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1、 J I S H*3309 89 D 4933b08 0050773 b I f _ . UDC 669.5-1 1 :543.062:546.72:%2- 3. 2- JAPANESE INDUSTRIAL STANDARD Methods for Determination of Iron in Zinc Metal Translated and Published by . Japanese Standards Association Printed in Japan 6 s Copyright Japanese Standards Association Provided by IHS
2、 under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:16 MDTNo reproduction or networking permitted without license from IHS -,-,- In the event of any doubt arising, the original Standard in Japanese is to be final authority. Copyright Japanese
3、Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:16 MDTNo reproduction or networking permitted without license from IHS -,-,- UDC 669.5-11:543.062546.72.062 JAPANESE INDUSTRIAL STANDARD JIS Methods for D
4、etermination of Iron i n Zinc Metal H 1109-1989 1. Scope specified in JIS H 2107. 2. General Matters JIS K 0116, and JIS K 0121. 3. T h i s Japanese Industrial Standard specifies the methods for determination of iron i n zinc metal General matters common to the analytical methods shall be i n accord
5、ance with JIS K 0050, JIS K 0115, Sampling and Treating of Analytical Sample 3.1 Sampling Method The sampling method shall be as follows: (1) The sampling method shall be, as a rule, in accordance with JIS H 0301. However, the sample scrapped off with a drill shall be cut to not more than about 5 mm
6、 by using clean scissors. (2) In the case where the above-mentioned specification can not be applied to the sampling method, the sampling method shall 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)
7、 In order to prevent an analytical sample from contamination by foreignmatters or the like, the analytical sample shall be put in a suitable glass container with a cover and shall be hermetically sealed to be reserved. (2) When there is a fear that oil or the like will adhere to the surface of an an
8、alytical sample, the analytical sample shall be preliminarilywashed with ethanol and diethyl ether to remove them. 3.3 Weighing Method of Sample The weighing method of a sample shall be as follows: (1) When an analytical sample is weighed out, sufficiently mix the sample by stirring carefully to rep
9、re- (2) For weighing out of an analytical sample, use a chemical balance as a rule, and read to the nearest sent its average composition. 10 mg. 4. Arrangement of Analytical Value a rule, in the same laboratory. 4.1 Number of Times of Analysis 4.2 Blank Test 4.3 Indication of Analytical Value For th
10、e number of times of analysis, repeat an analysis two times, as On analysis, carry out a blank test and correct measured values. lower place of the significant lowest figure used in expressing the numerical value specified in JIS H 2107, and round off in accordance with JIS Z 8401. Express an analyt
11、ical value by mass percentage, calculate to the nexl 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 Oll6 -General Rules for Emissio
12、n Spectrochemical Analysis JIS K 0121-GeneraRules for Atomic Absorption Spectrochemical Analysis JIS Z 8401-Rules for Rounding off of Numerical Values Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 0
13、3/12/2007 02:49:16 MDTNo reproduction or networking permitted without license from IHS -,-,- I J I S H*lLO 89 m 4733608 0050774 L I 2 H 1109-1989 5. Classification of Determination Methods The method for determination of iron shall be in accordance with either one of the following methods: (1) 1,lO-
14、phenanthroline absorptiometry This method applies to the sample of 0.001 wt % and over to 0.3 wt % including in iron content. (2) Chloride extraction separation 1,lO-phenanthroline absorptiometry This method applies to the sample of 0,0001 wt % and over to 0.002 wt % including in iron content. (3) A
15、tomic absorption method % including in iron content. (4) Inductively coupled plasma emission spectrochemical method sample of O.ooO1 wt % and over to 0.3 wt % including in iron content. This method applies to the sample of 0.0002 wt % and over to 0.3 wt This method applies to the 6. 1,lO-Phenanthrob
16、e Absorptiometry After decomposing a sample with a mixed acid of hydrochloric acid and nitric acid, add L-ascorbic acid and sodium ethylenediaminetetraacetate, hereinafter referred to as the “EDTA“, reduce iron, and mask zinc or the like, Thereafter, add 1, 10-phenanthroline, regulate pH by adding a
17、mmonium acetate, generate 1,lO-phenanthroline iron complex, and measure the absorbance thereof by using a photoelectric photometer. 6.1 Summary 6.2 Reagents The reagents shall be as follows: (1) Hydrochloric acid (1 + 1) (2) Mixed acid (45 parts of hydrochloric acid and 1 part of nitric acid) (3) L-
