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1、JAPANESE INDUSTRIAL STANDARD JIS K 0106 : 1995 Methods for determination of chlorine in flue gas January, 2004 ERRATA In pages 2, 3, 4, in the bottom box in the second column of Table 1, in (8) of 4.1.1, and i n ( c ) of 4 . 1 . 2 , respectively, the name of the reagent is changed as follows: Error:
2、 dime thylbenzidinium dichloride (o. tolidine Correct: dimethylbenzidinium dichloride (otolidine dihydrochloride) Remarks: This erratum is for correcting the first and second editions of this Standard. Japanese Standards Association - 13- Copyright Japanese Standards Association Provided by IHS unde
3、r license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 04:07:08 MSTNo reproduction or networking permitted without license from IHS -,-,- JAPANESE INDUSTRIAL STANDARD JIS KO106 : 1995 Methods for determination of chlorine in flue gas November, 2000 ERRATA Pag
4、e 9, line 24 In 6.1.2 (2)(b), the description of m is changed as follows: Error r n : Taken amount of potassium iodate (mi) Correct m : Taken amount of potassium iodate (g) Remarks: This erratum is for correcting the first edition of this Standard. Japanese Standards Association - I I - Copyright Ja
5、panese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 04:07:08 MSTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS K OLOb-ENGL 1995 Li933b08 O554053 078 I JAPANESE INDUSTRIAL STAN
6、DAFiD JTS K 0106: 1995 Methods for determination of chlorine in flue gas ERRATA March, 1999 PP. 2, 3, and 8 In Table 1, 4.1.1 (6), 4.1.2 (3) (a) and 6.1, the name of reagent is corrected as follows: Error 2,2-amino-bis Correct 2,2-azino-bis Remarks: This erratum is for correcting the first edition o
7、f this Standard. Japanese Standards Association Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 04:07:08 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S Ka0106
8、 95 4933608 0525986 945 = JIS UDC 662.61 3.5:543.274:546.13 . JAPANESE INDUSTRIAL STANDARD Methods for determination of chlorine in flue gas JIS K 0 1 0 6 - 1 9 9 5 Translated and Published bY Japanese Standards Association Printed in Japan 13 S Copyright Japanese Standards Association Provided by I
9、HS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 04:07:08 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S KJOLOb 75 4733608 O525987 881 W In the event of any doubt arising, the original Standard in Japanese is to b
10、e final authority. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 04:07:08 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S K*OLOb 95 m 9933608 0525988 718 m U
11、DC 662.613.5 : 543.274 : 546.13 JAPANESE INDUSTRIAL STANDARD J I S K 0106-1995 Methods for determination of chlorine in flue gas 1. Scope mination of chlorine in flue gas. This Japanese Industrial Standard specifies the methods for deter- Remarks 1. In this Standard, the flue gas means the gas exhau
12、sted into flue, chimney, and duct, etc. (hereafter they are referred to as “duct“) when burning, chemical reaction or the like is carried out, 2. The standards cited in this Standard are listed in Attached Table 1. 3. The units and numerical values given in 1 in this Standard are based on the tradit
13、ional units and are appended for informative reference. 2. Matters n common The matters commonly applied in chemical analysis, sampling off le gas, and absorptiometry, shall follow respectively JIS K 0050, JIS K 0095, and JIS K 0115. 3. methods shall be as shown in Table 1. Type and summary of analy
14、sis methods The type and summary of analysis Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 04:07:08 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S KxOL06 95
15、 4933608 0525989 654 m 2 K 0106-1995 Table 1. Type and summary of analysis methods Type of analysis methods 2,2-amino-bis (3- ethylbenzothiazoline- 6-sulfonic acid) absorptiometry (ABTS method) 4-pyridinecarboxylic acid-pyrazolone absorptiometry (PCP method) 3,3-dimethyl- benzidini um dichloride abs
16、orptometry (o- tolidine absorptiometry) Summary of analysis methods Outline Let chlorine in sample gas be absorbed into 2,2- amino-bis (3-ethylbenzo- thiazoline-6-sulfonic acid) absorbing liquid, color it, and measure its absorb- ance (400 nm). Let chlorine in sample gas be absorbed into p- toluenes
17、ulfonamide absorbing liquid, add potassium cyanide solution, color it with 4- pyridinecarboxylic acid- pyrazolone solution, and measure its absorbance (638 nm). Let chlorine in sample gas be absorbed into 3,3- dimethylbenzidinium di- chloride (o-tolidine) absorbing liquid, and measure the absorbance
