Use of FIA systems for on‐line dilution in multielement determination by ICP–MS (original) (raw)
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Microchemical Journal, 2014
This article describes the application of on-line isotope dilution mass spectrometry with inductively coupled plasma (OID-ICP-MS) to the field of trace metal analysis (B, Cd, Cr, Fe, Ni, Pb and Zn) in water samples by the certified reference material (CRM) characterization. Drinking, natural and waste water certified reference materials were analyzed. Emphasis is placed on OID-ICP-MS measurements of highest analytical quality and their validation against direct external calibration mass spectrometry with inductively coupled plasma analysis (ICP-MS). Differences in the calibration strategies such as single OID-ICP-MS versus direct external calibration ICP-MS were discussed. In general, it can be stated that OID-ICP-MS offers high accurate and precise results with small measurement uncertainties, when properly applied, compared to external calibration. Thus, OID-ICP-MS proved to be an ideal solution for routine water sample analysis, increasing sample throughput without any previous sample handling and improving the quality and reliability of the analytical results.
Talanta, 2001
A simple flow injection on-line dilution procedure with detection by inductively coupled plasma mass spectrometry (ICP-MS) was developed for the determination of copper, zinc, arsenic, lead, selenium, nickel and molybdenum in human urine. Matrix effects were minimized by employing a dilution factor of 16.5 with on-line standard addition, and (103)Rh was used as internal standard to compensate for signal fluctuation. The procedure was validated by the analysis of two standard reference materials SRM 2670 (NIST) and Seronormtrade mark Trace Elements in Urine. Recovery experiments were performed by spiking the reference materials as well as artificial urine. The detection limits (mug l(-1)) were 0.12,0.96,0.30,0.09,0.45,0.08,0.09, and the precisions (RSD,%) were 2.6,2.3,3.0,3.7,3.7,4.9,2.8 for Cu, Zn, As, Pb, Se, Ni and Mo, respectively. The procedure was applied to the analysis of 41 human urine samples. No correlations between the concentrations of the elements were observed.
Journal of Analytical Atomic Spectrometry, 2009
In this work, a new multiple nebulizer for liquid sample introduction in ICP-based spectrometers was developed and characterized on ICP-AES. The association of the Flow Focusing multiple nebulizer (FFMN) and a dedicated spray chamber was called Flow Focusing multi nebulization system (FFMNS). The nebulizer incorporates four nebulization nozzles with independent liquid feeding and a common gas inlet. Four different spray chambers were constructed and evaluated and the geometry of the best performing one was optimized. The FFNMS was characterized at 0.6-0.9 L min À1 nebulizing gas flow and 0.04-0.6 mL min À1 total liquid sample flow. Drop size and velocity distributions of primary and tertiary aerosols were studied together with total solvent and analyte transport rates. The system was characterized on ICP-AES in both axial and radial view modes and compared to a standard sample introduction system consisting in a concentric nebulizer and a cyclonyc spray chamber using model solutions and certified reference materials (CRM). In terms of sensitivity and LOD, the FFMNS showed a similar behavior to the reference system at half of the liquid sample uptake (0.5 mL min À1 for FFMNS vs. 1 mL min À1 for the standard system). The CRM (hard drinking water) analysis recovery results are ranged between 89%-106% for FFMNS, and between 78%-102% for the reference system. Finally, the FFMNS was applied to an ''in chamber'' standard addition analysis of synthetic samples and CRM (estuarine water). The results of the CRM analysis showed better recoveries with respect to the external calibration for Cd, Mn and Ni, and similar results for Cu and Pb.