18、ascorbic acid solution (10 g/l) (4) Ammonium acetate solution (500 gl) (5) EDTA solution ml of water and 10 ml of aqueous ammonia, and dilute to 100 ml with water. (6) 1,lO-Phenanthroline solution (3 gl) monohydrate in 1000 mi of water. Otherwise, dissolve 3.0 g of 1,lO-phenanthroline monohydratc in
19、 100 ml of ethanol (95), and dilute to 1000 ml with water. (7) Standard iron solution (20pg Fe/ml) Decompose 0.100 g of iron (99.9 wt % min.) with 20 ml o nitric acid (1 + 3). After cooling to ordinary temperature, transfer to a 1000 ml volumetric flask by using water, dilute to the mark with water,
20、 and take it as stock solution (100pg Fe/ml). Dilute a necessary amount of this stock solution accurately five times with water at each service, and take it as standard iron solution. Prepare this solution at each service. Dissolve 40 g of disodium ethylenediaminetetraacetate dihydrate by adding 50
21、Dissolve 3.6 g of 1,lO-phenanthroline chloride 6.3 Weighing Out Amount of Sample 6.4 Operation The weighing out amount of a sample shall be 5.0 g. 6.4.1 Preparation of Sample Solution cedure: (1) Weigh out a sample, and transfer to a beaker (300 mi). Prepare a sample solution inaccordance with the f
22、ollowing pro- (2) Cover with a watch glass, and decompose by adding 30 ml of mixed acid. When violent reaction ends, thoroughly decompose by gently heating, and successively concentrate by heating to a syrupy state. temperature, wash the bottom surface of the watch glass with water, remove the watch
23、 glass, trans- fer the solution to a 100 m volumetric flask by using water, and dilute to the mark with water. Separately take accurately 10 (3) Add about 50 ml of water, and dissolve salts by gently heating(). After cooling to ordinary from this solution to a 100 ml volumetric flask. Notes (l) When
24、 dissolution is incomplete, completely dissolve by adding 2 ml of hydrochloric acid (1 + 1). of aliquot solution so that the amount of iron becomes 50 to 300pg. (2) In the case where the amount of iron in this solution exceeds 3OOpg, reduce the amount -. Copyright Japanese Standards Association Prov
25、ided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:16 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS H*ll09 89 W 4933b08 0050775 3 W 3 H 1109-1989 6.4.2 Coloration (1) After making the amount of solut
26、ion 50 ml by adding water to the solution obtained in 6.4.1 (3), (2) Add 1 ml of EDTA solution 6.2 (5), 15 ml of 1,lO-phenanthroline solution 6.2 (6), and 5 ml of Coloration shall be performed in accordance with the following procedures: add 2 ml of Gascorbic acid solution 6.2 (3), and mix by shakin
27、g. ammonium acetate solution to this solution. After diluting to the mark with water, allow to stand for about 20 min. 6 6.4.3 Measurement of Absorbance Take a portionof the solution obtained in 6.4.2 (2) to the absorp- tion cell (10 mm) of a photometer, use water as contrast solution, and measure t
28、he absorbance near 510 nm in wavelength. the sample. 300 pg as iron) into several one mark volumetric flasks of 100 ml, and add water to make the amount of solu- tion about 50 ml. Thereafter, add 2 ml of L-ascorbic acid solution r6.2 (3), and mix by shaking. Hereinafter, operate following the proced
29、ures of 6.4.2 (2) and 6.4.3, prepare the relation curve between the obtained ab- sorbance and the amount of iron, parallel transfer the relation curve so as to pass through the origin, and take it as the working curve. 6.7 Calculation Obtain the amount of iron from the absorbance obtained in 6.4.3 a
30、nd 6.5 and the work- ing curve prepared in 6.6, and calculate the content of iron in a sample from the following formula: * 6.5 Blank Test 6.6 Preparation of Working Curve Carry out the same operation as that for a sample parallel to the sample without using Take stepwise O to 15.0 ml of standard ir
31、on solution r6.2 (7) (O to Ironwt% = A1-A2 X B x 100 -. ,. where Ai : detection amount of iron in aliquot sample solution (g) A2 : detection amount of iron in aliquot blank test solution (g) ni : weighing out amount of sample (g) B : aliquot ratio of sample solution and blank test solution 7. tract
32、iron from the hydrochloric solution with 4-methyl-2-pentanone and isopentyl acetate. Back extract iron by adding water to an organic phase, reduce iron by adding L-ascorbic acid and sodium ethylenediaminetetraacetate, hereinafter referred to as the “EDTA“, and besides, mask zinc or the like which co
33、exist. Thereafter, add 1, 10-phenanthroline, regulate pH by adding 1,iO-phenanthroline complex, and measure the absorbance thereof by using a photoelectric photometer. Chloride Extraction Separation 1,lO-Phenanthroline Absorptiometry 7.1 Summary After decomposing a sample with a mixed acid of hydroc
