containing
A 50 ml of sodium hydroxide
solution (200 giL)]
Source of
exhaust F: Suction pump (for replacing
of gas flow path)
G: Heater
B

Figure 1 Example of gas sampling apparatus

6.3.1.2 Reagents for washing solution

Reagents used for the washing solution of the gas sampling apparatus shall be as
follows.
a) Sodium hydroxide, specified in JIS K 8576.
b) Phosphoric acid, specified in JIS K 9005.

6.3.1.3 Preparation of washing solution

The preparation of washing solution shall be as follows.
a) For the washing solution which is to be poured in washing bottle (E), sodium
hydroxide solution shall be prepared by dissolving 200 g of sodium hydroxide in
water and adding water to make total 1 L.
b) For the washing solution which is to be used for a gas collecting container, phos-
phoric acid solution shall be prepared by adding water to 5.5 g of phosphoric acid
to make total 1 L.

6.3.1.4 Sample gas collecting container

In gas chromatography, the sample gas collecting container as indicated in figure 1
can be either of the following examples.
a) In the case where the sample gas is injected into gas chromatograph im-
mediately after sampling
1) Gas sampling syringe, 1 ml to 5 ml in capacity and made of glass, the inside
surface of which is expected to be with minimum adsorption. It shall be cleaned
by using the phosphoric acid prepared in 6.3.1.3 b) beforehand, and washed with
water and dried.

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b) In the case where the sample gas (sample in laboratory) carried to a labo-
ratory is injected into gas chromatograph
1) Gas sampling bag, which is a bag for sampling gas 1 L or over in capacity, made
of polyester resin, fluoroethylene resin, etc. unlikely to adsorb or absorb gas com-
ponents. This method is not suitable when the sample gas has to be stored for
a long time.
2) Gas collecting bottle, which is a glass bottle of about 1 L capacity exempli-
fied in b) 2) of figure 4 in JIS K 0095. It shall be cleaned by using the phos-
phoric acid prepared in 6.3.1.3 b) beforehand and then washed with water and
dried.
3) Gas collecting can, of stainless steel, 1 L or over in capacity, of which the in-
side surface is electrolytically polished and inactivated by silica-coating and
provided with a shut-out cock with the inside surface of gas flow path inacti-
vated.

6.3.1.5 Gas sampling procedure

The gas sampling procedure in the case of gas chromatography shall be as follows.
The suction pump (F) shall be operated beforehand and the gas flow path of the
gas sampling tube (A), filtering material (B), etc. shall be sufficiently replaced by sample
gas beforehand.
a) In the case of using gas sampling syringe Connect a gas sampling syringe
to the conduit tube (D) of the gas sampling apparatus in figure 1. Open the three-
way cock (C) and after repeating the pumping of syringe to replace sufficiently the
gas in flow path, perform suction of the sample gas. Sample the gas, close the three-
way cock (C), detach the gas sampling syringe and take it as the sample gas for
analysis.
b) In the case of using gas sampling bag An example of the gas sampling ap-
paratus using gas sampling bag is as shown in figure 2. Connect the gas sampling
bag (H) placed in the acrylic resin airtight container (I) as shown in figure 2 to
the conduit tube (D) of the gas sampling apparatus in figure 1 and open the three-
way cock (C). Operate the suction pump (L) in figure 2 and suction the sample
gas by opening the shut-out cocks (J) and (K). Take the sample gas, then close
the shut-out cock (J) and the preceding three-way cock (C), stop the suction pump
(L), take out the gas sampling bag (H) from the acrylic resin airtight container
(I), seal tightly the gas sampling bag and take it as the sample gas for analysis.
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A: Gas sampling tube

D: Conduit tube
H: Gas sampling bag
I : Acrylic resin airtight
container
J, K: Shut-out cock
L : Suction pump
M: Screw cock

Figure 2 Example of gas sampling apparatus using gas sampling bag

c) In the case of gas collecting bottle

1) Method of making vacuum Connect the gas collecting bottle which has been
made vacuum according to 7.4.2 and 7.4.5 a) of JIS K 0095 as the gas collecting
container to the conduit tube (D) of gas sampling apparatus in figure 1. Open
the three-way cock (C) and the shut-out cock of gas collecting bottle and suction
the sample gas. After the sample gas is taken, close the three-way cock (C) and
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the shut-out cock of the gas collecting bottle, then detach the gas collecting bottle
and take it as the sample gas for analysis.
2) Method of replacing with sample gas Connect a gas collecting bottle be-
tween the three-way cock (C) and the washing bottle (E) of the gas sampling ap-
paratus in figure 1. Open the three-way cock (C) and the shut-out cock of gas
collecting bottle, and absorb the sample gas in the collecting bottle by operat-
ing the suction pump (F). In this case, allow the sample gas of a volume 10 times
or over the capacity of the gas sampling tube, tubings and gas collecting bottle
to flow. After replacing the air in the bottle with sample gas, close the shut-out
cock of gas collecting bottle and the three-way cock (C), stop the suction pump
(F), then detach the gas collecting bottle and take it as the sample gas for analy-
SIS.

d) In the case of using gas collecting can Connect the gas collecting can which
has been made vacuum beforehand by using a pump to the conduit tube (D) of the
gas sampling apparatus in figure 1. Open the three-way cock (C) and the switch-
ing valve of gas collecting can and suction the sample gas. After suctioning the
sample gas, close the three-way cock (C) and the shut-out cock of collecting can,
then detach the gas collecting can and take it as the sample gas for analysis.

6.3.2 In the case of methylene blue absorptiometry and ion selective electrode
method

6.3.2.1 Apparatus and instruments for sampling gas

For the gas sampling apparatus and absorbing bottle in the case of methylene blue
absorptiometry and ion selective electrode method, the following shall be used depending
on the sampling amount of sample gas.

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a) In the case of sampling amount 1 L or over An example of gas sampling ap-

paratus is as shown in figure 3 and an example of absorbing bottle to be used is
as shown in figure 4.

Bypass
,.--_~A,- _ _- ,
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A: Gas sampling tube M: Absorbing bottle

B: Filtering material N: Trap (packed with
C: Three-way cock glass wool)
D: Conduit tube S: Wet gas meter
E: Washing bottle (containing 50 ml T: Thermometer
of washing solution) P: Manometer
F: Suction pump (1 L/min to 5 L/min) V: Flow rate controlling
G: Heater valve (cock)

Figure 3 Example of gas sampling apparatus Figure 4

Example of
absorbing
bottle

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b) In the case of sampling amount under 1 L An example of the gas sampling

apparatus is shown in figure 5 and an example of the absorbing bottle to be used
is shown in figure 6.

E
c

Source of
exhaust :::;:~::::::::::::::::::~ Inside

Q
L

A: Gas sampling tube G: Heater

B: Filtering material L: Absorbing bottle
C: Three-way cock P: Injector syringe (100 ml)
E: Washing bottle (containing Q: Absorbing bottle (1 L)
50 ml of washing solution)
F: Suction pump
NOTE: Land Q are connected when using an absorbing bottle.

Figure 5 Example of gas sampling apparatus Figure 6 Example of

absorbing
bottle

6.3.2.2 Reagents for absorbing solution and washing solution

In the case of methylene blue absorptiometry and ion selective electrode method,
the reagents to be used for the absorbing solution poured in the absorbing bottle of
(M) in figure 3 or (L) in figure 5 and for the washing solution poured in the washing
bottle (E) shall be as follows.
a) Zinc sulfate heptahydrate, specified in JIS K 8953.
b) Sodium hydroxide, specified in JIS K 8576.
c) Ammonium sulfate, specified in JIS K 8960.
d) Glycerin, specified in JIS K 8925.
e) Disodium dihydrogen ethylenediamine tetraacetate dihydrate, specified in
JIS K 8107.
f) L( + )-Ascorbic acid, specified in JIS K 9502.

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6.3.2.3 Method for preparation of absorbing solution and washing solution

In the case of methylene blue absorptiometry and ion selective electrode method,
the absorbing solution and washing solution shall be prepared as follows.
a) Absorbing solution for methylene blue absorptiometry Dissolve 5 g of zinc
sulfate pentahydrate in about 500 ml of water and add the solution in which 6 g
of sodium hydroxide is dissolved in about 300 ml of water. Further, add 70 g of
ammonium sulfate while stirring, and after the precipitate of zinc hydroxide is dis-
solved, add water to make total 1 L.
b) Absorbing solution for ion selective electrode method After dissolving 4 g
of sodium hydroxide, 200 ml of glycerin, 4 g of disodium dihydrogen ethylenedi-
amine tetraacetate dihydrate and 10 g of L( + )-ascorbic acid in water, add water
to make total 1 L.
c) Washing solution for gas sampling apparatus The method for preparation
of the gas washing solution for methylene blue absorptiometry and ion selective
electrode method shall be in accordance with 6.3.1.3 a).

6.3.2.4 Sample gas sampling procedure

The sample gas sampling procedure for methylene blue absorptiometry and ion se-
lective electrode method shall be as follows.
a) In the case of the sampling amount 1 L or over, prepare two absorbing bottles shown
in figure 4 and pour 50 ml of absorbing solution in each of them. In the case of
sampling amount under 1 L, prepare one absorbing bottle shown in figure 6 and
pour 10 ml of absorbing solution.
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b) In figure 3, before the sample gas is introduced, replace sufficiently the inside of
the conduit tube with sample gas by utilizing bypass, etc. When the conduit tube
for bypass can not be provided because of the restriction of space due to the cir-
cumstances of sampling site, the conduit tube for bypass may be omitted, provided
that the conduit tube (D) from the gas sampling tube (A) to the three-way cock
(C) is sufficiently replaced by sample gas.
c) The sampling amount and suction rate of sample gas shall be in accordance with
the values specified for each method.
d) Measure the temperature and pressure beforehand, at the same time as the mea-
surement of sample gas amount.

