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1、JIS This standard was revised in 2, 1995 JAPANESE I NDUSTRIAL STANDARD Methods for Emission Spectrochemical Analysis of Lead Metal JIS H 1123-1976 (Reaffirmed: 1984) This copy is an English version of Japanese Industrial Standard prepared by Japanese Standards Association, the copyright holder, Any
2、further reproduction without permission is prohibited. Translated Japanese Standards Association 1-24, Akasaka 4, Minato-ku Tokyo 107 Japan 0 JS* 1986 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 0
3、3/14/2007 07:16:01 MDTNo reproduction or networking permitted without license from IHS -,-,- . This English translation is prepared at the expense of Japan External Trade Organization (JETRO) . - 4 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/
4、1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:01 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS H LLZ3-.ENGL li115 E 3 Y133bU0 0544480 AZJ = UDC 669.44:543.423 b* Methods or Emission Spectrochemical Analysis of Lead Metal H 1123-1976 (Reaffirmed: 1
5、984) 1. Scope This Japanese Industrial Standard specifies the methods for photographic emission spectrochemical analysis of chemical composition (arsenic, iron, tin, antimony, bismuth, copper, silver and zinc) specified in JIS H 2105. 2. General Matters General matters common to the analytical metho
6、ds shall be in accordance with JIS K 0050 and JIS 2 2612. 3. Sampling and Treating of Sample The sample shal1,be taken in accordance with JIS H 0301 and prepared in accordance with 5.2.2, 5.3.2, 5.4.2, and 5.5.2 of this standard, or otherwise 7. of .TIS Z 2612. 4. Expression of Analytical Values Ana
7、lytical values shall be expressed by percentage and their numerical values shall be rounded off as follows: (1) The numerical values concerning impurities shall be limited to three places of decimals and the subsequent figure shall be rounded off in accordance with JIS 2 8401. However, the significa
8、nt numerical value of the content of element in impurity by this method shall be not more than two figures. Applicable Standards: JIS H 0301-General Rules for Tests and Inspection of Base Metals JIS H 2121-Methods for Chemical Analysis of Lead Metal JIS H 2105-Pig Lead JIS H 2121-Electrolytic Cathod
9、e Copper JIS K 0050-General Rules for Chemical Analysis J I S 2 2612-General Rules for Photographic Emission Spectrochemical Analysis of Mata1 Materials J I S Z 8401-Rules for Rounding off of Numerical Values - 1 - Copyright Japanese Standards Association Provided by IHS under license with JSALicens
10、ee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:01 MDTNo reproduction or networking permitted without license from IHS -,-,- (2) The contezt of lead shall be the remzfnder for which total sum of respective impurities obtained by (i) is subtracted from 100 and shall be
11、 obtained to two places of decimals. The third place of decimals shall be discarded. 5. - Determination Methods 5.1 Classification of Methods The determination methods shall be classified as follows according to the classification of pig lead. (i) Concentrated salt powder arc method (it is applicabl
12、e to the pig lead of not less than Class 2) (2) Salt powder arc method (it is applicable to the pig lead of not less than Class 2) (3) Solution arc method (it is applicable to the pig lead of not less than Class 2 ) ( 4 ) Metallic solid method ( a ) Metallic electrode intermittent arc method (it is
13、appli- cable to the pig lead of not more than Class 3) Metallic electrode spark method (it is applicable to the pig lead of not more than Class 3) . (b) 5.2 Concentrated Salt Powder Arc Method 5.2.1 Summary The solution prepared by decomposing a sample with nitric acid, is added with a fixed amount
14、of sulfuric acid, and a fixed amount of main components is separated by precipitation. A graphite supporting electrode is packed with the salt powder in which impurities are relztively concentrated and light is emitted therefrom by direct current arc method. and the intensity of spectral line is mea
15、sured. Its light is photographed by using a spectrograph 5.2.2 Preparation Method of Sample The method for prepararion of sample shall be as follows: (i) Analysis Sample Weigh out 2.00 g of the sample, transfer it into a beaker (100 mi), cover it with a watch glass, add - 15 ml of nitric acid (1 (1+
16、4) and decompose it by carefully heating it. dilute the amount of solution to 25 ml by adding water, drop 14.50 ml of 1 N sulfuric acid (2) with a burette while agitating it and precipitate about 75% of lead. Filter the precipitate by using the filter paper for determination, wash it 3 times by usin
