JIS-K-0303-2004-ENG.pdf

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1、J IS JAPANESE I N D USTR IAL STANDARD Translated and Published by Japanese Standards Association Methods for determination of formaldehyde in flue gas ICs 13.040.40; 71.040.40 Reference number : JIS K 0303 : 2004 (E) PROTECTED BY COPYRIGHT 22 s Copyright Japanese Standards Association Provided by IH

2、S under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 00:51:45 MDTNo reproduction or networking permitted without license from IHS -,-,- K 0303 : 2004 Foreword This translation has been made based on the original Japanese Industrial Standard revised

3、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 dra

4、ft 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 0303 : 1993 is replaced with this Standard. Attention is drawn to the possibility that some parts of this Stand

5、ard 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

6、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. Date of Establishment: 1993-04-01 Date of Revision: 2004-01-2

7、0 Date of Public Notice in Official Gazette: 2004-01-20 Investigated by: Japanese Industrial Standards Committee Standards Board Technical Committee on Environment and Recycling Policy JIS K 0303 : 2004, First English edition published in 2004-09 Translated and published by: Japanese Standards Assoc

8、iation 4-1-24, Akasaka, Minato-ku, Tokyo, 107-8440 JAPAN In the event of any doubts arising as to the contents, the original TIS is to be the final authority. O JSA 2004 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any m

9、eans, electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. Printed in Japan PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for

10、Resale, 03/13/2007 00:51:45 MDTNo reproduction or networking permitted without license from IHS -,-,- K 0303 : 2004 1 2 3 4 5 5.1 5.2 5.3 5.4 6 6.1 6.2 6.3 6.4 6.5 6.6 7 Contents Page Scope Normative references Common matters Classification of analytical methods and outline Taking method of sample g

11、as Case of 4.amino.3.hydrazino.5.mercapto.1,2, 4.triazol absorptiometry Case of 2, 4.dinitrophenylhydrazine collection-gas chromatography (collection in absorption bottle) and 2, 4.dinitrophenylhydrazine collection-high performance liquid chromatography (collection in Case of 2, 4.dinitrophenylhydra

12、zine collection-gas chromatography (collection in cartridge) and 2, 4.dinitrophenylhydrazine collection- high performance liquid chromatography (collection in cartridge) absorption bottle) . Gas sampling volume Method of determination 4-amino-3-hydrazino-5-mercapto-1,2, 4-triazol absorptiometry (AHM

13、T absorptiometry) 2, 4-dinitrophenylhydrazine collection-gas chromatography (collection in absorption bottle DNPH-GC method) 2, 4-dinitrophenylhydrazine collection-gas chromatography (cartridge collection DNPH-G method) . 2, 4-dinitrophenylhydrazine collection-high performance liquid chromatography

14、(collection in absorption bottle HPLC method) 2, 4-dinitrophenylhydrazine collection-high performance liquid chromatography (collection in cartridge DNPH-HPLC method) . 4-amino-3-hydrazino-5-mercapto-l,2, 4-triazol absorption-automated analysis (AHMT automated analysis method) . Rounding off of anal

15、ysis value . Attached Table 1 Normative references Attached Table 2 Saturated stream pressure . Annex (normative) 4.5.dihydroxy.2. 7.naphthalene disulfonic acid absorptiometry (chromotropic acid absorptiometry) 1 1 1 1 3 3 7 8 10 11 11 14 21 23 25 26 31 32 33 35 PROTECTED BY COPYRIGHT Copyright Japa

16、nese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 00:51:45 MDTNo reproduction or networking permitted without license from IHS -,-,- JAPANESE INDUSTRIAL STANDARD JIS K 0303 : 2004 Methods for determination

17、 of formaldehyde in flue gas 1 Scope This Japanese Industrial Standard specifies the methods of analyzing formaldehyde in flue gas. In this Standard, the flue gas means the gas exhausted in a flue, chimney, or duct (hereafter referred to as “duct”) in cases where such process is carried out as manuf

18、acturing of resin or the like, burning of methanol, other chemical reactions or the working process using or generating formaldehyde, or the gas exhausted to the exhaust pipe or the like of internal combustion engine. 2 Normative references Standards listed in attached table 1 contain provisions whi