6.3.2.5 Sampling amount of sample gas

The sampling amount of sample gas under the standard condition [273.15 K (0 °C),
101.32 kPa] shall be calculated as the dry-base gas amount (V SD ) or the wet-base gas
amount (Vsw ) according to formula (1) to formula (4) indicated as follows.
a) Calculation of dry-base gas amount
1) In the case of using wet gas meter

V
SD
= Vx 273.15 x Pa +Pm -Pv +22.41x(a+b) .................. (1)
273.15+t 101.32

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2) In the case of using dry gas meter

V. = Vx 273.15 x Pa +Pm +22.41x(a+b) ........................ (2)

SD 273.15+t 101.32

b) Calculation of wet-base gas amount

1) In the case of using wet gas meter

V. =Vx 273.15 x Pa + Pm - Pv + 22 .41 x (a+ b+c) ............. . (3)

sw 273.15+t 101.32

2) In the case of using dry gas meter

Vsw = Vx 273.15 x Pa +Pm +22.41x(a+b+c) .................... (4)

273.15+t 101.32
where, VSD : dry-base gas amount (L)
Vsw: wet-base gas amount (L)
V: gas amount measured by the gas meter (L)
t: temperature at the gas meter (OC)
Pa: atmospheric pressure (kPa)
Pm 1): gauge pressure at the gas meter (kPa)
Pv 2): saturation vapour pressure of water at t °C (kPa)
a 1): amount of analyzer species gas collected in absorb-
ing solution (mol)
b 1): amount of other coexisting gas than the analyzer
species collected in absorbing solution (mol)
c 1): moisture amount obtained according to clause 6 of
JIS Z 8808 (mol)
273.15: absolute temperature corresponding to 0 °C (K)
101.32: standard atmospheric pressure (kPa)
22.41: volume of 1 mol of gas under the standard condi-
tion (L)
Notes 1) Negligible in most cases.
2) As shown in table 2.

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Table 2 Saturation vapour pressure of water

Unit: kPa
Temperature °C
°C .0 .1 .2 .3 .4 .5 .6 .7 .8 .9
0 0.6105 0.6150 0.6195 0.6241 0.6286 0.6333 0.6379 0.6426 0.6473 0.6519
1 0.6567 0.6615 0.6663 0.6711 0.6759 0.6809 0.6858 0.6907 0.6958 0.7007
2 0.7058 0.7109 0.7159 0.7210 0.7262 0.7314 0.7366 0.7419 0.7473 0.7526
3 0.7579 0.7633 0.7687 0.7742 0.7797 0.7851 0.7907 0.7963 0.8019 0.8077
4 0.8134 0.8191 0.8249 0.8306 0.8365 0.8423 0.8483 0.8543 0.8603 0.8663
5 0.8723 0.8785 0.8846 0.8907 0.8970 0.9033 0.9095 0.9158 0.9222 0.9286
6 0.9350 0.9415 0.9481 0.9546 0.9611 0.9678 0.9745 0.9813 0.9881 0.9949
7 1.002 1.009 1.016 1.022 1.030 1.037 1.044 1.051 1.058 1.065
8 1.073 1.080 1.087 1.095 1.102 1.110 1.117 1.125 1.132 1.140
9 1.148 1.156 1.164 1.171 1.179 1.187 1.195 1.203 1.211 1.219
10 1.228 1.236 1.244 1.253 1.261 1.269 1.278 1.286 1.295 1.304
11 1.312 1.321 1.330 1.3388 1.3478 1.3567 1.3658 1.3748 1.3839 1.3998
12 1.4023 1.411 6 1.4209 1.4303 1.4397 1.4492 1.4587 1.4683 1.4779 1.4876
13 1.4973 1.5072 1.517 1 1.5269 1.5369 1.547 1 1.5572 1.5673 1.5776 1.5879
14 1.598 1 1.6085 1.619 1 1.6296 1.6401 1.6508 1.6615 1.6723 1.683 1 1.6940
15 1.7049 1.7159 1.7269 1.738 1 1.7493 1.7605 1.7719 1.7832 1.7947 1.8061
16 1.817 7 1.8293 1.8410 1.8529 1.8648 1.8766 1.8886 1.9006 1.9128 1.9249
17 1.9372 1.9494 1.9618 1.9744 1.9869 1.9994 2.012 1 2.0249 2.0377 2.0505
18 2.0634 2.0765 2.0896 2.1028 2.1160 2.1293 2.1426 2.1560 2.1694 2.1830
19 2.1968 2.2106 2.2245 2.2383 2.2523 2.2663 2.2805 2.2947 2.3090 2.3234
20 2.3378 2.3523 2.3669 2.3815 2.3963 2.4111 2.426 1 2.4410 2.456 1 2.4713
21 2.4865 2.5018 2.517 1 2.5326 2.5482 2.5639 2.5797 2.5955 2.6114 2.6274
22 2.6434 2.6595 2.6758 2.6922 2.7086 2.7251 2.7418 2.7584 2.775 1 2.7919
23 2.8088 2.8259 2.8430 2.8602 2.8775 2.8950 2.9124 2.9300 2.9478 2.9655
24 2.9834 3.0014 3.0195 3.0378 3.0560 3.0744 3.0928 3.1113 3.1299 3.1485
25 3.1672 3.1860 3.2049 3.2240 3.2432 3.2625 3.2820 3.3016 3.3213 3.3411
26 3.3609 3.3809 3.4009 3.4211 3.4413 3.4616 3.4820 3.5025 3.5232 3.5440
27 3.5649 3.5860 3.6070 3.6282 3.6496 3.6710 3.6925 3.7141 3.7358 3.757 7
28 3.7796 3.8016 3.8237 3.8460 3.8683 3.8909 3.9135 3.9363 3.9593 3.9823
29 4.0054 4.0286 4.0519 4.0754 4.0990 4.1227 4.1466 4.1705 4.1945 4.2186
30 4.2429 4.2672 4.2918 4.3164 4.3411 4.3659 4.3908 4.4159 4.4412 4.4667
31 4.4923 4.5180 4.5439 4.5698 4.5958 4.6219 4.6482 4.6745 4.7011 4.7279
32 4.7547 4.7816 4.8087 4.8359 4.8632 4.8907 4.9184 4.9341 4.9740 5.0020
33 5.0301 5.0585 5.0869 5.1154 5.1441 5.1730 5.2020 5.2312 5.2605 5.2898
34 5.3193 5.3490 5.3788 5.4088 5.4390 5.4693 5.4997 5.5302 5.5609 5.5918
35 5.6229 5.6541 5.6854 5.7169 5.7485 5.7802 5.8122 5.8443 5.8766 5.9088
36 5.9412 5.9739 6.0067 6.0396 6.0727 6.1060 6.1395 6.173 1 6.2070 6.2410
37 6.2751 6.3093 6.3437 6.3783 6.413 1 6.4480 6.483 1 6.5183 6.5537 6.5893
38 6.6251 6.6609 6.6969 6.7330 6.7693 6.8058 6.8425 6.8794 6.9166 6.9541
39 6.9917 7.0294 7.0673 7.1053 7.1434 7.181 7 7.2202 7.2589 7.2977 7.3367
40 7.3759 7.414 7.454 7.494 7.534 7.574 7.614 7.654 7.695 7.737
41 7.778 7.819 7.861 7.902 7.943 7.986 8.029 8.071 8.114 8.157
42 8.199 8.242 8.285 8.329 8.373 8.417 8.461 8.505 8.549 8.594
43 8.639 8.685 8.730 8.775 8.821 8.867 8.914 8.961 9.007 9.054
44 9.101 9.147 9.195 9.243 9.291 9.339 9.387 9.435 9.485 9.534
45 9.583 9.633 9.682 9.731 9.781 9.831 9.882 9.933 9.983 10.03
46 10.09 10.14 10.19 10.24 10.29 10.35 10.40 10.45 10.51 10.56
47 10.61 10.67 10.72 10.78 10.83 10.88 10.94 10.99 11.05 11.10
48 11.16 11.22 11.27 11.33 11.39 11.45 11.50 11.56 11.62 11.68
49 11.74 11.79 11.85 11.91 11.97 12.03 12.09 12.15 12.21 12.27

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Table 2 (concluded)
Unit: kPa
Temperature °C
°C .0 .1 .2 .3 .4 .5 .6 .7 .8 .9
50 12.33 12.39 12.46 12.52 12.58 12.64 12.70 12.77 12.83 12.89
51 12.96 13.02 13.09 13.15 13.22 13.28 13.347 13.412 13.479 13.544
52 13.611 13.678 13.746 13.812 13.880 13.948 14.016 14.084 14.154 14.223
53 14.292 14.361 14.431 14.500 14.571 14.641 14.712 14.784 14.856 14.928
54 15.000 15.072 15.144 15.217 15.291 15.364 15.439 15.513 15.588 15.663
55 15.737 15.812 15.887 15.963 16.040 16.117 16.195 16.272 16.349 16.427
56 16.505 16.585 16.664 16.743 16.823 16.903 16.983 17.064 17.145 17.227
57 17.308 17.391 17.473 17.556 17.639 17.721 17.805 17.889 17.973 18.059
58 18.143 18.228 18.313 18.400 18.486 18.573 18.660 18.748 18.836 18.924
59 19.012 19.101 19.190 19.280 19.369 19.460 19.550 19.641 19.732 19.824

