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1、JIS H*1339 87 4933608 0051013 2 E f i f b UDC 669.721.5 J JAPANESE INDUSTRIAL STANDARD Methods for Determination of Beryllium in Magnesium Alloys Translated and Published Japanese Standards Association -/ Printed in Japan - - .-/ 543 : 546.45.062 5 s Copyright Japanese Standards Association Provided
2、 by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 07:21:24 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 Jap
3、anese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 07:21:24 MDTNo reproduction or networking permitted without license from IHS -,-,- ! J I S H*iI339 87 4933608 005LO15 b - - UDC 669.721.5:543:546,45.062 .
4、 JAPANESE INDUSTRIAL STANDARD J I S Methods for Determination of Beryllium in H 1339-1987 Magnesium Alloys i. Scope This Japanese Industrial Standard specifies the methods for determination of beryllium in magnesium alloys. Y 4 e c e 2. General Items The general items common to the analysis method s
5、hall be in accordance with JIS H 1331 and JIS K 0121. 3. Classification of Determination Methods The method for determination of beryllium shall be as specified h either one This method applies to the sample of not less (2) Acetylacetone Extraction Atomic Absorption Method This method applies of the
6、 following methods: (1) Atomic Absorption Method than O. 001- % in beryllium content. to the sample of not less than O. O01 % in beryllium content. 4. Atomic Absorption Method 4.1 Purport peroxide and the absorbance of beryllium is measured by using an atomic absorp- tion photometer. A sample is dec
7、omposed with hydrochloric acid and hydrogen 4.2 Reagents The reagents shall be as follows: (1) Hydrochloric acid (1 + 1, 1 + 100) (2) Magnesium 99.90 % min. in purity, Class 1 of JIS H 2150 or that having quality equal or superior thereto (3) . Hydrogen peroxide (4) Standard beryllium solution (5 pg
8、Be/ml) min. ) is weighed out, transferred into a beaker (300 mi), cvered by a watch glass, joined by 50 ml hydrochloric acid (1 + 1) and decomposed by heating. After cooling to ordinary temperature, it is transferred hto a transfer flask of 500 ml by washing and diluted to the marked line with water
9、 to be the standard stock solution (200 pgBe/ml) . A necessary amount of standard stock solution is accurately diluted to 40 times with water to be the standard beryllium solution. 0.100 g beryllium (99.5 % Applicable Standards : JIS H 1331-General Rules for Chemical Analysis of Magnesium Alloys JIS
10、 H 2150-Magnesium Ingots . JIS K 0121-General Rules for Atomic Absorption Spectrochemical Analysis . Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 07:21:24 MDTNo reproduction or networkin
11、g permitted without license from IHS -,-,- J I S Hu1339 87 4933608 OOSLO1b 8 W 2 H 1339-1987 4.3 Weighing Out Amount of Sample The weighing out amount of a sample shall be 1.0 g. 4.4 Operation The determination operation shall be carried out i n ac- cordance with the following procedures : (1) Weigh
12、 out a sample, transfer it into a beaker (200 mi), add 20 ml water, cover it with a watch glass and add little by little 20 ml hydrochloric acid (1 + 1). When the reaction becomes slow, add 1 mi hydrogen peroxide, thoroughly decompose the sample by heating and decompose excess hydrogen peroxide by b
13、oiling ( ). Thereafter, cool it to ordi- nary temperature. (2) Transfer the solution into a transfer flask of 100 ml by washing and dilute it up to the marked line with water ( 2). (3) Use an atomic absorption photometer, spray the solution into the flame of dinitrogen oxide-acetylene, utilize the h
14、ollow cathode lamp of beryl- lium as a light source and measure the absorbance at 234.8 nm in wave- length ( 3 ) . Notes (l) When the precipitates of insoluble zirconium and silicic acid are observed, filter the solution with a filter paper (class 5 B) , sufficiently wash it with hydrochloric acid (
15、1 + 100) and join the filtrate and the washings. When the amount of beryllium contained in this solution is not less than 50 pg, separately take the solution into a transfer flask of 100 ml so that the amount of beryllium becomes 20 to 50 pg, add 20 ml hydrochloric acid (1 + 1) and dilute it up to t
16、he marked line with water. procedure of 4.4 (3) . ( 2 ) Thereafter, operate it in accordance with the ( ) When aluminium is contained in a sample, utilize a deuterium lamp as a light source, measure the absorbance under the same con- ditions as those in the case of utilizing a hollow cathode lamp as
17、 the light source and allow the value obtained by subtracting; that value from the absorbance in the case of utilizing the hollow cathode lamp as the light source to be the absorbance of the sample. 4.5 Blank Test following operation. into several pieces of beakers (200 mi), cover each of them with
