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1、UDC 669.296 + 669.296.5 : 543.272.6 i=& -. . - . . : . _, : JAPANESE INDUSTRIAL STANDARD Methods for Determination of Carbon in Zirconium and Zirconium Alloys JIS H 1 6 6 3 - 1 9 8 8 Translated and Published by Japanese Standards Association Printed in Japan Copyright Japanese Standards Association
2、Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:37 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS H*i,bb3 88 = 4933b08 0053438 3 I In the event of any doubt arising, the original Standard in Ja
3、panese is to be final authority. Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:37 MDTNo reproduction or networking permitted without license from IHS -,-,- J I S H*3bb3 88 4933608 0
4、053439 3 I i UDC 669.296+669.296.5:543.272.6 JAPANESE INDUSTRIAL STANDARD J I S Methods for Determination of Carbon H 1663-1988 in Zirconium and Zirconium Alloys 1. Scope This Japanese Industrial Standard specifies the methods for determination of carbon in zirconium and zirconium alloys. 2. General
5、 Matters General matters common to the methods for chemical analysis shall be in accordance with JIS H 1650 and JIS Z 2615. 3. Classification of Methods for Determination The methods for determination of carbon shall be in accordance with d, one of the following methods: (1) Combustion - Coulometric
6、 Method of not less than 0.002 wt % in carbon content. This method applies to the sample (2) Combustion - Infrared Absorption Method (Integral Method) This method applies to the sample of not less than 0.002 wt % in carbon content. (3) Combustion - Infrared Absorption Method (Circulating Method) Thi
7、s method applies to the sample of not less than 0.002 wt % in carbon content. (4) Combustion - Thermal Conductivity Method This method applies to the sample of not less than 0.002 wt % in carbon content. (5) Combustion - Electric Conductivity Method This method applies to the sample of not less than
8、 0.002 wt % in carbon content. 4. Combustion - Coulometric Method 4.1 Summary A sample is heated in the gas current of oxygen and carbon is oxidized to carbon dioxide. It is absorbed in weak alkaline barium salt solution adjusted at specific pH and the quantity of electricity required for returning
9、pH decreased by absorption to the original pH by electrolysis of barium salt solution, is measured. Applicable Standards: JIS H 1650-General Rules for Chemical Analysis of Zirconium and JIS Z 2615-General Rules for Determination of Carbon in Metallic Zirconium Alloys Materials Copyright Japanese Sta
10、ndards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:37 MDTNo reproduction or networking permitted without license from IHS -,-,- JIS H*l1bb3 88 4933608 005L440 T I 2 H 1663-1988 4.2 Apparatus For the apparatus
11、, a tubular electric resistance heating furnace of 5, (6) (a) in JIS Z 2615 is connected with an apparatus of 6.7,3 in JIS Z 2615 to be used. 4.3 Appliances, Materials and Reagents The appliances, materials, and reagents shall be in accordance with 5, of JIS Z 2615 and 6.7.2 of JIS Z 2615. 4.4 SamtA
12、e 4.4.1 Sampling and Preparation of Sample The sampling and preparation of a sample shall be in accordance with 4. of JIS H 1650 and 4. of JIS Z 2615 taking care for carbon not to be contaminated. An analysis sample shall be put into a clean glass bottle and hermetically sealed to be reserved, 4.4.2
13、 Weighing-Out Amount of Sample The weighing out amount of a sample shall be 0.5 g. 4.5 Operation 4.5.1 Preparatory Operation The preparatory operation shall be in accordance with 6.7.4 of JIS Z 2615. However, the temperature of a tubu electric resistance heating furnace shall be 130OOC , .ar Further
14、, for backing of a porcelain combustion boat, it shall be heated at not less than 13OOOC for not less than 2 h. 4.5.2 Determination Operation The determination operation shall be in accordance with 6.7.5 of JIS Z 2615. shall be used as ignition improvers ( I ) , (2), ( 3 ) . However, 1.0 g of tin an
15、d 1.0 g of iron Notes (l) When carbon is confirmed to be able to be sufficiently oxidized by using a standard sample, other ignition improvers may be used independently or otherwise by combining two or three kinds thereof. When tin and iron are used as ignition improvers, tin is placed on the bottom
16、 of a porcelain combustion boat and a sample is put thereon. Further, the sample is covered by iron. (2) ( 3 ) When iron to be used as ignition improver is pre- liminarily heated in the atmosphere of nitrogen at 8OOOC for 1 h, a blank test value may be controlled at a low level. 4.5.3 Blank Test Ign
17、ition improver used in 4.5.2 shall be used by the same amount as in 4.5.2 and the operation shall be carried out in ac- cordance with the procedure of 6.7.6 of JIS Z 2615. 4.5.4 Calculation The calculation shall be in accordance with 6.7.7 of JIS Z 2615. Copyright Japanese Standards Association Prov
18、ided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:37 MDTNo reproduction or networking permitted without license from IHS -,-,- 3 H 1663-1988 Remark: The high frequency induction heating furnace of 5, (6) (b) of JIS Z 2615 may be u
19、sed instead of the tubular electric resistance furnace. In this case, the procedure shall be as decribed in 5. (6) (6.2) of JIS Z 2615. However, the backing of a high frequency porcelain combustion crucible, ignition improver, etc shall be as described in 5.5.1 and 5.5.2. 5. Combustion - Infrared Ab
20、sorption Method (Integral Method) d 1 5.1 Summary A sample is heated in the gas current of oxygen and carbon is oxidized to carbon dioxide. an infrared absorption detector and the infrared absorption quantity by carbon dioxide is measured by an integral method. It is sent together with oxygen to 5.2
21、 Apparatus For the apparatus , the high frequency induction heating furnace of 5. (6) (b) in JIS Z 2615 is connected with the apparatus of - - 6.9.3 in JIS Z 2615 to be used. 5.3 Appliances and Materials The appliances and materials shall be as described in 5 . of JIS Z 2615 and 6.9.2 of JIS Z 2615.
