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1、STD-JIS K 0090-ENGL 3998 m 4933b08 0553804 Tb4 111 J IS JAPANESE INDUSTRIAL STANDARD Translated and Published by Japanese Standards Association JIS K 0090:1998 Method for determination of phosgene in flue gas ICs 13.040.40; 71.040.40 Descriptors : carbonyl chloride, exhaust gases, gas analysis, indu
2、strial air pollutants, industrial wastes, sampling methods, spectrophotometry, gas chromatography, determination of content Reference number : JIS K O090 : 1998 (E) 8s Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie
3、Not for Resale, 03/14/2007 08:23:04 MDTNo reproduction or networking permitted without license from IHS -,-,- STD*JIS K 0090-ENGL 3798 4933b08 0553805 9TO D K O090 : 1998 Foreword This translation has been made based on the original Japanese Industrial Standard revised by the Minister of Internation
4、al Trade and Industry through deliberations at Japanese Industrial Standards Committee in accordance with the Industrial Standardization Law: Date of Establishment: 1975-08-01 Date of Revision: 1998-03-20 . Date of Public Notice in Official Gazette: 1998-03-20 Investigated by: Japanese Industrial St
5、andards Committee Divisional Council on Environment Technical Committee on Air Quality JIS K 0090:1998, First English edition published i n 1998-10 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 t
6、he contents, the original TIS is to be the final authority. O JSA 1998 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
7、 from the publisher. Printed in Japan Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 08:23:04 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS K CIOSO-ENGL
8、 1778 H 4733b08 055180b 837 = JAPANESE INDUSTRIAL STANDARD JIS K O090 : 1998 Method for determination of phosgene in flue gas 1 phosgene (carbonyl chloride) in flue gas. Scope This Japanese Industrial Standard specifies the method for determination of 1 Remarks 1 In this Standard, flue gas means one
9、s which is generated by being accom- panied with manufacturing processes of various chemical products, combus- tion, other chemical reactions and manufacturing process using phosgene, etc., and exhausted to flue, chimney or duct. The normative references are shown in Attached Table 1. 2 2 Common ite
10、ms The common items of chemical analysis, sampling methods of flue gas and molecular absorptiometric analysis shall be in accordance with JIS K 0050, JIS K 0095 and JIS K 0115, respectively. 3 methods and their outlines shall be as shown in Table 1. Classification of analytical methods and their out
11、lines Classification of analytical Table 1 Classification of analytical methods and their outlines Classification of analytical method Outlines of analytical method Summary Sampling I I Diphenylurea ultraviolet - . absorptiometry After absorbing phosgene in the sample gas into absorbent, gen- erated
12、 diphenylurea is extracted by solvent and the absorbance (257 nm in wavelength) of this extracted solution is measured. Absorption bottle met hod Absorbent : Aniline solution (2.5 gll, pH 7 to pH 9) Absorption volume : 10 mlx 1 vol ppm dance with I 4 Sampling method of sample gas Sampling position o
13、f gas for analysis shall be selected the point where the typical gas can be collected and, after collected at least twice in the same position within adjacent time, and these gases shall be analyzed respectively. 4.1 Sampling method Absorption bottle method 4.2 Reagents and preparation method of rea
14、gent solution (1) Reagents (a) Water A2 grade specified in JIS K 0557. (b) Hydrochloric acid Specified in JIS K 8180. (c) Sodium hydroxide Specified in JIS K 8576. (d) Aniline Specified in JIS K 8042. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employe
15、es/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 08:23:04 MDTNo reproduction or networking permitted without license from IHS -,-,- STD=JIS K 0070-ENGL 1998 4933b08 0553807 773 M 2 K O090 : 1998 (2) Preparation method of reagent solution (absorbent) Dissolve 25g of aniline in hydrochloric
16、 acid (1 mol/Z) to dilute to 1 1, Take 100 ml of this solution at the time of use and add sodium hydroxide (1 mol/Z) to adjust pH 7 to pH 9 and dilute it to 1 1. 4.3 Apparatus and device (1) Absorption bottle Only one absorption bottle which has 40 ml to 50 ml in volume and is shown in Fig. 1 as an
17、example shall be used. t Remarks: This absorption bottle shall be as the same as that of Fig. 3 (d) in JIS K 0095 or equivalent to the example. Though the absorption bottle may be attached with nozzle Fig. 3 (b), inside diameter of nozzle in this case shall be 1 mm and connected 2 nozzles in series.
