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1、STD-JIS K 0087-ENGL 1798 W 4733b08 0558033 949 JAPANESE INDUSTRIAL STANDARD JIS KOO87: 1998 Methods for determination of pyridine in flue gas October, 1999 ERRATA Page 6, line 13 Error 5.1.2 Correct 5.1.3 Page 6 In Remarks of 5.1.5, the phrase “and 10 ml of water” is eliminated. Page 7 In 5.1.6, the
2、 formula and definition of “A” is replaced as follows: Error C= 50/25 XA/ 71.040.40 Descriptors : pyridine, exhaust gases, gas analysis, industrial air pollutants, industrial wastes, sampling methods, spectrophotometry, gas chromatography, determination of content Reference number : JIS K 0087 : 199
3、8 (E) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 02:25:53 MSTNo reproduction or networking permitted without license from IHS -,-,- K 0087 : 1998 Foreword This translation has been made
4、based on the original Japanese Industrial Standard revised by the Minister of International Trade and Industry through deliberations at Japanese Industrial Standards Committee in accordance with the Industrial Standardization Law: Date of Establishment: 1975-10-01 Date of Revision: 1998-03-20 Date o
5、f Public Notice in Official Gazette: 1998-03-20 Investigated by: Japanese Industrial Standards Committee Divisional Council on Environment Technical Committee on Air Quality I JIS K 0087:1998, First English edition published in 1998-10 Translated and published by: Japanese Standards Association 4-1-
6、24, Akasaka, Minato-ku, Tokyo, 107-8440 JAPAN .L T In the event of any doubts arising as to the contents, the original JIS 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,
7、electronic or mechanical, including photocopying and microfilm, without permission in writing from the publisher. Printed in Japan Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 02:25:53 MST
8、No reproduction or networking permitted without license from IHS -,-,- JAPANESE INDUSTRIAL STANDARD JIS K 0087 : 1998 Methods for determination of pyridine i n flue gas 1 Scope This Japanese Industrial Standard specifies the methods for determination of pyridine in flue gas. L L Remarks 1 In this St
9、andard, flue gas means ones which are generated by being ac- companied with the manufacturing process of various kinds of chemi- cals, combustion, other chemical reaction, production process dealt with pyridines and exhausted out to flue, chimney or duct. 2 The normative references to this Standard
10、are shown in Attached Ta- ble l. 2 Common items The common items concerned with chemical analysis, sampling method of flue gas, molecular absorptiometric analysis and gas chromatograph shall be in accordance with JIS K 0050, JIS K 0095, JIS K 0115 and JIS K 0114 respectively. 3 methods and their out
11、line shall be as follows. Classification of analytical methods and their outlines Classification of analytical Table 1 Classification of analytical methods and their outlines Classification of analytical meth- ods Diaminostilbene - disulfonic acid absorptiometry Gas chromatogra- PhY Outline of Summa
12、ry After absorbing pyridine in flue gas into diluted sulfuric acid, add 4,4-diaminostilbene- -2, 2-disulfonic acid solution and cyanogen bromide solu- tion to colour development. Measure its absorbance at 490 nm in wavelength and deter- mine the pyridine. Absorb pyridine in flue gas which was collec
13、ted in a collec- tion bottle into sulfuric acid solution. After extracting it in carbon disulphide, determine the pyridine by the chromato- gram obtained with gas chro- matograph provided with a hydrogen flame ionization detector. ialytical method Sampling Absorption bottle method Absorbent : 0.01 m
14、ol/ 1 Sulfuric acid so- lution 20 ml X 2 Vacuum flask method Absorbent : 0.01 moU Sulfuric acid so- lution 50 ml Range of deter- mination volppm 0.1 to For 20 1 of sample gas ( 1 ) I 0.6 to For 1 1 of sample gas( 2 ) Applica- tion re- quirement According to 6 . 1 . 1 Notes () It is the case of the s
15、ample solution in which 10 I to 20 E of sample gas is collected and the absorbent is diluted to 200 ml. It is the case of the sample solution in which 1 1 of sample gas is collect- (2) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, U