34、hloric acid and nitric acid, ex- 7.2 Reagents The reagents shall be as follows: (1) Hydrochloric acid (1 + 1) . (2) Nitric acid (1 + 1) (3) Mixed acid (45 parts of hydrochloric acid and 1 part of nitric acid) (4) Washing solution Take about 300 ml of hydrochloric acid (6 + 5) into a separatory funne
35、l (500 mi), add about 50 ml of 4-methyl-2-pentanone and isopentyl acetate mixed solvent, mix by shaking, and remove the organic phase. (5) L-ascorbic acid solution (10 gi) (6) Ammonium acetate solution (500 gi) (7) EDTA solution As described in 6.2 (5). (8) 1,lO-phenanthroline solution (3 g i ) As d
36、escribed in 6.2 (6). (9) 4-methyl-2-pentanone and isopentyl acetate mixed solvent (1 part of 4-methyl-2-pentanone and 1 As described in 6.2 (3). part of isopentyl acetate) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Ber
37、nie Not for Resale, 03/12/2007 02:49:16 MDTNo reproduction or networking permitted without license from IHS -,-,- r J I S H*:LLOS 89 4933608 005C177b 5 I 4 H 1109-1989 (10) Standard iron solution (20pg Fehl) As described in 6.2 (7). 7.3 Weighing Out Amount of Sample 7.4 Operation The weighing out am
38、ount of a sample shall be 5.0 g. 7.4.1 Preparation of Sample Solution cedures: (1) Operate in accordance with the procedures of 6.4.1 (1) and (2). (2) Add 20 ml of hydrochloric acid (1 + l), and dissolve salts by gently heating. 7.4.2 Separation of Iron (1) Transfer the solution obtained in 7.4.1 (2
39、) to a separatory funnel (100 ml) by using hydrochloric acid (1 + l), and make the amount of solution to 50 ml by using hydrochloric acid (1 + 1). (2) Add 20 ml of 4-methyl-2-pentanone and isopentyl acetate mixed solvent 7.2 (!I), mix by violently shaking for about 1 min, and separate into two layer
40、s by standing still. Thereafter, remove the aqueous phase. (3) Add 15 ml of washing solution 7.2 (4) to the organic phase, mix by shaking for about 1 min, and separate into two layers by standing still. Thereafter, remove the aqueous phase. Further, repeat this washing operation once. (4) Add about
41、20 ml of water to the organic phase, and mix by vigorously shaking for about 1 min. After separation into two layers by standing still, transfer the aqueous phase to a beaker (50 mi). Add about 5 ml of water to the organic phase, and mix by violently shaking for about 1 min. After separation into tw
42、o layers by standing still, join the aqueous layer to the aqueous phase in the beaker (50 mi). Discard the organic layer. (5) Add 5 ml of nitric acid (1 + l), and evaporate to dryness by heating. After standing to cool, add 2 ml of hydrochloric acid (1 + l), dissolve salts by heating, and cool. 7.4.
43、3 Coloration Perform coloration in accordance with the following procedures: (1) Add 2 ml of L-ascorbic acid solution j7.2 (5) to the solution obtained in 7.4.2 (9, and allow to stand for about 15 min. (2) Add 0.5 ml of EDTA solution 7.2 (7), 2 ml of 1,lO-phenanthroline solution 7.2 (S), and 10 ml o
44、 ammonium acetate solution to this solution, and transfer to a 25 ml volumetric flask by using water. After dilution to the mark with water, allow to stand for about 20 min. Take a portion of the solution obtained in 7.4.3 (2) to the absorp- Prepare a sample solution in accordance with the following
45、 pro- Separate iron in accordance with the following procedures: 7.4.4 Measurement of Absorbance tion cell (10 mm) of a photometer, utilize water as contrast solution, and measure the absorbance near 510 nm in wavelength. 7.5 Blank Test the sample. 7.6 Preparation of Working Curve 1OOpg as iron) int
46、o several beakers (50 mi), add 2 ml of hydrochloric acid (1 + 1) and 2 ml of L-ascorbic acid solution 7.2 (5), and allow to stand for about 15 min. Hereinafter, operate following the procedures of 7.4.3 (2) and 7.4.4, prepare the relation curve between the obtained absorbance and the amount of iron,
47、 paral- lel transfer the relation curve so as to pass through the origin, and take it as the working curve. Obtain the amount of iron from the absorbance obtained in 7.4.4 and 7.5, and the work- ing curve prepared in 7.6, and calculate the content of iron in a sample from the following formula: Carr
48、y out the same operation as that for a sample parallel to the sample without using Take stepwise O to 5.0 ml of standard iron solution 7.2 (lo) (O to 7.7 Calculation Ironwt% = x 100 where Ai : detection amount of iron in sample solution (g) A2 : detection amount of iron in blank test solution (g) ni
49、 : weighing out amount of sample (g) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:16 MDTNo reproduction or networking permitted without license from IHS -,-,- . J I 5 H*LLO 89 493360