18、 Inner Fig. 1 An example of absorption bottle (2) Gas sampling apparatus The apparatus shall be constructed as shown in Fig. 2 for example and provided with the following conditions. This apparatus is the construction of Fig. 2 (a) in JIS K 0095 absorption bottle method (in case of measuring the vol
19、ume of sample gas by gas meter). (a) Gas sampling apparatus shall be made of such materials that are not corroded by Co-existing components in flue gas. For example, glass, stainless steel, quartz glass and fluoride resin shall be used. (b) In order to prevent against mixing dust into sample gas, fi
20、lter medium without alkali shall be inserted into a suitable place of gas sampling apparatus ( ). Note () As phosgene has tendency to decompose easily at high temperature, heating shall be avoided stubbornly and, in an unavoidable case such as much condensation of water, the heating temperature shal
21、l be 100 “C or lower. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 08:23:04 MDTNo reproduction or networking permitted without license from IHS -,-,- 1 Gas 3 K O090 : 1998 By pass A : Ga
22、s sampling tube F : Trap (filling up glass wool) B : Filter medium G : Flow rate adjusting cock C : Three way stopcock H : Closed type suction pump (1 to 5 Umin) D : Absorption bottle I : Wet type gas meter (1 to 5 Uper revolution) J :Heater K : Thermometer L : Pressure gauge Washing bottle put in 5
23、0 ml of sodium hydroxide solution (200 g/Z) Fig. 2 An example of gas sampling apparatus Sampling gas The method of sampling gas shall be as follows. Put 10 ml of absorbent into absorption bottle (*). Note () In case of absorption bottle having larger inside diameter than that of Fig. 1, the distance
24、 of absorbent level in still from glass wool filter shall be more than 3 cm. In case of the distance smaller than 3 cm, add absorbent to maintain this level. in case of using absorption bottle with nozzle, the distance of nozzle from absorbent level in still condition shall be more than 6cm. In case
25、 of the distance lower than 6 cm, add absorbent to maintain this level. Place the gas sampling apparatus at a position as near the sampling position as possible. Prior to introducing gas into absorption bottle, substitute sufficiently with sample gas in the piping. Keep the flow rate of sample gas n
26、ot exceeding 0.7 Zlmin, and take 20 Z of the sampling volume, and increase or decrease this volume according to the concentration of phos- gene in sample gas. At the same time as the measurement of sample gas volume, measure the temperature and pressure of gas in flow meter. 5 Determination of phosg
27、ene 5.1 In case of coexisting with acidic gas such as chlorine and nitrogen dioxide, as the results of analysis are affected positively, this method shall be applied when these effects can be ignored or eliminated. Applicable requirements Copyright Japanese Standards Association Provided by IHS unde
28、r license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 08:23:04 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS K 0070-ENGL 1978 4733b08 0553809 54b I 4 K 0090 : 1998 5.2 Reagents and preparation of reagent solution (1) Rea
29、gents (a) Sulfuric acid Specified in JIS K 8951. (b) Hexane Specified in JIS K 8848. (c) 1-penthanol (d) Methanol Specified in JIS K 8891. (e) 1,3-diphenyIurea (melting point at 238 O C to 239 O C ) (2) Preparation of reagent solution (a) Sulfuric acid (1+4) Prepared with sulfuric acid. (b) Extracti
30、ng solvent Mix hexane and 1-penthano1 in each equal volume. (c) Stock solution for 1, 3-diphenylurea working curve Dissolve 94.9mg of 1, 3-diphenylurea into methanol, put it in a 100 ml volumetric flask and dilute to 100 ml with methanol. Solution for 1, 3-diphenylurea working curve Put 1 ml of stoc
31、k solution for 1, 3-diphenylurea working curve into a volumetric flask and dilute to 100 ml with water. 1 ml of this solution corresponds to 1 pl of phosgene (O O C , 101.32 kPa). (d) 5.3 Preparation of sample solution for determination After finishing the operation of 4.4, transfer all volume of ab
32、sorbent in absorption bottle to a separatory funnel of 100ml. Wash absorption bottle with approx. 20ml of absorbent thoroughly and combine the wash- ings into the separatory funnel and take it as the sample solution for determination (3). Note ( 3 ) In case of using two absorption bottles, carry out
33、 the same operation for the two bottles and combine these solutions in the same bottle to use as the sample solution for determination. 5.4 Apparatus and device (1) S,pectrophotometer (2) Absorption cell (made of quartz glass) 5.5 Operation (1) Add 5 ml of sulfuric acid (1+4) and extracting solvent