19、ch, through reference in this Standard, constitute provisions of this Standard. The most recent editions of the standards (including amendments) shall be applied. 3 Common matters The common matters shall be as follows: General rule in accordance with JIS K 0050. Definitions 0211 or JIS K 0215 apply

20、. Sampling of flue gas The general matters in common to sampling of flue gas shall be in accordance with JIS K 0095. The general matters in common to chemical analysis shall be For the purposes of this Standard, the definitions given in JIS K Reagents and water The general matters in common to reage

21、nts and water shall be accordance with JIS K 8005 and JIS K 0557. Absorptiometry The general matters in common to absorptiometry shall be in accordance with JIS K 0115. Gas chromatography phy shall be in accordance with JIS K 0114. High performance liquid chromatography The general matters in common

22、 to high performance liquid chromatography shall be in accordance with JIS K 0124. The general matters in common to gas chromatogra- 4 Classification of analytical methods and outline lytical methods and outline shall be in accordance with table l. The classification of ana- PROTECTED BY COPYRIGHT C

23、opyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 00:51:45 MDTNo reproduction or networking permitted without license from IHS -,-,- 2 K 0303 : 2004 Table 1 Classification of analytical method

24、s and outline Classification of analytical methods (Abbreviation) Outline of analytical method Matters that require attention on appli- cation Summary Sampling Range of determina- tion (I) vol ppm (mg/m3) 4-amino-3-hydrazino- 5-mercapto-1,2,4- triazol absorptiometry :AHMT absorptiometryj After colle

25、cting formaldehyde in sample gas into boric acid solution, alkalize it, add AHMT to colour it and mea- sure its absorbance. Collection in absorp- tion bottle Absorption solution: boric acid solution (5 g/L) Absorption volume: 40 ml x 2 bottles Standard sampling volume: 2 L to 20 L 0.4 to 75 (0.5 to

26、100) According to 6.1.1 After collecting formaldehyde in sample gas into DNPH solution, extract it by chloro- form or the like, and sepa- rate to determine it by gas chromatograph. Collection in absorp- tion bottle Absorption solution: DNPH hydrochloric acid solution (2 g/L) Absorption volume: 40 ml

27、 Standard sampling volume: 2 L to 10 L 0.4 to 56 (0.5 to 75) According to 6.2.1 2,4-dinitrophenyl- hydrazine collection- :as chromatography 1DNPH-GC method) After collecting formaldehyde in sample gas in the cartridge packed with collector impreg- nated with DNPH solution, elute with acetonitrile, a

28、nd then dissolve it again by chloroform and separate to determine it by gas chromato- graph. Collection in car- tridge Standard sampling volume: 2 L to 10 L 0.4 to 45 (0.5 to 60) According to 6 . 3 . 1 2,4-dinitrophenyl- aydrazine collection- nigh performance liquid chromatography :DNPH-HPLC method)

29、 After collecting formaldehyde in sample gas in DNPH solu- tion, extract it by chloroform and the like, dissolve it again in acetonitrile and separate to determine it by high per- formance liquid chromato- graph. Collection in absorp- tion bottle Absorption solution: DNPH hydrochloric acid solution

30、(2 g/Lj Absorption volume: 40 ml Standard sampling volume: 2 L to 10 L 0.2 to 56 (0.3 to 75) According to 6 . 2 . 1 Collection in car- tridge Standard sampling volume: 2 L to 10 L 0.2 to 45 (0.3 to 60) According to 6.5.1 After collecting formaldehyde in sample gas in the cartridge packed with collec

31、tor impreg- nated with DNPH solution, elute with acetonitrile and separate to determine it by high performance liquid chromatograph. PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resa

32、le, 03/13/2007 00:51:45 MDTNo reproduction or networking permitted without license from IHS -,-,- 3 K 0303 : 2004 Table 1 (concluded) Classification of analytical methods (Abbreviation) 4-amino-3-hydrazino- 5-mercapto-i ,2,4-triazol absorption-automated analysis method (AHMT automated analysis metho

33、d) Outline of analytical method Range of determina- tion() vol ppm (mg/m3) - Carry out periodically the automatic analysis of formal- dehyde in sample gas with using the automatic measur- ing apparatus of AHMT absorptiometry . Collection in absorp- tion bottle Absorption solution: potassium hydrox-

