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1、 STD-JIS G 1229-ENGL 1774 4733bU8 0594027 750 UDC 669,14/, 15 ;543,062 : 546.815 This copy is an English version of Japanese -I Industrial Standard prepared by Japanese Standards Association, the copyright holder. Any further reproduction without permission is prohibited. JIS This standard was revis
2、ed in 9, 1994 JAPANESE I NDUSTRIAL STANDARD Methods for Determination of Lead in Steel J IS G 1229-1980 L I Translated Japanese Standards Association 1-24, Akasaka 4, Minato-ku Tokyo 107 Japan 0 JSA, 1985 COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Ja
3、panese Standards Association Licensed by Information Handling Services ., , . . mis English translation is prepared at the expense of Japan External Trade Organizaion (JETRO) . COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association
4、 Licensed by Information Handling Services UDC 669.14/.15:543.062:546.815 4733b08 0544031 507 1. Scope This Japanese Industrial Standard specifies the methods for determination of lead in steel. 2. General Items General items common to determining methods shall be in accordance with JIS G 1201. 3. C
5、lassification of Methods The method for determination of lead in steel shall be in accordance with one of the following: (1) Lead molybdate gravimetric method This method applies to the sample of 0.05 46 and over in lead content (2) Dithizone extraction absorptiometry This method applies to the samp
6、le of 0.01 2 and over, up to 0.5 2 in lead content. (3) Iron separation dithizone extraction absorptiometry This method applies to the sample of 0.0001 46 and over, up to 0.01 2 in lead content. Applicable Standards: JIS G 1201-General Rules for Chemical Analysis of Iron and Steel JIS R 3503-Glass A
7、pparatus for Chemical Analysis - 1 - COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services 4. Lead Molybdate Gravimetric Method 4.1 Summary The sample is decomposed with hydrochloric acid
8、and excessive acid is removed. hydrogen sulfide, filtered and this precipitate is decomposed with nitric acid. Thereafter, lead sulfide is precipitated by Lead molybdate is precipitated by ammonium molybdate, filtered and its mass is measured by igniting that. 4.2 Applicable Fields When the sample c
9、ontains a large amount of silicon, tungsten, niobium, tantalum, zirconium and chromium and is difficult to be decomposed with hydrochloric acid, the preparation of sample solution shall be in accordance with other operation. 4.3 Reagents The reagents shall be as follows: Hydrochloric acid Hydrochlor
10、ic acid (l+l) Nitric acid Nitric acid (l+l) Sulfuric acid (1+20) Aqueous ammonia Hydrogen sulfide hydrogen sulfide generator is used. The hydrogen sulfide originated from bomb or Hydrogen sulfide saturated hydrochloric acid passing hydrogen sulfide through 1 R hydrochloric acid (1+99) for about 10 m
11、in, it is used. After violently Ammonium chloride - 2 - COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services Ammonium nitrate solution (5 w/v X) Lead-saturated sulfuric acid wherein 300 m
12、l of sulfuric acid is added gradually into 1800 ml of water, this hot solution being added with 1 g of lead acetate, sufficiently mixed with stirring, stood for 24 h or more, and thereafter filtered with a filter paper (Class 5 C ) . The acid prepared by a method Ammonium molybdate solution method w
13、herein after dissolving 10 g of ammonium molybdate The solution prepared by a (4 hydrate) with 200 ml water during heating it, it is filtered with a filter paper (Class 5 B ) . lead is precipitated by 1 ml of this solution. About 0.055 g of Tartaric acid Ammonium acetate solution Ammonium acetate sa
14、turated water solution at the ordinary temperature is diluted 2 times with water, added with 1 to 2 drops of Methyl Red-alcohol solution (0.1 w/v X) and neutralized by acetic acid or aqueous ammonia. The ammonium acetate solution is prepared by adding 30 ml of acetic acid per 1 R of this solution. A
15、mmonium acetate cleaning fluid diluting ammonium acetate solution l 4 . 3 ( 1 4 ) l 10 times with water. The fluid prepared by Ethyl alcohol (95 v/v X min,) 4.4 Apparatus The following apparatus shall generally be used. Hydrogen Sulfide Generator The hydrogen sulfide generator of a suitable size is
16、selected among Kipps gas generators given in Attached Fig. 35 of JIS R 3503 according to the using amount and let generate hydrogen sulfide with iron sulfide and hydrochloric acid (l+l). - 3 - COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Stand
17、ards Association Licensed by Information Handling Services 4.5 Weighing-Out Amount of Sample weighed out in accordance with Table 1. The sample shall generally be Weighing-out amount of sample g Table 1 Using amount of hydrochloric acid (1+1) ml Lead content % 0 . 1 and over 5.0 50 0.05 and over, up
