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1、 STD-JIS H 1353-ENGL L99Li 4933b08 0544bLl Lob H UDC 669.714+669.715 : 543.062 : 546.72 JIS This standard was revised in 11, 1994 JAPANESE I NDUSTRIAL STANDARD Methods for Determination of Iron in Aluminium and Aluminium Alloy J IS H 1353-1972 This copy is an English version of Japanese Industrial S
2、tandard prepared by Japanese Standards Association, the copyright holder. Any further reproduction without permission is prohibited. I Translation wihout guarantee I ! in the event of any doubt arising, the original i . standard i n Japanese is to be evidence j I Translated Japanese Standards Associ
3、ation 1-24, Akasaka 4, Minataku Tokyo 107 Japan 0 JSA, 1984 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:29 MDTNo reproduction or networking permitted without license from IHS -,-,
4、- This English traslation is prepared at the expense of Japan External Trade Organization (JETRO) . - - .- - - -. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:29 MDTNo reproduction
5、 or networking permitted without license from IHS -,-,- UDC 669.714+669.7151:543.062:546.72 JAPANESE STANDARD AsscATooN JAPANESE INDUSTRIAL STANDARD J I S Methods for Determination of Iron in H 1353-1972 Aluminium and Aluminium Alloy (Reaffirmed: 1978) i. Scooe This Japanese Industrial Standard spec
6、ifies the methods for determi- nation of iron in aluminium and aluminium alloys. 2. General Reauirements The general requirenentc to JIS H 1351. 3. Classification of Methods used in common for analysis shall conform The methods for determination of iron shall conform to the appropriate one among tho
7、se specified in the following: (1) Potassium permanganate titration method: This method is applica- .ble for the sample of iron conterit greater than or equal to 0.1 2. (2) Sulfosalicylic acid absorptiometry: This method is applicable for the sample of iron content greater than or equal to 0.1 %. (3
8、) o-phenanthroline absorptiometry: This method is applicable for the sample of iron content up to and including 0.5 %. Reference Standards: JIS H 1351-General Rules for Chemical Analysis of Aluminium and JIS Ei 3108-Tiri Netal JIS K 8005-Primary Standard Substances for Volumetric Determination Alumi
9、nium A1 loy - 1 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:29 MDTNo reproduction or networking permitted without license from IHS -,-,- 4 . Pbtassium Permaneanate Titration Met
10、hod 4.1 Summary Decompose the sample with sodium hydroxide, oxidize iron with the addition of hydrogen peroxide solution and boil. Separate the precipitation by filtering, dissolve with nitric acid, and allow to settle. iron hydroxide with aqueous ammonia. filtering, reduce by the stannous chloride
11、reducing method, and titrate with potassium permanganate standard solution. Separate the precipitation by . 4.2 Reagent The reagent shall be as follows: Hydrochloric acid (l+l, 1+3, 1+100) Nitric acid Nitric acid (1+3, 1+100) Aqueous ammonia Sodium hydroxide solution: in 100 ml of water, and store i
12、n a bottle of polyethylene. And use the supernatant liquid. Hydrogen peroxide solution (1+9) Ammonium chloride Dissolve 20 g of sodium hydroxide Ammonium chloride solution (2 w / % 1 Stannous chloride solution: Take 100 ml of hydrochloric acid in a beaker, add 50 g of stannous chloride (dihydrate) l
13、ittle by little to dissolve while heating on a water bath, dilute with.water and make up the volume to 1 R. granulated tin (99.9 Z min., equal to or superior than the quality of Class 1A specified in JIS H 2108) into this solu- tion, and store in a brown reagent bottle. Put a little Mercuric chlorid
14、e solution (saturated one) c # - 2 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:29 MDTNo reproduction or networking permitted without license from IHS -,-,- Manganese sulphate so
15、lution: sulphate (tetrahydrate) i n 200 ml of water, add 175 m 1 of phosphoric acid, pour 350 m l of sulphuric acid (l+l) gradually t o this mixed solution, after cooling i n cool water, dilute with water t o make up the volume t o 1 I , and blend sufficiently. This solution shall be used on third o
16、r fourth day after preparation. Dissolve 90 g of manganese N/50 potassium permanganate standard solution: 0.63 g of potassium permanganate in 1 I of water, boil for 1 t o 2 hours gently with a flask, then allow to stand for a whole day and night at a dark place. Dissolve Filter the supernatant liqui
17、d with refined asbestos or sintered-glass f i l t e r , pour into a brown bottle that is steam washed for approximtely 30 minutes and without washed with water, and store at a dark place. The standardization of this solution shall be conducted as follows: Weigh out accurately 1.000 g of sodium oxala
