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1、JIS JAPANESE INDUSTRIAL STANDARD Translated and Published by Japanese Standards Association Methods for in stack gas determination of mercury ICs 13.040.40; 71.040.40 Descriptors : gases, pollutant gases, exhaust gases, mercury, determination of content, chemical analysis and testing, gas analysis,
2、spectrophotometry, absorptiometry Reference number : JIS K 0222 : 1997 (E) 10 s Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:54:01 MDTNo reproduction or networking permitted without l
3、icense from IHS -,-,- K 0222 : 1997 This translation has been made 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: Da
4、te of Establishment: 1981-03-01 Date of Revision: 1997-08-20 Date of Public Notice in Official Gazette: 1997-08-20 Investigated by: Japanese Industrial Standards Committee Divisional Council on Environment JIS K 0222 : 1997, First English edition published in 1998-01 Translated and published by: Jap
5、anese 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. O JSA 1998 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in
6、 any form or by any means, 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=Wing, Bernie Not for Re
7、sale, 03/15/2007 08:54:01 MDTNo reproduction or networking permitted without license from IHS -,-,- . . t STD-JI.5 K 0222-ENGL 1997 4933bO 0548554 28T 9 JAPANESE INDUSTRIAL STANDARD JIS K 0222: 1997 Methods for determination of mercury in stack gas 1 gaseous mercury in stack gas. Scope This Japanese
8、 Industrial Standard specifies the methods for determination of Remarks 1 The concentration of mercury is expressed by the concentration of mercury in dry gas under standard condition. The normative references to this Standard are listed in Attached Table 1. 2 2 Definitions JIS K 0095, and the follo
9、wing definitions apply. For the purposes of this Standard, the definitions given in JIS K 0211 and (1) stack gas The gas exhausted from such as a flue, chimney or duct (hereafter referred to as “duct”) due to burning of fuels, roasting of ores, metal refining, and treatment of sludge or waste. Gener
10、ic term of mercury and mercury compounds which are present in stack gas as the style of gas. ( 2 ) gaseous mercury 3 JIS K 0095, JIS K 0121, JIS K 8001, and JIS Z 8808. Matters in common The matters commonly used in this Standard follow JIS K 0050, 4 Classification of methods for determination The m
11、ethods for determination are classified into the following three. (1) Wet absorption-atomic absorption spectrometry by reducing vaporization Make gaseous mercury in sample be absorbed in sulfuric acidic solution of potassium perman- ganate, catch it, reduce mercury in absorption liquid, aerate throu
12、gh this solution to isolate mercury, and determine the mercury by atomic absorption spectrometry. This method can be used for the determination of gaseous mercury existing in every stack gas. Determination range shall be from 1 ng to 1 O00 ng as mercury. Gold-amalgam catching- atomic absorption spec
13、trometry by heating vaporization After catching mercury in sample gas as gold amalgam, heat the caught mercury in a heating vaporization furnace to vaporize mercury, and determine isolated mercury by atomic absorption spectrometry. This method is used for the analysis of stack gas after treatment, a
14、nd applicable to the determination of metal mercury in stack gas. Determination range shall be from 0.01 ng to i O00 ng as mercury mass. (3) Continuous measuring method Introduce directly sample gas into an absorption cell, vaporize it by reduction, and determine continuously it by atomic absorption
15、 spec- trometry. (2) This method is applicable lo the stack gas exhausted from city garbage burning plant. Determination range shall be from 1 g/m to 5 mg/m as mercury concentration. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, Use
16、r=Wing, Bernie Not for Resale, 03/15/2007 08:54:01 MDTNo reproduction or networking permitted without license from IHS -,-,- - STD-JIS K 0222-ENGL 1997 4933b08 0548555 Llb 2 K 0222 : 1997 5 Wet absorption-atomic absorption spectrometry by reducing vaporization 5.1 follow JIS K 0095. Sampling of samp
17、le gas The general matters on sampling method of sample gas 5.1.1 Sampling place Choose the place where distribution of flow rate is uniform. 5.1.2 Sampling device for sample be as follows. An example of sampling device for sample is shown in Fig. 1. Except the prescription in 4 of JIS K 0095, it sh
18、all A : D : G : J : Filtering material B : Sampling tube for sample gas C : Warmth retaining heater By pass E : Absorption bottle F : Cooling chamber Selector cock H : Drying tube I : Suction pump Adjusting cock for flow rate K : Wet gas meter Fig. 1 Construction of sampling device for sample (examp