34、ide solution (0.12 mol/L) 40 ml Absorption volume: Standard sampling volume: 25 L o to 20 (O to 27) Matters that require attention on appli- cation According to 6.6.1 Note (1) The range of determination is the value given when, in case of absorptiometry, sample gas is taken by 20 L for low concentra

35、tion side and by 2 L for high concen- tration side, and in the case of gas chromatography and high performance liquid chromatography, sample gas is taken by 10 L for low concentration side and by 2 L for high concentration side individually. Moreover, the value in AHMT automated analysis shall be th

36、e one indicating Remarks 1 There is the detecting tube method for the simplified measuring method of form- aldehyde concentration in flue gas. The sample gas of approximately 100 ml is sucked in a detecting tube, reacted with the reagent in the tube and the form- aldehyde concentration is obtained f

37、rom the coloured length of reagent. The range of determination varies depending on the type of tube and the sucked volume, and 20 vol pprn to 1 500 vol ppm when 100 ml is sucked. When the moisture in flue gas is condensed, formaldehyde is dissolved in the condensed water and it gives a negative erro

38、r, and the existence of other aldehydes in flue gas gives a positive error. It is usable for setting up a standard of formalde- hyde concentration or the self-control of concentration. In addition to the methods in table 1, this Standard specifies 4,5-dihydroxy-2,7- naphthalene disulfonic acid absor

39、ptiometry (chromotropic acid absorptiometry) in annex (normative). 3 The vol ppm and mg/m3 as shown in this Standard mean the volume concen- tration and mass concentration under the standard condition (O “C, 101.325 kPa). range. 2 5 Taking method of sample gas 5 . 1 Case of 4-amino-3-hydrazino-5-mer

40、capto-1,2,4-triazol absorptiometry 5 . 1 . 1 Taking of sample gas The taking position of sample gas to be used for analy- sis shall be the point where the representative gas can be taken, and the sample gas shall be taken usually at least 2 times, which are in adjacent interval of time, at the same

41、taking position, and they shall be used for analysis respectively. PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 00:51:45 MDTNo reproduction or networking permitted

42、 without license from IHS -,-,- 4 K 0303 : 2004 5.1.2 Reagents and preparation of reagent solution 5.1.2.1 Reagents The reagents shall be as follows: a) b) 5.1.2.2 Preparation of reagent solution a) Absorption solution (5 gH3BOJL) 1 L in total. Prepare this solution when used. Water, class A2 specif

43、ied in JIS K 0557. Boric acid, specified in JIS K 8863. Dissolve 5 g of boric acid in water to make 5.1.3 Apparatus 5.1.3.1 in capacity) as shown in figure 1 shall be used with connecting two bottles. 5.1.3.2 Apparatus for sampling gas The apparatus shall be constructed as shown in figure 2 and be p

44、rovided with the following requirements. Absorption bottle For the absorption bottle, the absorption bottle (100 ml For the gas sampling tube (BI, glass tube, quartz glass tube, polytetrafluoro- ethylene tube and the like, which is not attached by or does not absorb such corrosive gas as formaldehyd

45、e, etc. in flue gas. For the purpose of preventing the sample gas from being mingled with dust, etc., stuff with suitable media(2) at the top of the gas sampling tube or an ad- equate position. For the purpose of preventing the moisture in the sample gas from condensa- tion, the portion between the

46、gas sampling tube and the stop cock (Pl) shall be constructed to be heated(3). For the connecting part between those, a ground joint tube, silicone rubber tube or polytetrafluoroethylene tube and the like shall be used. The apparatus shall be assembled so as not to generate gas leakage at the con- n

47、ecting of each part in it. Notes (2) The material in quality, which does not produce the chemical reac- tion with the component in flue gas, for example, silica wool or non- alkali glass wool shall be used. The piping shall be as short as possible, and when the moisture is possibly condensed, the po

48、rtion between the gas sampling tube (BI and the stop cock (Pl) shall be heated at 100 O C to 110 OC. (3) PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 00:51:45 MDTNo reproduction or networking permitted without license from IHS -,-,- 5 K 0303 : 2004 Unit: mm Outside diameter d 40 Glass ball filter lass filter Glass ball filter: maximum pore diameter 40 pm to 120 pm (No. 1 to No. 2) Glass filter: maximum pore diameter 60 pm Figur

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