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1、 1 I J I S H*:lbb4 88 4933b08 0053447 2 t- a rdk JAPANESE INDUSTRIAL STANDARD Methods for Determination of Hydrogen in Zirconium and Zirconium Alloys JIS H 1 6 6 4 - 1 9 8 8 Translated and Published by Japanese Standards Association Printed in Japan 8s I I JIS H*Klbb4 88 m 4933b08 0053448 4 m I In t
2、he event of any doubt arising, the original Standard in Japanese is to be final authority. . . UDC 669.296: 669.296.5: 543.062: 546.11.062 JAPANESE INDUSTRIAL STANDARD J I S Methods for Determination of Hydrogen in H 1664-1988 Zirconium and Zirconium Alloys i. Score This Japanese Industrial Standard
3、 specifies the methods for determination of hydrogen in zirconium and zirconium alloys. Remark: The units given in 1 in this Standard are in accordance with the International System of Units (SI) and are appended for informative reference. Further, the part where conventional units and units by SI g
4、iven in 1 thereafter are given in this Standard shall be converted to units specified in Appendix on and after January 1, 1991. 2, General Matters General matters common to the methods of chemical analysis shall be in accordance with JIS H 1650 and JIS Z 2614. 3. Classification of Determination Meth
5、ods 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 0.005 wt % excl. in hydrogen content. (2) Inert Gas Fusion-Gas Chromatograph
6、y sample of 0.0001 wt % and over to 0.005 wt % excl, in hydrogen content. This method applies to the 4. PreDaration of SamDle The preparation of a sample shail be in accordance with either one of the following met hods : (1) File Polishing (1) of JIS Z 2614. The file polishing shall be as prescribed
7、 in 4.5.1 (2) _ Chemical Polishing After dipping a sample into the mixed solution of 100 ml nitric acid (1 + 1) and 5 ml hydrofluoric acid, it is successively washed with water, ethanol, and acetone for each one minute by using an ultrasonic cleaner and dried by sending air. Applicable Standards: JI
8、S H 1650-General Rules for Chemical Analysis of Zirconium and JIS Z 2614-General Rules for Determination of Hydrogen in Metallic Zirconium Alloys Materials JIS H*1bb4 88 4933608 0051450 2 1 2 H 1664-1988 5. Weighing-Out Amount of Sample The weighing-out amount of a sample shall be 0.3 g, 6. Vacuum H
9、eating-Constant Volume Manometric Method 6.1 Summary A sample is heated with an electric resistance heating furnace under vacuum and hydrogen together with other gases are extracted to be collected in a constant volume. Then, its pressure is measured. Hydrogen in this collected gas is oxidized by he
10、ated copper (II) oxide to prepare water. After absorbing it in diphosphorus pentoxide, the pressure is measured. 6.2 Materials and Reagents The materials and reagents shall be in ac- cordance with 3.2.2 (1) of JIS Z 2614. 6.3 Apparatus JIS Z 2614( 1) (2) is connected to the gas analysis part of 3.3.
11、1 (2) in JIS Z 2614 to be used. For the apparatus, the gas extraction part of 3.2.2 (2) in 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 transpar
12、ent quartz tube of 25 to 40 mm in bore and 300 to 400 mm in length and fitting another end thereof to a water cooling type glass cap by grinding is used as the extraction furnace, The furnace tubeis equipped with a side tube for connecting the furnace tube to a gas extraction pump and a side tube fo
13、r filling a sample. An example of the extraction furnace is given in Attached Fig, 1. 6.4 Operation 6.4.1 Preparatory Operation The preparatory operation shall be carried out in accordance with the following procedures : (1) Connect a furnace tube to a water cooling type glass cap by using I vacuum
14、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 centre of the heating part. Carry out the operation in accordance with the procedures of 5.1.3 (1) (b) t
15、o 5.1.3 (2) (d) of JIS Z 2614(3). (2) , Note (3) In the operation of 5.1.3 (2) (c) to (d) of 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 temperatur
16、e. However, instead of this operation, apply power to a tubular electric resistance heating furnace and heat the furnace tube at 1100 to 1150OC in gas extraction temperature. J I S H*kLbb4 88 W 4933608 0051451 4 mp 3 H 1664-1988 6.4.2 Determination Operation The determination operation shall be carr
17、ied out in accordance with 5.1.4 (2) of JIS Z 2614. However, though a graphite crucible is heated at a gas extraction temperature in the opera- tion of 5.1.4 (2) (a-1) of JIS Z 2614, a furnace tube is kept at a gas extraction temperature instead of it. The gas extraction temperature shall be 1100 to
18、 1150% and gas collection time shall be 15 minutes. 6.5 Blank Test The determination operation of 6.4.2 shall be carried out without using a sample. 6.6 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, a conversion facto