18、a watch glass and decompose hydrogen peroxide by boiling. Thereafter, cool it When Note () has been applied, carry out the same filtration washing operation as that of a sample. When Note (2) has been applied, after accurately diluting the amount of each solution to 100 ml with water, respectively s
19、eparately take the same amount as that of each sample solution into a beaker (200 mi) and add 20 ml hydrochloric acid (1 + 1) thereto . . After stepwise accurately adding O to 10 ml standard beryllium solution (O to 50 p g as beryllium), respectively transfer each of them into a transfer flask of 10
20、0 ml and dilute it up to the marked line with water. Hereinafter, operate it in accordance with the procedure of 4.4 (3) parallel to Obtain the value of a blank test in accordance with the Take 20 ml water, 20 ml hydrochloric acid (1 + 1) and 1 ml hydrogen peroxide c Copyright Japanese Standards Ass
21、ociation Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 07:21:24 MDTNo reproduction or networking permitted without license from IHS -,-,- I j JIS H*1339 7 4933608 0051017 T S 3 H 1339-1987 the sample In this case, allow the corr
22、ection by a deuterium lamp of Note (3) not to be carried out., prepare the relation curve between the obtained ab- sorbance and the amount of beryllium, carry out the parallel shifting thereof so that it passes through the origin and allow that to be the blank test working curve. from the absorbance
23、 of the solution without addition of standard beryllium solution to be the blank test value. . Use this blank test working curve and obtain the amount of beryllium Further , when the absorbance of the solution without addition of standard beryllium solution is remarkably low, use only reagents, carr
24、y out the operation in accordance with the procedures of 4.4 (1) to (3) parallel to the sample When Note (2) has been applied, separately take the same amount as that of a sample solution. to be carried out. and allow the blank test value to be obtained by using the working curve prepared in 4.6. We
25、igh out each 1. O g magnesium, trans- fer it into each of several pieces of beakers (200 mi), decompose it in accordance with the procedure of 4.4 (1) and cool it to ordinary temperature. respectively transfer the solution into a transfer flask of 100 ml by washing with water When Note (2) is applie
26、d , after further diluting it up to the marked 2d line with water, respectively separately take the same amount as that of sample solution of each solution into a transfer flask of 100 ml and add 20 ml hydrochlo- ric acid (1 + 1) thereto. solution ( O to 50 yg as beryllium) and dilute it up to the m
27、arked line with water. Hereinafter, operate it in accordance with the procedure of 4.4 (3) parallel to the sample In that case, allow the correction by a deuterium lamp of Note ( 3 ) not to be carried out .I , prepare the relation curve between the obtained ab- sorbance and the amount of beryllium a
28、nd carry out the parallel shifting thereof -so that it passes through the origin and take that curve as the working curve. curve prepared in 4.6 and the content of beryllium in the sample. shall be cal- culated from the following formula: Further, allow the correction by a deuterium lamp of Note (3)
29、 not 4.6 Preparation of Working Curve Thereafter, Stepwise accurately add O to 10 ml standard beryllium 4.7 Calculation The amount of beryllium shall be obtained from the working A W Beryllium (%) = -xi00 where A : detection amount of beryllium in sample solution (g) W : weighing o amount of sample
30、(g) Acetylacetone Extraction Atomic Absorption Method 5. 5.1 Purport A sample is decomposed with hydrochloric acid and hydrogen The generated peroxide, joined by EDTA and EDTA complex is generated by heating. After masking coexisting elements such as aluminium or the like, acetylacetone and sodium a
31、cetate are added and its pH is regulated at 6, O to 6.2. acetylacetone complex of beryllium is extracted with butyl acetate and the absorbance of beryllium of an organic phase is measured by using an atomic - absorption photometer. 5.2 Reagents The reagents shall be as follows: (1) Hydrochloric acid
32、 (1 + 1, 1 + 100) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 07:21:24 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S H*L339 87 9 4933608 005L018 L m 4
33、H 1339-1987 Sodium hydroxide solution (2 w/v %) Magnesium Ditto in 4.2 (2). Hydrogen peroxide Sodium Sulfat e (an hydride) Sodium acetate solution 60 g sodium acetate (trihydrate) is dissolved with water and the amount of solution is diluted to 200 ml with water. Disodium ethylenediaminetetraacetate