--`,`,,,,`,``,````,``````,,,`,-`-`,,`,,`,`,,`---
60 19.916 20.008 20.101 20.194 20.288 20.381 20.476 20.570 20.665 20.760
61 20.856 20.952 21.048 21.144 21.241 21.340 21.438 21.542 21.636 21.734
62 21.834 21.934 22.034 22.134 22.236 22.337 22.438 22.541 22.643 22.746
63 22.849 22.953 23.057 23.162 23.267 23.373 23.478 23.585 23.691 23.798
64 23.906 24.013 24.121 24.230 24.339 24.449 24.558 24.669 24.779 24.891
65 25.003 25.115 25.227 25.339 25.453 25.567 25.682 25.797 25.911 90.054
66 26.143 26.259 26.376 26.494 26.611 26.728 26.847 26.966 27.086 27.206
67 27.326 27.447 27.568 27.690 27.812 27.935 28.058 28.180 28.304 28.428
68 28.554 28.679 28.806 28.932 29.059 29.186 29.314 29.442 29.570 29.699
69 29.828 29.959 30.090 30.220 30.352 30.484 30.617 30.751 30.884 31.017
70 31.16 31.29 31.42 31.56 31.70 31.84 31.97 32.12 32.25 32.38
71 32.52 32.66 32.80 32.94 33.08 33.22 33.37 33.52 33.65 33.80
72 33.94 34.09 34.24 34.38 34.53 34.68 34.82 34.97 35.13 35.28
73 35.42 35.57 35.73 35.88 36.04 36.18 36.34 36.49 36.65 36.80
74 36.96 37.12 37.26 37.42 37.58 37.74 37.90 38.06 38.22 38.38
75 38.54 38.70 38.86 39.04 39.20 39.36 39.53 39.69 39.85 40.02
76 40.18 40.36 40.52 40.69 40.86 41.02 41.20 41.37 41.54 41.72
77 41.88 42.05 42.22 42.40 42.57 42.76 42.93 43.10 43.29 43.46
78 43.64 43.82 44.00 44.18 44.36 44.54 44.73 44.90 45.09 45.28
79 45.46 45.65 45.84 46.02 46.21 46.40 46.58 46.77 46.96 47.16
80 47.34 47.53 47.73 47.92 48.12 48.32 48.50 48.70 48.90 49.10
81 49.29 49.49 49.69 49.89 50.22 50.30 50.64 50.70 50.90 51.12
82 51.32 51.52 51.73 51.93 52.14 52.36 52.56 52.77 52.98 53.20
83 53.41 53.62 53.84 54.05 54.26 54.48 54.70 54.92 55.13 55.36
84 55.57 55.78 56.01 56.22 56.45 56.68 56.90 57.13 57.36 57.58
85 57.81 58.04 58.26 58.49 58.73 58.96 59.18 59.42 59.65 59.89
86 60.12 60.34 60.58 60.82 61.06 61.29 61.53 61.77 62.01 62.25
87 62.49 62.73 62.97 63.21 63.46 63.70 63.95 64.19 64.45 64.69
88 64.94 65.19 65.45 65.69 65.94 66.19 66.45 66.70 66.97 67.22
89 67.47 67.73 67.99 68.25 68.51 68.78 69.03 69.30 69.57 69.70
90 70.096 70.362 70.630 70.898 71.167 71.437 71.709 71.981 72.254 72.527
91 72.801 73.075 73.351 73.629 73.907 74.186 74.465 74.746 75.027 75.310
92 75.592 75.876 76.162 76.447 76.734 77.022 77.310 77.599 77.890 78.182
93 78.474 78.767 79.060 79.355 79.651 79.948 80.245 80.544 80.844 81.145
94 81.447 81.749 82.052 82.356 82.661 82.968 83.274 83.582 83.892 84.202
95 84.513 84.825 85.138 85.452 85.766 86.082 86.400 86.717 87.036 87.355
96 87.675 87.997 88.319 88.643 88.967 89.293 89.619 89.947 90.275 90.605
97 90.935 91.266 91.598 91.931 92.266 92.602 92.939 93.276 93.615 93.954
98 94.295 94.636 94.979 95.323 95.667 96.012 96.359 96.707 97.056 97.407
99 97.757 98.109 98.463 98.816 99.172 99.528 99.885 100.24 100.60 100.96
100 101.32 101.69 102.05 102.42 102.78 103.15 103.52 103.89 104.26 104.63
101 105.00 105.37 105.75 106.12 106.50 106.88 107.26 107.64 108.02 108.40

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7 Sample gas sampling procedure and preparation of sample solutions for

analysis

7.1 In the case of gas chromatography

The gas sampling procedure shall be in accordance with 6.3.1.

7.2 In the case of methylene blue absorptiometry and ion selective electrode
method
The preparation of sample solutions for analysis, after sampling the sample gas in
an absorbing bottle by means of the sample gas sampling apparatus as shown in fig-
ure 3 or figure 5 according to 6.3.2.4, shall be as follows.
a) After suction of sample gas, transfer the solution in the absorbing bottle into a
200 ml volumetric flask, if the absorbing bottle in figure 4 is used, and into a 20 ml
volumetric flask, if the absorbing bottle in figure 6 is used. Wash the inside of
the absorbing bottle with absorbing solution, and join the washings to the previ-
ous volumetric flask.

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b) Add absorbing solution up to the mark and seal tightly. Take this solution as the
sample solution for analysis.

8 Gas chromatograph

8.1 Summary
Analysis is performed by using a packed column or a capillary column as a separa-
tion column and using a thermal conductivity detector, a flame photometric detector
or an atomic emission detector as a detector. The flue gas taken in 6.3.1.5 is intro-
duced into the gas chromatograph, and hydrogen sulfide is determined from the chro-
matogram obtained. The determination range, when 100 ~l of sample gas is introduced,
is 200 vol ppm to 20 vol % for a thermal conductivity detector, 0.2 vol ppm to 50 vol ppm
for a flame photometric detector, 0.05 vol ppm to 50 vol ppm for an atomic emission
detector.

8.2 Reagen ts and gas

The following reagents and gas shall be used.

8.2.1 Phosphorus acid, specified in 6.3.1.2 b).

8.2.2 Helium, with purity of 99.999 vol % min. or 99.999 9 vol % min.

8.2.3 Nitrogen, of Grade 1 or Grade 2 as specified in JIS K 1107.

8.2.4 Argon, of Grade 1 or Grade 2 as specified in JIS K 1105.

8.2.5 Hydrogen, of Grade 1 to Grade 3 as specified in JIS K 0512.

8.2.6 Oxygen, with purity 99.5 vol % min. as specified in JIS K 1101.

8.2.7 High purity air, which is clean and dry.

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8.3 Apparatus and instruments

The following apparatus and instruments shall be used.

8.3.1 Sample introducing instrument of gas chromatograph The sample in-

troducing instrument of gas chromatograph shall be as follows.
a) Gas sampling syringe, for gas sampling apparatus, as specified in 6.3.1.4 a) 1).
b) Gas sample introducing instrument (loop injector), composed of a measur-
ing tube (sample loop tube) for filling a certain amount of sample gas for analysis
attached to a rotary valve made offluoroethylene resin or the like or a sliding valve,
which is capable of heating up to 150 cC. In the case of sample of low concentra-
tion, an introducing instrument in which the measuring tube and tubings have the
inner surface composed of inactivated stainless steel, fluoroethylene resin or any
other material at least equivalent to these in inactivation, so that adsorption of
gas component is minimum. An example of gas sample introducing apparatus is
shown in figure 7.

Measuring tube
Pressure
control for
Sample ~ injection
opening
--`,`,,,,`,``,````,``````,,,`,-`-`,,`,,`,`,,`---

Injection

Figure 7 Example of gas sample introducing apparatus

Connect the suction pump to the position 3 (out) shown in figure 7, and suction
the sample gas for analysis into the measuring tube. After filling the measuring
tube with the sample gas, allow the temperature and pressure of the sample gas
for analysis to stabilize, connect positions 1 and 2, positions 5 and 6 by switching
the valve, and introduce the sample gas for analysis in measuring tube into the
injection opening of the gas chromatograph.

8.3.2 Constitution of gas chromatograph The constitution of gas chromatograph

shall be as follows.
a) Packed column, in accordance with the following 1), which is filled with anyone
of column packings in 2).
1) Tube for column, a tube the inside surface of which has been washed well with
acid, and after being cleansed with phosphoric acid in 6.3.1.3 b), washed with
water and dried, or a tube made of fluoroethylene resin 3).
Note 3) When using a tube of fluoroethylene resin, make sure that the con-
nection is without any leakage of gas.

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2) Column packing
2.1) Distributor type packing, prepared by impregnating polymer beads of 74 ~m
to 250 ~m diameter, high purity diatomaceous earth based support or support
made of inert material 4) with an adequate stationary liquid [for example, 1,2,3-
tris (2-cyanoethoxy) propane] among those given in table 4 of JIS K 0114.
Note 4) The particles of terephthalic acid, particles of fluoroethylene resin,
etc.
2.2) Porous polymer type packing, composed of organic high polymer compound,
superior in chemical stability and mechanical strength.
b) Capillary column, composed of the column tube in 1) in the following, the inside
surface of which is chemically bonded with the stationary liquid in 2) or stabilized
with the adsorbent in 3).
1) Tube for column, a tube based on molten silica or a tube of stainless steel of
which the inside surface is inactivated.
2) Stationary liquid, of methyl silicone, or methyl silicone in which a part of
methyl group is replaced by another functional group (for example, phenyl group)
or polyethylene glycol.
3) Adsorbent, composed of silicon oxide, aluminium oxide or organic high polymer
compound, superior in chemical stability and mechanical strength.

--`,`,,,,`,``,````,``````,,,`,-`-`,,`,,`,`,,`---
c) Detector, a thermal conductivity detector, a flame photometric detector or an
atomic emission detector 5).
Note 5) In some atomic emission detectors, the packed column can not be used.
d) Carrier gas, in the case of thermal conductivity detector, helium in 8.2.2, nitrogen
in 8.2.3 or argon in 8.2.4, and in the case of the flame photometric detector, helium
in 8.2.2 or nitrogen in 8.2.3, and in the case of atomic emission detector, helium
in 8.2.2 with purity 99.999 9 vol % min.
e) Gas for detector The gas used for each detector shall be as follows.
1) Addition gas for thermal conductivity detector, the same kind of gas as
the carrier gas.
2) Flame photometric detector The gas for flame photometric detector shall
be selected from among the followings given according to each usage.
2.1) Addition gas, helium in 8.2.2 or nitrogen in 8.2.3.
2.2) Combustion gas, hydrogen specified in 8.2.5.
2.3) Supporting gas, oxygen in 8.2.6 or high purity air in 8.2.7.
3) Atomic emission detector The gas for atomic emission detector shall be as
follows.
3.1) Addition gas (purge gas), nitrogen in 8.2.3.
3.2) Combustion gas (plasma gas), helium in 8.2.2, with purity of 99.999 9 vol %
mIn.