19、le) Sampling tube Introducing tube introducing tube made of special vinyl chloride resin can be used. Collecting bottle has 250 ml capacity are connected in series ( I ). Made of borosilicate glass, quartz glass, titanium, or ceramics. Made of tetrafluoroethylene resin. When heating is not needed, t
20、he Follow 4.7 of JIS K 0095. Two absorption bottles each of which Note ( I ) Ordinally, one bottle is enough. 5.1.3 Sampling Except the prescription in 5 . 1 of JIS K 0095, the sampling shall be as follows (). Note (*) In case of stack gas containing high concentration of sulfur dioxide as in ore ro
21、asting gas, wash the gas with absorption liquid prepared by potas- sium hydroxide. Absorption liquid sulfuric acid (1+15). Store it in a colored glass bottle. Sampling tube, introducing tube gas on sampling tube or introducing tube, if necessary, heat or keep its warmth. Mix in equivolume potassium
22、permanganate solution (3 gll) and In order to avoid the condensation of water in stack . Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:54:01 MDTNo reproduction or networking permitted
23、without license from IHS -,-,- 3 K 0222 : 1997 (3) Absorption bottle Absorption bottle shall be previously washed with nitric acid (1+9) and water, and be dried. Put 100ml of absorption liquid, and cool it in a cooling chamber. Connect 2 absorption bottles in series. While sucking, the flow rate sha
24、ll be 0.5 Zlmin to 1.0 llmin, and sucked quantity shall be about 20 1. However, dont suck in until the color of potassium permanganate of absorption liquid disappears. (4) Sucked quantity 5.1.4 Preparation of reagent for determination (i) Reagents If necessary, the reagents shall be for analysis for
25、 deleterious metal or for precision determination. Sulfuric acid (l+l) Take one unit of water in a beaker, and add gently one unit of sulfuric acid specified in JIS K 8951 while cooling and stirring the water. Potassium permanganate solution (50 gll) Dissolve 50 g of potassium perman- ganate specifi
26、ed in JIS K 8247 in water, filtrate it through a glass filter (G4), and add water to make total 1 1. Store it in a colored glass bottle. (c) Hydroxylammonium chloride solution (200 gll) Dissolve 20 g of hydroxylammo- nium chloride specified in JIS K 8201 in water to make total 100 ml. (d) Hydroxylam
27、monium chloride solution (20 gll) Add several drops of sulfuric acid (1+1) into 10 mi of hydroxylammonium chloride solution (200 gil), and add water to make total 100 ml. (a) (b) (2) Implements Implements shall be as follows. (a) Flask reflux condenser. Made of glass. 500ml flask capable of being eq
28、uipped with a ground-in (b) Reflux condenser With about 30 cm in length (3) Procedures Procedures shall be as follows. (a) Transfer the absorption liquid, in which sample gas has passed, into a flask. Wash the absorption bottle with a little quantity of hydroxylammonium chloride solution (20 gll) an
29、d water, and put the washings into the flask (). Note () When sample gas does not contain organic gas, the procedure at (b) can be omitted. In this case, transfer the absorption liquid at (a) into a suitable beaker, and then carry out the procedures stated at (c) and thereafter. (b) Attach a reflux
30、condenser, heat gently it avoiding bumpings, and boil it for 1 h. During this heating, if color of potassium permanganate disappears (), lower the temperature down to about 60 “C, add 2 ml of potassium permanganate solution (50 gil), boil it again, and repeat these procedures until the color of pota
31、ssium perman- ganate lasts for about 10 min. Then cool the tetnperature of solution to 40 “C or lower. Note ( 4 ) Even when the color of potassium permanganate disappeared, if manga- nese dioxide exists, the supplementation of potassium permanganate solution is not carried out. Copyright Japanese St
32、andards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:54:01 MDTNo reproduction or networking permitted without license from IHS -,-,- 4 K 0222 : 1997 (c) While shaking the solution, add drop by drop hydroxylammoni
33、um chloride solution (200 gll), and decompose the superfluous potassium permanganate ( ). Note () Avoid to add excessively hydroxylammonium chloride solution. After cooling, transfer the solution into a 500 ml measuring flask, add water up to the marked line, and make it sample solution. Take absorp
34、tion liquid that is the same quantity as that used for sampling, carry out the procedures from (a) to (d), and make it the solution for blank test. (d) (e) 5.2 Method for determination (i) Reagents If necessary, the reagents shall be for analysis for deleterious metal or for precision analysis. Sulf
35、uric acid (1+35) Tin (II) chloride solution Add 60 ml of sulfuric acid (1+20) onto 10 g of tin (n) chloride dihydrate specified in JIS K 8136, and heat it to dissolve while stirring them. After cooling, add water to make total 100 ml. This solution shall be used up within one week from preparation.