34、 (EDTA) solution 100 g disodium ethylenediaminetetraacetate (dihydrate) is joined by 300 ml water, dis- solved by dropping sodium hydroxide solution (20 w/v %) and the amount of solution is diluted to 500 m l with water. Acetylacetone solution (15 v/v %) Butyl, acetate Standard beryllium solution (
35、1 pgBe/ml) standard beryllium solution of 4.2 (4) is accurately diluted 5 times with water at each service. A necessary amount of 5.3 Weighing Out Amount of Sample The weighing out amount of a sample shall be 0.50 g. 5.4 Operation The determination operation shall be carried out in ac- cordance with
36、 the following procedures : Carry out the operation in accordance with the procedure of 4.4 (1) ( 4). Add 20 m l EDTA solution and boil it for approx. 1 min by heating. After cooling, add 2 ml acetyl acetone solution and 10 ml sodium acetate solution, regulate ( 5 , pH of the solution at 6. O to 6.2
37、 by using sodium hydroxide solution and hydrochloric acid (1 + 1) and leave the solution as it is for approx. 10 min. Transfer the solution into a separately funnel (200 mi) by washing with water and dilute the amount of solution to 150 ml with water. Accurately add 10 ml butyl acetate and mix them
38、by violently shaking for 2 min. solution phase and dehydrate the organic phase ( 6 ) . After separating it into two layers, discard the aqueous Utilize an atomic absorption photometer, spray the organic phase into the flame of dinitrogen oxide - acetylene and measure the absorbance at 234.8 nm in wa
39、velength. Notes (4) When the amount of beryllium contained in this solution is not less than 5 pg, transfer the solution into a transfer flask of 100 ml by washing with water and dilute it up to the marked line with water. so that the amount of beryllium becomes 2 to 5 p g and adjust the amount of s
40、olution at approx. 40 m l by adding water. Thereafter, separately take it into a beaker (200 mi) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 07:21:24 MDTNo reproduction or networking pe
41、rmitted without license from IHS -,-,- I 1 , JI$ H*1339 87 I 4733608 005L019 3 I 5 I H 1339-1987 I , Notes ( ) Utilize a pH meter. ( 6, Pack dry filter paper (class 2) or absorbent cotton into the leg part of a separatory funnel for dehydration and pass the organic phase therethrough. Otherwise, tra
42、nsfer it into the Erlenmeyer flask with ground-in stopper containing sodium sulfate (an- hydride) and mix them by shaking. 5.5 Blank Test Obtain the value of a blank test in accordance with the following operation : 7 Take 20 ml water., 20 ml hydrochloric acid (1 + 1) and 1 ml hydrogen per- oxide in
43、to several pieces of beakers (200 mi), cover each of them with a watch glass,. and decompose hydrogen peroxide by boiling. Note () is applied, carry out the same filtration washing operation as that for a sample. Further, when Note ( 4 , is applied, accurately dilute the amount of each solution to 1
44、00 ml with water. Thereafter , respectively separately take the same amount thereof as that of the sample solution into a beaker (200 mi) and control the amount of solution at approx. 40 ml by adding water. Step- wise accurately add O to 5 ml standard beryllium solution (O to 5 vg as beryllium), her
45、einafter carry out the operation thereof parallel to the sample in accordance with the procedures of 5.4 (2) to (4), prepare the relation curve between the obtained absorbance and the amount of beryllium, carry out its parallel shifting so that the relation curve passes through the origin and allow
46、it to be the blank test working curve. Use this blank test working curve and obtain the amount it of beryllium from the absorbance of the solution without addition of standard beryllium solution to be the blank test value. Thereafter, cool it When -5) Further, when the absorbance of the solution wit
47、hout addition of standard . beryllium solution is remarkably low, use only reagents , carry out the operation thereof parailel to the sample in accordance with 5.4 (1) to (4) When Note ( 4 , has been applied, separately take the same amount thereof as that of sample solution. and allow the blank tes
48、t value to be obtained by using the working curve prepared in 5.6. transfer them into several pieces of beakers (200 mi) , decompose each of them in accordance with the procedure of 5.4 (I) and cool it to ordinary temperature When Note () is applied, after accurately diluting the amount of each solu
49、tion to 100 ml with water, respectively separately take the same amount thereof as that of the sample into each beaker (200 mi) and adjust the amount of solution at approx. 40 ml by adding water. beryllium solution ( O to 5 vg as beryllium), hereinafter operate each of them . parallel to the sample in