skip to main content
OSTI.GOV title logo U.S. Department of Energy
Office of Scientific and Technical Information

Title: Sample introduction into a direct current plasma by filament vaporization

Abstract

This dissertation describes sample introduction into a direct current plasma by a tungsten filament vaporizer. The filament heater was designed to resistively heat a 0.1 mm diameter tungsten wire quickly and efficiently. The heating system is under microprocessor control for precise power application to the filament. The cell volume is small, less than 4 mL, and the accessibility of the primary emission zone allowed placement of the filament less than 5 cm from the confluence point of the plasma. The first study describes some of the fundamental design considerations, as well as performance of the interface. The absolute mass detection limits for Ca, Fe, Al, and Cu are 80, 2,000, 90, and 200 fg respectively. The blackbody emission temperature of the filament was measured. The initial heating rate was 50,000{degree}C/s. Observations are reported for optimization of operating parameters, as well as how to locate the region of maximum analyte emission intensity. Finally, the application of this technique to the analysis of a biological sample, swine blood, is reported. The second study examines the sources of noise and their components. Noise is grouped into additive and multiplicative noise occurring in three frequency ranges. The largest contribution, greater than 90%, was shotmore » to shot multiplicative variations in sample vaporization and excitation. The third study examines the effect of addition of concomitant substances to the analyte. The substances were added both as metal salts to the aqueous analyte solution and as dopant gases to the carrier gas. Measured transport efficiencies ranged from 60 to 103% for manganese under various concomitant conditions. A 1% doping of the carrier gas with hydrogen caused significant enhancement of the emission signal of three metals, Fe, Al, and Ca. Enhancement correlated with volatility of the reduced form of the element.« less

Authors:
Publication Date:
Research Org.:
North Carolina State Univ., Raleigh, NC (United States)
OSTI Identifier:
7201070
Resource Type:
Miscellaneous
Resource Relation:
Other Information: Thesis (Ph.D.)
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; METALS; QUANTITATIVE CHEMICAL ANALYSIS; ALUMINIUM; CALCIUM; COPPER; EXPERIMENTAL DATA; FLASH HEATING; IRON; PLASMA; SAMPLE PREPARATION; ALKALINE EARTH METALS; CHEMICAL ANALYSIS; DATA; ELEMENTS; HEATING; INFORMATION; NUMERICAL DATA; TRANSITION ELEMENTS; 400102* - Chemical & Spectral Procedures

Citation Formats

Buckley, B T. Sample introduction into a direct current plasma by filament vaporization. United States: N. p., 1989. Web.
Buckley, B T. Sample introduction into a direct current plasma by filament vaporization. United States.
Buckley, B T. 1989. "Sample introduction into a direct current plasma by filament vaporization". United States.
@article{osti_7201070,
title = {Sample introduction into a direct current plasma by filament vaporization},
author = {Buckley, B T},
abstractNote = {This dissertation describes sample introduction into a direct current plasma by a tungsten filament vaporizer. The filament heater was designed to resistively heat a 0.1 mm diameter tungsten wire quickly and efficiently. The heating system is under microprocessor control for precise power application to the filament. The cell volume is small, less than 4 mL, and the accessibility of the primary emission zone allowed placement of the filament less than 5 cm from the confluence point of the plasma. The first study describes some of the fundamental design considerations, as well as performance of the interface. The absolute mass detection limits for Ca, Fe, Al, and Cu are 80, 2,000, 90, and 200 fg respectively. The blackbody emission temperature of the filament was measured. The initial heating rate was 50,000{degree}C/s. Observations are reported for optimization of operating parameters, as well as how to locate the region of maximum analyte emission intensity. Finally, the application of this technique to the analysis of a biological sample, swine blood, is reported. The second study examines the sources of noise and their components. Noise is grouped into additive and multiplicative noise occurring in three frequency ranges. The largest contribution, greater than 90%, was shot to shot multiplicative variations in sample vaporization and excitation. The third study examines the effect of addition of concomitant substances to the analyte. The substances were added both as metal salts to the aqueous analyte solution and as dopant gases to the carrier gas. Measured transport efficiencies ranged from 60 to 103% for manganese under various concomitant conditions. A 1% doping of the carrier gas with hydrogen caused significant enhancement of the emission signal of three metals, Fe, Al, and Ca. Enhancement correlated with volatility of the reduced form of the element.},
doi = {},
url = {https://www.osti.gov/biblio/7201070}, journal = {},
number = ,
volume = ,
place = {United States},
year = {Sun Jan 01 00:00:00 EST 1989},
month = {Sun Jan 01 00:00:00 EST 1989}
}

Miscellaneous:
Other availability
Please see Document Availability for additional information on obtaining the full-text document. Library patrons may search WorldCat to identify libraries that may hold this item.

Save / Share: