JIS-H-1619-1988-ENG.pdf

T L J I S H*lb19 88 4933608 0051259 1i I UDC 669.295 : 669.295.5 : 543.062 : 546.1 1 .O62 ,'JIS Q) JAPANESE INDUSTRIAL STANDARD Methods for Determination of Hydrogen in Titanium and Titanium Alloys Translated and Published by Japanese Standards Association Printed in Japan Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 04:28:47 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS H * l b l î 88 I 4933608 005l260 B UDC 669.295: 669.295.5: 543.062: 546.11.062 JAPANESE INDUSTRIAL STANDARD J I S Methods for Determination of Hydrogen H 1619-1988 in Titanium and Titanium Alloys 1. Scope This Japanese Industrial Standard specifies the methods for determination of hydrogen in titanium and titanium alloys. Remark: The units given in with the International System of Units (SI) and appended for informative reference. 1 in this Standard are in accordance Further, the part where conventional units and units by SI given in 1 thereafter are given in this Standard shall be converted to units specified in Appendix on and after January 1st , 1991, 2. General Matters General matters common to the methods of chemical analysis shall be in ac- cordance with JIS H 1611 and JIS Z 2614. 3, Classification of Determination Methods The method for determination of hydrogen shall be in accordance with either one of the following methods: (1) Vacuum Heating-Constant Volume Manometric Method This method applies to the sample of 0.0001 wt % and over to 0.02 wt % excl. in hydrogen content. (2) Vacuum Heating-Gas Chromatography This method applies to the sample of 0.0001 wt % and over to 0.02 wt % excl. in hydrogen content. (3) Inert Gas Fusion-Gas Chromatography This method applies to the sample of 0.0001 wt % and over to 0.02 wt % excl. in hydrogen content. 4. Vacuum Heating-Constant Volume Manometric Method 4.1 Summary A sample is heated with an electric resistance heating furnace in a vacuum and hydrogen together with other gases are extracted. They are collected in a definite volume and the pressure thereof is measured. Hydrogen in this collected gas is oxidized with heated copper (II) oxide to make water. After absorbing it in diphosphorus pentoxide, the pressure is measured. Applicable Standards: JIS H 1611-General Rule for Chemical Analysis of Titanium JIS Z 2614-General Rules for Determination of Hydrogen in Metallic Materials . Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 04:28:47 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS H*Iib19 88 4933b08 005L2bL T I Hydrogen content wt % 2 H 1619-1988 Weighing-out amount of sample g 4.2 Materials and Reagents Materials -and reagents shall be in accordance with 3.2.2 (1) of JIS Z 2614. 4.3 Apparatus For the apparatus, the gas extraction part.( 1)(2) of 3.2.2 (2) in JIS Z 2614 is connected to the gas analysis part of 3.3.1 (2) in JIS Z 2614 to be used. Notes () For the heating apparatus , a tubular electric resistance heating furnace is used and a high frequency induction heating system is not used. (2) A furnace tube prepared by sealing one end of a quartz tube of 25 to 40 mm in bore diameter and 300 to 400 mm in length and fitting another end thereof to a water cooling glass cap by grinding is used as the extraction furnace. The furnace tube is equipped with a side tube for connecting the furnace tube to a gas extraction pump and a side tube for filling a sample. An example of the extraction furnace is given in Attached Fig. 1. 4.4 ,Weighing out Amount of Sample A sample shall be weighed out to the nearest 1 mg in accordance with Table 1. Table 1. Weighing out Amount of Sample 4.5 Operation 4.5.1 Preparatory Operation The preparatory operation shall be carried out in accordance with the following procedures : (1) Connect a furnace tube to a water cooling glass cap by using vacuum grease, insert the furnace tube into the heating part of a tubular electric resistance heating furnace and fix the heating furnace so that the bottom part of the furnace tube is positioned at the center of the heating part, (2) Carry out the operation in accordance with the procedures of 5.1.3 (1) (b) to 5.1.3 (2) (d) in JIS Z 2614(3). Note (3) In the operation of 5.1.3 (2) (c) to 5.1.3 (2) (d) in JIS Z 2614, operate a high frequency induction oscillator and a blower, heat a graphite crucible at a degassing temperature and degas it for several hours. Thereafter, lower it to a gas extraction temperature. However, instead of this operation, pass electric current to a tubular electric re- sistance heating furnace and heat the furnace tube at 1100 to 115OOC in gas extraction temperature. 