36、Solution for mercury dilution Put 10 mg of L-cysteine into a 1 O00 ml measuring flask, add water, shake to dissolve it, add 2 ml of nitric acid specified in JIS K 8541, and add water up to the marked line. Mercury reference solution (100 mgHg/l) Put 67.7 mg of mercury (n) chloride specified in JIS K
37、 8139 into a 500 ml measuring flask, dissolve it in the solution for mercury dilution, then add the solution for mercury dilution up to the marked line, and make it stock solution. Store the stock solution in a refrigerator. Reference solution shall be prepared by diluting this stock solution with t
38、he solution for mercury dilution. ( 2 ) Apparatus Apparatus is composed of an atomic absorption spectrometer, reduction vessel, absorption cell, air pump, flowmeter, drying tube, connecting tube, and others. Fig. 2 shows an example of a closed circulation type, and Fig. 3 shows an example of open ai
39、r-supplying type apparatus. The detail of each constructing part is as follows. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:54:01 MDTNo reproduction or networking permitted without l
40、icense from IHS -,-,- STD-JIS K 0222-ENGL 1777 4733b08 0548558 925 E A C - F D 7 c 5 K 0222 : 1997 A : B : C : D : E : F : Reduction vessel Drying tube Absorption cell Air pump Mercury removal device Cock for bypass rl Fig. 2 Construction of closed circulation type apparatus (example) A : Reduction
41、vessel B : Drying tube C : Flowmeter D : Absorption cell E : Air pump F : Mercury removal device Fig. 3 Construction of open air-supplying type apparatus (example) (a) Atomic absorption spectrometer Atomic absorption spectrometer or atomic ab- sorption spectrometer for mercury. Reduction vessel by t
42、he measuring apparatus. The tube, measuring 100 mm to 300mm in length, is made of quartz glass, glass, or plastics (not adsorbing mercury), and its both ends are covered with a quartz glass window. (b) Aeration tube with a filter for bubbling. Its capacity is specified (c) Absorption cell (d) Air pu
43、mp Diaphragm pump capable of sending air by 0.5 Ilmin to 3 Ilmin, or air pump having equivalent performance. In case of closed circulation type, pay attention about the adsorption of mercury. Flowmeter Capable of measuring flow rate of 0.5 Ilmin to 3 Ilmin (). Note ( 6 ) (e) When closed circulation
44、type is adopted, there is apprehension that mercury is adsorbed on a flowmeter, therefore flowmeter is not attached. Beforehand, flow rate is controlled by the flow rate of an air pump, and thus the optimum flow rate shall be determined. (f) Drying tube which granular-type desiccant is stuffed (). T
45、hermoelectronic refrigeration type, or the straight tube or U tube in Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 08:54:01 MDTNo reproduction or networking permitted without license fro
46、m IHS -,-,- STD-JIS K 0222-ENGL 6 K 0222 : 1997 Note () If the temperature in absorption cell is designed to be about 10 “C higher than ambient, the drying tube is unnecessary. (g) Connecting tube Made of soft vinyl-chloride resin. (h) Mercury removal device taining potassium permanganate (50 gll) i
47、s put. Gas washing bottle in which sulfuric acid (1+4) con- (3) Procedures Procedures shall be carried out as follows. (a) Take suitable quantity of sample solution (*) in a reduction vessel, and add sulfuric acid (1+35) () in the sample solution. Notes (*) The quantity of sample solution to be take
48、n is specified depending on the measuring apparatus. () The quantity of sulfuric acid to be added is specified depending on the measuring apparatus. Remarks: The sample containing a lot of chloride ion may give positive error because, when preparing sample solution, the chlorine absorbs light which was produced from chloride ion by means of the oxidation resulted from the adding of potassium permanganate. In this case, add in excess of quantity of hydroxylammonium chloride solution to reduce chlorine. The chlorine existing in a reduction vessel shall be expel