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3.3) Supporting gas, hydrogen of Grade 2 or superior in 8.2.5 and oxygen in 8.2.6,
with purity of 99.999 vol % min.

8.4 Introduction of sample gas for analysis into gas chromatograph

The introduction of sample gas for analysis into gas chromatograph shall be as fol-
lows.
a) Introduction using gas sampling syringe When the sample gas is taken in
a gas sampling syringe in 6.3.1.5 a), attach a needle to the syringe and introduce
directly the sample gas for analysis into a gas chromatograph. When the sample
gas is taken in a gas sampling bag, gas collecting bottle or gas collecting can, seal
tightly the opening of the collecting container, with, for example, silicone rubber,
and penetrate the needle attached to the gas sampling syringe into the stopper.
Carry out the operation in 6.3.1.5 a) and introduce the sample gas taken in the
gas sampling syringe into the gas chromatograph.
b) Introduction using gas sample introducing apparatus Connect the opening
of the gas sampling bag, a gas collecting bottle or a gas collecting can in 6.3.1.4 b)
to the sampling part of the gas sample introducing apparatus in figure 7. Open
the cock or valve of the collecting container, switch the valve of gas sample intro-
ducing apparatus and suction the sample gas by pump so as to allow the amount
of sample gas which is five times or over the capacity of the measuring tube to
pass through the measuring tube until the measuring tube is filled with the sample
gas, then switch the valve of the gas sample introducing apparatus, and introduce
the sample gas for analysis in the measuring tube into the gas chromatograph.
In addition, connect the sample injecting opening of the gas sample introduc-
ing apparatus in figure 7 to the sample gas sampling tube (A) in figure 1, and the
--`,`,,,,`,``,````,``````,,,`,-`-`,,`,,`,`,,`---

sample gas may be directly introduced into a gas chromatograph.

8.5 Operation conditions of gas chromatograph

8.5.1 Conditions of sample introducing part

The optimum conditions for sample introducing part can differ depending on the
type of column and equipment to be used. The conditions, therefore, should be opti-
mized by referring to the operation manual for respective equipments. Examples of
setting conditions are as follows.
a) Packed column
1) In the case of using a gas sampling syringe The packed column injection
method shall be employed. The temperature at the sample introducing part shall
be set to about 150°C.
2) In the case of using a gas sample introducing apparatus The tempera-
ture of the gas sample introducing apparatus shall be set to about 150 °C.
b) Capillary column
1) In the case of using a gas sampling syringe The split injection method or
direct injection method shall be employed. The temperature at the sample in-
troducing part shall be set to about 150°C.

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2) In the case of using a gas sample introducing apparatus The split in-
jection method or direct injection method shall be employed. The temperature
at the sample introducing part and the temperature of the sample introducing
apparatus shall be set to about 150°C.

8.5.2 Example of operation conditions for column

The conditions for column shall be a column temperature and a carrier gas flow rate
at which the column would fully exhibit the separation performance as described in
8.3.2 a) or 8.3.2 b). Table 3 shows examples of conditions for column.

Table 3 Examples of conditions for column a), b)

Separation Case of Packings Col umn dimensions Temperature of Carrier gas

column condition col umn and the flow rate
rise and fall of
temperature
Packed Case 1 1,2,3-tris (2- Inside diameter: 3 mm, 60°C to 80 °C 10 mllmin to
column cyanoethoxy) Length: 3 m to 5 m 50 mllmin
propane (25 %) c)
Case 2 Polymer beads Inside diameter: 3 mm, 80°C to 100°C 40 mllmin to
Length: 0.75 m to 2 m 60 ml/min

Capillary Case 3 Stationary liquid: Inside diameter: 0.25 mm 50°C (5 min) 3 ml/min
column 100 % methyl to 0.53 mm, ---720 °C/min---7
silicone Length: 60 m to 105 m, 250°C (0 min)
Film thickness: 1 !-lm to
5!-lm
Case 4 Porous polymer: Inside diameter: 0.52 mm, 80°C (5 min) 3 mllmin
silica gel Length: 30 m to 60 m ---720 °C/min---7
250°C (0 min)
Notes a) For both the packed column and capillary column, a column with separation performance
equivalent or superior to that exemplified may be used.
b)
The column temperature and carrier gas flow rate shall match the conditions where the
hydrogen sulfide separates from the interferring substance.
c)
When separation is impossible due to coexistence of sulfur dioxide, polyphenylether
(6 ring) shall be used.

8.5.3 Operation conditions for detector

The temperature and gas flow rate of each equipment shall be set to the optimum
conditions. The optimum conditions can differ depending on the type of column and
equipment to be used, and therefore, conditions should be optimized by referring to
the operation manual for respective equipments. Examples of operation conditions are
as follows.
a) In the case of using thermal conductivity detector Example of condition
Temperature of detector: 250°C, flow rate of addition gas: 45 mllmin.
b) In the case of using flame photometric detector Example of condition
Temperature of detector: 200°C, flow rate of addition gas (helium): 50 mllmin, flow
rate of combustion gas: 50 ml/min, flow rate of supporting gas (air): 60 mllmin.

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c) In the case of using atomic emission detector Example of condition Tempera-

ture of detector: 300°C, flow rate of addition gas (purge gas, nitrogen): 0.5 L/min,
flow rate of combustion gas (plasma gas, helium): 35 mlimin, flow rate of supporting
gas (hydrogen): 20 mlimin, flow rate of supporting gas (oxygen): 20 mlimin, wave-
length of sulfur monitor: 181 nm.

8.6 Determination procedure

The procedure of determination shall be as follows.
a) Maintaining the analytical conditions of the gas chromatograph to be equivalent
to the conditions for preparation of working curve, inject a certain amount of sample
gas for analysis which has been obtained in the sampling procedure in 6.3.1.5 into
the gas chromatograph, and record the resultant gas chromatogram.
b) Measure the peak height or peak area of hydrogen sulfide in sample gas, and obtain
the amount (ng) of hydrogen sulfide from the working curve prepared beforehand.
In the case of measuring hydrogen sulfide content by using a fluorescence photo-
metric detector, the response of the detector is proportional to approximately the
square of the absolute amount of injection. The inclination (power multiplier, etc.)
of working curve differs depending on the state of the column, the combustion
condition of the detector, etc., therefore, the prepared working curve shall be the
multi-point working curve.

8.7 Preparation of working curve

The preparation of working curve shall be as follows.
a) Set the conditions of the apparatus according to the analytical and operation con-
ditions of the gas chromatograph.
b) Prepare gas 6) for working curve of appropriate concentration in a gas sampling bag,
gas collecting bottle or gas collecting can equivalent those specified in 6.3.1.4 b).

--`,`,,,,`,``,````,``````,,,`,-`-`,,`,,`,`,,`---
Using a gas sampling syringe 7), inject different amounts of sample gas into the
gas chromatograph, and record the resultant gas chromatogram.
Notes 6) As an alternative to the standard gas available on the market, gas
prepared by permeation tube method may also be used. For the method
of preparing standard gas by the permeation tube method, see JIS K
0055 :2002.
7) For introduction of sample, as an alternative to using a gas sampling
syringe, a gas sample introducing apparatus may also be used. In the
analysis for lower concentration of gas, there is a possibility of
adsorbing to the inside wall surface and gas sample introducing ap-
paratus, therefore care shall be taken when it is used.
c) Measure the peak height or peak area of hydrogen sulfide in the gas for working
curve, and create a relation curve between the mass (ng) of hydrogen sulfide and
the peak height or peak area.

8.8 Calculation of hydrogen sulfide concentration

Calculate the concentration of hydrogen sulfide in the sample gas according to the
following formulae and round off to two significant figures according to JIS Z 8401.

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C = 0.657 x A x 10~6 xl 0 6
y V
A
Cm = - = l.521 x Cy
V
where, Cv : volume concentration of hydrogen sulfide in flue gas
(vol ppm)
Cm : mass concentration of hydrogen sulfide in sample
gas (mg/m 3 )
A: mass of hydrogen sulfide in sample gas for analy-
sis obtained by working curve (ng)
V: sample gas injection amount (ml)
0.657: volume of hydrogen sulfide corresponding to 1 mg
of hydrogen sulfide (ml)
1.521: mass concentration of 1 vol ppm of hydrogen sulfide
(mg/m 3 ), (34.086/22.41)
10-6 : factor to convert the unit of mass from ng to mg
106 : factor to convert ml/ml to vol ppm

9 Methylene blue absorptiometry

9.1 Reagents and preparation of reagent solutions

9.1.1 Reagents
The following reagents shall be used.
a) N,N-Dimethyl-para-phenylenediammonium dichloride, specified in JIS K
8193.
b) Iron (III) chloride hexahydrate, specified in JIS K 8142.
c) Sulfuric acid, specified in JIS K 8951.
d) Potassium iodide, specified in JIS K 8913.
e) Iodine, specified in JIS K 8920.
f) Hydrochloric acid, specified in JIS K 8180.
g) Sodium thiosulfate pentahydrate, specified in JIS K 8637.
h) Sodium carbonate, specified in JIS K 8625.
i) Potassium iodate, specified in JIS K 8005.
j) Starch, soluble, specified in JIS K 8659.
k) Sodium sulfide nonahydrate, specified in JIS K 8949.

9.1.2 Preparation of reagent solutions

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The preparation of reagent solutions shall be as follows.

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9.1.2.1 Absorbing solution, prepared in accordance with 6.3.2.3 a).

9.1.2.2 N,N-Dimethyl-para-phenylenediammonium solution Dissolve 0.2 g of

N,N-dimethyl-para-phenylenediammonium dichloride in 100 ml of sulfuric acid (1+3).

9.1.2.3 Iron (III) chloride solution Dissolve 1 g of iron (III) chloride hexahydrate
in 100 ml of sulfuric acid (1+99).

9.1.2.4 Iodine solution (0.05 mol/L) 8) Dissolve 40 g of potassium iodide in about

25 ml of water, then add and dissolve 13 g of iodine and make 1 L with water. Add
three drops of hydrochloric acid to this solution, mix, and pour in an opaque and air-
tight bottle and store in a dark place.
Note 8) The solution available on the market may also be used.