18、 of colored solution (435 nm). Sampling Absorbing-bottle method Absorbing liquid: ABTS solution (0.01%) Quantity of absorbing liquid: 20 ml x 2 Standard sampling volume: 20 I Absorbing-bottle method Absorbing liquid: p-toluenesulfon- amide solution (0.1%) Quantity of absorbing liquid: 20 ml x 2 Stan
19、dard sampling volume: 20 1 Absorbing-bottle method Absorbing liquid: 3,3-dime thyl- benzidinium dichloride solution (0.0 1 %) Quantity of absorbing liquid: 20 ml x 2 Standard sampling volume: 2.5 I Determinatioi range() volppm (mgCldrn3) 0.06 to 10 (0.2 to 32) 3.08 to 10 10.3 to 32) 1.1 to 10 0.3 to
20、 32) Applicable condi tion Follow 6.1.1 Follow 6.2.1 Follow 6.3.1 Note(1) This value shows when sample solution for analysis is prepared by means of diluting the absorbing liquid (40 mi), through which sample gas has been passed, to make 50 ml. Remarks: In Annex, the continuous analysis method using
21、 3,3-dimethyl- benzidinium dichloride (o-tolidine continuous analysis method) is stated. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 04:07:08 MSTNo reproduction or networking permitted wi
22、thout license from IHS -,-,- J I S K*OltOb 95 4333608 0525990 376 3 K 0106-1995 4. be as follows. Sampling method of sample gas The sampling method of sample gas shall When sampling the sample gas for analysis, choose the spot where repre- sentative sample gas can be taken, sample the gas principall
23、y at least 2 times in a short time at the same sampling spot, and use each of them for analysis. 4.1 Reagents and preparation of reagent solution 4.1.1 Reagents Water Class A2 specified in JIS K 0557. Hydrochloric acid Specified in JIS K 8180. Sulfuric acid Specified in JIS K 8951. Potassium dihydro
24、genphosphate Specified in JIS K 9007. Disodium hydrogenphosphate Specified in JIS K 9020. 2,2-amino-bis( 3-ethylbenzothiazoline-6-sulfonic acid) sulfate (ABTS) p-toluenesulfonamide Recrystallize in benzene, and dry in a desiccator. 3,3-dimethylbenzidinium dichloride (o-tolidine) Specified in JIS K 8
25、669. Benzene Specified in JIS K 8858. 4.1.2 PreDaration of reagent solution (1) Sulfuric acid (0.02 mol/) Add 1.2 ml of sulfuric acid into 1 1 of water. (2) Buffer solution (pH 7) Dissolve 4.5 g of potassium dihydrogenphosphate in water to make total 1 1 (U30 mol/), dissolve 4.7 g of disodium hydrog
26、en- phosphate solution in water to make total 1 1 (1/30 mol/), mix them equally in volume, and control its pH to be 7 . (3) Absorbing liquid (a) Case of ABTS absorptiometry ABTS solution Dissolve O. 1 g of 2,2-amino-bis(3-ethylbenzothiazoline- 6-sulfonic acid) sulfate (ABTS sulfate) in 100 ml buffer
27、 solution (pH 7), and add sulfuric acid (0.02 mol/l) to make total 1 1. Storage period of this solution is for 2 days in cold and dark place. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 0
28、4:07:08 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S K*OLOb 95 = 4933608 0525993 202 4 K 0106-1995 (b) Case of PCP absorptiometry p-toluenesulfonamide solution of dried p-toluenesulfonamide, place 100 ml of water on it, heat it to 50C Recrystallize using benzene, t
29、ake O. 1 g to 60C on a water bath, shake sufficiently to dissolve it, and allow it to cool. (c) Case of 3,3-dimethylbenzidinium dichloride absorptiometry 3,3-dimethylbenzidinium dichloride solution dimethylbenzidinium dichloride (o-tolidine) in about 500 ml of water, and add 15 ml of hydrochloric ac
30、id and water to make total 1 1. Take 100 ml of this solution and add water to make total 1 1. Store this stock solution in a brown bottle. Storing period is about 6 months. Dissolve 1 g of 3,3- 4.2 Implements and apparatus (i) Absorbing bottle Connect 2 absorbing bottles (capacity 50 mi), shown in F
31、ig. 1, when they are to be used(2). (2) Sampling apparatus for sample gas Fig. 2, shall be equipped with the following conditions. Apparatus, constructed as shown in (2.1) The sampling pipe of sample gas (BI shall be made of the material which resists corrosive gas in flue gas such as chlorine, for
32、instance, glass pipe, quartz pipe, or polytetrafluoroethylene pipe. (2.2) In order to prevent dust to mix into sample gas, plug end of sampling pipe or suitable place with filter medium(3). (2.3) In order to keep the moisture contained in sample gas from being condensed, provide a device to heat fro
33、m gas sampling pipe to cock (Pi)(4). To connect these parts, use commonly ground connecting pipe, silicone rubber pipe, or polytetrafluoroethylene pipe. (2.4) Set up the whole apparatus to get rid of any leakage at each connection. Notes (2) When it is confirmed that chlorine is completely captured,