17、g 7 ml of water by decantation, transfer little by little the filter paper and wash liquid into an evaporating dish (50 mi) and carefully evaporate them to dryness. After standing to cool, transfer all the dried salt into an agate mortar with a nonmetallic spatula and nix them by sufficiently grindi
18、ng them to be the analytical sample. After standing to cool a t room temperature, c - 2 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:01 MDTNo reproduction or networking permitted
19、 without license from IHS -,-,- Notes ( I ) For the nitric acid used in this nethod, nitric acid of not less than Cless 1 is refined by using an all glass still and water is refined in the same way by using the all glass still. (2) For 1 N sulfuric acid, the reagent sulfuric acid of guaranteed grade
20、 is accurately diluted to 1 N to be used. (2) Standard Sample Weigh out 3.20 g of lead nitrate (equiva- lent to 2.00 g of lead) refined in accordance with 5.2.3, transfer. it into a beaker (100 mi) and dissolve it by adding 4 ml of nitric acid (1+4) and 15 ml of water. the equivalent amounts of vari
21、ous impurity metal standard solutions of 5.2.4 (calculated amounts to lead) thereto by using a microburet or a measuring pipette ( 3 ) , dilute the amount of solution to 25 nl by using water, hereinafter carry out the operation on and after the addition of 1 N sulfuric acid of 5.2.2 ( l ) and allow
22、this sample to be the standard sample. However, prepared several pieces of this standard samples corresponding to purities of respective steps. Note (3) After adding A microburet or measuring pipette of 0.01 ml in graduation shall be corrected to be used. 5.2.3 Refining Method of Lead Nitrate Put 20
23、0 g of lead (not less than 99.9 X ) into a beaker (3000 mi), add 800 ml of water and 250 ml of nitric acid, decompose it by heating and filter it with a sintered-glass filter (No. 4) while it is warm. Settle lead chloride by adding a calculated amount of hydrochloric acid (i+l to this solution with
24、mixing them. After washing the precipitate several times by using cold water according to decantation, filter it by suction. Dissolve this lead chloride in 10000 ml of hot water by dividing it by 3 times, immediately pass hydrogen sulfide gas through this hot solu- tion and precipitate lead sulfide.
25、 After washing the precipitate with warm water several tines, dissolve it with hot nitric acid (i+l and add the water of about one half of the amount of solution. After boiling it for about 1 0 to 20 min, filter this warm solution, and cool the filtrate with water while mixing it with stirring at ti
26、mes to deposit lead sulfate. Further, recrystallize this crystal with redistillation water three times After filtering the crystal by suction, dry it at 120 to 125OC. Carry out the qualitative test of the crystal obtained herein by emission spectrochemical analysis method. Idhen impurities such as a
27、rsenic, iron, tin, antimony, bismuth, copper, silver, zinc, etc. are confirmed, further refine it by recrystallization. 5.2.4 Preparation Method of Standard Pletal Solution The nitric acid solutions or the mixed solutions of nitric acid and tartaric acid of various impurity metals shall be prepared.
28、 Their concentrations shall be ones in which 1 mg, 0.1 mg o r 0.01 mg of metal element are - 3 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:01 MDTNo reproduction or networking pe
29、rmitted without license from IHS -,-,- respectively contaized in 1 1 of the solution. metals of not less than 49.9 % in purity shall be used. However, various (1) 1 mg/ml Standard letal Solution The preparation method thereof shall be as follows: Standard Zinc Solution transfer it into a beaker (100
30、 mi), cover it with a watch glass, add 8 ml of nitric acid (19-2) and carefully decom- pose it by heating. After standing to cool to room temperature, transfer it into a measuring flask of 500 ml by using water and dilute it up t o the marked line. Weigh out 0.500 g of zinc, Standard Iron Solution-
31、Weigh out 0.500 g of iron, transfer it into a beaker (100 mi), cover ft with a watch glass, add 15ml of nitric acid (Ir-3) and carefully decoinpose it by hearting. After standing to cool to rooui temprature, transfer it into a measuring flask of 500 nl and dilute it up to the marked line, Standard C
32、opper Solution transfer it into a beaker (100 mi), cover it with a watch glass, add 15 ml of nitric acid (1+3) and carefully decompose it by heating. After standing to cool to room temperature, transfer it into a measuring flask of 500 ml by using water and diiut it up the the marked line. Weigh out
33、 0.500 g of copper, Standard Silver Solution nitrate, transfer it into a beaker (100 mi) and dissolve it by adding 1 ml of nitric acid and water. Thereafter, transfer it into a measuring flask of 500 ml by using water and dilute it up to the marked line. Weigh out 0.7857 g of silver Standard Bismuth