9.1.2.5 0.1 mol/L Sodium thiosulfate solution Weigh out 13 g of sodium thiosul-
fate pentahydrate and 0.1 g of sodium carbonate and dissolve in 500 ml of water free
from dissolved oxygen (see NOTE 3 to clause 4 of JIS K 0557). Store the solution in
an airtight container and leave to stand for 2 days. After standing, standardize using
potassium iodate. The standardization procedure shall be as follows.
Standardization
a) Heat potassium iodate at 130°C for about 2 h, allow it to cool in a desiccator, then
weigh out about 0.36 g of it to the nearest 0.1 mg.
b) After dissolving it in water, transfer it into a 250 ml volumetric flask by washing
with water and add water up to the mark.
c) Weigh out accurately 25 ml of this solution in a 300 ml Erlenmeyer flask with
ground stopper, add water to make about 100 ml, add 2 g of potassium iodide, 5 ml
of sulfuric acid (1+5), stopper and shake it gently and leave it in dark place for
10 min.
d) Titrate the isolated iodine with 0.1 mollL sodium thiosulfate solution. After the
yellow colour of the solution has become faint, add about 1 ml of starch solution
as an indicator, and continue the titration to the end point where the blue colour
of starch iodine vanishes, and obtain the volume consumed in titration.
e) Separately, carry out a blank test under the same conditions and obtain the vol-
ume consumed in titration.
f) Calculate the factor of 0.1 mollL sodium thiosulfate solution according to the fol-
lowing formula:
25 1 B
f=mx--x x--
. 250 Cal +ao)xO.003567 100

where, f: factor of 0.1 mollL sodium thiosulfate solution

m: sampling amount of potassium iodate (g)
B: purity of potassium iodate (mass ratio %)

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al: amount of 0.1 mollL sodium thiosulfate solution

consumed in titration in d) (ml)
ao: amount of 0.1 mollL sodium thiosulfate solution
consumed in blank test in e) (ml)
0.003 567: amount of potassium iodate corresponding to 1 ml
of 0.1 mollL sodium thiosulfate solution (g)

9.1.2.6 Starch solution (10 gIL) Mix 1 g of starch (soluble) with about 10 ml of water
sufficiently, add this to 90 ml of hot water while stirring, boil for about 1 min, and allow
to cool. Prepare this solution immediately before use.

9.1.2.7 Sulfide ion standard solution (S2- 1 mg/ml) Weigh out approximately 3.B g
of crystal of sodium sulfide nonahydrate, wash the surface with small amount of water,
and after filtering through a filter paper to remove moisture, dissolve in water free
from dissolved oxygen (see NOTE 3 to clause 4 of JIS K 0557) to make 500 ml. The
concentration of this solution shall be obtained according to the following.
a) Weigh out accurately 20 ml of iodine solution (0.05 mollL), pour it into a 300 ml
Erlenmeyer flask with ground stopper and add 1 ml of hydrochloric acid. Weigh
out accurately 20 ml of this sulfide ion standard solution and add 9) to the iodine
solution by dipping the tip of the pipette in it. Immediately stopper it tightly, shake
to mix, and leave it to stand for 10 min.
Note 9) The sulfide ion standard solution (S2- 1 mg/ml) is added to the acidic
iodine solution of hydrochloric acid.
b) Titrate it with 0.1 mollL sodium thiosulfate solution, and when the yellow colour
of solution has become faint, add 1 ml of the starch solution (10 giL) as an indica-
tor and titrate it until the blue colour of starch iodine generated vanishes.
c) Separately, weigh out accurately 20 ml of iodine solution (0.05 mol/L), pour it into
a 300 ml Erlenmeyer flask with ground stopper, add 1 ml of hydrochloric acid, then
similarly, titrate it with 0.1 mollL sodium thiosulfate solution.
d) Calculate the concentration Cs (S2- mg/ml) of the sulfide ion standard solution
according to the following formula.
Cs =(b-a)xJxl/20x1.603

where, Cs : concentration of sulfide ion standard solution (S2-

mg/ml)
a: amount of 0.1 mollL sodium thiosulfate solution
consumed in titration (ml)
b: amount of 0.1 mollL sodium thiosulfate solution cor-
responding to 20 ml of iodine solution (0.05 mol/L)
(ml)
f: factor of 0.1 mollL sodium thiosulfate solution
1.603: mass of sulfide ion of 1 ml of 0.1 mollL sodium thio-
sulfate solution (mg)

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9.1.2.8 Sulfide ion standard solution (S2- 10 ~g/ml) Weigh out accurately 1 ml
of the sulfide ion standard solution (8 2 - 1 mg/ml) in a 100 ml volumetric flask and add
water free from dissolved oxygen (see NOTE 3 to clause 4 of JIS K 0557) up to the
mark. However, the concentration of this solution shall be calculated from the con-
centration of sulfide ion standard solution (8 2 - 1 mg/ml) in 9.1.2.7.

9.2 Apparatus and instrument

The following apparatus and instrument shall be used.
Photometer A spectrophotometer or a photoelectric photometer shall be used.

9.3 Determination procedure

The procedure of determination shall be as follows.

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a) Take 20 ml of the sample solution for analysis prepared according to 7.2 in a 25 ml
vol umetric flask.
b) Add 2 ml of N,N-dimethyl-para-phenylenediammonium solution, stopper it, tumble
it gently to mix 10), immediately add 1 ml of iron (III) chloride solution, again stopper
it and tumble it gently to mix 10), then add water free from dissolved oxygen (see
NOTE 3 to clause 4 of JIS K 0557) up to the mark.
Note 10) The solution shall not be shaken.
c) Leave it to stand at a certain temperature in the vicinity of the ordinary tempera-
ture for 30 min.
d) Transfer a portion of the solution into the absorption cell of a spectrophotometer
or photoelectric photometer as the analytical sample, and measure the absorbance
at the wavelength of around 670 nm. For the contrast solution, take 20 ml of
absorbing solution in a 25 ml volumetric flask, and perform the procedures in b)
and c).
e) Obtain the mass (mg) of sulfide ion from the working curve prepared according to
9.4.

9.4 Preparation of working curve

The preparation of working curve shall be as follows.
a) Take stepwise amounts from 0.5 ml to 2.0 ml of sulfide ion standard solution (8 2 -
10 !lg/ml) in 9.1.2.8 in as many 25 ml volumetric flasks, and add 20 ml of absorb-
ing solution in 6.3.2.3 a).
b) Perform the procedures in 9.3 b) to 9.3 d).
c) Create a relation curve between the amount (mg) of sulfide ion and the absorbance.

9.5 Calculation of hydrogen sulfide concentration

Calculate the concentration of hydrogen sulfide in the sample gas according to the
following formulae and round it off to two significant figures according to JIS Z 8401.

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200
0.698xax-
Cy = _ _ _---=2=-.:0=___ x 1 000
Vs

l.063 x a x 200
Cm = _ _ _---=2::..;:0'--x 1 000 = 1.521 x Cy
Vs

where, Cv : volume concentration of hydrogen sulfide in sample

gas (vol ppm)
Cm : mass concentration of hydrogen sulfide in sample
gas (mg/m 3 )
a: mass of sulfide ion obtained in 9.3 e) (mg)
20: aliquot amount 20 of sample solution for analysis
(ml)
Vs: sampling amount of sample gas under the standard
condition calculated in 6.3.2.5 (L)
0.698: volume of hydrogen sulfide corresponding to 1 mg
of sulfide ion (8 2 -) (ml)
1.063: mass of hydrogen sulfide corresponding to 1 mg of
sulfide ion (8 2 -) (mg)
1.521: mass concentration of 1 vol ppm of hydrogen sulfide
(mg/m 3 ), (34.086/22.41)

10 Ion selective electrode method

10.1 Reagents and preparation of reagent solutions

10.1.1 Reagents
The following reagents shall be used.
a) Sodium thiosulfate pentahydrate, specified in JIS K 8637.
b) Sodium sulfide nonahydrate, specified in JIS K 8949.
c) Glycerin, specified in JIS K 8295.
d) Sodium hydroxide, specified in JIS K 8576.

10.1.2 Preparation of reagent solutions

The preparation of reagent solutions shall be as follows.

10.1.2.1 Absorbing solution, prepared in accordance with 6.3.2.3 b).

10.1.2.2 0.1 mol/L Sodium thiosulfate solution, prepared in accordance with

9.1.2.5.

10.1.2.3 Starch solution, prepared in accordance with 9.1.2.6. Prepare this solu-
tion immediately before use.

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10.1.2.4 Sulfide ion standard solution (S2- 1 000 mg/L) Dissolve 3.8 g of sodium
sulfide nonahydrate, 100 ml of glycerin and 2 g of sodium hydroxide in water to make
500 ml. 8tore this solution in an airtight container and standardize it immediately
before use. The concentration of this solution shall be determined according to 9.1.2.7
a) to d).

10.1.2.5 Sulfide ion solution for working curve (S2- 10 mg/L) Dilute the sul-
fide ion standard solution (8 2 - 1 000 mg/L) 100 times with absorbing solution. The con-
centration of this solution shall be calculated by the concentration of sulfide ion standard
solution (8 2- 1 000 mg/L) in 10.1.2.4.

10.1.2.6 Sulfide ion solution for working curve (S2- 1 mg/L) Dilute the sulfide
ion standard solution (8 2- 1 000 mg/L) 1 000 times with absorbing solution. The con-
centration of this solution shall be calculated by the concentration of sulfide ion stan-
dard solution (8 2- 1 000 mg/L) in 10.1.2.4.

10.1.2.7 Sulfide ion solution for working curve (S2- 0.1 mg/L) Dilute the sul-
fide ion standard solution for working curve (8 2 - 10 mg/L) 100 times with absorbing
solution. The concentration of this solution shall be calculated by the concentration
of sulfide ion standard solution (8 2 - 1 000 mg/L) in 10.1.2.4.