18、te (JIS K 8005) i n a beaker (300 mi), dissolve with the addition of w a t e r , transfer to a 500 ml measuring flask, and dilute with water until it reaches t o the marked line. Take 25 ml aliquot from this solution i n a beaker (500 m1) with a pipette, add 200 rnl of hot water of 80 t o 90C and 10
19、 ml of sulphuric acid (l+l), keeping the liquid temperature at 60 to 70C, carry out titration gradually with potassium permanganate solution, and the t i m e when the liquid is slightly converted t o red shall be deemed as the end point. Since 0.05 g of sodium oxalate is equivalent t o 37.32 ml of N
20、/50 potassium permanganate standard solution and 1 mLof this is equivalent t o 0.001117 g of iron, the quantity of iron that is equivalent to 1 r n l of potassium permanganate solution which is consumed shall be calculated by the following formula: - 3 - Copyright Japanese Standards Association Prov
21、ided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:29 MDTNo reproduction or networking permitted without license from IHS -,-,- STD-JIS H 1353-ENGL L77LI I Li733b08 05LI4blb 798 JAPANESE STANDARDS O . 001117 ( g ) 37.32 (ml) A - f-
22、 where f = quantity of irm that is equivalent to 1 m l of N/50 potassium permanganate standard solution (g) A = consumption of N/50 potassium permanganate - standard solution (ml) 4.3 Weight of Sample t o Be Weighed out Weigh out 3.0 g of the sample. 4.4 Procedure The determination procedure shall b
23、e conducted as follows : Weigh out the sample (I) in a beaker (500 mi), cover with a watch glass, add 50 ml of sodium hydroxide solution, and heat t o decompose when the reaction becomes weak. tion of decomposition,of sample, dilute w i t 6 the addition of approximately 300 ml of warm water, add 5 m
24、 l of hydrogen peroxide solution (1+9) gradually while stirring to oxidize, and boil for several minutes. After the. comple- In this case, i f oxidation of iron is considered as not suffici- ent, add further hydrogen peroxide solution (1+9), allow t o stand until precipitation deposits completely, s
25、eparate by filtering with a filter paper (Class 5A), and wash with warm water. Dissolve and put the precipitation l e f t on the f i l t e r paper as f a r as possible with a little hot n i t r i c acid (1+3) into the former beaker. When it is difficult t o dissolve, dissolve with a little hydrogen
26、peroxide solution (1+9), and wash the f i l t e r paper with n i t r i c acid (1+100). Add approximately 100 m l of warm water and 5 g of ammonium chloride to the f i l t r a t e and the washing, then add aqueous ammonia, to produce precipita- tion of hydroxide, add further 5 ml of excess aqueous am
27、onia, heat until it is going t o boil, after settling of precipitation, - 4 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:29 MDTNo reproduction or networking permitted without lic
28、ense from IHS -,-,- STD*JIS H 1353-ENGL 1774 4933LOO 0544b17 b24 JAPANESE STANDARDS separate by filtering, and wash sufficiently with warmammonium chloride solution (*l. (4) Dissolve and put the precipitation with hot hydrochloric acid (1+3) as l i t t l e as possible into the former beaker, and was
29、h the f i l t e r paper with hot hydrochloric acid (1+100). Then heat this liquid to condense until the volume of liquid becomes up to and incl. approximately 5 ml, wash the inside w a l l of the beaker with a l i t t l e warm water, add stannous chloride drop by drop while shaking, at the time the
30、colour of ferric chloride i n the solution vanishes, add one to two drops of excess stannous chloride, and cool Sufficiently with cold water. (5) Add thereto 5 ml of mercuric chloride solution a t a time, allow to stand for 1 to 2 minutes, dilute with water to make up the volume t o 150 m l , add 30
31、 ml of manganese sulphate solution, and titrate with potassium permanganate standard solution while shaking. Notes (I) In the case of sample of rich silicon content, weigh out 1 g of sample, add 30 m l of hydrochloric acid (l+l), when vigorous reaction is completed, add 2 to 3 ml of sulphuric acid a
32、nd heat t o dissolve copper and the like. After separation of insoluble silicon, etc. by filter- ing with the addition of approximately 30 ml of warm water thereto, wash sufficiently with warm water. Neutralize the f i l t r a t e with the addition of sodium hydroxide solution, and continue t o add