34、 one absorbing bottle will do. (3) Use the material, making no chemical reaction with the components in flue gas, such as silica wool, or alkaliless glass wool. (4) Set up the line of piping as short as possible, and if it is apprehended that condensed water affects measured value, heat from the sam
35、pling pipe to cock Pl at about 120C. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 04:07:08 MSTNo reproduction or networking permitted without license from IHS -,-,- JIS K+0106 95 4933608 0
36、525992 I149 5 K 0106-1995 Fig. 1 Example of absorbing bottle Unit: mm Glass ball filter: Maximum pore diameter 40 nm to 120 nm Glass ball filter Fig. 2 Example of sampling apparatus for sample gas A : Filter medium(3) B : Sampling pipe for sample gas C : Insulator D : Thermometer E : Heater F, F, :
37、Absorbing bottle (50 ml capacity) L : Suction pump M :Wet gas meter G : Glass filter H : Washing bottle J : Drying pipe (50 ml capacity) K, K, : Adjusting cock of flow rate - N : Thermometer O :Manometer P,P, : Three way cock to switch flow way Copyright Japanese Standards Association Provided by IH
38、S under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 04:07:08 MSTNo reproduction or networking permitted without license from IHS -,-,- J I S K*OLOb 95 4933608 0525993 085 6 K 0106-1995 4.3 Procedures for sampling symbols adopted here follow Fig. 2. P
39、rocedures shall be carried out as follows. The (i) Put respectively 20 ml of any absorbing liquid of (a), (b), or (c) in 4.1.2(3), which has been specified in each analysis method, into absorbing bottles (Fl, F2)(2). (2) Turn switching cocks (Pl, P2) to bypass side, run suction pump (L), and displac
40、e inside from gas sampling pipe (B) to cock (Pl) by sample gas. (3) After stopping suction pump (LI, turn the switching cocks (Pl, Pz) toward absorbing bottles (Fl, F2) side. Then, read indication (V,) on a gas meter (M) to the nearest 0.01 1. (4) Run the suction pump (L) to pass the sample gas thro
41、ugh the absorbing bottles (F, F2)(5). In this time, control flow-rate controlling cocks (Kl, K,) to make flow rate about 1 Ilmin O 5 llmin(6) in case of 3,3-dimethylbenzidinium dichloride absorptiometryl. Take about 20 l(2.5 1 in case of 3,3-dimethyl- benzidinium dichloride absorptiometry)(7) of sam
42、ple gas, stop the suction pump (L), shut the switching cocks (Pl, P , ) , and read the indication (V,) on the gas meter (M) to the nearest 0.01 1. At the same time, measure temperature and gauge pressure of the gas using the thermometer (NI and manometer (O) attached on the gas meter (M). Simultaneo
43、usly, measure atmospheric pressure. (5) As occasion demand, measure the moisture in sample gas according to 6. of JIS Z 8808. Notes(5) When absorbing liquid may be likely warmed by prettily high temperature of gas to be sampled, place the absorbing bottle in a cooling tank. ( 6 ) When it is beforeha
44、nd known that chlorine concentration is completely absorbed in absorbing liquid, the flow rate about 1 Zlmin may be permitted. (7) It may be suitably adjusted according to the concentration of chlorine. 4.4 amount of gas sampled at standard condition (OOC, 101.32 kPa (760 mmHg) shall be converted in
45、to dry-base gas amount (VSD) or wet-base gas amount (Vsw). Sampled amount of sample gas According to the following formula, the 4.4.1 When obtaining dry-base gas amount (i) Case of using a wet gas meter 273.15 P, + P, - P “ VSD = vx X + 22.41 (a + b) 273.15 + t 101.32 Copyright Japanese Standards As
46、sociation Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Japan, IHS Not for Resale, 02/16/2008 04:07:08 MSTNo reproduction or networking permitted without license from IHS -,-,- JIS KxOLOb 95 4933608 0525994 TIL 7 K 0106-1995 (2) Case of using a dry gas meter VSD = v x
47、 X P a + Pm + 22.41 (a+b) 273.15 273.15 + t 101.32 4.4.2 When obtaining wet-base gas amount (1) Case of using a wet gas meter 273.15 Pa + Pm - P v v , , = v x X + 22.41 (a+b+c) 273.15 + t 101.32 (2) Case of using a dry gas meter + 22.41 (a+b+c) P a + Pm X 273.15 v,= vx 273.15 + t 101.32 where, VsD :
48、 Dry-base gas amount (I) Vsw : Wet-base gas amount (I) V : Amount of gas measured by gas meter (I) t : Temperature at gas meter (OC) equals to V, - VI at the procedures of 4.3(3) and (4)l Pa : Atmospheric pressure (kPa) (mmHg) P , : Gauge pressure at gas meter (kPa) (mmHgI(8) Pv : Saturated water vapor pressure at toc (kPa) (mmHg) a(8) : Target gas for anal