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1、UDC 669.5-11:543.062:546.811.062 JIS JAPANESE I NDUSTRIAL STANDARD Methods f o r Determination o f Tin in Zinc Metal Translated Japanese Standards Association 1-24, Akasaka 4, Minato-ku Tokyo 107 Japan 0 JSA, 1989 PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under
2、license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/10/2007 23:37:31 MSTNo reproduction or networking permitted without license from IHS -,-,- This English translation is prepared at the expense of Japan External Trade Organization (JETRO). PROTECTED BY COPYRIGHT
3、Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/10/2007 23:37:31 MSTNo reproduction or networking permitted without license from IHS -,-,- UDC 669.5-11:543.062:546.811.062 JAPANESE INDUSTRIAL STAND
4、ARD J I S Methods for Determination of Tin in Zinc Metal H 1111-1989 1. Scope in JIS H 2107. 2. General Matters K 0115, and J I S K 0116. This Japanese Industrial Standard specifies the methods for determination of tin in zinc metal specified General matters common to the determination methods shall
5、 be in accordance Vnth ES K 0050, . T I S 3. Sampling and Treating Methods of Analytical Sample 3.1 Sampling Method The sampliig method shall be as follows: (1) The sampling method shall be, as a d e , in accordance with JIS H 0301. However, the sample scraped off with a drill shall be cut to not mo
6、re than about 5 IIIII by using clean scissors. (2) When the provision above-mentioned can not be applied to the sampling, it shail be as agreed upon between the parties concerned with delivery. 3.2 Treating Method of Sample The treating method of a sample shall be as follows: (1) In order to prevent
7、 an analytical sample from contamination due to foreign matter or the like, the analytical sample shall be put into a suitable container with a cap and shall be hermetically sealed to be reserved. (2) When it is feared that oil or the like may adhere to the surface of the analytical sample, they sha
8、ll be removed by preliminarily washing the sample with ethanol and diethyl ether. 3.3 Weighing Method of Sample The weighing method of a sample shall be as follows: (1) When the analytical sample is weighed out, the sample shail be sufficiently mixed by stirring care- fully to represent an average c
9、omposition. (2) For weighing out of the analytical sample, a chemical balance shall, as a rule, be used, and the weight shall be read to the nearest 10 mg. 4. Arrangement of Analytical Value a rule in the same chemical laboratory. 4.1 Number of Times of Analysis 4.2 Blank Test For the number of time
10、s of analysis, execute the analysis two times as When an analysis is performed, carry out a blank test, and correct measured values. 4.3 Expression of Analytical Value Express an analytical value by mass percentage, calculate to the next lower place of the lowest significant figure of a numerical va
11、lue specified in JIS H 2107, and round off in - accordance with JIS Z 8401. - Applicable Standards: JIS H 0301-General Rules for Tests and Inspection of Base Metals JIS H 2107-Zinc Metal JIS K 0050-General Rules for Chemical Analysis JIS K 0115-General Rules for Absorptiometric Analysis JIS K 0116-G
12、eneral Rules for Emission Spectrochemical Analysis JIS Z 8401 -Rules for Rounding off of Numerical Values PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/10/2007 23:37:31 MST
13、No reproduction or networking permitted without license from IHS -,-,- 2 H 1111-1989 5. Classification of Determination Methods The method for determination of tin shall be i n accordance with either one of the following methods: (1) Quercetin extraction absorptiometry to 0.002 wt % including in tin
14、 content. (2) Inductively coupled plasma emission spectrochemical method sample of 0.0005 wt % and over to 0.002 wt % including in tin content. (3) Iron hydroxide coprecipitation separation inductively coupled plasma emission spectrochemical method This method applies to the sample of 0.0001 wt % an
15、d over to 0.002 wt % including in tin content. This method applies to the sample of O.OOO1 wt % and over This method applies to the 6. L-ascorbic acid, and mask copper and iron. Add quercetin, extract the generated quercetin tin complex with 4-methyl-2-pentanone, and measure the absorbance by using
16、a photoelectric photometer. 6.1 Summary Decompose a sample with hydrochloric acid and hydrogen peroxide, add thiourea and 6.2 Reagents The reagents shall be as follows: (1) Hydrochloric acid (2) Hydrochloric acid (1 + 1) (3) Sulfuricacid(1 + 19) (4) Zinc (5) Hydrogen peroxide (6) Nickel chloride sol
17、ution (7) L-ascorbic acid solution (20 gll) (8) Thiourea solution (50 g Z ) (9) Quercetin solution Zinc of 99.99 wt % min. in purity and 0.0005 wt % max. in tin content. Dissolve 2 g of nickel chloride hexahydrate in water to lo00 ml. Prepare this solution at each service. Prepare this solution at e
