Multielement trace metal determination by electrodeposition, scanning electron microscopic X-ray fluorescence, and inductively coupled plasma mass spectrometry

Journal Article · Tue May 15 00:00:00 EDT 1990 · Analytical Chemistry (Washington); (USA)

DOI:https://doi.org/10.1021/ac00209a015· OSTI ID:6144039

Chong, Ngeesing; Norton, M L; Anderson, J L ^[1]

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1. Univ. of Georgia, Athens (USA)

Multielement analysis of multicomponent metallic electrodeposits is described, based on scanning electron microscopy with energy dispersive X-ray fluorescence (EDXRF) detection, followed by dissolution and inductively coupled plasma mass spectrometry (ICP-MS) detection. Application of the method is described for determination of trace elements in seawater, including Zn, Mn, Co, Cu, Cr, Ni, Fe, Cd, Pb, and Hg. These elements are simultaneously electrodeposited onto a niobium wire working electrode at {minus}1.40 V vs an Ag/AgCl reference and subjected to EDXRF analysis. Internal standardization is practical for quantitative calibration at the 1 ppm analyte concentration level in an analyte:internal standard concentration ratio range of 0.02-50. Detection limits for EDXRF range from 1.9 ppb for Fe to 50 ppb for Cd. The deposit is dissolved for subsequent ICP-MS determination. Significant reduction in ICP-MS matrix interferences by Na, Ca, Mg, K, and Cl ions is achieved by deposition at potentials more positive than their very negative reduction potentials. Measurement of elemental isotope ratios is achieved with 0-8% relative error. ICP-MS detection limits for all elements except Zn and Fe are superior to those of EDXRF.

• OSTI ID: 6144039
• Journal Information: Analytical Chemistry (Washington); (USA), Vol. 62:10; ISSN 0003-2700
• Country of Publication: United States
• Language: English

Related Subjects

54 ENVIRONMENTAL SCIENCES
37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
SEAWATER
MULTI-ELEMENT ANALYSIS
CADMIUM
CHROMIUM
COBALT
COPPER
IRON
LEAD
MANGANESE
MASS SPECTROSCOPY
MERCURY
NICKEL
SCANNING ELECTRON MICROSCOPY
X-RAY FLUORESCENCE ANALYSIS
ZINC
CHEMICAL ANALYSIS
ELECTRON MICROSCOPY
ELEMENTS
HYDROGEN COMPOUNDS
METALS
MICROSCOPY
NONDESTRUCTIVE ANALYSIS
OXYGEN COMPOUNDS
SPECTROSCOPY
TRANSITION ELEMENTS
WATER
X-RAY EMISSION ANALYSIS
540320* - Environment
Aquatic- Chemicals Monitoring & Transport- (1990-)
400102 - Chemical & Spectral Procedures