22、 5.4 Sample 5.4.1 Sampling and Preparation of Sample The sampling and preparation of a sample shall be as described in 4.4.1. 5.4.2 Weighing-Out Amount of Sample The weighing-out amount of sample shall“ be O. 5 g. 5.5 Operation 5.5-. 1 Preparatory Operation The preparatory operation shall be as desc
23、ribed in 6.9.4 of JIS Z 2615. However, for the backing of a high frequency porcelain combustion crucible, it is heated at not less than 130OOC for not less than 2 h (4). Note (4) A backing can be substituted by the operation that a fixed amount of the same metal as metals used as ignition improver i
24、n determination operation is put into a high frequency porcelain combustion crucible and heated in a high frequency induction heating furnace for a fixed time. In this case, because the amount of metal to be put into the crucible, and heating time are different according to the kind of metal to be u
25、sed as ignition improver, an optimum amount thereof and an optimum time are preliminarily examined. ignition improvers, 0.5 g of iron and 0.5 g of copper are put into the crucible and should preferably be heated for 1 min. However, in determination operation, 1.0 g of iron and 1.0 g of copper are us
26、ed as ignition improvers as specified in 5.5.2 separately therefrom. Further, when iron and copper are used as Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:37 MDTNo reproduction or
27、 networking permitted without license from IHS -,-,- J I S H*1bb3 88 m 4933b08 0051442 3 m ! 4 H 1663-1988 5.5.2 Determination Operation The determination operation shall be as described in 6.9.5 of JIS Z 2615. However, 1.0 g of iron and 1.0 g of copper are used as ignition improvers (l) , ( 3), ( 5
28、). Note ( 5 , When iron and copper are used as ignition improvers, a sample is put into a high frequency porcelain combustion crucible and its upside is covered by iron and copper in this order. 5.5.3 Blank Test Ignition improvers used in 5.5.2 are used by the same amount as that in 5.5.2 and the op
29、eration is carried out in accordance with the procedure of 6.9.6 in JIS Z 2615. 5.5.4 Calculation The calculation shall be as described in 6.9.7 of JIS Z 2615. Remark: The tubular electric resistance heating furnace of 5 . (6) (a) in JIS Z2615 may be used instead of the high frequency induction heat
30、ing furnace. the operation shall be as described in 5. (6) (6.1) of JIS Z 2615. However, the temperature of the tubular electric resistance heating furnace, the backing of a porcelain combustion boat, ignition improver, etc. shall be as described in 4.5.1 and 4.5.2. In this case, 6. Combustion - Inf
31、rared Absorption Method (Circulating Method) at a fixed pressure in a fixed volume and carbon is oxidized to carbon dioxide and carbon monoxide. to an infrared absorption detector of a circulating loop and the infrared absorption quantities of carbon dioxide and carbon monoxide are respectively meas
32、ured. 6.1 Summary A sample is heated in the circulating gas current of oxygen They are sent together with excess oxygen 6 2 Apparatus For the apparatus, the high frequency induction heating furnace of 5. (6) (b) in JIS Z 2615 is connected with the apparatus of 6.10.2 in JIS Z 2615 to be used. 6.3 Ap
33、pliances and Materials The appliances and materials shall be as described in 5.3. 6.4 Sample 6.4.1 Sampling and Preparation of Sample The sampling and preparation of a sample shall be as described in 4.4.1. 6.4.2 Weighing-Out Amount of Sample The weighing-out amount of a sample shall be 0.5 g. 6.5 O
34、peration 6.5.1 Preparatory Operation The preparatory operation shall be as described in 6.10.3 of JIS Z 2615. frequency porcelain combustion crucible, it is heated at not less than 130OOC for not less than 2 h (4). However, for the backing of a high rib Copyright Japanese Standards Association Provi
35、ded by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:37 MDTNo reproduction or networking permitted without license from IHS -,-,- e a 5 H 1663-1988 6.5 2 Determination Operation described in 6.10.4 of JIS Z 2615. copper are used as ig