18、ach service. Dissolve 0.5 g of quercetin in about 300 mi of ethanol (95). After adding 25 ml of hydrochloric acid, dilute with ethanol (95) to lo00 ml. (10) 4-me t hyl-Zpent anone 11) Standard tin solution (5pg Sdml) Decompose 0.100 g of t i n (99.9 wt % min.) with 100 ml of hydrochloric acid (1 + 1
19、) by heating. After cooling to ordinary temperature, transfer to a one mark volumetric flask of lo00 ml by using hydrochloric acid (1 + i), dilute to the mark with hydrochloric acid (1 + i), and take it as stock solution (1Opg Sdml). Dilute a necessary amount of this stock solution accurately 20 tim
20、es with hydrochloric acid (1 + i), and take it as standard tin solution. 6.3 Weighing Out Amount of Sample 6.4 Operation The weighing out amount of a sample shall be 2.0 g. 6.4.1 Preparation of Sample Solution procedures: (1) Weigh out a sample, and transfer to a beaker (300 mi). (2) Cover with a wa
21、tch glass. After decomposing() by adding 20 ml of hydrochloric acid, thoroughly decompose by adding several drops of hydrogen peroxide. After cooling to ordinary temperature, wash the bottom face of the watch glass with water, and remove the watch gass. (3) Transfer to a one mark volumetric flask of
22、 50 ml by using water, and dilute to the mark with water. Note (*) When decomposition is difficult, add 2 ml of nickel chloride solution 6.2 (6) Prepare a sampIe solution in accordance with the following 6.4.2 Coloration Separately take accurately 25 ml from the solution obtained in 6.4.1 (3) into a
23、 separating funnel (100 d) preliminarily containing 20 ml of thiourea solution 6.2 ( 8 ) , 5 mi of L-ascorbic acid solution 6.2 (7), and 20.0 rnl of quercetin solution 6.2 (9), and mix by shaking. Thereafter, cool in water for about 15 min. PROTECTED BY COPYRIGHT Copyright Japanese Standards Associa
24、tion Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/10/2007 23:37:31 MSTNo reproduction or networking permitted without license from IHS -,-,- 3 H 1111-1989 6.4.3 Extracting Separation Add accurately 15 ml of 4-methyl-2-pentanone to the
25、solution obtained in 6.4.2, mix by violently shaking for about 1 min, and separate into two layers by standing still. Thereafter, remove the aqueous phase. Add 25 ml of sulfuric acid (1 + 19) to the organic phase, and mix by shaking for about 30 sec. After separation into two layers by standing stil
26、l, remove the aqueous phase. using a dry filter paper, take a portion of the filtrate into the absorption cell (10 mm) of a photometer, use 4-methyl-2-pentanone as contrast solution, and measure the absorbance near 440 nrn in wavelength. 6.4.4 Measurement of Absorbance Filter(2) a portion of the org
27、anic phase obtained in 6.4.3 by Note (2) Perform filtration in order to remove water drops in the organic phase. Discard the ini- tial filtrate. Absorbent cotton may be used instead of the filter paper. 6.5 Blank Test 6.6 Preparation of Working Curve Perform the same operation as that for a sample p
28、arallel to the sample without using the sample. with the following procedures: Preparation of working curve shali be carried out in accordance (1) Weigh out each 2.0 g of zinc 6.2 (4), transfer to several beakers (100 mi), decompose by adding 15 ml of hydrochloric acid and several drops of hydrogen
29、peroxide, and continuously heat to dry- ness. Further, add 5 ml of hydrochloric acid, and heat again to dryness(3). After standing to cool, dissolve salts by adding 10 ml of hydrochloric acid. (2) Stepwise add O to 8.0 ml of standard tin solution 6.2 (il) (O to 4Opg as tin). Further, add hydrochlori
30、c acid (1 + 1) so that the amount of hydrochloric acid in each solution becomes 15 mie). Hereinafter, carry out operation parallel to the sample foilowing the procedures of 6.4.1 (3) to 6.4.4, prepare the relation curve between the obtained absorbance and the amount of tin in the aliquot solution, p
31、arallel transfer the relation curve so as to pass through the origin, and take it as the working curve. Notes ( 3 ) Almost all the tin contained in zinc can be removed by this operation. e) When, for instance, O, 4.0, and 8.0 mI of standard tin solution are added, it is suitable to add respectively
32、10,6, and 2 ml of hydrochloric acid (1 + i). 6.7 Calculation Obtain the amount of tin from the absorbance obtained in 6.4.4 and 6.5, and the work- ing curve prepared in 6.6, and calculate the content of tin in the sample from the following formula: Thwt%= Ai- m x B A2 x 100 where Ai : detection amou
33、nt of tin in aliquot sample solution (g) A2 : detection amount of tin in aliquot blank test solution (g) ni : weighing out amount of sample (g) B : aliquot ratio of sample solution, and 1/2 herein 7. Decompose a sample with a mixed acid of hydrochloric acid and nitric acid, spray the solution into t
