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1、? *3 STD-JIS H L355-ENGL 1772 m 4733b08 05gVb83 TZ m UDC 669.71+669.7151:543.062:546.711 Th19 standard was revised in 12, 1992 JAPANESE I NDUSTRIAL STANDARD Methods for Determination of Manganese in Aluminium and Aluminium Alloy J IS H 1355-1972 This copy is an English version of Japanese Industrial
2、 Standard prepared by Japanese Standards Association, the copyright holder. Any further reproduction without permission is prohibited. I Transiation without guarantee In the event of any doubt arising, the original standard i n Japanese is to be evidence I l i Translated Japanese Standards Associati
3、on 1-24, Akasaka 4, Minato-ku Tokyo 107 Japan 0 J S A , m 4 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:22 MDTNo reproduction or networking permitted without license from IHS -,-,
4、- I. . . . , . .-:-. _, : + - . .-. . . , . - .- _.- , -.- . . _. . . . . r. y. - -7. ._ . . . . , I This English translation is prepared at the expense of Japan External Trade Organization (JETRO) . .- _ - i k Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=I
5、HS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:22 MDTNo reproduction or networking permitted without license from IHS -,-,- JAPANESE INDUSTRIAL STANDARD Methods for Determination of Manganese in J I S H 1355-1972 Aluminium and Aluminium Alloy (Reaff inned: 1984) 1. Scope
6、 This Japanese Industrial Standard specifies the methods for deter- mination of manganese in luminium and aluminium alloys. 2. General Requirements The general requirements in common with the chemical analysis shall be in accordance with JIS H 1351. 3. Methods for Determination 3.1 Classification of
7、 Methods The methods for determination of manganese shall be in accordance with one of the following methods: (1) Ammonium peroxydisulfate oxidizing sodium arsenite titration method and over i n manganese content. This method is applicable t o the sample of 0.05% (2) Ammonium peroxydisulfate oxidizi
8、ng absorptiometry (Method A) This method is applicable to the sample of manganese content ranging from 0.01 to 1.0% inclusive. (3) Ammonium peroxydisulfate oxidizing absorptiometry (Method B) This method is applicable to the sample of manganese content ranging from 0.001 to 0.025% inclusive. Referen
9、ce Standards: JIS H 1351-General Rules for Chemical Analysis of Aluminium and Aluminium A l 1 oy JIS K 8005-Primary Standard Substances for Volumetric Determination - 1 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bern
10、ie Not for Resale, 03/13/2007 08:22:22 MDTNo reproduction or networking permitted without license from IHS -,-,- STDOJIS H 1355-ENGL 1772 Li733b08 05LiLib8b 001 JAPANESE TANDARDS 3.2 Ammonium Peroxydisulfate Oxidizing Sodium Arsenite Titration Method 3.2.1 Surmnary The sample is dissolved with sodiu
11、m hydroxide solution, and it is acidified by adding mixed acid, and after manganese has been to permanganate with silver nitrate and ammonium persulfate, it is with the sodium arsenite standard solution. Reagents The reagents shall be as given in the following: Mixed acid: of water and after this ha
12、s been cooled, admix 250 mR of nitric acid and 150 mR of phosphoric acid. Add 200 mll of sulfuric acid carefully into 400 mR Sodium hydroxide solution: in 100 mR of water, store in a-polyethylene bottle, and use this supernatant. Dissolve 20 g of sodium hydroxide Hydrogen peroxide water (1+9) Ammoni
13、um persulfate. Silver nitrate solution (1 Wlv X) Standard manganese solution (0.2 mg Mnlml): Weigh out 0.200 g of metallic manganese (99.9% and over) into a beaker, add 20 mi2 of nitric acid (l+l) to decompose, and after nitrogen oxides have been expelled by boiling for several minutes, cool and dil
14、ute to 1000 mR correctly. - 2 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:22 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS H 1355-ENGL 1772 L
15、i733bO 05YLib7 T4 STANDARDS (7) Sodium arsenite standard solution: Weigh out 0.65 g of arsenic trioxide (arsenious acid) (JIS R 8005) correctly into a beaker, add 2 g of sodium carbonate (anhydrous) and approxi- mately 150 mR of water to this, heat to dissolve completely, transfer to a 1000 m i Z me
16、asuring flask and, after it has been diluted to the marked line with water, allow to stand for one day and night, then filter and use. solution corresponds to about 0.2 mg of manganese, the stan- dardization shall be carried out as given in the following: Although 1 mR of this Weigh out 1 g of high