36、nition improvers (l) , (3) , ( 5 ) . The determination operation shall be as However, 1.0 g of iron and 1.0 g of 6.5.3 Blank Test The ignition improvers used in 6.5.2 are used by the same amount as that in 6.5.2 and the operation is carried out in ac- cordance with the procedure of 6.10.5 in JIS Z 2
37、615. 6.5.4 Calculation The calculation shall be as described in 6.10.6 of JIS Z 2615. Remark: The tubular electric resistance heating furnace of 5. (6) (a) in JIS Z 2615 may be used instead of the high frequency induction heating furnace. the operation shall be as described in 5. (6) (6.1) of JIS Z
38、2615. However, the temperature of the tubular electric resistance heating furnace, the backing of a porcelain combustion boat , ignition improvers, etc. shall be as described in 4.5.1 and 4.5.2. In this case , 7. Combustion - Thermal Conductivity Method 7.1 Summary A sample is heated in the gas curr
39、ent of oxygen and carbon is oxidized to carbon dioxide. tube containing adsorbent, this collection tube is heated and carbon dioxide adsorbed is released. conductivity detector and the change of thermal conductivity by carbon dioxide is measured. After adsorbing it in a collection It is sent togethe
40、r with oxygen to a thermal 7.2 Apparatus For the apparatus , the high frequency induction heating furnace of 5. (6) (b) of JIS Z 2615 is connected with the apparatus of 6.8.3 in JIS Z 2615 to be used. 7.3 Appliances, Materials, and Reagents The appliances , materials , and reagents shall be as descr
41、ibed in 5. of JIS Z 2615 and 6.8.2 of JIS Z 2615. 7.4 Sample 7.4.1 Sampling and Preparation of Sample The sampling and preparation of a sample shall be as described in 4.4.1. 7.4.2 Weighing-Out Amount of Sample The weighing-out amount of a sample shall be 0.5 g. 7.5 Operation 7.5.1 Preparatory Opera
42、tion The preparatory operation shall be as described in 6.8.4 of JIS Z 2615. frequency porcelain combustion crucible, it is heated at not less than 1300OC for not less than 2 h (4). However, for the backing of a high 7.5.2 Determination Operation The determination operation shall be as described in
43、6.8.5 of JIS Z 2615. However, 1.0 of iron and 1.0 g of copper are used as ignition improvers ) , (3) , ( % ). Copyright Japanese Standards Association Provided by IHS under license with JSALicensee=IHS Employees/1111111001, User=Wing, Bernie Not for Resale, 03/12/2007 02:49:37 MDTNo reproduction or
44、networking permitted without license from IHS -,-,- - , JISH*1tsb3 88 m 4933608 0051444 7 m I 6 H 1663-1988 7 5.3 Blank Test For the blank test, ignition improvers used in 7.5.2 is used by the same amount as in 7.5.2 and the operation is carried out in accordance with the procedure of 6.8.6 in JIS Z
45、 2615, 7.5.4 Calculation The calculation shall be as described in 6.8.7 of JIS Z 2615. Remark: The tubular electric resistance heating furnace of 5 (6) (a) in JIS Z 2615 may be used instead of the high frequency induction heating furnace. the operation shall be as described in 5. (6) (6.1) of JIS Z
46、2615. However, the temperature of a tubular electric resistance heating furnace, the backing of a porcelain combustion boat y ignition improvers y etc. shall be as described in 4.5.1 and 4.5.2. In this case 8. Combustion - Electric Conductivitv Method 8.1 Summary A sample is heated in the gas curren
47、t of oxygen and carbon is oxidized to carbon dioxide, alkali solution and the change in conductivity of the solution before and after absorption is measured. It is absorbed in a fixed amount of 8.2 Apparatus For the apparatus, the tubular electric resistance heating furnace of 5. (6) (a) in JIS Z 26
48、15 is connected with the apparatus of 6.6.3 in JIS Z 2615 to be used. 8.3 Appliances, Materials and Reagents The appliances, materials, and reagents shall be as described in 5. of JIS Z 2615 and 6.6.2 of JIS Z 2615. 8.4 Sample I 8.4.1 Sampling and Preparation of Sample The sampling and preparation of a sample shall be as described in 4.4.1. 8.4.2 Weighing-Out Amount .of Sampl The weighing-out amount of sample shall be 0.5 g. 8 5 Operation 8.5.1 Preparatory Operation The preparatory operation shall be as described in 6.6.4 of JIS Z 2615. a tubular electric resistance