19、r shall be preliminarily calculated in 7. Inert Gas Fusion-Gas Chromatography 7.1 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
20、 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 through the separation column, hydrogen or water is separated from other gases, introduced to a heat conductivity detector and the variation of heat conductiv
21、ity due to hydrogen or water is measured. 7.2 Materials and Reagents The materials and reagents shall be as follows: (1) Tin (Granular or Disklike) (2) Argon or Helium(4) That of not less than 99.99 vol %. (3) Hydrogen That of not less than 99.99 vol %. (4) Graphite Crucible That conforming to an im
22、pulse furnace. Its example is given in Attached Fig. 2. Note ( 4 , Argon is used in the case where the extracted hydrogen is measured as it is and helium is used in the case where it is measured after conversion to water. 7.3 Apparatus The apparatus is composed of an inert gas cleaning part, a gas e
23、xtraction part, a gas separation part, a gas measurement part, a hydrogen cleaning part for inspection, a gas inspection part , etc. (Attached Fig. 3 and Attached Fig. 4) ( 5 ) . Note ( 5, The constitution, structure and use conditions of an apparatus is different according to the apparatus to be us
24、ed. (i) Inert Gas Cleaning Part The inert gas cleaning part is composed of an oxidation tube, a carbon dioxide absorption tube, a dehydration tube , an electric resistance heating furnace, etc. (a) Oxidation Tube A stainless steel tube packed by copper (II) oxide (granular). It is heated in the elec
25、tric resistance heating furnace to be used. I J I S H*3bb4 88 m 4733608 0053452 b I 4 H 1664-1988 (b) Carbon Dioxide Absorption Tube A glass tube packed by soda lime, soda asbestos, or sodium hydroxide. (c) Dehydration Tube A glass tube packed by magnesium perchlorate or diphosphorus pentoxide. (2)
26、Gas Extraction Part projecting device, an impulse furnace, etc, The gas extraction part is composed of a sample (a) Sample Projecting Device into an impulse furnace in an inert gas atmosphere. A device which can project a sample (b) Impulse Furnace This furnace is composed of an upper water cooling
27、electrode which is made of copper to be fixed, a lower water cooling electrode which can be vertically moved, etc., of which a graphite crucible 7.2 (4) pinched between both electrodes can be heated to 1700 to 250OOC in several seconds by application of electric power. (3) Gas Separating Part The co
28、nstitution of a gas separation part differs in the case of measuring extracted hydrogen as it is and in the case of measurement after conversion to water. In the Case of Measurement of Hydrogen as It Is separation part is composed of a dust collection tube, an oxidation tube, a carbon dioxide absorp
29、tion tube, a de- hydration tube, a separation column, etc, (Attached Fig, 3). The gas Dust Collection Tube A glass tube packed by glass wool. Oxidation Tube (diiodine pentoxide as main constituent) . Carbon Dioxide Absorption Tube (1) (b). A glass tube packed by Schutze reagents As prescribed in 7.3
30、 Dehydration Tube As prescribed in 7.3 (1) (c) . Separation Column A stainless steel tube or ethylene tetra- fluoride resin tube packed by synthetic zeolite or silica gel. In the Case of Measurement after Conversion to Water The gas separation part is composed of a dust collection tube, an oxidation
31、 tube, a separation column, etc. (Attached Fig. 4). Dust Collection Tube As prescribed in 7.3 ( 3) (3.1) (a), Oxidation Tube As prescribed in 7.3 (1) (a). Separation Column tetrafluoride resin tube packed by filler of a porous polymer series. A stainless steel tube or a ethylene I (4) Gas Measuremen
32、t Part heat conductivity detector, an indicating instrument, etc The gas measurement part is composed of a J I S H*:1bb4 88 W 4933b08 0053453 8 5 H 1664-1988 (a) Heat Conductivity Detector It is composed of a contrast cell into which thermistors having uniform characteristics are inserted, a sample
33、cell, . etc (b) Indicating Instrument It is an indicating instrument by which an electric signal based on hydrogen or water detected with a heat conductivity detector can be read out. (5) Measuring Hydrogen Cleaning Part The measuring hydrogen cleaning part is composed of a carbon dioxide absorption
34、 tube, a dehydration tube, etc. (a) Carbon Dioxide Absorption Tube As prescribed in 7 . 3 (1) (b) . (b) Dehydration Tube As prescribed in 7.3 (1) (c) . (6) Gas Inspection Part inspection tube, and others( 5 ) . Gas inspection tube The gas inspection part is composed of a gas A stainless steel tube o