18、 to 0.1 I 10.0 1 1 O0 4.6 Operat ion 4.6.1 Preparation of Sample Solution (1) Sample Easy to Be Decomposed with Hydrochloric Acid (1.1) Transfer the weighed-out sample into a beaker (500 mi), cover it with a watch glass, add hydrochloric acid (l+l) according to Table 1 and decompose it by heating. A
19、fter salts begin to be deposited by continuing to heat it, remove the watch glass and evaporate it to dryness as far as possible to the degree that the bottom of beaker does not turn brown due to burn and seizing. After cooling, dissolve salts by adding about 400 ml of hot water, add 1 0 g of ammoni
20、um chloride (), precipitate lead as sulfide by violently passing hydrogen sulfide 4,3 (7)l for 1 0 min, filter it with a filter paper (Class 5 A) and wash it several times with hydrogen sulfide saturated hydrochloric acid l4.3 (8)l. Discard the filtrate and washings. (1.2) Receive a beaker (300 mi)
21、under a funnel, decompose lead sulfide by pouring 10 ml of hot nitric acid (l+l) onto the precipitate on filter paper and further wash it several times with hot water. Combine the filtrate with the washings, dilute it t o about 100 ml by adding water and add 2 g of tartaric acid thereto. After disso
22、lving tartaric acid by mixing with stirring, neutralize it with aqueous ammonia and further add 5 ml of aqueous ammonia in excess. - 4 - COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Servic
23、es (2) Sample Difficult to Be Decomposed with Hydrochloric Acid (2.1) Operate the weighed-out sample in accordance with the procedure of 4.6.1 ( 1 . 1 ) . Transfer the precipitate and filter paper into a porcelain crucible (15 mi) and dry it. Thereafter, incinerate the filter paper by heating it at
24、400 to 500C and transfer the residue into a beaker ( 1 0 0 m i ) . Decompose the residue fixed to porcelain crucible by heating after adding about 5 ml of hydrochloric acid and transfer it to the previous beaker (100 mi) by washing it with water. Add 10 ml of nitric acid thereto, decompose it by hea
25、ting, add about 20 ml of water, filter the insoluble residue with a filter paper (Class 5 C) and sufficiently wash it with hot water. Discard the residue. Collect the filtrate and washings into a beaker (300 mi), make it about 10 ml by heating concentration, add 40 ml of lead saturated sulfuric acid
26、 L4.3 (li) and generate white fume by continuing heating. After cooling it a little, wash the wall of beaker with a small amount of sulfuric acid (1+20). Thereafter, generate white fume by heating it again. After cooling, dilute the amount of solution to about 40 ml by adding water, dissolve soluble
27、 salts by heating, stand it for one night and mature the precipitate of lead sulfate. Filter it with a filter paper (Class 5 C) and sufficiently wash it with lead saturated sulfuric acid 4 . 3 (il). Thereafter, wash it several times with sulfuric acid (1+20) and wash it once with ethyl alcohol (95 v
28、/v % min.) at last. Discard the filtrate and washings. Transfer the precipitate on filter paper into the original beaker (300 mi) with warm water with washing, add 50 ml of ammonium acetate solution 4.3 (14)1, dissolve lead sulfate by heating, filter it with the original filter paper and COPYRIGHT J
29、apanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services sufficiently wash it with hot ammonium acetate cleaning fluid 4.3 (15)l. beaker (300 mi) and make it about 250 ml with water. Discard the residue
30、. Collect the filtrate and washings into a Note () pH of solution at that time is most suitable at 2.0 to 2.5. 4.6.2 Generation of Precipitate and Filtration When the sample solution obtained in 4.6.1 is heated and begun to be boiled, add 10 ml of ammonium molybdate solution l4.3 (12)l and let the p
31、recipitate of lead molybdate aggregate by boiling it for several minutes. Filter it with a small amount of filter paper pulp and filter paper (Class 5 B ) , rub off the precipitate adhered to the inner wall of beaker by the glass rod with rubber tube, transfer it on filter paper and sufficiently was
32、h it with the hot ammonium nitrate solution (5 w/v X) slightly made ammoniac. Discard the filtrate and washings, 4.6.3 Incineration and Weighing Transfer the precipitate filtered in 4.6.2 into the porcelain crucible (15 mi) having known mass together with filter paper and dry it by slowly heating it
33、. Incinerate the filter paper by gradually raising temperature, heat it within a range of 600 to 650C to constant weight and leave it cool in a desiccator to ordinary temperature. molybdate. Thereafter, weigh its mass as lead 4.7 Calculation The lead content in sample shall be calculated from the fo