10.1.2.8 Sulfide ion solution for working curve (S2- 0.01 mg/L) Dilute the sul-
fide ion standard solution for working curve (8 2 - 10 mg/L) 1 000 times with absorbing
solution. The concentration of this solution shall be calculated by the concentration
of sulfide ion standard solution (8 2 - 1 000 mg/L) in 10.1.2.4.

10.2 Apparatus and instruments

The following apparatus and instruments shall be used.

10.2.1 Potentiometer, of high input resistance capable of reading response poten-

tial of 0.1 mV or under (e.g. digital type pH-mV meter, pH-mV meter with expanded
span, ion meter, etc.).

10.2.2 Sulfide ion selective electrode, the solid state membrane type sulfide ion
selective electrode in which silver sulfide is to be the main component.

10.2.3 Reference electrode, of the silver-silver chloride internal electrode type.

10.2.4 Magnetic stirrer, coated with fluoroethylene resin, provided with a rotor.

10.3 Determination procedure

The procedure of determination shall be as follows.
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a) Connect a sulfide ion selective electrode and a reference electrode to a potentiom-

eter.
b) Wash the part of the sulfide ion selective electrode and the reference electrode which
has been in contact with the solution with water, and wipe off the water.
c) Transfer the sample solution for analysis 11) prepared according to 7.2 to a 50 ml
dry beaker, immerse the sulfide ion selective electrode and the reference electrode,

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and measure the response potential (Eo) while agitating with a magnetic stirrer
at a definite rate.
Note 11) If the amount of sample solution is 200 ml, a part of it is transferred
to a beaker, and if 20 ml, the whole amount. It should be noted that
washing with water should not be performed.
d) Obtain the approximate value of the concentration of sulfide ion in sample solu-
tion from the working curve prepared according to 10.4 and prepare the solution
for sulfide ion working curve (mg/L) which is 100 times to 1 000 times the obtained
concentration according to 10.1.2.4 to 10.1.2.8.
e) Add 0.2 ml of the solution for sulfide ion working curve prepared in d) to the sample
solution measured in c), and measure similarly the response potential (E l ).
f) Add 0.2 ml of the solution for sulfide ion working curve of a different concentra-
tion prepared in d) to the solution measured in e), and measure the response po-
tential (E 2 ) similarly to e). Carry out the similar operation again, and measure
the response potential (E3).

10.4 Preparation of working curve

The preparation of working curve shall be as follows.
a) Transfer a proper amount of the solution for sulfide ion working curve (8 2 -
0.01 mg/L) prepared in 10.1.2.8 in a 50 ml beaker, perform the procedure in 10.3
and measure the response potential from a potentiometer 12).
Note 12) When an ion meter which displays the measured value in concentra-
tion of ion is used as a potentiometer, instead of preparing the work-
ing curve according to a) to c) in 10.4, perform correction on the ion
meter with two types of solutions for working curve with different
concentrations of sulfide ion, and then measure the sample solution
to determine the sulfide ion concentration.
b) Repeat the procedure in a) on the solution for sulfide ion working curve (8 2 -
0.1 mg/L) in 10.1.2.7, the solution for sulfide ion working curve (8 2 - 1 mg/L) in
10.1.2.6 and the solution for sulfide ion working curve (8 2- 10 mg/L) in 10.1.2.5,
in this order, and measure the response potential corresponding to each solution.
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c) Plot the logarithm of sulfide ion concentration on the abscissa and the response
potential on the ordinate to prepare the relation curve between the concentration
of sulfide ion (mg/L) and the response potential.

10.5 Calculation of hydrogen sulfide concentration

The calculation shall be as follows.
a) Calculation of sulfide ion concentration in sample solution for analysis
Calculate the concentration (A) of sulfide ion in sample solution for analysis ac-
cording to the following formulae, and round it off to two significant figures
according to JIS Z 8401.

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C C C
Al = LlE A2 = - - - - - - - A3 = LlE
_1 LlE2 _3

101 x lOs - 100 102 x lOs - 100 103 x lOs - 100

where, A: mean value of measured values of sulfide ion con-

centration in sample solution for analysis (mg/L)
A 1 , A 2 , A3: sulfide ion concentration in sample solution for
analysis obtained by adding 0.2 ml, 0.4 ml, 0.6 ml
--`,`,,,,`,``,````,``````,,,`,-`-`,,`,,`,`,,`---

of the solution for sulfide ion working curve to the

sample solution for analysis (mg/L)
C: concentration of the solution for sulfide ion work-
ing curve prepared in 10.3 d) (mg/L)
i1El, i1E2, i1E3: difference between the response potential Eo ob-
tained in 10.3 c) and response potentials E1, E2 ,
E3 obtained in 10.3 e) and 10.3 f) (i1E 1 = Eo- E 1,
AE2 = Eo - E 2, i1E3 = Eo - E 3)
S: potential slope in the vicinity of the concentra-
tion of sample solution for analysis in the work-
ing curve obtained in 10.4, and the difference of
response potential corresponding to tenfold con-
centration change (V)
b) Calculation of hydrogen sulfide concentration in flue gas Calculate the hy-
drogen sulfide concentration in flue gas according to the following formulae.
C = 0.698 x A x V
y V
s

C
m
= 1.063 x A x V = 1.521 x C y
Vs

where, Cv : volume concentration of hydrogen sulfide in sample gas

(vol ppm)
Cm : mass concentration of hydrogen sulfide in sample gas
(mg/m 3 )
A: mean value of the concentration of sulfide ion in the
sample solution for analysis obtained in a) (mg/L)
V: amount of sample solution for analysis prepared in 7.2
(ml)
v~: sampling amount of sample gas under the standard
condition calculated in 6.3.2.5 (L)
0.698: volume of hydrogen sulfide corresponding to 1 mg of
sulfide ion (8 2 -) (ml)

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1.063: mass of hydrogen sulfide corresponding to 1 mg of sul-

fide ion (8 2 -) (mg)
1.521: mass concentration of 1 vol ppm of hydrogen sulfide
(mg/m 3 ), (34.086/22.41)

11 Record of analysis results

The items to be recorded as analysis results shall be as follows.
a) Name of person who performed gas sampling, and date and time of sampling
b) Details of sampling method and preparation of analysis sample
c) Determination method
d) N arne of person who performed analysis, and time and date of analysis
e) Analysis values
f) Other matters required to be noted

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Annex A (informative)
Silver nitrate potentiometric titration

A.l Summary of silver nitrate potentiometric titration

The summary of silver nitrate potentiometric titration is shown in table A.I.

Table A.l Silver nitrate potentiometric titration

Determination method Sampling Determination NOTE

range
Flue gas is allowed to be absorbed Absorbing bottle 10 vol ppm to The drawing method
in absorbing solution, then the method 500 vol ppm shall be as follows.
potentiometric titration is carried Absorbing solution: 100 vol ppm or over:
out by using silver nitrate methanol as specified in A.2.2.1 according to the
solution to determine hydrogen titration curve.
sulfide. Sampling amount
of sample gas: 20 L 100 vol ppm or under:
Gran plotting method
shall be applied.

A.2 Reagents and preparation of reagent solutions

The reagents and preparation of reagent solutions are as follows.

A.2.1 Reagents The following reagents are used.

a) Potassium hydroxide, specified in JIS K 8574.
b) Methanol, specified in JIS K 8891.
c) Ammonia solution, specified in JIS K 8085.
d) Sodium chloride, specified in JIS K 8005.
e) Silver nitrate, specified in JIS K 8550.
f) Potassium nitrate, specified in JIS K 8548.

A.2.2 Perparation of reagent solutions The preparation of reagent solutions is

as follows.

A.2.2.1 Absorbing solution Dissolve 60 g of potassium hydroxide in 50 ml of water,

and add methanol to the mark to make 1 L.

A.2.2.2 Ammonia solution (1+14) It is prepared by adding 1 volume of ammonia

solution and 14 volume of water.

A.2.2.3 0.01 mol/L silver nitrate methanol solution Take 0.17 g of silver nitrate,
add 100 ml of methanol to dissolve completely, and add methanol to the mark. The
factor of this solution is obtained by the following standardization.

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Standardization
a) Heat sodium chloride at 600°C for 1 h, put it in a desiccator and leave it to cool.
Weigh out about 0.58 g of it to the nearest 0.1 mg, dissolve it in about 20 ml of
water, then wash it into a 100 ml volumetric flask and add water to the mark.
b) Take accurately 10 ml of this solution in a 250 ml beaker and add about 40 ml of
methanol.
c) Immerse an ion selective electrode and a reference electrode 1) in a beaker and carry
out the potentiometric titration 2) by using 0.01 moliL silver nitrate methanol so-
lution. Plot the added amount of 0.01 mol/L silver nitrate methanol solution (ml)
on the abscissa and the response potential difference (V) on the ordinate to pre-
pare a titration curve. Obtain the amount (ml) of 0.01 mollL silver nitrate methanol
solution consumed in titration from the titration curve, and calculate the factor
(j) of 0.01 moliL silver nitrate methanol solution according to the following formula.

f=~
a

where, f: factor
a: amount of silver nitrate methanol solution con-
sumed in titration (ml)
b: 0.01 moliL sodium chloride solution (ml)
Notes 1) A salt bridge of potassium nitrate or a double liquid junction type
reference electrode is used, in order to prevent potassium chloride
solution from mixing in the titration solution.
2) As an alternative to the potentiometric titration, the silver nitrate
titration method using an adsorption indicator (for example, fluores-
cein sodium, etc.) may be applied.

A.3 Apparatus and instruments

The following apparatus and instruments are used.

A.3.1 Sample gas sampling apparatus and absorbing bottle, as shown in fig-
ure 3 and figure 4, respectively.

A.3.2 Potentiometer, as shown in 10.2.1.

A.3.3 Silver ion selective electrode, of solid state membrane type, of which the
main component is silver sulfide.

A.3.4 Reference electrode, of double liquid junction type, having silver-silver chlo-
ride internal electrode, in which a potassium nitrate solution not containing chloride
ion is used for the internal liquid of outer tube.

A.3.5 Magnetic stirrer, as shown in 10.2.4.

