《JIS-Z-2614-1990-R2005-ENG.pdf》由会员分享，可在线阅读，更多相关《JIS-Z-2614-1990-R2005-ENG.pdf（45页珍藏版）》请在三一文库上搜索。
1、UDC 543.272.2:669 JAPANESE INDUSTRIAL STANDARD General rules for determination of hydrogen in metallic materials JIS 2 2614-1990 Translated and Published by Japanese Standards Association Printed in Japan 23 S Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IH
2、S Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 22:28:37 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
3、IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 22:28:37 MDTNo reproduction or networking permitted without license from IHS -,-,- UDC 543.272.2:669 JAPANESE INDUSTRIAL STANDARD J I S General rules for determination of hydrogen in metallic ma
4、terials 2 2614-1990 1. Scope method of hydrogen in metallic materials. This Japanese Industrial Standard specifies the following general matters in determination (1) Method (2) Apparatus (3) Sampling and preparation of sample (4) Operation (5) Arrangement of results (6) Other matters Remark: The uni
5、ts and numerical values given in in this Standard are in accordance with the International System of Units (SI) and, appended for informative reference. Further, in this Standard the traditional units and the numerical values and the units according to SI and the converted value based on them in the
6、 thereafter are exchanged to the units and numerical values shown in on and after January 1, 1991. 2. Method This method is the method to determine by separating the hydrogen from other coexisting gases by heating or heat melting metallic sample in vacuum or inert gas flow and by extracting hydrogen
7、 in sample and is shown as follows. 2.1 Gas Extraction Method (a) High-temperature Vacuum Melting Method (b) Low-temperature Vacuum Melting Method Melt the sample in vacuum in a graphite In vacuum add tin as flux in a crucible, and extract the hydrogen together with other gases. refractories crucibl
8、e such as quartz to the sample, melt at a temperature not higher than the melting point of sample, and extract hydrogen together with other gases. In vacuum heat the sample at a temperature not higher than the melting point under the solid condition as it is to extract hydrogen together with other g
9、ases. Informative reference: There are a high temperature method and a low temperature method. (c) Vacuum Heating Method (d) Inert-gas Fusion Method (e) Inert-gas Heating Method Fuse the sample in a graphite crucible in an inert-gas flow, and discharge hydrogen together with other gases. melting poi
10、nt under the solid condition as it is in an inert-gas flow, and discharge hydrogen together with other gases. Heat the sample at a temperature not higher than the 2.2 Gas Analysis Method (a) Manometric Method at Constant Volume Collect the gas extracted from the sample into a vacuum container of a d
11、efinite volume to measure the pressure, remove the water generated by passing through oxidizing agent and dehydrating agent, again measure the pressure and calculate the hydrogen amount. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001,
12、 User=Wing, Bernie Not for Resale, 03/12/2007 22:28:37 MDTNo reproduction or networking permitted without license from IHS -,-,- 2 Z 2614-1990 (b) Gas Volumetric Method Together with collection of gas extracted from the sample, add oxygen, burn with a microgas analysis apparatus connected with burni
13、ng pipette, absorption pipette, and gas burette to absorb and calculate the hydrogen amount from oxygen consumption amount. (c) Palladium Transmission Method heated palladium tube, collect the transmitted hydrogen to measure the pressure, and calculate the hydrogen amount. Feed the gas extracted fro
14、m the sample into a (d) Thermal Conductivity Method Collect the gas extracted from the sample into a definite volume containing a thermal conductivity cell, measure the change of thermal conductivity due to hydrogen, and calculate the hydrogen amount. volume, introduce together with the carrier gas
15、such as argon into a thermal conduc- tivity cell through an absorption type separating tube, measure the change of thermal conductivity due to hydrogen, and calculate the hydrogen amount. (e) Gas Chromatography Collect the gas extracted from the sample into a definite 3. Apparatus gas extraction sys
16、tem, gas analytical system and others, and according to the method each unit apparatus in connected to be consisted. An example of constitution of apparatus is shown in Fig. 1. 3.1 Constitution of Apparatus The analytical apparatus to be used usually shall consist of , Copyright Japanese Standards A