35、f a known volume. 7.4 Operation( 6 , 7.4.1 Preparatory Operation The preparatory operation shall be carried out in accordance with the following procedures : (1) After supplying cooling water and argon or helium 7.2 (2) 3 to an apparatus, turn on the power source. Set each part of the apparatus at s
36、pecific conditions and stabilize each part of the apparatus. Install a new graphite crucible 7.2 (4) at a specific position, apply power to an impulse furnace and heat the graphite crucible at a degassing temperature( 7). (2) (3) Heat the graphite crucible of (2) at a gas extracting temperature( ) a
37、nd read out the value of an indicating instrument Repeat this operation until a stable value of the indicating instrument can be obtained( ). Notes (6) ( 7 Since the fine procedure of the operation differs according to the apparatus to be used, follow the procedure designated for said apparatus. Rea
38、d a current value flowing to a graphite crucible by taking it as a parameter for a temperature of the graphite crucible and confirm that it is higher than a current value in gas extraction. Preliminarily obtain the optimum current value in gas ex- traction by using zirconium or zirconium alloy havin
39、g a known hydrogen content. Repeatedly use the graphite crucible degassed in 7.4.1 (2). J I S H33bb4 88 W 4933b08 0053454 T E I 6 H 1664-1988 7.4.2 Determination Operation The determination operation, in succession to the preparatory operation, the blank test, and the preparation of working curve, s
40、hall be carried out in accordance with the following procedures: (i) (2) Weigh out a sample and put it into a sample projecting device, Put tin( O) into a new graphite crucible 7.2 (4) 1 and install it at a specific position, Apply. power to an impulse furnace, heat the graphite crucible at a degass
41、ing temperature(7) and degas the graphite crucible and the tin, (3) Project the sample into the graphite crucible, heat the graphite crucible at a gas extracting temperature( by applying power to the impulse furnace and read out the value of an indicating instrument. Note ( O ) Since an additional a
42、mount of tin differs according to the apparatus to be used, preliminarily obtain an amount suitable for the apparatus by using zirconium or zirconium alloy having a known hydrogen content. 7.5 Blank Test The blank test, in succession to the preparatory opera- tion, shall be carried out in accordance
43、 with the following procedures( 6, : (1) Put the same quantity of tin as that of tin used in 7.4,2 (2) into a new graphite crucible 7.2 (4) and install it at a specific position. Apply power to an impulse furnace under the same conditions as in 7.4.2 (2) , heat the graphite crucible at a degassing t
44、emperature and degas the graphite crucible and the tin. Apply power to the impulse furnace under the same conditions as in 7.42 (3), heat the graphite crucible at a gas extracting tempera- ture and read out the value of an indicating instrument. (2) (3) Repeat the operations of (1) and (2) and obtai
45、n average value of values which have been read out. 7.6 Preparation of Working Curve The preparation of a working curve, in succession to the preparatory operation and the blank test, shall be carried out in accordance with the following procedures( ) : (1) Install a new graphite crucible 7.2 (4) at
46、 a specific position. Apply power to an impulse furnace under the same conditions as in 7.4.2 (2) and heat the graphite crucible at a degassing tempera- ture * (2) Use a gas inspection part, supply. a specific volume of hydrogen 7.2 (3) and read out the value of an indicating instrument. (3) Measure
47、 atmospheric pressure and the temperature of supplied hydrogen. (4) Repeat the operation of (2) several times and obtain average of read out values. 7 H 1664-1988 (5) Plot the average value of (4) to the mass( verted from the volume of hydrogen supplied in (2). Prepare the straight line connecting t
48、he plotted point to the origin and take it as the working curve. of hydrogen con- Note (”) The conversion from the volume of hydrogen to the mass of hydrogen shall be in accordance with the following formula (applicable to December 31, 1990). 2.016X P X V Mass Of hydrogen (g) = 6:236XlX(273+ t ) whe
49、re P : atmospheric pressure measured in (3) (mmHg) kPa) volume of gas inspection tube (mi.) temperature of hydrogen measured in (3) (OC) Y : f : However, in the case of the International System of Units (SI), the part of 6.236 x lo4 is made 8.314 x lo3. 7.7 Calculation The mass of hydrogen shall be obtained from the value read out in 7.4.2 (3) , the average value obtained in 7.5 (3), and the working curve prepared in 7.6 and the content of hydrogen in a sample shall be calculated from the following formula: Hydrogen content wt % = (Ai-Az)X1OO
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