1	High Resolution Glow Discharge Mass Spectrometry An Overview: How and Where it is Applied Richard Balamut SHIVA Technologies Syracuse, NY ILAP 2007 – July 27, 2007 Breckenridge, CO
2	Outline The three major components of HR-GDMS instrumentation Ion source Mass analyzer Detector Review of sample data Generation of data Applications Summary of the technique’s strengths and limitations
3	Three major components of HR-GDMS instrumentation Three major components of HR-GDMS instrumentation Ion Source Mass Analyzer Detector
4	The VG9000 HR-GDMS
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6	Three major components of HR-GDMS instrumentation Ion source Glow discharge The luminous effect of passing current through a gas with a large potential difference (voltage) between electrodes
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8	Three major components of HR-GDMS instrumentation Ion source Glow discharge The ability to generate stable analyte ion population directly from a solid sample – eliminating the problems of dissolution, dilution, and contamination from sample handling Separation of atomization and ionization (dark space), this is not the case with Spark Source, Thermal Ionization, Laser Ion-desorption, and Secondary Ion – Mass Spectrometry [SSMS, TIMS, LIMS, SIMS]
9	VG9000 HR-GDMS GLOW-DISCHARGE ION PRODUCTION
10	Sample Size Requirements
11	Three major components of HR-GDMS instrumentation Mass Analyzer Double focusing magnetic sector Uniform high mass resolution using a single set of tuning conditions High ion transmission - characteristic at > 75% Mass resolution (m/Dm) better than 4000m Extremely low background allows for ultra-trace detection
12	The High Resolution Glow Discharge Mass Spectrometer
13	Three major components of HR-GDMS instrumentation Detector Dual detector system Faraday cup for major elements Daly detector for trace and ultra-trace element concentration Dynamic working range of eleven orders of magnitude
14	Detection Principle
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16	Example of a Low Resolution Mass Analyzer
17	Example of VG9000 Spectral Output
18	Generation of Data What does the technique measure? HR-GDMS measures the number of ions arriving at the detector(s) – ion beam intensity The number of ions is proportional to the number of atoms in the sample
19	Generation of Data Semi-quantitative - Ion Beam Ratio Assumes that the ratio of ion current for any single isotope, with respect to the total ion current, is representative of the ratio of the number of atoms of that isotope in the sample to the other constituent atoms of the sample C_i= (I_i / I_m) C_m This is a variation on internal standard calibration – the matrix element serving as the internal standard Result within a factor of 2 or 3 are typical
20	Generation of Data Quantitative - Relative Sensitivity Factors In a given matrix the proportionality factor varies from element to element - this factor is measured by analyzing a standard Parameter RSF(i/m), which is the slope of the calibration line, is commonly understood as the Relative Sensitivity Factor (RSF)
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23	Example of RSF values
24	Generation of Data Quantitative - Relative Sensitivity Factors The factors (RSF’s) are then applied to the ion beam ratio for quantification Below is application of RSF to a single element matrix C_i= (RSF_i / RSF_m ) x (I_i / I_m)
25	Application of HR-GDMS Ideal uses for HR-GDMS Trace and ultra-trace element determination in high purity metals, alloys, carbides, ceramics, semiconductors, and electronic materials Depth profiling of flat surfaces for major, minor, and trace elements Identification of unknowns from minute amount of specimen Full element characterization of powder and particulate materials
26	Application of HR-GDMS Relative Industries served Sputter target manufacturing Aerospace Refractory metals and alloys Rare earth metals and oxides Precious metals High purity materials production
27	Application of HR-GDMS
28	ASTM F2405 GDMS on Cu
29	ASTM F2405 GDMS on Cu
30	Application of HR-GDMS Published GDMS Method (ASTM F01.17) ASTM F1593 – 97 Aluminum ASTM F1710 – 97 Titanium ASTM F1845 – 97 Aluminum-Copper, Aluminum-Silicon, and Aluminum-Copper-Silicon Alloys ASTM F2405 – 04 Copper ASTM Fxxxx- xx In progress for Ta
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32	HR-GDMS Application
33	HR-GDMS Application
34	HR-GDMS Strengths and Limitations HR-GDMS Limitations Sample heterogeneity Volatile samples Not suited for organic materials Time allotment per sample analysis
35	HR-GDMS Strengths and Limitations HR-GDMS Strengths Full periodic table coverage (except H) Sub-ppb to ppt detection Minimal matrix effects Linear and simple calibration Depth profiling of layers and coatings (at ~0.1 microns/minute)
36	High Resolution Glow Discharge Mass Spectrometry An Overview: How and Where it is Applied Rich Balamut ILAP 2007 – July 27, 2007 Breckenridge, CO