Report of the Inductively Coupled Plasma - Mass Spectrometry (Icp-MS) Facility, University of Notre Dame 1993-1996 (original) (raw)
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Journal of Radioanalytical and Nuclear Chemistry, 1998
The subrnined manuscript has been authored by a contractor of the US. Government under contact No. DE-ACOS-960R22464. Accordingly. the U.S. Government retains a nonexclusive. royalcy-free license to publish or reproduce the published form of this contribution. or allow others to do so. for U.S. Government purposes." Research sponsored by U.S. Department of Energy, under contract number DE-AC05-960R22464 with Oak Ridge National Laboratory, managed by Lockheed Martin Energy Research C o p. 19980402 003 DISCLAIMER This report was prepared as an account of work sponsored by an agency of the United States Government. Neither the United States Government nor any agency thereof, nor any of their employees, makes any warranty, express or implied, or assumes any legal liability or responsibility for the accuracy, completeness, or usefulness of any information, apparatus, product, or process disclosed, or represents that its use would not infringe privately owned rights. Reference herein to any specific commercial product, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof. The views and opinions of authors expressed herein do not necessarily state or reflect those of the United States Government or any agency thereof.
Sources of contamination and remedial strategies in the multi-elemental trace analysis laboratory
Analytical and Bioanalytical Chemistry, 2010
In theory, state of the art inductively coupled plasma mass spectrometry (ICP-MS) instrumentation has the prerequisite sensitivity to carry out multi-elemental trace analyses at sub-ng L −1 to sub-pg L −1 levels in solution. In practice, constraints mainly imposed by various sources of contamination in the laboratory and the instrument itself, and the need to dilute sample solutions prior to analysis ultimately limit detection capabilities. Here we review these sources of contamination and, wherever possible, propose remedial strategies that we have found efficacious for ameliorating their impact on the results of multi-elemental trace analyses by ICP-MS. We conclude by providing a list of key points to consider when developing methods and preparing the laboratory to routinely meet the demands of multi-elemental analyses at trace analytical levels by ICP-MS.
2021
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Tests of the Contamination Analysis Unit, Phase 2
2003
Lawrence Livermore National Laboratory (LLNL) has developed a mass spectrometer-based system that measures organic surface residues in situ. This system, called the Contamination Analysis Unit (CAU), can detect and quantify a variety of volatile surface residues on a range of different substrates. Residue samples are removed from the substrate using a combination of vacuum and thermal desorption, and are then ionized and quantified by a quadrupole mass spectrometer. The current effort (Phase 2) was carried out in accordance with Thiokol Project Test Plan PTP-0467. A first phase of tests was completed under PTP-0327 and the results reported in TWR-75385. The Phase 2 test plan, PTP-0467, is a follow-on to PTP-0327, and was conducted in order to more fully determine the capabilities of the CAU. This report summarizes experiments in which the CAU was evaluated for application in reusable solid rocket motor production scenarios. The report has been ordered by the tasks requested by ATK T...
Atomic spectrometry update – a review of advances in environmental analysis
Journal of Analytical Atomic Spectrometry, 2021
Introduction 2 Air analysis 2.1 Sampling techniques 2.2 Reference materials and calibrants 2.3 Sample preparation 2.4 Instrumental analysis 2.4.1 Atomic absorption and emission spectrometries 2.4.2 Mass spectrometry 2.4.2.1 Inductively coupled plasma mass spectrometry 2.4.2.2 Other mass spectrometry techniques 2.4.3 X-ray spectrometry 2.4.4 Combustion-based techniques 2.4.5 Other instrumental techniques 3 Water analysis 3.1 Certification of reference materials and metrological investigations Page 12 of 125 235 U 1 H + isobaric interference on 236 U. By cleverly exploiting the fact that the hydride form of UO + (UOH +) is less prone to formation in the plasma than UH + , together with the use of a desolvating nebuliser, it was possible to constrain the 235 U 16 O 1 H + / 235 U 16 O + formation rate to ca. 10-7 so 236 U/ 238 U ratios of <10-8 could be determined successfully for material deposited from the Fukushima Daiichi nuclear incident. Siloxanes in gaseous fuels, even at low concentrations, can be problematic because, upon combustion, amorphous Si can deposit and cause damage within combustion systems or fuel cells. The LOQ for Si of ca. 0.01 mg m-3 for a new GC-ICP-MS approach to the analysis of fuels was 37 below the benchmark limit of ≤0.1 mg m-3 designed to protect machinery. The Hg 0 concentration output from the NIST prime calibrator (see section 2.1) was certified 38 using ID-CV-ICP-MS at selected span points over the range 0.25 to 38 µg m-3. Two procedures were used, a direct gas analysis approach and a preconcentration method that involved trapping defined gas volumes on activated carbon. The direct measurement approach yielded expanded MU ranging from 5.5% at 0.5 µg m-3 to 1% at 38 µg m-3 with a LOQ of 0.06 µg m-3 , whereas sample preconcentration yielded an expanded MU of 1% across this range with a LOQ of 0.001 µg m-3. The single particle ICP-MS analysis of atmospheric particles deposited in ice-core samples was performed 39 for the first time using CFA coupled to ICP-TOF-MS. The fact that Al and Mg signals were associated with Fe signals emanating from Fe-rich particles suggested that clay minerals such as illite were the dominant components in the particles being examined. Use of a dry aerosol provided 40 a significant gain in ion extraction from a plasma thereby making it possible to now size silver and titanium NPs at 3.5 and 12.1 nm, an improvement of 29 and 37% over that achievable under wet plasma conditions.
