JIS-H-1695-1976-R1986-ENG.pdf
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1、JIS UDC 669.294 : 543.272.1 JAPANESE INDUSTRIAL STANDARD Methods for Determination of Oxygen in Tantalum JIS H 1695-1976 Translated and Published Japanese Standards Association Printed in Japan I 5 s Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employee
2、s/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 07:21:54 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 Standards Association Provided by IHS under
3、license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/11/2007 07:21:54 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S H*3695 76 = 4933608 0053643 2 M UDC 669.294:543.272.1 4.1 Summary Heat in vacuum the sample in graphite crusible as
4、 it is in solid state, make the oxygen in sample to carbon monoxide to extract together with other gases and collect in adefined volume to measure the pressure. Oxidize this collected gases by heated copper oxide to make the carbon monoxide to carbon dioxide and hydrogen to water. water by phosphoru
5、s pentoxide, freeze the carbon dioxide by liquid nitrogen and measure the pressure at every stage, Absorb the 4.2 Apparatus As for apparatus, use that in which the gas extraction system of 3.2.1 (2-1) of JIS Z 2613 and gas analysis system of 3.3.1 (2) are connected. h JAPANESE INDUSTRIAL STANDARD J
6、I S Methods for Determination of H 1695-1976 Oxygen in Tantalum (Reaffirmed: 1986) 1. Scope This Japanese Industrial Standard specifies the methods for determina- tion of oxygen in tantalum. 2. General Items The general items common to the methods for determination shall be in accordance with JIS H
7、1680 and JIS Z 2613. 3. Divisions of Methods For the determination of oxygen, one of the following methods applies: (1) Method by heating in vacuum and measuring pressure in constant volume . (2) Method by fusing in vacuum and measuring pressure in constant volume (3) Method by fusing in inert gas a
8、nd measuring of quantity of electricity 4. Method by Heating in Vacuum and Measuring Pressure in Constant Volume 4.3 Materials and Reagents The materials and reagents shall be in accordance with 6.1.2 of JIS Z 2613. 4.4 Sample 4.4.1 Sampling and Preparation of Sample The method of sampling and prepa
9、ration of sample shall be as follows: Applicable Standards : JIS H 1680-General Rules for Chemical Analysis of Tantalum JIS Z 2613-General Rules for Determination of Oxygen in Metallic Materials Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/111
10、1111001, User=Wing, Bernie Not for Resale, 03/11/2007 07:21:54 MDTNo reproduction or networking permitted without license from IHS -,-,- 2 H 1695-1976 (1) Elongation Material Sample A s for elongation material sample, sample specimen according to 4.3-1 of JIS Z 2613 and prepare the analytical sample
11、 according to 4.4.1 (1) or (2). However, use as cleaning solvent petroleum benzine and conduct warm air drying Further, set the conditions of electrolytic polishing as follows. An example of electrolytic polishing device is shown in Fig. 1. Electrolytic solution : hydrofluoric acid 1 + sulfuric acid
12、 3 (volume ratio) Electrolytic cell : Cathode : lead plate synthetic resin beaker (300 ml) Anode : sample (hold the sample by alumi- nium small pincette and hold this by stainless steel pincette) Electrolysis voltage : 1.1 to 1.7 V or 13.5 V Current density of anodic electrolysis : 5 to 9 A/dm2 or 8
13、 A/dm2 (2) Powder Sample As for powder sample, sample the specimen according to 4.3.2 of JIS Z 2613 and prepare analytical sample according to 4.4.2 (2). 4.4.2 Amount of Sample to Be Taken by Weighing According to oxygen content rate of sample, take, in general, by weighing to the nearest 1 m g acco
14、rding to Table 1. Table 1 Amount of analytical sample I to be taken by weighing g Oxygen content rate % Up to 0.05 0.05 and over, up to 0.5 0.10 to 0.30 0.30 to 5.0 4.5 Operation 4.5.1 Preparatory Operation Conduct the filling of analytical sample, evacuation ofing of graphite crucible according to
15、6.1.3 (i) to (2) of JIS Z 2613. However, do not use bath metal. Take the outgassing temperature as 2200 to 230OOC and the outgassing time as 2 to 3 h. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 0
16、3/11/2007 07:21:54 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS H%Lb95 76 W 4933608 0051b45 b 3 H 1695-1976 4.5.2 Operation for Determination Conduct the blank test, analysis of sample and calculation according to 6.1.4 (2) to (4) of JIS Z 2613 and determine the conv
17、ersion coefficient according to 6.1.4 (5) (b) . take the temperature of gas extraction as 21OO0C( l). However, Note ( l ) In this case, the gas collecting times are frequently 3 to 15 min. 5, Method by Fusing in Vacuum and Measuring Pressure in Constant Volume 5.1 Summary Heat in vacuum the sample w
18、ith using metal bath in graphite crucible to fuse, make the oxygen in sample to carbon monoxide to extract together with other gases and collect in a defined volume to measure the pressure. Oxidize this collected gas by heated copper oxide to make the hydrogen to water and the carbon monoxide to car
19、bon dioxide. water by phosphorus pentoxide, freeze carbon dioxide by liquid nitrogen and measure the pressure at each stage. Absorb 5.2 Apparatus As for apparatus, use that in which the gas extraction system of 3.2.1 (2-1) of JIS Z 2613 and gas analysis system of 3.3.1 (2) are connected. e 5.3 Mater
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