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A.4 Sampling of sample gas and preparation of sample solution for analysis
The sampling of sample gas and preparation of sample solution 3) for analysis are
as follows.
a) Add 50 ml of absorbing solution in A.2.2.1 to each of the two absorbing bottles
shown in figure 3.
b) Before introducing the sample gas into the absorbing bottle, replace the air inside
the conduit tube with sample gas thoroughly using a bypass, etc.
c) The sampling amount of sample gas and the suction rate should be as shown in
table A.2.

Table A.2 Sampling amount of sample gas and suction rate

Concentration of hydrogen sulfide vol ppm Sampling amount L Suction rate L/min
Under 100 20 to 30 Approx.1
100 to 1 000 10 to 20 Approx.1

d) Measure the temperature and pressure at the same time as measurement of the
sample gas.
e) After suction of sampled gas is finished, wash the solution in the absorbing bottle
into a 200 ml volumetric flask by using absorbing solution, add the absorbing so-
lution to the mark and take it as the sample solution for analysis.
Note 3) Perform all of the procedures avoiding direct sunshine.

A.5 Titration procedure

The procedure of titration is as follows.
a) Take a portion of the sample solution of an amount calculated to be suitable in a
250 ml beaker based on the approximate value of the concentration of sample gas
measured by hydrogen sulfide detector beforehand and on the values in table A.2.
b) Dilute the ammonia solution (1+14) 20 times (0.05 mol/L), transfer 2.5 ml of this
solution to the beaker, and add water to make about 50 ml.
c) Immerse the silver ion selective electrode and the reference electrode in the bea-
ker, and connect these electrodes to a potentiometer. After the response poten-
tial has stabilized, drop 0.01 mollL silver nitrate methanol solution from a burette.
d) Read the response potential corresponding to the dropped amount and continue
this operation until it passes the end point of titration.
e) Obtain the amount (ml) of 0.01 mollL silver nitrate methanol solution consumed
up to the end point of titration.
f) For the blank test, take the same amount of absorbing solution as the aliquot of
sample solution for analysis taken in A.4 a) in a 250 ml beaker, perform the pro-
cedures of A.4 b) to e) and obtain the amount of 0.01 mollL silver nitrate metha-
nol solution (ml) consumed in the procedures as the blank test value.

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A.6 Drawing
The drawing is performed as follows, depending on the concentration of hydrogen
sulfide.
In addition, when a potentiometer with built-in function of A.6.l or A.6.2 is used,
the function may be utilized.

A.6.l In the case of 100 ppm or over (titration curve method)

a) For the sample solution and the blank test solution, plot the values of the added
amount (ax) of 0.01 mollL silver nitrate methanol solution on the abscissa and those
of the response potential (E) on the ordinate on the section paper to prepare a
titration curve.
b) Obtain the titration curve by drawing and take it as the amount (a and b) of
0.01 mollL silver nitrate methanol solution consumed in titration of the sample
solution and the blank test solution respectively.

A.6.2 In the case of under 100 ppm (Gran plotting method)

An example of drawing according to Gran plotting method is given in figure A.I.

'-~ 0
'-
a
Added amount of 0.01 mol/L silver nitrate
methanol solution ax (ml)

Figure A.l Example of Gran plotting method

The procedures of creating Gran plot are as follows.

--`,`,,,,`,``,````,``````,,,`,-`-`,,`,,`,`,,`---

a) Calculate 4) the added amount of 0.01 mollL silver nitrate methanol solution (ax)
and the corresponding response potential difference (V2 + ax) 10e/s (E).
Note 4) V2 is the aliquot amount of sample solution, S is the potential inclina-
tion of silver ion selective electrode and the difference between the
response potential (E 1) of 0.01 mollL silver nitrate methanol solution
consumed in the titration and the response potential (E 2 ) of the said
solution diluted 10 times. Usually it is 57 m V to 59 m V at 25°C.
b) Plot ax (ml) on the abscissa and (V2 + ax) 10e/s on the ordinate on the section paper,
and draw the straight line passing through each point.

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c) Take the point where the extension of this straight line intersects with the abscissa
as the end point of titration, and obtain the amount (a) of 0.01 mollL silver nitrate
methanol solution consumed in the titration. In this case, the blank test need not
be carried out.

A.7 Calculation of concentration of hydrogen sulfide

Calculate the volume concentration of hydrogen sulfide in the sample gas by the
following formulae, and round the result to two significant figures according to JIS Z
8401.

C = O.112x(a-b) xfxlOOO
v
Vs x r

where, Cv : volume concentration of hydrogen sulfide in sample

gas (vol ppm)
Cm : mass concentration of hydrogen sulfide in sample
gas (mg/m 3 )
0.112: volume of hydrogen sulfide corresponding to 1 ml
of 0.01 mollL silver nitrate methanol solution (ml)
1.521: mass concentration of 1 vol ppm of hydrogen sulfide
(mg/m 3 ), 34.086/22.41
a: amount of 0.01 mol/L silver nitrate methanol solu-
tion obtained in A.5 a) to e) (ml)
b: blank test value obtained in A.5 f) (ml)
Vs: sampling amount of sample gas under standard con-
ditions obtained in 6.3.2.5 (L)
r: aliquot ratio [ratio of the solution amount of aliquot
taken (ml) to the amount of sample solution for
analysis (ml)]
f: factor of 0.01 mollL silver nitrate methanol solution
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Annex B (informative)
Sulfur dioxide conversion ultraviolet ray
fluorescent method

B.I Summary
The summary of the sulfur dioxide conversion ultraviolet ray fluorescent method
is as shown in table B.1.

Table B.I Sulfur dioxide conversion ultraviolet ray fluorescent method

Determination method Sampling Determination NOTE

range al
The sample gas is sucked by The sample From 0 vol ppm This method, with which continuous
pump, and the hydrogen gas is sucked to 0.01 vol ppm, measurement is possible, can be
sulfide is made to pass through by pump and to 0 vol ppm to effectively applied for the continuous
oxidation catalyst. The sulfur introduced 10 vol ppm. automatic measurement of hydrogen
dioxide produced is measured into the sulfide in flue gas or the air. When
according to the ultraviolet ray detector. aromatic hydrocarbon is contained in
fluorescent method and the the sample gas, the same fluorescence
concentration of hydrogen as sulfur dioxide is radiated and a
sulfide is obtained by conver- positive interference is given to the
sion. measured values. Therefore, the

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concentration of hydrogen sulfide
should be determined after passing
through a scrubber for removing
aromatic hydrocarbon.

Note a) The range divided adequately according to the concentration of hydrogen sulfide in sample
gas. Dilution with air is permissible in the case of samples with high concentration.

B.2 Measurement principle

Ultraviolet rays are radiated to the sample gas in which the hydrogen sulfide has
been converted to sulfur dioxide with oxidation catalysis, and the fluorescence emit-
ted by the excited sulfur dioxide molecule which is generated by irradiation of ultra-
violet ray is detected. The concentration of sulfur dioxide in the sample gas is measured
from the intensity of the detected fluorescence and obtained by converting to the con-
centration of hydrogen sulfide.
The first stage of this reaction is generation of excited sulfur dioxide molecules (80 2 *)
by radiation of light (hVl) at a wavelength in the range 200 nm to 220 nm.
80 2 + hVl ~ 80 2 *
The second stage of the reaction mechanism is the generation of fluorescence (hV2)
at a wavelength in the range 240 nm to 420 nm when the excited sulfur dioxide mol-
ecule (80 2 *) returns to the ground state (80 2 ).
80 2 * ~ 802 + hV2
In this case, the intensity of fluorescence hV2 is proportional to the intensity of ex-
citation light and the number of sulfur dioxide molecules [concentration (80 2 )].

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B.3 Constitution of apparatus

An example of constitution of sulfur dioxide conversion ultraviolet ray fluorescence
measuring apparatus is shown in figure B.lo

Light source
part
I I
Sample ----+ Dust ~ Dehumidi- ----+ ----+ Oxidation r---+ f-- Fluorescence
introducing filter fication Scrubber catalyst f-- photometric
Fluorescence
opening unit part
room
Exhaust gas +--
Sample air
pump l
I I Indication
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Ie Comparison recorder
Pressure photometric
gauge part

Figure B.I Example of constitution of sulfur dioxide conversion

ultraviolet fluorescence measuring apparatus

The apparatus should be constituted as shown in the following example.

a) Sample introducing opening The opening is the part connected to the sample
introducing tube, and should be made of a material with minimum adsorption of
hydrogen sulfide, for example, fluoroethylene resin.
b) Dust filter The filter is for removing dust, which should be made of a material
with minimum adsorption of hydrogen sulfide, for example, fluoroethylene resin.
It should be exchanged regularly so that the sample suction flow rate is not re-
duced.
c) Dehumidification unit The unit is for dehumidifying or conditioning the sample
gas for reducing the influence due to moisture, and a transmitted membrane type
dehumidifier, or an electric cooler is used. When the influence due to moisture is
negligible, this unit is not necessary.
d) Scrubber 1) The scrubber is used for removing mainly the sulfur dioxide in sample
gas. When aromatic hydrocarbon is contained in the sample, a transmitted mem-
brane type, adsorption type or other type of scrubber is used together.
Note 1) If the influence is negligible, the scrubber is not necessary.
e) Oxidation catalyst The catalyst is for converting the hydrogen sulfide in sample
gas to sulfur dioxide. The catalyst is maintained at a definite temperature and
some catalysts are capable of monitoring the set temperature.
f) Fluorescence room The parts of the fluorescence room which are in contact with
the sample gas should be made of a material with minimum adsorption of sulfur
dioxide and minimum deterioration due to ultraviolet ray.
g) Light source part A lamp which irradiates ultraviolet rays by electric discharge,
etc. is used.

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h) Fluorescence photometric part The part receives fluorescence through an op-

tical filter which transmits only the florescence of sulfur dioxide, and converts the
fluorescence to an electric signal proportional to the intensity.
i) Comparison photometric part The part receives the excited light irradiated
from the light source part and converts it to an electric signal proportional to the
intensity.
j) Sample air pump The pump for suctioning the sample. In the sample line, a
needle valve or a capillary tube should be used for maintaining the suction flow
rate to be constant.
k) Pressure gauge The gauge is used for measuring the pressure in fluorescence
room.