17、purity aluminium, add a definite quantity of the standard manganese solution, and carry out titration in accordance with the procedure specified in 3.2.4(1) “addition of the sodium hydroxide solution“ and the following, as ap- propriate, and obtain the quantity of manganese corresponding to 1 mR of
18、the sodium arsenite standard solution from the following formula: where f-= quantity of manganese corresponding to 1 mR of the sodium arsenite standard solution (g) !G = quantity of manganese in 1 mR of the manganese standard solution (g) VI = added quantity of the manganese standard solut ion (mR)
19、V2 = consumption of the sodium arsenite standard solution (ma) - 3 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:22 MDTNo reproduction or networking permitted without license from
20、 IHS -,-,- STD-JIS H 1355-ENGL L992 4933b08 05?!4b88 904 JAPANESE STANDARDS 3.2.3 Weight of Sample to Be Weighed out The sample shall generally be weighed out in accordance with Table 1, according to the assumed manganese contents. Table 1 Weight of sample to be weighed out (g Assumed manganese cont
21、ent (X) 1.0 I 0.05 and over, up to 1.0 1.0 and over, up to and incl. 2.0 0.50 3.2.4 Procedure The procedure for determination shall be carried out in accordance with the following steps: Weigh out the sample into a conical beaker (500 ma), cover it with a watch glass, add 20 mi of the sodium hydroxi
22、de solution, and wait until it becomes quiet, and then wash the watch glass and the inner wall of the beaker, add 5 ma of the hydrogen peroxide water (1+9), and heat to decompose completely. After cooling, add 45 mR of the mixed acid, heat to make up as the transparent solution, further boil to expe
23、l nitrogen oxides, add warm water to make up to approximately 200 mR. Add 3 m l l of the silver nitrate solution and 3 g of the ammonium persulfate, heat to boil for 2 to 3 min. ( ), make it colourate sufficiently, cool to 25C or under in current water. Iuune- diately titrate with the sodium arsenit
24、e standard solution. 1 1 ( ) Boil to such a degree that small bubbles could disappear, as almost all of the ammonium Dersulfate being decomoosed. - 4 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale,
25、03/13/2007 08:22:22 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS H 1355-ENGL 2772 9933b08 0599b87 810 STANDARDS 3.2.5 Calculation The manganese content in the sample shall be calculated from the following fofmula. Manganese ( % i - - v x f x100 w where V = consum
26、ption of the sodium arsenite standard solution (mg) f = quantity of manganese corresponding to 1 mi of the sodium arsenite standard solution (g) -. - IV = weighed out quantity of the sample (8) 3.3 Ammonium Persulfate Acidified Absorptiometrv (Method A) 3.3.1 Summary The sample, after it has been de
27、composed with sodium hydroxide solution, is acidified by adding mixed acid, and this is boiled, adding silver nitrate and ammonium persulfate, oxidize the manganese to permanganate, and the absorbance is measured. 3.3.2 Reagents The reagents shall be as given in the following: (1) Mixed acid A: Add
28、200 mR of sulfuric acid into 400 mR of water carefully and, after this has been cooled, admix 250 mR of nitric acid and 150 mR of phosphoric acid. (2) Mixed acid B: Add 60 mR of sulfuric acid into 370 mR of water carefully and, after this has been cooled, admix 100 mR of nitric acid and 70 mR of pho
29、sphoric acid. (3) Sodium hydroxide solution: Refer to 3.2.2(2). ( 4 ) Ammonium persulfate (5) Silver nitrate solution (i v/v X) - 5 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:2
30、2 MDTNo reproduction or networking permitted without license from IHS -,-,- STD JIS 0.3 and over, up to and incl. 1.0 H 1355-ENGL o. 20 JAPANESE STANDARDS ( 6 ) Urea solution (10 “/v X) (7) Sodium nitrite solution (10 “il- X) (8) Manganese standard solution ( 0 . 1 mg Mn/mi): Weigh out 0.100 g of me
31、tallic manganese (99.9% min.) into a beaker, add 20 mR of nitric acid (l+l) to decompose and, after it has been boiled for several minutes, cool to an ordinary temperature, then transfer it to a 1000 m2 measuring flask, and dilute up to the marked line with water. 3.3.3 Weight of Sample to Be Weighe
32、d out be weighed out in accordance with Table 2, according to the assumed manganese contents. The sample shall generally . . . Table 2 Weight of sample to be weighed out ( 8 ) Assumed manganese content (2) 0.01 and over, up to 0.05 I 1.0 - 1 0.05 and over, up to 0.3 0.50 3.3.4 Procedure The procedur
33、e for determination shall be carried out in the following steps. 1 (1) Weigh out the sample ( into a beaker (300 me), cover it with a watch glass, add 15 m l , of sodium hydroxide solution gradually, and heat quietly to decompose perfectly. After cooling, after it has been acidified by adding 3.0 me
