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Title: High-Throughput Method for Strontium Isotope Analysis by Multi-Collector-Inductively Coupled Plasma-Mass Spectrometer

Abstract

This technical report presents the details of the Sr column configuration and the high-throughput Sr separation protocol. Data showing the performance of the method as well as the best practices for optimizing Sr isotope analysis by MC-ICP-MS is presented. Lastly, this report offers tools for data handling and data reduction of Sr isotope results from the Thermo Scientific Neptune software to assist in data quality assurance, which help avoid issues of data glut associated with high sample throughput rapid analysis.

Authors:
 [1];  [2];  [2];  [2];  [1];  [1];  [1]
  1. National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States)
  2. Univ. of Pittsburgh, PA (United States)
Publication Date:
Research Org.:
National Energy Technology Lab. (NETL), Pittsburgh, PA, (United States)
Sponsoring Org.:
USDOE
OSTI Identifier:
1361494
Report Number(s):
NETL-PUB-20755
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
47 OTHER INSTRUMENTATION; Strontium isotope

Citation Formats

Wall, Andrew J., Capo, Rosemary C., Stewart, Brian W., Phan, Thai T., Jain, Jinesh C., Hakala, Alexandra, and Guthrie, George D.. High-Throughput Method for Strontium Isotope Analysis by Multi-Collector-Inductively Coupled Plasma-Mass Spectrometer. United States: N. p., 2016. Web. doi:10.2172/1361494.
Wall, Andrew J., Capo, Rosemary C., Stewart, Brian W., Phan, Thai T., Jain, Jinesh C., Hakala, Alexandra, & Guthrie, George D.. High-Throughput Method for Strontium Isotope Analysis by Multi-Collector-Inductively Coupled Plasma-Mass Spectrometer. United States. doi:10.2172/1361494.
Wall, Andrew J., Capo, Rosemary C., Stewart, Brian W., Phan, Thai T., Jain, Jinesh C., Hakala, Alexandra, and Guthrie, George D.. Thu . "High-Throughput Method for Strontium Isotope Analysis by Multi-Collector-Inductively Coupled Plasma-Mass Spectrometer". United States. doi:10.2172/1361494. https://www.osti.gov/servlets/purl/1361494.
@article{osti_1361494,
title = {High-Throughput Method for Strontium Isotope Analysis by Multi-Collector-Inductively Coupled Plasma-Mass Spectrometer},
author = {Wall, Andrew J. and Capo, Rosemary C. and Stewart, Brian W. and Phan, Thai T. and Jain, Jinesh C. and Hakala, Alexandra and Guthrie, George D.},
abstractNote = {This technical report presents the details of the Sr column configuration and the high-throughput Sr separation protocol. Data showing the performance of the method as well as the best practices for optimizing Sr isotope analysis by MC-ICP-MS is presented. Lastly, this report offers tools for data handling and data reduction of Sr isotope results from the Thermo Scientific Neptune software to assist in data quality assurance, which help avoid issues of data glut associated with high sample throughput rapid analysis.},
doi = {10.2172/1361494},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Thu Sep 22 00:00:00 EDT 2016},
month = {Thu Sep 22 00:00:00 EDT 2016}
}

Technical Report:

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  • This technical report presents the details of the Sr column configuration and the high-throughput Sr separation protocol. Data showing the performance of the method as well as the best practices for optimizing Sr isotope analysis by MC-ICP-MS is presented. Lastly, this report offers tools for data handling and data reduction of Sr isotope results from the Thermo Scientific Neptune software to assist in data quality assurance, which help avoid issues of data glut associated with high sample throughput rapid analysis.
  • The INL made an assessment of the commercially available inductively coupled plasma mass spectrometers (ICPMS) for actinide analysis; emphasizing low detection limits for plutonium. INL scientists subsequently determined if plutonium was present on a swipe, at a 10 million atom decision level. This report describes the evaluation of ICPMS instruments and the operational testing of a new process for the dissolution, separation and analysis via ICPMS of swipes for plutonium and uranium. The swipe dissolution, plutonium and uranium isolation, separation and purification are wet chemistry methods following established procedures. The ICPMS is a commercially available multi-collector magnetic sector mass spectrometermore » that utilizes five ion counting detectors operating simultaneously. The instrument includes a sample introduction system allowing for sample volumes of < 1 mL to be reproducibly injected into the instrument with minimal waste of the sample solution, while maximizing the useable signal. The performance of the instrument was measured using SRM 996 ( 244Pu spike) at concentrations of 12 parts per quadrillion (ppq, fg/mL) and with SRM 4350B Columbia River Sediment samples spiked onto swipes at the 10 million atom level. The measured limit of detection (LOD, defined as 3s) for 239Pu is 310,000 atoms based upon the instrument blank data. The limit of quantification (LOQ defined as 10 s) for 239Pu is 105,000 atoms. The measured limit of detection for 239Pu from the SRM 4350B spiked onto a swipe was 2.7 million atoms with the limit of quantification being 9.0 million atoms.« less
  • The sampling of ions from an atmospheric pressure inductively coupled plasma for mass spectrometry (ICP-MS) with a supersonic nozzle and skimmer is shown to follow similar behavior found for neutral beam studies and for ion extraction from other plasmas and flames. In particular, highest ion beam intensity is found if the skimmer tip is close to the Mach disk and at a calculated skimming Knudsen number close to the recommended value of 1. Our ICP-MS instrument with an off-axis detector and conventional cylindrical electrostatic ion focusing in the transition flow regime gives intense count rates of 1 to 5 MHzmore » per mg L/sup -1/ of analyte superimposed on a background of 1 to 10 kHz. The dependence of count rates for metal oxide and doubly charged ions on ICP operating parameters, and sampling interface configuration are discussed for this instrument. A simple method is described for the approximate measurement of the ion energy distribution in ICP-MS. The average ion kinetic energy, kinetic energy spread, and maximum kinetic energy are evaluated from a plot of ion signal as a function of retarding voltage applied to the quadrupole mass analyzer. The effects of plasma operating parameters on ion signals and energies are described. In particular, kinetic energy is a sensitive function of aerosol gas flow rate. This behavior is attributed to a non-thermal, possibly electrical, interaction between the plasma and the sampling interface, which is induced by the presence of the axial channel in the ICP. The interference on the ionization of cobalt by five salts, NaCl, MgCl/sub 2/, NH/sub 4/I, NH/sub 4/Br and NH/sub 4/Cl, in an ICP is first considered theoretically and subsequently the theoretical trends are established experimentally by ICP-MS. The interference trends are found to be in the order of the most easily ionized element in the matrix salt, i.e., Na > Mg > I > Br > Cl.« less
  • The document is an appendix to Method 200.7, Inductively Coupled Plasma-Atomic Emission Spectrometric Method for Trace Analysis of Water and Wastes. The procedure is not a stand along method, but as an appendix is intended to be used in connection with Method 200.7 for the analysis of drinking water. Revision 1.3 replaces an earlier revision of the appendix dated September, 1985. The method is applicable to the analyses of certain primary contaminants (Ag, As, Ba, Cd, Cr and Pb) for their respective existing maximum contaminant levels (MCL) as of that date. However, at such time the Agency promulgates new MCL'smore » all methods including the appendix to Method 200.7 will be reevaluated to determine their continued approval. The original document on EPA Method 200.7 is also included. The method describes the requirements for the use of the inductively coupled plasma in the analysis of water and wastes for some 25 elements.« less