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Determination of micro-amount carbon in sodium metal by vacuum distillation-gas chromatography

Technical Report:

Abstract

The amount of carbon in sodium metal which is used as a coolant of fast reactors has the effect on physical and mechanical properties of construction materials for reactors. A method to determine microamounts carbon in sodium metal by vacuum distillation-gas chromatography in the ppm level has been developed. Under the argon atmosphere, 1 {approx} 6 g sodium samples are put into silica crucibles, then crucibles are placed in a stainless steel distillation pot at 673 K and 6.7 x 10{sup -3} Pa to remove the sodium. The residue is combusted at 1373 K with pure oxygen for 30 minutes. The CO{sub 2} formed is collected in a silica gel cold trap (193 {approx} 173 K) and measured by gas chromatography after dis-adsorption by boiling water. Many experimental conditions such as distillation, combustion, cold trap, treatment of apparatus and quantitative method have been studied. By this method the relative deviation is less than 12% with the content of carbon in sodium at the range of 5 {approx} 100 ppm. Standard addition experiments are carried out with nuclear grade graphite and sodium carbonate standards. Within the above range, the recoveries are (104.9 +- 11.1)% and (100.8 +-19)%, respectively. This method has  More>>
Authors:
Ximent, Wen; Qingzhou, Guo; Shiping, Sun [1] 
  1. Academia Sinica, Beijing, BJ (China). Inst. of Atomic Energy
Publication Date:
Jun 01, 1993
Product Type:
Technical Report
Report Number:
CNIC-00766; IAE-0121.
Reference Number:
SCA: 400102; PA: AIX-26:009361; EDB-95:029992; SN: 95001322981
Resource Relation:
Other Information: PBD: Jun 1993
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; CARBON; DISTILLATION; CARBON DIOXIDE; GAS CHROMATOGRAPHY; SODIUM; ACCURACY; ADSORPTION; COMBUSTION; COOLANTS; FAST REACTORS; HIGH VACUUM; RESIDUES; TRACE AMOUNTS; 400102; CHEMICAL AND SPECTRAL PROCEDURES
OSTI ID:
10111236
Research Organizations:
China Nuclear Information Centre, Beijing, BJ (China)
Country of Origin:
China
Language:
Chinese
Other Identifying Numbers:
Other: ON: DE95611763; ISBN 7-5022-0962-X; TRN: CN9402340009361
Availability:
OSTI; NTIS (US Sales Only); INIS
Submitting Site:
INIS
Size:
10 p.
Announcement Date:
Jun 30, 2005

Technical Report:

Citation Formats

Ximent, Wen, Qingzhou, Guo, and Shiping, Sun. Determination of micro-amount carbon in sodium metal by vacuum distillation-gas chromatography. China: N. p., 1993. Web.
Ximent, Wen, Qingzhou, Guo, & Shiping, Sun. Determination of micro-amount carbon in sodium metal by vacuum distillation-gas chromatography. China.
Ximent, Wen, Qingzhou, Guo, and Shiping, Sun. 1993. "Determination of micro-amount carbon in sodium metal by vacuum distillation-gas chromatography." China.
@misc{etde_10111236,
title = {Determination of micro-amount carbon in sodium metal by vacuum distillation-gas chromatography}
author = {Ximent, Wen, Qingzhou, Guo, and Shiping, Sun}
abstractNote = {The amount of carbon in sodium metal which is used as a coolant of fast reactors has the effect on physical and mechanical properties of construction materials for reactors. A method to determine microamounts carbon in sodium metal by vacuum distillation-gas chromatography in the ppm level has been developed. Under the argon atmosphere, 1 {approx} 6 g sodium samples are put into silica crucibles, then crucibles are placed in a stainless steel distillation pot at 673 K and 6.7 x 10{sup -3} Pa to remove the sodium. The residue is combusted at 1373 K with pure oxygen for 30 minutes. The CO{sub 2} formed is collected in a silica gel cold trap (193 {approx} 173 K) and measured by gas chromatography after dis-adsorption by boiling water. Many experimental conditions such as distillation, combustion, cold trap, treatment of apparatus and quantitative method have been studied. By this method the relative deviation is less than 12% with the content of carbon in sodium at the range of 5 {approx} 100 ppm. Standard addition experiments are carried out with nuclear grade graphite and sodium carbonate standards. Within the above range, the recoveries are (104.9 +- 11.1)% and (100.8 +-19)%, respectively. This method has met the technical requirements for carbon analysis in nuclear grade sodium.}
place = {China}
year = {1993}
month = {Jun}
}