33、excess sodium hydroxide solution until the formed aluminium hydroxide is dissolved completely. of hydrogen peroxide solution (1+9), heat and boil, allow t o stand for a while t o settle precipitation, separate by filtering, and wash Sufficiently with warm water. Further operations shall be conducted
34、 conform- ing to the procedure specified i n 4.4 ( 3 ) and the following t o determine iron. Then add approximately 5 ml - 5 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:29 MDTNo
35、 reproduction or networking permitted without license from IHS -,-,- STDOJIS H 1353-ENGL 1774 ii33b08 05114b38 5b0 m JAPANESE STANDARDS ASS PATION (2) In this case, if precipitation has blue of copper ion, dissolve this precipitation with hydrochloric acid (1+3), allow to precipitate once again with
36、 aqueous ammonia, and repeat the procedure until copper is remove d. 4.5 Calculation The content of iron contained in the sample shall be calculated according to the following formula: iron (%) = 7 x f x100 where V= consumption of N/50 potassium permanganate standard - -. solution (mi) f= quantity o
37、f iron equivalent t o 1 ml of N/50 potassium permanganate standard solution (8) - w= weighed out quantity of sample (g) 5. Sulfosalicylic Acid Absorptiornetry 5.1 Summary Dissolve the sample with mixed acid, dilute with water, adjust pH with aqueous ammonia and sulphuric acid, colourate with the add
38、ition of sulfosalicylic acid, and measure the absorbancy. 5.2 Reagent The reagent shall be as follows: Mixed acid (hydrochloric acid 3, nitric acid 2, water 8) Nitric acid (l+l) Sulphuric acid (1+3) Aqueous ammonia (1+3) Sodium acetate solution: water and make up the volume to 100 m l . Dissolve 10
39、g of sodium acetate i n - 6 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07:16:29 MDTNo reproduction or networking permitted without license from IHS -,-,- (6) Sulfosalicylic acid solu
40、tion: Dissolve 10 g of sulfosalicylic acid (dihydrate) i n water and make up the volume t o 70 to 80 ml, then adjust pH to f a l l i n the range of 2.0 to 2.5 with aqueous awonia (1+3), and dilute with water. to make up the volume to 100 ml. (7) Iron standard solution (0.1 mgFe/nl): Weigh out 0.100
41、g of pure iron (99.5 % min.), dissolve with 15 ml of n i t r i c acid (1+3), add 3 ml of sulphuric acid (1+3) and heat t o vaporize until the white fume of sulphuric acid is generated. After allow to cool, dissolve with the addition of water, cool up t o the room temperature, and dilute with water t
42、 o make up the volume to accurately 1000 mi. 5 . 3 Weight of Sample t o Be Weighed out Weigh out 1.0 g of the sample. 5.4 Procedure The determination procedure shall be conducted as Weigh out the sample i n a beaker (300 mi), cover with a watch glass, and add 50 ml of mixed acid t o dissolve (3). Bo
43、il for several minutes, cool up t o room temperature ( 4 ), transfer to a 250 ml measuring flask, and dilute with water until it reaches t o the marked line. Take exactly each 50 ml aliquot i n two beakers (200 ml) respectively, add 10 ml of sodium acetate solution respectively, add 5.0 ml of sulfos
44、alicylic acid to one of them, while no addition t o another beaker, and adjust pH to f a l l i n the range of 2.0 t o 2.5 by using aqueous ammonia (1+3) and sulphuric acid (1+3) so as t o the Thymol Blue test paper is colourated t o faint red. Transfer the liquids to two 100 ml measuring flasks resp
45、ectively , dilute with water until they reach to the marked lines, add sulfosalicylic acid and shake sufficiently to colourate iron. - 7 - Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/14/2007 07
46、:16:29 MDTNo reproduction or networking permitted without license from IHS -,-,- ( 4 ) Take a part of each solution i n the absorption cell of the photometer respectively, take the solution without the addition of sulfosalicylic acid as the contrast solution, and measure the absorbancy of wavelength
47、 of approximately 500 nm. Notes (3) When it is difficult to decompose the sample completely because of rich content of copper, add a little n i t r i c acid (l+l) to decompose ccmpletely . (4) In t h i s case, i f precipitation of silicon and the l i k e are appreciated, separate by filtering and wa
48、sh with warm water. 5.5 Calculation The quantity o.f iron shall be obtained from the analytical curve prepared by 5.6, and the content of iron in the sample shall be calculated according to the following formula: - - - Iron (%) = - A x100 W x B -_ where A= . W= -_ detected quantity of iron contained i n the sample solution (g) ratio of aliquot of the sample solution weighed out quantity of sample (g) 5.6 Preparation of Analytical Curve Weigh out a certain quantity