0,0001 and over to 0.01 excl.1 O. 30 0.01 and over to 0.02 excl. I o. 10 Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 04:28:47 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S H*LbLï 88 4733608 00512b2 L Hydrogen content wt % 0.0001 and over to 0.005 excl. 0.005 and over to 0.02 excl. 3 H 1619-1988 Weighing out amount of sample g O. 30 o. 10 4.5.2 Determination Operation The determination operation shall be carried out in accordance with 5.1.4 (2) of JIS Z 2614. However, though a graphite crucible is heated to a gas extraction temperature in the operation of 5.1.4 (2) (a-1) in JIS Z 2614, a furnace tube is kept at a gas extraction temperature instead of this. The gas extraction temperature shall be 1100 to 1150% and gas collection time shall be 15 minutes. 4.6 Blank Test The same determination operation as that of a sample shall be carried out without using the sample. 4.7 Calculation The calculation shall be as prescribed in 5.1.4 (3) of JIS Z 2614. accordance with 5.1.4 (4) of JIS Z 2614. However, conversion factor shall be preliminarily calculated in 5. Vacuum Heating-Gas Chromatography 5.1 Summary A sample is heated by using a graphite crucible in a vacuum and hydrogen is extracted together with other gases. After collecting the extracted gas into a gas buret by using a Toepler pump, hydrogen is separated from other gases by passing the collected gas through a separation column, conducted to a heat conductivity detector and the variation of heat conductivity due to hydrogen is measured. 5.2 Materials and Reagents The materials and reagents shall be as pre- scribed in 3.2.1 (1) of JIS Z 2614 and as follows: (1) Argon Argon of not less than 99.99 vol % (2) Hydrogen Hydrogen of not less than 99.99 vol % (3) Synthetic zeolite A type-calcium salt (for instance, molecular sieve 5 A) of 355 to 250 p m (equivalent to 40 to 60 mesh) 5.3 Apparatus For the apparatus, a mercury ejector pump for gas collection, a Toepler pump for gas collection, a gas buret, and a gas chromatograph are successively connected to the gas extraction part of 3.2.1 (2) in JIS Z 2614. separation column filled by synthetic zeolite 5.2 (3) and a heat con- ductivity detector shall be used. An example of the apparatus is given in Attached Fig. 2. However, the gas chromatograph equipped with a 5.4 Weighing out Amount of Sample A sample shall be weighed out to the nearest 1 mg in accordance with Table 2. Table 2. Weighing out Amount of Sample 5.5 Operation Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 04:28:47 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S H*1617 ô8 W 4933608 00512b3 3 4 H 1619-1988 5.5.1 Preparatory Operation The preparatory operation shall be carried out in accordance with the following procedures: Fill a sample in accordance with the procedures of 5.1.3 (1) in JIS Z 2614. Close a total cock, operate a oil rotary pump (T) and quietly open a cock Ci. After exhausting gas for about five minutes, operate a high frequency oscillator, heat a graphite crucible (i) at 2200 to 2300% and carry out degassing. When the indication of a Pirani gauge (k) becomes almost constant, operate a mercury diffusion pump for gas extraction (m) and a mercury ejector pump for gas collection (n) , open a cock C, close the cock Cl and continue degassing for about three hours. Flow argon 5.2 (i) by 20 ml per minute from an argon cylinder (W) about one hour before completion of degassing, turn on the power source of a gas chromatograph and set the temperature of a thermostatic tank at 5OOC. Open a cock C6 toward the introduction side of the gas chromato- graph and successively open cocks C 8 and C 9. When the mercury of a Toepler pump for gas collection (o) has completed to rise in a gas buret (p) , close the cock C 8. Then, open a cock C 5 and raise a mercury leveling bulb (r) . When the surface of mercury in the gas buret (p) has reached the inlet of the cock C6 , close the cock C 6 , ,return the mercury leveling bulb (r) to the original position and close the cock C5. Close the cock Cg, open a cock C7 on the exhaust gas system side connected to the oil rotary pump (T) and exhaust gas for five minutes. Thereafter, close the cock C 7 and keep a hydrogen gas reservoir (9) under vacuum. Regulate the temperature of the graphite crucible (i) at 1180 to 1220% in gas extraction temperature, close the cock C, and open a cock C3 and the cock CS. Alternately open and close the cock C 9 and the cock C 1 O , repeat the operation that the mercury of the Toepler pump for gas collection (o) is raised and lowered for about 15 minutes and collect extraction gas in the gas buret (p) . Thereafter, close the cock C 8. Open the cock C5, open the cock C6 on the introduction side of the gas Chromatograph while operating the mercury leveling bulb (r) and introduce the gas collected in the gas buret (p) into the gas chromatograph. Thereafter, close the cocks C6 and CS and measure the peak area of the gas chromatograph of hydrogen. Open the cock C 8 , repeat the operations of (8) and (9) until the peak height of the gas chromatograph of hydrogen becomes not more than 10 mm(4) and measure the peak area of the gas chromatograph of hydrogen obtained lastly. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 04:28:47 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS H*Lb19 88 W 4933b08 0053264 5 I 5 H 1619-1988 Note ( 4 , Regulate the sensitivity of a recorder so that the peak height per 1 p1 of hydrogen under standard state becomes about 10 mm. 5.5.2 Determination Operation The determination operation, in suc- cession to the preparatory operation, shall be carried out in accordance with the following procedures: (1) Keep a graphite crucible (i) at 1180 to 1220OC. (2) Project a sample and operate it in accordance with the procedures of 5.5.1 (8) and (9). 5.6 Blank Test The peak area measured in 5.5.1 (10) shall be taken as the peak area of a blank test. 5.7 Preparation of Working Curve The preparation of a working curve shall be carried out in accordance with the following procedures: ( 1) Open a cock C 7, fill a hydrogen gas reservoir (q) by hydrogen 5.5 (2) from a hydrogen cylinder (H) and close the cock C 7. Open a cock C 6 to the hydrogen gas reservoir (q) side, open a cock C5, take hydrogen into a gas buret (p) by operating the mercury leveling bulb (r) and close the cock C 6. Thereafter, measure the volume of hydrogen by operating the mercury leveling bulb (r) and besides, measure the atmospheric pressure and room temperature. Open the cock C 6 on the introduction side of the gas chormatograph, operate the mercury leveling bulb (r) , introduce hydrogen in the gas buret (p) into the gas chromatograph, close the cock C6 and the clock C5 and measure the peak area of the gas chromatograph of hydrogen. Repeat the operations of (2 1 and (3) so that the quantity of hydrogen introduced into the gas chromatograph becomes stepwise. Convert the volume of hydrogen introduced into the gas chromato- graph to the mass of hydrogen from the following formula (applicable till December 31, 1990). where p : atmospheric pressure measured in (2) (mmHg) EkPa) volume of hydrogen taken in gas buret in (2) (mi) However, in the case of International System of Units (SI), the part of 6.236 x lo4 shall be made 8.314 x lo3. V : t : room temperature measured in (2) (OC) Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/15/2007 04:28:47 MDTNo reproduction or networking permitted without license from IHS -,-,- ! J I S H*i(lbL9 88 m 4933b08 0053265 7 m 6 H 1619-1988 (6) Prepare the relation curve between the mass of hydrogen intro- duced into the gas chromatograph and the peak area, parallel transfer the relation curve so as to pass the origin and take said relation curve as the working curve. 5.8 Calculation Obtain the mass of hydrogen from the peak area obtained in 5.5.2 (2) and 5.6 and the working curve prepared in 5.7 and calculate the content of hydrogen in a sample from the following formula: Hydrogen content.wt % = exloo where A, : A2 : m : weighing out amount of sample (g) mass of hydrogen obtained from the peak area of mass of hydrogen obtained from the peak area of 5.6 (g) 5.5.2 (2) (g) 6. Inert Gas Fusion-Gas Chromatography' 6.1 Summary A sample together with tin is fused by heating with a graphite crucible according to an impulse system in a current of inert gas and hydrogen is extracted together with other gases. By passing the extracted gas as it is through a separation column, or otherwise by oxidizing the hydrogen in the extracted gas to be converted to water and then, passing it through the separation column, hydrogen or water is separated from other gases, introduced to a heat conductivity detector and the variation of heat conductivity due to hydrogen or water is measured. 6.2 Materials and Reagents The materials and reagents shall be as follows: (1) Tin (granular or disklike) (2) Argon or helium( 5 , (3) Hydrogen As prescribed in 5.2 (2). (4) Graphite crucible That conforming to an impulse furnace. That of not less than 99.9 vol %. Its example is given in Attached Fig. 3. Note ( 5 , In the case where the extracted hydrogen is measured as it is, argon shall be used, and in the case where it is measured after converting to water, helium, used. 6.3 Apparatus( ') The apparatus is composed of an inert gas cleaning part, a gas extraction part, a gas sep