Capabilities of production-oriented laboratories in water analysis using ICP-ES and ICP-MS
Journal of Geochemical Exploration, 1993
This study describes and evaluates the results of a round-robin wherein 22 lake water samples were submitted to eight private sector laboratories for application of their inductively coupled plasma emission spectrometry (ICP-ES) or mass spectrometry (ICP-MS) analytical packages. An objective of the project was to gain an appreciation for the quality of water analyses amongst production-oriented laboratories, and hence to use this information to assist in the design of sample collection and analytical programs in support of hydrogeochemical surveys. The 22 samples were in fact 11 duplicate pairs in order to provide data to facilitate an estimation of precision both within a laboratory and across laboratories; precision control charts were employed to this end. The accuracy observed for each element was more difficult to quantify, but was assessed by the degree of convergence of results using these independent analytical methods and techniques. The samples were spiked with varying amounts of Ba, Be, Cd, Co, Cu, Cr, Mn, Mo, Ni, Pb, V and Zn in order to raise their concentrations to levels above the detection capability of both techniques. The best estimate of precision (defined as twice the relative standard deviation) observed across the laboratories is: 10% for Mg, Mn, Na and Sr; 15% for Ba, Be, Ca, Cd, Co, Mo and V; 20% for As (ICP-MS only), Cu and Pb; 25% for Cr and K (ICP-ES only); 30% for AI and Sb (ICP-MS only); 35% for Zn; and 60% for Fe. Good precision was not necessarily a guide to good accuracy and the range in mean values for duplicates across laboratories was particularly wide for A1, B, Ca, Fe, K, Na and Zn. Most of the data from one laboratory had to be excluded from assessment of both precision and accuracy as their values deviated greatly from the average. A bias in absolute values between the two techniques was shown for AI only, ICP-MS yielding the lower results. Superior reproducibility was observed in the MS data for A1, Cr, Ni and Zn. The higher detection power of ICP-MS allowed the measurement of additional elements, namely As,
Quantitative aspects of inductively coupled plasma mass spectrometry
Philosophical transactions. Series A, Mathematical, physical, and engineering sciences, 2016
Accurate determination of elements in various kinds of samples is essential for many areas, including environmental science, medicine, as well as industry. Inductively coupled plasma mass spectrometry (ICP-MS) is a powerful tool enabling multi-elemental analysis of numerous matrices with high sensitivity and good precision. Various calibration approaches can be used to perform accurate quantitative measurements by ICP-MS. They include the use of pure standards, matrix-matched standards, or relevant certified reference materials, assuring traceability of the reported results. This review critically evaluates the advantages and limitations of different calibration approaches, which are used in quantitative analyses by ICP-MS. Examples of such analyses are provided.This article is part of the themed issue 'Quantitative mass spectrometry'.
Spectrochimica Acta Part B: Atomic Spectroscopy, 1998
A method for the determination of Cu, As, Se, Cd, In, Hg, Tl, Pb and Bi in waters and in biological materials by inductively coupled plasma mass spectrometry, after an on-line separation, is described. The matrix separation and analyte preconcentration is accomplished by retention of the analytes complexed with the ammonium salt of O,O-diethyl dithiophosphoric acid in a HNO 3 solution on C 18 immobilized on silica in a minicolumn. Methanol, as eluent, is introduced in the conventional pneumatic nebulizer of the instrument. In order to use the best compromise conditions, concerning the ligand and acid concentrations, the analytes were determined in two separate groups. The enrichment factors were in the range from 5 to 61, depending on the analyte. The limits of detection varied from 0.43 ng L −1 for Bi to 33 ng L −1 for Cu. The sample consumption is only 2.3 mL for each group and the sampling frequency is 21 h −1 . The accuracy was tested by analysing five certified reference materials: water, riverine water, urine, bovine muscle and bovine liver. The agreement between obtained and certified concentrations was very good, except for As. The relatively small volume of methanol, used as eluent, minimizes the problems produced by the introduction of organic solvent into the plasma. ᭧
Journal of Analytical Atomic Spectrometry, 1999
Recent and ongoing work in the author's laboratory is described with particular reference to the use of flow injection, continuous flow and HPLC procedures for the development of improved analytical methodology for (a) the determination of trace concentrations of As, Cd, Pb and Se and (b) the determination of various arsenic and selenium compounds. The methods have been applied to the analysis of several different sample matrices, including urine, soil, sediments, waters, plants (garlic, onion, apple leaves), yeast, fruit juices, wine, calcium supplements and marine plankton. The dependence of the LOD of an FI HG method on sample volume is examined and the validity
Analytica Chimica Acta, 1991
A study was made of the capabilities of immodtacetic acrd/ethylcellulose (IDAEC) to serve as the chelatmg resin for preconcentratmg trace elements together with a computer-assisted on-line flow mjection analysis-inductively coupled plasma atomrc emission spectrometry technique. The system was tested with a few analytes of particular climcal and enwonmental tmportance (Cd, Co, Cu and Pb) m matrices such as water, sea water and urine. The performance of IDAEC resin was compared with that of carboxymethylated polyethyleneimine-polymethylenepolyphenylene lsocyanate (CPPI) and Chelex 100 wrth regard to ennchment factor, analytical throughput and recovery. With several obvious advantages over the batch procedure, the on-hne mode unproved the detection power by one to two orders of magmtude and allowed twelve samples per hour to be treated IDAEC appears to be the most convement resin m terms of efficiency and long-term performance.