16、ser=Japan, IHS Not for Resale, 02/16/2008 02:25:53 MSTNo reproduction or networking permitted without license from IHS -,-,- ed in a vacuum flask and extract into 1 ml of carbon disulfide. 4 Sampling method of gas Sampling method of gas shall be in accordance with methods of absorption bottle and va
17、cuum flask. Sampling position of gas for analysis shall be selected the point where the typical gas is collected and, after collected at least two times in a same position within adjacent time , these gases shall be analyzed re- spectively. A 4.1 try. Method with absorption bottle This method shall
18、be applied for the absorptiome- 4.1.1 Reagents and preparation of reagent solution (1) Reagents (a) Water A2 grade specified in JIS K 0557. (b) Sulfuric acid SpeciFied in JIS K 8951. (2) Preparation of reagent solution (absorbent) (a) Absorbent : Sulfuric acid (Approx. 0.01 moVl) Dilute 1 g of sulfu
19、ric acid to 1 1 with water. 4.1.2 Device and apparatus Device and apparatus shall be as follows: (1) Absorption bottle Connected two absorption bottles which have 100 ml in each volume as an example shown in Fig. 3 (a) ( an example of absorption bottle ) of JI$ K 0095 shall be used. (2) Sampling app
20、aratus The apparatus shall be constructed as shown in Fig. 1 and provided with the following requirements. (a) The sampling tube shall be made of such material which are not reacted chemi- cally with pyridine, not adsorbed it in flue gas and have a greater heat-resistance for the temperature of flue
21、 gas. For example, glass tube, quartz tube, stainless steel tube and fluoride resin tube, etc. shall be used. (b) In order to prevent against mixing-in of dust in flue gas, appropriate fdter medium such as silica wool, etc. shall be put into the end part of gas sampling tube. (e) For connecting part
22、 .between the sampling tube and absorption bottle, glass grinding tube, silicon rubber tube shall be used. d I Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 02:25:53 MSTNo reproduction or n
23、etworking permitted without license from IHS -,-,- STD-JIS K 0087-ENGL 1778 4933b08 0553783 b37 E 3 K 0087 : 1998 A : Filter medium N : Thermometer B : Sampling tube O : Desiccant (Silica gel) C : Insulated material P, : Flow-rate adjusting cock D : Fluorine-containing rubber tube J : Gas washing bo
24、ttle P, : Flow-rate adjusting cock E : Thermometer F : Heater G : Spherical ground joint H, : No.1 absorption bottle H,: No.2 absorption bottle I : Glass filter K : Silicone rubber tube L : Suction pump M : Gas meter Q : Manometer R, : Passage change cock R, : Passage change cock 7 Fig. 1 Sampling a
25、pparatus of gas with absorption bottle (an example) 4 . 1 . 3 Procedure of gas sampling The sampling of gas shall be carried out according to the following procedures. The symbols of the apparatus shown in the following sen- tences shall be in accordance with ones shown in Fig. 1. (1) Take 20 ml of
26、the absorption solutions into each absorption bottle (HI. H2) sepa- rately. (2) After turning the passage change cock (R, R,) to the side of bypass, start the suction pump (L) and substitute air in the piping (between B and R,) with sample gas. (3) After stopping the suction pump (L), turn the passa
27、ge change cock (RI, R,) to the side of absorption bottles (HI, H,) read off the indication (V,) of gas meter (M) 0.01 1 (li- ter) orders of magnitude. (4) Start the suction pump (L) and pass the sample gas into absorption bottles (HI, H,). Adjust the flow rate to approx. 0.1 2 Imin with the flow-rat
28、e adjusting cock (P, P, ) and take approx. 10 1 of the sample gas. Stop the suction pump (L), close the passage change cock (R, R,) and read off the indication (V,) of gas meter (M) 0.01 1 orders of magnitude. At the same time, re- cord indication value of thermometer (N), and manometer (&). Atmosph
29、eric pres- sure shall be also measured. (5) According to necessity, measure the moisture in the sample gas according to 6 of JIS Z 8808. (6) Calculation sampling volumes of the gas A volume of dry gas (V, ) or a volume of Copyright Japanese Standards Association Provided by IHS under license with JS
30、ALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 02:25:53 MSTNo reproduction or networking permitted without license from IHS -,-,- 4 K 0087 : 1998 wet gas (Vsw) in the normal state (O ?c, 101.32 kPa) shall be calculated in accor- dance with 5 . 1 . 7 in JIS K 0095. 4 .