34、 of the mixed acid A while mixing up, heat to dissolve soluble salts, and 2 boil quietly to expel nitrogen oxides ( 1. - 6 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:22 MDTNo r
35、eproduction or networking permitted without license from IHS -,-,- STD=JIS H 1355-ENGL 1992 m 4733b 0544b71 477 W STANDARDS (2) After this has been made up to approximately 80 mR by adding warm water, add 5 mR of silver nitrate solution and, at the same time when it begins boiling by heating, add 3
36、g O amonium persulfate dividing into several times, furthermore, after it has been boiled succeedingly for about 1 min, cool down to about 25C or under using cold water. t o a 100 mR measuring flask, and dilute to the marked line with water. Transfer this ( 3 ) Take a part of this solution into the
37、absorption cell O the photometer, and measure the absorbancy at a wavelength of about 550 nm ( 4 using contrast solution ( 3 ) . 3.3.5 Calculation The manganese content in the sample shall be calculated from the following formula, obtaining the quantity of manganese from the calibration curve prepar
38、ed by 3.3.6. 4 W Manganese (/“)=-xlOo where -A-= detected quantity of manganese in the sample solution (g) _ - W = weighed out quantity of the sample (8) 3.3.6 Preparation of Analytical Curve Add 15 mR of the sodium hydroxide solution and 30 mR of the mixed acid A into several pieces of beakers, tak
39、e from O to 20 mR (from O to 2 mg a s manganese) of the manganese standard solution into these stepwisely, and dilute these to make up to approximately 80 mR by adding water. Hereinafter, operate in accordance with the procedure specified in 3.3.4(2) “addition of the silver nitrate solution“ and the
40、 following and prepare a correlation curve, between the obtained absorbances and quantities of manganese to serve as the analytical curve. - 7 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2
41、007 08:22:22 MDTNo reproduction or networking permitted without license from IHS -,-,- 1 Notes ( ) In the case of sample of high silicon content, add 30 mg of the mixed acid B to the sample, heat quietly to decompose, add 30 mQ of water and filter insolubles, and rinse thoroughly with warm water. Co
42、mbine the filtrate with washing, and heat to evaporate until the volume of solution becomes approxi- mately 80 mQ. accordance with the procedure specified in 3.3.4(2) “addition of the silver nitrate solution“ and the following. Hereinafter, determine the manganese. in 2 ( ) If any precipitates of si
43、licon and other have been observed, filter and rinse with warm water. 3 ( ) The contrast solution shall be prepared, extinguishing the colour of permanganate by dripping 10 mR of the. urea soJution and several drops of the sodium nitrite solution into the coloured residual solution in the measuring
44、flask. 4 ( Measure the absorbancy within 30 min after colouration. 3.4.1 Summary The sample is decomposed with sodium hydroxide solution, and after its acid concentration has been regulated by adding mixed acid, silver nitrate and ananoniun persulfate are added, and manganese is oxidized into perman
45、ganate by boiling, and then the absorbancy is measured. 3 . 4 . 2 Reagents The reagents shall be as given in the following: (1) Mixed acid A. Refer to 3.3.2(1). (2) Sodium hydroxide solution. Refer to 3.3.2(2). - 8 - Copyright Japanese Standards Association Provided by IHS under license with JSALice
46、nsee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/13/2007 08:22:22 MDTNo reproduction or networking permitted without license from IHS -,-,- STDmJIS H 1355-ENGL 1992 Li933b08 0544b73 241 (3) Silver nitrate solution (i w/v %l. ( 4 ) Annnonium persulfate solution (20 “IV X) . A solut
47、ion which is within 10 hours after preparation is t o be used for this solution. ( 5 ) Sodium nitrate solution (10 wlv X) (6) Urea solution (10 “IV %l. (7) Manganese standard solution (20 ug Mn/mR) take a definite volume of solution which has been prepared i n accordance with 3.3.2(8), and dilute to
48、 5 times correctly with water. 3.4.3 Weight of Sample to Be Weighed out A sample of 2.0 g shall be weighed out. 3.4.4 Procedure The procedure for determination shall be carried out i n accordance with the following steps: (1) Weigh out the sample in a beaker (300 ma), cover it with a watch glass, add 30 ma af the sodium hydroxide solution gradually, and heat quietly t o decompose completely. Cool, and after this has been acidifi