34、llowing formula: w x O. 5644 loo Lead (2) = where z u : mass of lead molybdate ( 8 ) IV: weighing-out amount of sample (g) - 6 - COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services 4.8 A
35、nalysis Precision The analysis precision on this method shall be as given in Table 2. Lead content Table 2 Unit: X Standard deviation Standard deviation within same laboratory between different laboratories O. 0288xCPb(%)+O. 0042 I o. o5 and over, up to 0.22() O . 0117XPb(%)+O. 0089 Note (2) This nu
36、merical value means the maximum value of lead content of sample used for determination of analysis precision. 5 . Dithizone Extraction Absorptiometry 5.1 Summary After decomposing the sample with hydrochloric acid, nitric acid and perchloric acid, the maskings of iron, nickel, etc. are carried out w
37、ith tartaric acid, sodium sulfite and sodium cyanide. Then, lead is extracted to benzene as dithizone complex and the absorbancy is measured. 5.2 Applicoble Fields This method is not applicable to the case where 1 mg of titanium and 0.05 mg and over of niobium are contained in the sample solution se
38、parately taken. 5.3 Reagents The reagents shall be as follows: (1) Hydrochloric acid (2) Hydrochloric acid (1+100) (3) Nitric acid ( 4 ) Perchloric acid ( 5 ) Aqueous ammonia - 7 - COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Associa
39、tion Licensed by Information Handling Services (6) Aqueous ammonia (1+2) (7) Iron The iron having as high purity as possible without containing lead, or of which lead content is as low as possible and known. ( 8 ) Cleaning fluid The fluid prepared by adding 100 ml of aqueous ammonia (1+100) with 5 m
40、l of sodium sulfite solution (saturated) (9) Sodium sulfite solution (saturated, bout 20 w/v X) (10) Sodium cyanide solution (3) 20 g of sodium cyanide is dissolved in 100 nl water, put into a separating funnel (200 mi), added with 1 0 to 15 ml of dithizone-benzene solution 15.3 ( 1 2 ) l and mixed
41、with shaking. two layers after standing still, the lower layer of water solution phase is taken out as sodium sulfite solution. When organic phase indicates red, the lower layer of water solution phase is transferred to another separating funnel and extracting operation is repeated. When it is separ
42、ated into (il) Tartaric acid solution (20 w/v A) Dithizone-benzene solution The solution obtained by the following preparing method shall be teken as the dithizone-benzene solution. O. O1 g of dithizone (diphenylthiocarbazone) (C,H,NHNHCSN : NC,H,) is dissolved in 10 ml of benzene, put into a separa
43、ting funnel (100 mi), further added with 50 ml of cleaning fluid 15.3 (8)l and mixed by shaking for 1 min. When the solution is separated into two layers by standing still, the lower layer of water solution phase is transferred into another separating funnel (100 mi), added with hydrochloric acid (l
44、+l) and made slightly acidic. Thereafter, it is added with 20 ml of benzene and mixed by shaking for 1 min. When the solution is separated - 8 - COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handlin
45、g Services into two layers by standing still, the lower layer of water solution phase is discarded, the upper layer of organic phase is diluted to 100 ml with benzene, put into a brown bottle and stored. When dithizone is impure, it is refined as follows: 0 . 1 g of dithizone is dissolved in 50 ml o
46、f benzene, put into a separating funnel (200 m i ) , further added with 50 ml of cleaning fluid l5.3 (8)l and mixed by shaking for 1 min. the solution is separated into two layers by standing still for a while, the lower layer of water solution phase is taken out, added with hydrochloric acid and ma
47、de slightly acidic. The precipitated dithizone is filtered with a filter paper (Class 5 A), washed with water and dried in a desiccator. When (13) Benzene (14) Standard lead solution (100 vgPb/ml) The solution prepared by a method wherein water, added with about 1 0 ml of nitric acid, transferred in
48、to a measuring flask of 1000 ml and diluted up to the marked line with water. 0.1599 g of lead nitrate is dissolved in Note (3) Because sodium cyanide solution is violently poisonous, cares shall necessarily be taken about handling the solution containing it. 5.4 Weighing-Out Amount of Sample 1.0 g
49、of the sample shall generally be weighed out. 5 . 5 Operation 5.5.1 Preparation of Sample Solution - 9 - COPYRIGHT Japanese Standards Association Licensed by Information Handling Services COPYRIGHT Japanese Standards Association Licensed by Information Handling Services Transfer the weighed-out sample into an Erlenmeyer flask (300 mi), add 1 0 ml of hydrochloric acid and 3 ml of nitric acid and decompose it by heating. acid thereto, generate thick white fume of perchloric acid by successively heating it and oxidize chromium to dichromic acid. Further continue