17、ssociation Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 22:28:37 MDTNo reproduction or networking permitted without license from IHS -,-,- Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=
18、IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 22:28:37 MDTNo reproduction or networking permitted without license from IHS -,-,- .JIS Z*:2634 90 4933608 0083807 II 4 Z 2614-1990 3.2 Gas Extraction System 3.2.1 Vacuum Fusion Method The vacuum fusion method shall be as follows
19、: (1) Materials and Reagents (a) Graphite crucible and graphite funnel (b) Graphite powder 74 to 44 pm (corresponding to 200 to 325 mesh) (c) Wax for high vacuum (d) Grease for vacuum apparatus, extraction furnace, gas extraction pump, exhaust gas apparatus, etc. (2) Apparatus The gas extraction sys
20、tem consists of high frequency induction heating (a) High Frequency Induction Heating Apparatus The high frequency induction heating apparatus is to be able to keep the crucible, sample, etc. in the extrac- tion furnace at a temperature not lower than the degasing temperature and consists of high fr
21、equency power source and heating coil. graphite crucible outer tube and inner tube and graphite funnel thereinto and fix the quartz cylinder filled with graphite powders or molybdenum cylinder put-into with quartz crucible, Allow fixing of them to be hanging down method (Figs, 2 and 3) and the metho
22、d to support with furnace-tube bottom-part furnace plug (Fig. 4). At the upper part of furnace tube, provide the prism for temperature measurement, temperature measurement window, sample injection opening, gas transfer tube, etc. Let the cooling of furnace tube be the method to carry out with water
23、(Fig. 3) and the method to carry out with a blower (Figs. 2 and 4). (c) Gas Extraction Pump The pump having the purpose to extract gas from the sample and a mercury diffusion pump of high exhaust gas speed, or the like is used. The apparatus having the purpose to exhaust gas in the apparatus to vacu
24、um, and connected with a mercury diffusion pump or the like and oil hydraulic rotary pump. (b) Extraction Furnace Allow the furnace tube to be made of hard glass, put the (d) Exhaust-gas Apparatus (3) Assembling of Crucibles (3-1) In the Case of Using a Graphite Crucible (a) Fill graphite powder int
25、o a quartz cylinder up to the height of 30 to 35 mm from the bottom. In the case of making the graphite crucibles double (Fig. 4), preliminarily lap them,and place highly on the graphite powder so as to be same axis as that of quartz cylinder. (b) Place a lid of cone shape on the graphite crucible s
26、o as the graphite powder not to enter into the graphite crucible, and gently add graphite powder between the graphite crucible and the quartz cylinder up to the approximately upper end of graphite crucible. (c) Detach the conical-shape lid, attach it to graphite funnel, place the lid of conical shap
27、e on it and add graphite powder up to the upper end of graphite funne. Insert a copper wire of approximately 1 mm in diameter into graphite powder, rotate it once around the graphite crucible to extinguish voids of graphite powder. Add the insufficient content and remove the conical-shape lid. (d) F
28、it the quartz cylinder entered with a graphite crucible with a furnace plug (Figs. 2 and 4), insert from under part of furnace tube and seal the ground joint part with furnace plug with the wax for high vacuum. (3-2) In the Case of Using a Quartz Crucible Hang down the molybdenum cylinder containing
29、 a quartz crucible entered with bath metal (Fig. 3) and connect the furnace tube. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 22:28:37 MDTNo reproduction or networking permitted without
30、 license from IHS -,-,- O Fig. 2. Example of Extraction Furnace 5 Z 2614-1990 a b - - C d e h k 1 m - n O - P - Quartz cylinder Quartz heat shielding cylinder Graphite crucible Graphite funnel Graphite powder Graphite plug Platinum wire Glass hook Tantalum wire Molybdenum wire Soft iron bar Side tub
31、e for filling sample Iron bar for projection of sample Right angular prism for temperature measurement Blower Heating coil Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 22:28:37 MDTNo rep
32、roduction or networking permitted without license from IHS -,-,- J I S Z*ZbL4 90 W V933b08 0083809 5 W 6 Z 2614-1990 Fig. 3. Example of Extraction Furnace - a b - C d e f - h k 1 - Right angular prism made of quartz for temperature measurement Shutter Double cock Side tube for filling of sample Wate
33、r cooling tube Platinum wire Quartz-sample guide tube Transparent quartz furnace tube Molybdenum wire Heating coil Molybdenum cylinder Quartz crucible Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 0