34、into sample solution and mix this solution by shaking thoroughly. (2) After allowing to stand, transfer the solvent layer into a volumetric flask of 25 ml. (3) Add 10 ml of extracting solvent to water layer again and mix it by shaking thoroughly. (4) After allowing to stand, transfer the solvent lay
35、er into the above volumetric flask of 25 ml. (5) Add extracting solvent up to the marked line. 7 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 08:23:04 MDTNo reproduction or networking pe
36、rmitted without license from IHS -,-,- 5 K 0090 : 1998 Take 40 ml of absorbent to a separatory funnel of 100 ml and carry out the operation of (1) to (5) to use as the solution for blank test. Take sample solution for determination of (5) and solution for blank test of (6) into absorption cells resp
37、ectively. Measure and record absorption spectra in the range of 210 nm to 300 nm with spectrophotometer, in contrast to the blank test solution. The example is shown in Fig. 3. Connect points A and B indicating the minimum absorbance in Fig. 3 and take it as an base line. Draw down a vertical line f
38、rom point P indicating maximum absorbance, take the intersecting point with base line AB as point C and obtain the absorbance PC. Obtain the concentration of phosgene with the working curve prepared preliminarily. P Absorbance I I I I I l I l l I I I t LA A - - C I- I I I - I I, 23 O 250 270 210 Wav
39、elength (nm) Fig. 3 An example of ultraviolet absorption spectrum Preparation of working curve Take solution for 1, 3-diphenylurea working curve O 5m1, 10m1, 20ml into respective separatory funnels of 100ml and add absorbent to make 40 ml. Concerning this solution, perform the operation of 4.4 (1) t
40、o (9) and prepare the relation curve between the concentration of phosgene ( I/ml) and absorbance. 5.7 ing to the following formula, and rounded to 2 digits of significant figures. Calculation The concentration of phosgene in sample gas shall be calculated accord- where Ch : Concentration of phosgen
41、e in flue gas (vol ppm) A : Concentration of phosgene in sample solution for determination Vs: Collected volume of gas obtained in 5.1.7 of JIS K 0095 obtained from working curve ( l/ml) (collected volume of gas) (1) 6 Record of analytical results 6.1 Items for record Items to be recorded shall be a
42、s follows. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 08:23:04 MDTNo reproduction or networking permitted without license from IHS -,-,- 6 K 0090 : 1998 (i) Analytical value (2) Classi
43、fication of analytical method (3) Sampling date and time for sample gas (4) Other items for requirement to be recorded 6.2 Determination method for analytical value of flue gas Determination shall be performed twice for the same sample solution in each sampling, calculated the average value and roun
44、ded it to 2 digits of significant figures. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 08:23:04 MDTNo reproduction or networking permitted without license from IHS -,-,- 7 K O090 : 1998
45、 Informative reference This Informative reference is supplemented to the specified items of the text according to the form of this standard and is not a part of the provision. Informative reference Table 1 Classification of informative methods and outlines classification Outlines of analytical metho
46、d of analytcial method Summary High speed liquid chro- matography After absorbing into absor- bent, determine the gener- ated diphenylurea by high speed liquid chromatography (UV detector) Detective tube method Determine the length of red coloring layer in the detec- tive tube, generated by the reac
47、tion of 4-paranitroben- zylpyridine with benzyla- niline Sampling Absorption bottle method Absorbent : Aniline solution (2.5 gll, pH 7 to PH 9) Absorption volume: 10 ml X 1 Suck by gas sampler for detec- tive tube (vacuum method, 0.1 I ) Range of determination vol ppm 0.05 to 7 (10 1) 0.5 to 20 (0.1
48、 ij O. 1 to 4 (0.5 1) Applicable condition In case of inter- ferencial effect by coexisting gas In case of pos- sible ignoring in- terference by hydrogen chlo- ride, chlorine and nitrogen dioxide Informative . . reference 1 High performance liquid chromatography Refer to JIS K 0124 General rules for high performance liquid chromatographic analysis. Determination shall be carried out in accordance with absolute working curve method. 1.1 Sampling of gas 1.1.1 Reagents and preparation of reagent solution (1) Reagents