34、 Solution Weigh out 0.500 g of bismuth, transfer it into a beaker (lo nl), cover it with a watch glass and decompose it by adding 20 ml of nitric acid (l+l). Thereafter, transfer it into a measuring flask of 500 ml by using water and dilute it up to the marked line. Standard Arsenic Solution trioxid
35、e refined by sublimation, transfor it into a beaker (100 mi), add as small amount (about 5 mi) of potassium hydroxide solution (about 10 X ) as possible and dissolve it by heating. After standing to cool to room tempera- ture, add 20 ml of nitric acid (l+l) while sufficiently mixing them by shaking,
36、 transfer it into a measuring flask of 500 ml by using water and dilute it up to the marked line. Weigh out 0.6602 g of arsenic Standard Antimony Solution mony, transfer it into a beaker (100 mi), cover it with a watch glass, add 20 ml of nitric acid (l+l) and 5 g of tartaric acid and carefully deco
37、mpose it by heating. After standing to cool to room temperature, transfer it into a measuring fleck of 500 ml by using water and dilute it up to the marked line. Weigh out 0.500 g of anti- - 4 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/111
38、1111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:01 MDTNo reproduction or networking permitted without license from IHS -,-,- STD.JIS H 1123-ENGL 1995 Li933b08 054Li484 477 W (h) Standard Tin Solution Weigh out 0.500 g of tin, transfer it into a beaker (100 m i ) , cover it with a watch g
39、lass, add 30 ml of nitric acid (1+4) and 10 g of tartaric acid and dissolve them by standing for one night at room temperature with mixing the solution by shaking at times. Thereafter, transfer it into a measuring flask of 500 ml by using water and dilute it up to the marked line. However, when prec
40、ipitate is generated during storage, prepare it newly. 0.1 mg/ml Standard Metal Solution fixed amount of 1 mg/ml standard metal solution of (1) into a measuring flask and accurately dilute it; 10 times by using water. However, use tartaric acid solution (2 X ) instead of water for standard tin solut
41、ion, use nitric acid (1+15) instead of water for standard bismuth solution and dilute each of them 10 times respectively. Accurately weigh out a 0.01 mg/ml Standard Metal Solution Accurately weigh out a fixed amount of 0.1 mg/ml standard metal solution of (2) into a measuring flask and accurately di
42、lute it 10 times by using water. instead .of water for standard tin solution, use nitric acid (1+20) instead of water f.or standard bismuth solution and dilute each of them 10 times respectively. all 0.01 mg/ml standard metal solutions at each use without storage. However, use tartaric acid solution
43、 (1 X ) However, prepare 5.2.5 Preparation Method of Sample Supporting Electrode The graphite bar for spectrochemical analysis of 5 to 6 mm in diameter is cut by a length of about 30 mm and one end thereof is finished per- pendicular to its axis. drilled by a fixed depth of 3 to 4 mm by using a dril
44、l of 3 mm in diameter. Thereafter, the centre of emission surface is Further, the end of counter electrode should preferably be pointed to diameter of 3 rmn. Its example is given in Fig. 1. - 5 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/11
45、11111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:01 MDTNo reproduction or networking permitted without license from IHS -,-,- Fig. i. Exaaple O Dimensions of Graphite Electrode for Powder Arc Unit: mm 5.2.6 Apparatus and Operating Conditions The apparatus and operating conditions shall b
46、e as follows: (1) Spectral Apparatus The middle type quartz spectroscope having the optical system of intermediate image method shall be used. The slit of spectroscope shall be 20 Firn and a step filter or a rotating sector shall be provided just before the slit-. Emission Method After respectively
47、packing the analysis sample and the standsrd sample prepzred according to 5.2.2 into the holes of graphite supporting electrode with a fixed hardness by using nonmetal spoons, the powder on the enission surface is removed and the sample electrode is mede the lower electrode (anode) of electrode supp
48、ort stand to be prepared. For the upper electrode, a graphite counter electrode is attached and both electrodes are, as a rule, opposed with each other by a fixed clearance of 5 to 10 m. The gap between both electrodes is given with a fixed voltage (100 t o 200 V) of direct current and a fixed current (5 to 10 A) and light is emitted by direct current arc. The exposure time shall be 10 to 20 sec just after emission. In that case, the light emitted from the white heat part of electrode and the neighbourhood of both electrodes shall be regulated with the screen of th