34、3/12/2007 22:28:37 MDTNo reproduction or networking permitted without license from IHS -,-,- 7 Z 2614-1990 a b c d e f g h i j k 1 m n Quartz right angular prism for temperature measurement Shutter Side tube for filling of sample Side tube for opening-and-closing of graphite plug Gas transfer tube G
35、raphite plug Graphite funnel Quartz cylinder Graphite powder High frequency heating coil Inside graphite crucible Outside graphite crucible Furnace-tube bottom-part furnace . Pl% Blower 3.2.2 Vacuum Heating Method The vacuum heating method shall be as follows. (1) Material and Reagent Grease for vac
36、uum furnace, gas-extraction pump, exhaust gas apparatus, etc. (a) Heating Apparatus (2) Apparatus The gas extraction system consists of a heating apparatus, extraction The heating apparatus is to be able to maintain the extrac- tion furnace at a temperature not lower than degasing temperature. As to
37、 the heating apparatus, generally resistance heating system is used, and to the rapid analysis of small type sample, high frequency induction heating system may be used. Use a furnace tube (Fig. 5) of which one end of quartz tube of 25 to 40 mm in inner diameter and 300 to 400 mm in length is sealed
38、 and of which other end is ground joint with water cooling type glass cap and connect the water cooling cap with the extraction pump. Informative reference: There are vertical type and lateral type and the lateral (b) Extraction Furnace type is convenient for use. (c) Gas Extraction Pump The gas ext
39、raction pump is to be in accordance with the case of 3.2.1 (2) (c) vacuum fusion method, as appropriate. (d) Exhaust-gas Apparatus The exhaust-gas apparatus is to be in accordance with 3.2.1 (2) (d). Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employee
40、s/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 22:28:37 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S Z*E!hL4 90 W 4933bO 00838LL 3 0 8 Z 2614-1990 Fig. 5. Example of Vacuum Heating Method Furnace Tube Unit: mm C 300 t o m a 3.2.3 Inert-gas Heating Metho
41、d (1) Material and Reagent The inert-gas heating method shall be as follows. (a) Inert gas (b) Denitrification-deoxydation agent (c) Dehydrating agent furnace, inert gas cleaning apparatus, etc. (a) Heating Apparatus Argon (it is preferable to be 99.999 % or more) or helium (it is preferable to be 9
42、9.99 % or more). Sponge titanium or the like. Phosphorus pentaoxide or the like. (2) Apparatus The gas extraction system consists of a heating apparatus, extraction The heating apparatus is to be able to maintain the extrac- tion furnace at a temperature not lower than the degasing temperature. For
43、heating apparatus, generally the resistance heating system is used. to 600 mm in length and it is to be provided with a quartz furnace tube having inert-gas introduction opening and sample injection opening. The ground joint part is cooled with water, as required. to remove nitrogen, oxygen, moistur
44、e, etc. in used inert gas, and is connected with a tube filled with denitrification-deoxidation agent, a small type electric fur- nace for heating it at approximately 500C and a tube filled with dehydrating agent. However, in the case of using argon of not less than 99.999 %, the denitrification-deo
45、xidation agent tube may be omitted. (b) Extraction Furnace Its furnace tube is 25 to 40 mm in inner diameter and 400 - (c) Inert-gas Cleaning Apparatus The inert-gas cleaning apparatus has the object 3.3 Gas Analysis System 3.3.1 Manometric Method at Constant Volume The manometric method at constant
46、 volume shall be as follows. (1) Material and Reagent (a) Oxidizing agent, copper oxide, etc. (b) Dehydrating agent, phosphorus pentaoxide, etc. (c) Silicone oil Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not fo
47、r Resale, 03/12/2007 22:28:37 MDTNo reproduction or networking permitted without license from IHS -,-,- 9 Z 2614-1990 (2) Apparatus The gas analysis system consists of a gas collection apparatus, oxidizing apparatus for collected gas, dehydrating tube, micro-pressure measuring apparatus, etc. (a) Ga
48、s Collection Apparatus The gas collection apparatus capable of colIecting the gas extracted from the sample into a definite volume gas reservoir by using a mercury ejector pump (combined with gas circulation) of high back pressure characteristic. The oxidizing apparatus having the purpose to make the collected hydrogen, carbon monoxide, respectively water, carbon dioxide, and provided with a tube filled with oxidizing agent and a small type electric furn