34、he argon plasma of an inductively coupled plasma emission spectrochemical apparatus, and measure the emission intensity. Inductively Coupled Plasma Emission Spectrochemical Method 7.1 Summary 7.2 Reagents The reagents shall be as follows: (1) Hydrochloric acid (1 + 1) (2) Mixed acid (45 parts of hyd
35、rochloric acid and 1 part of nitric acid) (3) Zinc solution (200 mg Zdml) Decompose 100 g of zinc 6.2 (5) in 400 ml of hydrochloric acid, and evaporate by heatin to dryness. After cooling, add 5 ml of hydrochloric acid, and heat again to evaporate to dryness( ). After cooling, add 10 ml of hydrochlo
36、ric acid (1 + 5) and water, and dissolve the salts by heating. After cooling to room temperature, transfer to a 500 ml volumetric flask by using water, and dilute to the mark with water. 5 PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=
37、IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/10/2007 23:37:31 MSTNo reproduction or networking permitted without license from IHS -,-,- 4 H 1111-1989 ( 4 ) Standard tin solution (5pg Sn/ml) 7.3 Weighing Out Amount of Sample 7.4 Operation As described in 6.2 (11). The weighing out a
38、mount of a sample shall be 5.0 g. 7.4.1 Preparation of Sample Solution (1) Weigh out a sample, and transfer to a beaker (300 ml). (2) Cover with a watch glass, and decompose by adding 30 ml of mixed acid. When violent reaction ends, thoroughly decompose by gently heating, successively heat, and conc
39、entrate until the amount of solution becomes about 25 mi(). After coolmg to ordinary temperature, wash the bottom face of the watch glass, and remove the watch glass. (3) After addmg about 20 mi of water and 20 ml of hydrochloric acid (1 + i), transfer to a 100 ml volumetric flask by using water, an
40、d dilute to the mark with water. Note () When the solution is concentrated to 20 ml max., it is feared that a portion of tin may be Prepare a sample solution i n accordance with the following procedures: vaporized. 7.4.2 Measurement of Emission Intensity Spray a portion of the solution obtained i n
41、7.4.1 (3) into the argon plasma of an inductively coupled plasma emission spectrochemical apparatus, and measure the emission intensity(6) at 189.989 nm in wavelength. Note (6) When precision and accuracy have been confirmed, measurement may be performed by using other wavelengths. For an apparatus
42、for which high order spectral lines can be used, the high order spectral lines may be used. Further, for an apparatus equipped with a background correction mechanism, the background correction mechanism may be used. 7.5 Blank Test 7.6 Preparation of Working Curve Carry out the same operation as that
43、 for a sample parallel to the sample without using the sample. 7.6.1 Preparation of Working Curve for Sample (1) Take 25 ml of zinc solution 7.2 (3) into several volumetric flasks of 100 ml. (2) Stepwise add O to 20.0 ml of standard tin solution 7.2 (4) (O to 100,ug as tin), further add hydrochloric
44、 acid (1 + 1) so that the amount of hydrochloric acid in each solution becomes 10 ml, and dilute to the mark with water. (3) Spray a portion of the solution into the argon plasma of an inductively coupled plasma emission spectrochemical apparatus, measure the emission intensity at 189.989 nm in wave
45、length parallel to the sample, prepare the relation curve between the obtained emission intensity and the amount of tin, parallel transfer the relation curve so as to pass through the origin, and take it as the working curve for the sample. Stepwise deal out O to 12.0 ml standard tin Prepare the wor
46、king curve for a sample in accord- ance with the following procedures: 7.6.2 Preparation of Working Curve for Blank Test(7) solution 7.2 (4) (O to pg as tin) into several 100 ml volumetric flasks, add 20 ml of hydrochloric acid (1 + 1) volumetric flasks, add 20 ml of hydrochloric acid (1 + i), and d
47、ilute to the mark with water. Spray a portion of the solution into the argon plasma of an inductively coupled plasma emission spectrochemical ap- paratus, measure the emission intensity at 189.989 nm in wavelength parallel to the blank test, prepare the relation curve between the obtained emission i
48、ntensity and the amount of tin, parallel transfer the relation curve so as to pass through the origin, and take it as the working curve for the blank test. Note (7) When the emission intensity of the blank test solution is considerably weak by comparing it with the emission intensity of the sample s
49、olution, the working curve prepared in 7.6.1 may be used. PROTECTED BY COPYRIGHT Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/10/2007 23:37:31 MSTNo reproduction or networking permitted without license from IHS -,-,