B.4 Preliminary operation of measuring apparatus

B.4.1 Gas
The following gas is used.
a) Zero gas The zero gas to be used for calibration should not contain the sulfur

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dioxide and hydrogen sulfide of the concentration detectable by measuring instru-
ment. The concentration of oxygen in zero gas should be (20.9 ± 2.0) vol % as in
the usual composition in the air.
b) Span gas The span gas to be used for calibration should be the gas prepared by
methods equal to one or multiple preparation methods of 1.2 in Annex 3 of JIS B
7952, and should be packed in container or diluted to an adequate concentration
as required and should be oxygen-based. The concentration of oxygen in span gas
should be the same as that of the zero gas.
c) Other gas The gas to be used for the test should be the same as the span gas.

B.4.2 Calibration
For the calibration of the measuring apparatus, the following zero adjustment or
span adjustment is carried out.
a) Zero adjustment Introduce the zero gas at the set flow rate and after the indi-
cation has stabilized, carry out the zero adjustment on the apparatus.
b) Span adjustment Introduce the span gas at the set flow rate and after the in-
dication has stabilized, carry out span adjustment of apparatus.

B.4.3 Catalytic oxidation efficiency test

When the calibration is carried out by using the gas containing sulfur dioxide as
the span gas by not passing it through a scrubber, the oxidation efficiency of the hy-
drogen sulfide should be grasped beforehand. After the zero adjustment and the span
adjustment are carried out, introduce the gas for test (hydrogen sulfide), read the
indicated value of it and calculate the oxidation efficiency according to the following
formula.

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b
a =-xlOO
c
where, a: oxidation efficiency (%)
b: indicated value of the apparatus after the gas for
test is passed through the scrubber (vol ppm)
c: volume concentration of the gas for test (vol ppm)

B.4.4 Adsorption efficiency test

It is required to grasp the efficiency of scrubber to adsorb sulfur dioxide beforehand.
After the zero adjustment and the span adjustment are carried out, introduce the gas
for test (sulfur dioxide), read the indicated value of it and examine the adsorption
efficiency according to the following formula.

d = (1 - e / C v ) x 100

where, d: adsorption efficiency (%)

e: indicated value of the apparatus after the gas for
test is passed through the scrubber (vol ppm)
Cv : volume concentration of gas for test introduced
(vol ppm)

B.5 Measurement of sample gas

Sample the gas under the condition that the temperature of the apparatus and oxi-
dation catalyst have sufficiently stabilized 2).
Note 2) It should be at least 4 h after the measuring apparatus has been elec-
trified.

B.6 Reading of the measurement value

a) Read the value of the hydrogen sulfide concentration off the indication recorder.
Perform the oxygen efficiency correction if required 3).
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Note 3) For one method of correction, when oxygen efficiency obtained in B.4.3
is, for example, 98 %, the obtained data can be multiplied by 1/0.98, i.e.,
approximately 1.02 as a correction factor.
b) In the case of an apparatus liable to be influenced by temperature, the tempera-
ture correction should be performed.

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Annex C (informative)
Detecting tube method

C.l Applicable condition

The detecting tube method is the simplified method which is carried out for the pur-
pose of daily environmental control or screening by the business owner and the results

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obtained by it are not to be compared directly with the emission regulation values.
The detecting tube method is applied where the interference of coexisting gases is
negligible. Since the degree of the influence of other gas components coexisting in the
flue gas can differ depending on the reaction principle of the detecting tube, the speci-
fications, technical data, etc. of the detecting tube should be studied before applying
this method.

C.2 Summary of determination method

The summary of detecting tube method is as follows.

Table C.l Summary of detecting tube method

Determination method Sampling Determination NOTE

range
The method is based on the 50 ml to 300 ml, The range The graduation of concentration
princi pIe of the following two by the gas sampler between printed on the detecting tube, as
kinds of reactions. of vacuum method 1 vol ppm and the standard sampling amount,
Silver sulfide method: Silver for detecting tube. 2 000 vol ppm is typically 100 ml. When
sulfide is produced by reacting in volume ratio measurement is carried out by
with silver nitrate. is measured by other sampling amount than the
selecting from standard sampling amount, the
Lead sulfide method: Lead (II) several kinds of conversion of concentration
sulfide is produced by reacting detecting tubes. val ue should be in accordance
with lead (II) acetate. with the instruction manual.

C.3 Apparatus and instrument

The apparatus and instrument to be used for the detecting tube method are as fol-
lows.

C.3.l Detecting tube, for hydrogen sulfide use specified in 5.2 of JIS K 0804.

C.3.2 Gas sampler, of cylindrical type specified in 4.1 of JIS K 0804, and satisfy-
ing the requirements specified in 5.1 of JIS K 0804.

C.3.3 Gas sampling apparatus The gas sampling apparatus should be in accor-
dance with either of the following.
a) Sampling by gas sampling bag Use the gas sampling bag in 6.3.1.4 b) 1) as
the sampling apparatus and instrument for sample gas specified in 6.3, for sam-
pling the gas.

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b) Direct sampling For direct sampling, the apparatus used should be of the con-
stitution as exemplified in figure C.l. The suction flow rate 1) of sample gas in this
case should be 0.5 L/min to 1 L/min.
Note 1) Attention should be paid when the inside of the flue is under negative
pressure, since it may be impossible to pass the specified amount of
sample gas into the detecting tube, and the detecting tube may indi-
cate a lower value. During sampling by the detecting tube, it should
be constantly checked that the pointer or the counter of the wet gas
meter is rotating.

A Gas sampling tube

E
B Inserting opening for
detecting tube (silicone
rubber)
h C Detecting tube
D Gas sampler

0 E Thermometer
F Attaching opening for
~ detecting tube
G Piston
H Drying tube
D
L,I 2 Flow rate controlling
cock
J Suction pump
K Wet gas meter
L Tetrafl uoroethylene resin
tube a)
M Connection rubber tube
G (silicone rubber)
a) Example of sampling when the temperature of flue gas is high
(combustion flue gas, etc.)

b) Example of sampling for reaction flue gas, etc.

Note a) When the resin tube (L) of reaction flue gas is long, dead space can become a cause of
error. In this case, the measurement should be carried out after the inside of the resin
--`,`,,,,`,``,````,``````,,,`,-`-`,,`,,`,`,,`---

tube is sufficiently replaced.

Figure C.I Example of gas sampling apparatus

C.4 Measurement procedure

C.4.1 Preparation of measurement

The preparation of measurement is performed as follows.

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a) Measure the temperature at the measuring point and confirm that it is within the
service range indicated in the specification of the detecting tube.
b) Bring the temperature 2) of the detecting tube to be used to the temperature at the
measurement place. In this case, take care so as not to expose it to the direct
sunlight.
Note 2) When the detecting tube has been stored in a cool and dark place such
as in a refrigerator, allow it to rest until its temperature becomes equal
to the temperature of the outside air before use.
c) Carry out the leak test of gas sampler according to the instruction manual.

--`,`,,,,`,``,````,``````,,,`,-`-`,,`,,`,`,,`---
C.4.2 Measurement
The measurement is performed as follows.
a) Break off both ends of the detecting tube with a chip cutter or the like and con-
nect the sample gas inlet side of the tube to connection opening of the gas sam-
pling bag, if a gas sampling bag is used as a gas sampling container, to the
position B in the case of direct sampling in figure C.1 a), and to the connection
rubber tube (M) in the case of direct sampling in figure C.1 b), in such a way that
the sample air flows in the direction of the arrow mark printed on the surface of
the detecting tube.
b) Lock the shaft by pulling at a stretch the handle of the gas sampler and leave it
for the time specified for the detecting tube.
c) After the suction is finished, immediately detach the detecting tube and read the
graduation of concentration at the tip of the discolouration layer 3) 4).
Notes 3) In some detecting tubes, the discoloured colour can fade or the length
of discoloured layer can change with the elapse of time after the aera-
tion is finished, therefore, the discoloured layer should be marked at
its end immediately after completion of aeration, and the reading
performed.
4) When the tip surface of the discoloured layer is oblique, the interme-
diate point is read as the concentration value.
d) When the conversion of concentration unit is required, the following formula is used:

C=C/X~x 273.15 x p
22.41 (273.15+t) 101.32

where, C: mass concentration of hydrogen sulfide (mg/m 3 )

C': read value of detecting tube (vol ppm)
M: molecular weight (hydrogen sulfide 34.086)
t: temperature at measuring point (OC)
p: atmospheric pressure at measuring point (kPa)
101.32: standard atmospheric pressure (kPa)

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C.4.3 Examination of interfering substances

The principle behind discolouration of detecting tube, in most cases, is not a reac-
tion specific to the target substance but common to substances having similar chemi-
cal properties. When a substance which reacts similarly to the target substances are
coexistent, they cause the indication to be higher than the concentration of the target
substance (positive error), while, on the contrary, such coexisting substances can in-
terfere with the discolouration reaction and cause negative error, or blur the
discolouration boundary. For measurements, therefore, possible coexisting substances
should be previously examined and their influence should be studied by referring to
the specifications or technical data, etc. of the detecting tube.

C.5 Disposal of detecting tube

It is basically disposed as industrial waste, but since some can contain harmful ma-
terial, the instruction manual should be referred to for the proper disposal. In cases
where it is not clear in the manual, inquire the manufacturer.

Bibliography
JIS B 7952 Continuous analyzer for sulfur dioxide in ambient air
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JIS K 0055: 2002 General rules for calibration method of gas analyzer
JIS K 0804 Gas detector tube measurement system (Length-of-stain type)
JIS K 8085 Ammonia solution (Reagent)
JIS K 8548 Potassium nitrate (Reagent)
JIS K 8550 Silver nitrate (Reagent)
JIS K 8574 Potassium hydroxide (Reagent)
JIS K 8891 Methanol (Reagent)

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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:
Standards Publishing Department, Japanese Standards Association
4-1-24, Akasaka, Minato-ku, Tokyo, 107-8440 JAPAN
TEL. 03-3583-8002 FAX. 03-3583-0462

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