2016
I would like to express my deepest gratitude to the following individuals, whose patience, support and guidance have contributed towards the success of this research study. First and foremost, I am most thankful to my research Supervisor at Necsa, Dr. Molahlehi Sonopo, for encouraging my research and encouraging me to grow in the research field, without his guidance and his continuous support; I would not have finished this research. To my research Co-Supervisor, Professor Shadung Moja, I would like to express my special appreciation for his guidance, motivation and immense knowledge. To my Manager at RadioAnalysis at Necsa, Mr. Sello Mokhobo, I am forever grateful for the opportunity to conduct this research, for the time he`s given me, for the financial support granted and for his continuous support. To the RadioAnalysis laboratory expert, Mr. Deon Kotze, I would like to express my gratitude for his brilliant comments, suggestions and his immense knowledge. I am forever grateful to Ms Immanda Louw for her patience, guidance and encouragement; I could not have imagined a better mentor. To my laboratory Supervisor, Ms. Monika Buys, for her continuous support and for her encouragement. I would also like to express my deepest appreciation to my colleagues at RadioAnalysis for being supportive, for always willing to help and for allowing me to use the instruments whenever there was a chance. Lastly, I would like to express my deepest gratitude to The South African Nuclear Energy Corporation SOC Limited-Necsa for financial support and the time that the company has provided for me to be able to complete this research in time.
Environmental monitoring at the Lawrence Livermore National Laboratory: Annual report, 1987
1988
It reports the results of the Environmental Quality Verification Group, which is responsible for environmental monitor ing. Data are obtained through the combined efforts of the Environmental Protection Department, the Nuclear Chemistrv Division, an J the Hazards Control Department. In addition to the authors listed, the following personnel made significant contributions to this report: M. L. Alviso (2) C. Aracne (1) V. E. Arganbright (1) ]. A. Behne (2) 1. Beiriger (1) S. A. Bishop (2) 1. I-. Boyer (2) S. L. Brigdon (2) M. Brown (1) T. Carlsen (1) D. VV. Carpenter (2) ]. 1.. Cate, ]r. (2) C. DeGrange (2) E. Dranev (2) T. Ellis (1) R. A. 1'ailor (2) L. Finnie (1) L. A. Pry (1)). Garrison (1) A. R. Gravson (2) K. S. Griggs (2) M. Heaton (1) R. Henry (2) F. Hoffman (2) S. Jackson (2) M. Johansen (1) Environmental Quality Verification Personnel (1) Administrative and Technical Support Personnel (2)
Radiocarbon, 2016
Substances enriched with 14 C can easily contaminate samples and laboratories used for natural abundance measurements. We have developed a new method using wet chemical oxidation for swabbing laboratories and equipment to test for 14 C contamination. Here we report the findings of 18 months work and more than 800 tests covering studies at multiple locations. Evidence of past and current use of enriched 14 C was found at all but one location and a program of testing and communication was used to mitigate its effects. Remediation was attempted with mixed success and depended on the complexity and level of the contamination. We describe four cases from different situations. 2. Introduction The use of radiochemicals enriched with 14 C can contaminate work areas used for natural abundance measurements. The concentration of naturally occurring 14 C is 10-12 and blanks measured by accelerator mass spectrometry (AMS) are <10-15. Therefore, commercially available radiochemicals containing 100% atom 14 C are >15 orders of magnitude above blank levels and pose a catastrophic danger to AMS laboratories. Several laboratories have reported experiences of contamination and recovery from a single 'hot' sample and we are aware of a number of other unreported examples (Jull et al. 1990; Vogel et al. 1990; Zhou et al. 2012). Practices for preventing contamination, evaluating and monitoring potential workspaces and cleaning contaminated workspaces and laboratory equipment have been described for both natural abundance and bio-AMS preparation laboratories (Buchholz et al. 2000; Zermeno et al. 2004). In the case of a graphitization of a hot sample, it was found that the majority of the contamination occurred in the graphitization system where cross talk between samples occurs due to extended manipulation of the gases during sample preparation. It was possible to recover from a contamination event from a single hot sample in the 10-6-10-9 range by extensive cleaning of the apparatus and replacement of parts that have been in direct contact with the hot sample. The ion source of the AMS system recovered quickly where it had been in
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,