31、 2 Vacuum flask method This method shall be applied to the gas chromatograph. 4 . 2 . 1 Reagents (1) Reagents (a) Water A2 grade specified in JIS K 0557. (b) Phosphoric acid Specified in JIS K 9005. (c) Acetone Specified in J I S K 8034. 4 . 2 . 2 Device and apparatus The apparatus and device shall
32、be as follows: Bottle which has 1 Z of volumes as shown in Fig. 4 (b - 2) of JIS K 0095 and its in- ternal capacity (VsD) has measured by weight of water filled it in accordance with JIS K 0095 (3) (4) shall be used. Notes (3) The vacuum flask shown in Fig. 2 shall be taken care that the grease does
33、 not put into it at the time of use. (4) The inside of vacuum collecting bottle shall be washed with 0.01 mol/Z phosphoric acid- acetone solution and dried previously. Sampling apparatus The apparatus shall be constructed as shown in Fig. 2 and provided with the requirements shown in 4 . 1 . 2 (2) (
34、a) to (c). F A : Gas sampling tube B : Insulated material C : Filter medium D :Heater E : Gas collecting bottle with silicone rubber stopper F : Mercury switching manometer G : Empty bottle (for prevention of back flow) H : Gas washing bottle (contained diluted sulfuric acid) I : Dryingtube J : Vacu
35、um pump Q, R : Three way stopcock SI, S, S3 : Silicone rubber tube F i g . 2 Sampling apparatus of gas with a vacuum flask (an example) t Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 02:25
36、:53 MSTNo reproduction or networking permitted without license from IHS -,-,- , STD*JIS K 0087-ENGL 1998 W 4933b08 0551783 4UT 5 K 0087 : 1998 4.2.3 Procedure of gas sampling The sampling of gas shall be in accordance with 5.4.5 of JIS K 0095. (1) Calculation of sampling gas volumes A volume of dry
37、gas (V, ) or a volume of wet gas (V,) in the normal state (O “c, 101.32 kPa) shall be calculated in accordance with 5.4.6 in JIS K 0095. 5 Procedures of determination 5.1 Diaminostilbene-disulfonic acid spectrophotometric method 5.1.1 Application requirement This method shall be applied to the gas i
38、n which (Y - picoline is not more than the same concentration as pyridine and 1 3 -picoline is not more than -!- of the pyridine concentration. 10 1 5.1.2 Reagents and preparation of reagent solution (1) Reagents (a) Water A2 grade specified in JIS K 0557. (b) Hydrochloric acid Specified in JIS K 81
39、80. (c) Sulfuric acid Specified in JIS K 8951. (d) Cyanogen bromide (e) Sodium tetraborate (borax) Specified in JIS K 8866. (0 Sodium acetate trihydrate Specified in JIS K 8371. (g) Ethanol Specified in JIS K 8101. (h) 4,4-diaminostilbene-2, 2-disulfonic acid (i) Pyridine Specified in JIS K 8777. I
40、(2) Preparation of reagent solution (a) 4,4-Diaminostilbene-2,2-disulfonic acid solution Emulsify to disperse 1.0 g of 4, 4-diaminostilbene-2, 2-disulfonic acid in approx. 20 ml of water, add this solution little by little in 30 ml of sodium acetate solution (30 WN %) and dissolve it with mixing by
41、stirring. Dilute the solution to 100 ml with ethanol. (This acid solution which has elapsed not less than one month after preparation shall not be used.) (b) Cyanogen bromide solution Dissolve 1.5 g of cyanogen bromide in water and di- lute to 100 ml with water. (The solution which has elapsed not l
42、ess than one month after preparation shall not be used.) (c) Sodium tetraborate buffer solution Dissolve 38 g of sodium tetraborate decahy- drate (borax) in 950 ml of water, add hydrochloric acid to make pH 7.8, and dilute to 1 1 with water. (d) Solution for pyridine working curve Dissolve 1.00 ml o
43、f pyridine in water and Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 02:25:53 MSTNo reproduction or networking permitted without license from IHS -,-,- STD=JIS K 0087-ENGL 1998 M 4933b08 0
44、553784 34b = 6 K 0087 : 1998 dilute to 1 I with water. Take 1.8 ml of this solution and dilute to 1 1 with 0.01 moUZ sulfuric acid solution. This solution of 1 ml corresponds to 0.000 5 ml (C,H,N O “c, 101.32 kPa). 5.1.3 Preparation of sample solution After carrying out the procedure of 4.1.3, trans
45、- fer the absorption solution in No.1 absorption bottle (Hl) into a volumetric flask of 200 ml. Wash inside of No.1 absorption bottle (Hl) with the absorption solution in No.2 absorption bottle (H2) and combine the washings into the former flask. Repeat washing procedure with new absorption solution
46、. Dilute to the mark of the flask with absorption solution and use for the sample solution (). t Note (5) The absorption bottles shall be immersed in water with ice when tempera- ture of sampling gas is high. 5.1.4 Operation Operation shall be carried out the following procedure. (1) Take 25 ml of s
47、ample solution prepared in 5.1.2 into a volumetric flask of 50 ml. (2) Add 15 ml of sodium tetraborate buffer solution, 3 ml of 4, 4-diaminostilbene-2, 2- disulfonic acid solution, further 3 ml of cyanogen bromide solution, and dilute the solution up to the marked line with buffer solution. thermost
48、at (). Allow to stand the solution for 30 min to 60 min at the content temperature in a Note () The color development becomes larger as the standing time increases, but it become smaller with the passing of the time. The time to reach the maximum value is different according to temperature of the reaction and other causes. It needs approx. 60 minutes at 20 “c of temperature, and approx. 20 minutes at 30 “c. Therefore the standing time and temperature after adding colorating agent shall be under the same conditions as those at the time of preparing t