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Inductively Coupled Plasma Spectrometry for Speciation Analysis: Development and Applications
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry.
2007 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

In analytical chemistry the main goal is normally to determine the identity and/or concentration of one or more species in a sample. The samples analyzed are often natural samples, containing numerous different species in a complex matrix and the choice of technique for multi-elemental detection is in general inductively coupled plasma spectrometry. The chemical forms of an element can affect many of its characteristics e.g. toxicity, which makes speciation analysis important. Therefore, determination of the identity and quantity of an element is still important, but for many applications measurements of total element concentration provides insufficient information. To be able to perform speciation analysis, separation, identification and/or characterization of the various forms of elements in the sample has to be accomplished. Speciation analysis has been employed in a wide range of disciplines, including for example environmental science, biology and clinical chemistry.

This thesis describes work to improve and understand the elemental speciation analysis with liquid chromatography coupled to plasma spectrometry and also highlights the importance and potential of the synergy between atomic spectrometry and molecular mass spectrometry. The combination of the matrix tolerant, robust and very sensitive plasma spectrometry used together with molecular mass spectrometry, which provides structural information and the possibility to identify unknown species, is demonstrated to be a very powerful tool for speciation analysis. In this thesis methods are developed for on-line sample clean-up and pre-concentration coupled to liquid chromatography and plasma spectrometry, which makes handling of small sample volumes easier and also decreases the risk of contamination. The problems associated with organic modifiers in plasma spectrometry are also addressed. Applications of speciation analysis are exemplified by analysis of aluminium-chelated siderophores in field-soil solutions and organic phosphorous species in aquatic sediments. The possibility to analyze un-dissolved samples as slurries with minimal sample preparation is also discussed.

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis , 2007. , p. 56
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 327
Keywords [en]
Analytical chemistry, Speciation analysis, Atomic emission spectrometry (AES), Mass spectrometry (MS), Inductively coupled plasma (ICP), Liquid Chromatography (LC), on-line sample pre-treatment, Organic phosphour, Siderophores, Slurry nebulization, matrix effects
Keywords [sv]
Analytisk kemi
Identifiers
URN: urn:nbn:se:uu:diva-8169ISBN: 978-91-554-6945-0 (print)OAI: oai:DiVA.org:uu-8169DiVA, id: diva2:170564
Public defence
2007-09-25, B41, BMC, Uppsala, 13:15 (English)
Opponent
Supervisors
Available from: 2007-09-04 Created: 2007-09-04 Last updated: 2011-05-10Bibliographically approved
List of papers
1. Investigation of matrix effects in boron determination using organic solvents as modifiers for liquid chromatography coupled to ICP-MS
Open this publication in new window or tab >>Investigation of matrix effects in boron determination using organic solvents as modifiers for liquid chromatography coupled to ICP-MS
2006 In: Journal of Analytical Atomic Spectrometry, ISSN 0267-9477, Vol. 21, no 3, p. 305 - 310Article in journal (Refereed) Published
Identifiers
urn:nbn:se:uu:diva-96096 (URN)
Available from: 2007-09-04 Created: 2007-09-04Bibliographically approved
2. On-line electrochemically controlled solid-phase extraction interfaced to electrospray and inductively coupled plasma mass spectrometry
Open this publication in new window or tab >>On-line electrochemically controlled solid-phase extraction interfaced to electrospray and inductively coupled plasma mass spectrometry
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2005 In: The Analyst, ISSN 0003-2654, Vol. 130, no 10, p. 1358-1368Article in journal (Refereed) Published
Identifiers
urn:nbn:se:uu:diva-96097 (URN)
Available from: 2007-09-04 Created: 2007-09-04Bibliographically approved
3. Screening and identification of aluminium-containing biomolecules by column-switched LC-ICP-MS and LC-ESI-MS/MS
Open this publication in new window or tab >>Screening and identification of aluminium-containing biomolecules by column-switched LC-ICP-MS and LC-ESI-MS/MS
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2007 (English)In: Journal of Analytical Atomic Spectrometry, ISSN 0267-9477, E-ISSN 1364-5544, Vol. 22, no 11, p. 1397-1402Article in journal (Refereed) Published
Abstract [en]

Column-switching liquid chromatography followed by low resolution ICP-MS was evaluated as a tool for speciation analysis of aluminium-containing biomolecules. The strategy was applied on siderophores, small organic molecules (Mr < 1500) which normally act as strong iron chelators. The drawbacks normally encounterd with aluminium detection using low resolution ICP-MS are the formation of polyatomic ions causing isobaric overlaps and space-charge effects. When adding a carbon rich solvent, such as methanol or acetonitrile, the 13C14N+, 12C15N+ and 12C14N1H+ with the same mass as 27Al+ will form in the plasma. The nitrogen is either entrained from the surrounding atmosphere or added with the constituents in the mobile phase. These disadvantages were successfully counteracted by the use of nitrogen free organic modifier in the mobile phase and the use of cool plasma conditions. Detection limits for standard solutions of aluminium-chelated ferrichrome in sub-nanomolar range were obtained by monitoring the aluminium-27 isotope. The combined use of LC-ICP-MS and LC-ESI-MS/MS was also evaluated as a tool to identify unknown metal complexes, here siderophores, in field soil solution samples. Two aluminium-chelated siderophores, Al-desferrichrom and Al-desferricrocin, were identified and quantified. Both aluminium-siderophore complexes were present in the low nanomolar range (1.1 and 0.7 nM, respectively).

National Category
Chemical Sciences
Identifiers
urn:nbn:se:uu:diva-96098 (URN)10.1039/b707948f (DOI)000250399600015 ()
Available from: 2007-09-04 Created: 2007-09-04 Last updated: 2017-12-14Bibliographically approved
4. Screening for Organic Phosphorus Compounds in Aquatic Sediments by Liquid Chromatography Coupled to ICP-AES and ESI-MS/MS
Open this publication in new window or tab >>Screening for Organic Phosphorus Compounds in Aquatic Sediments by Liquid Chromatography Coupled to ICP-AES and ESI-MS/MS
Show others...
2008 (English)In: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 80, no 17, p. 6689-6697Article in journal (Refereed) Published
Abstract [en]

The structures of organic phosphorous (P) compounds in aquatic sediments are to a large extent unknown although these compounds are considered to play an important role in regulating lake trophic status. To enhance identification of these compounds, a liquid chromatography (LC) method for their separation was developed. The stationary phase was porous graphitic carbon (PGC), and the mobile phases used in the gradient elution were compatible with both inductive coupled plasma atomic emission spectroscopy (ICP-AES) and electrospray ionization tandem mass spectrometry (ESI-MS/MS). With LC-ICP-AES, eight different P containing peaks could be observed in the P chromatogram indicating that at least eight different P compounds were separated. With the setup of an information dependent acquisition (IDA) with ESI-MS/MS, the mass over charge (m/z) of compounds containing a phosphate group (H2PO3, m/z 97) could be measured and further fragmentation experiments gave additional information on the structure of almost 40 separated P compounds, several were verified to be nucleotides. ICP-AES was very suitable in the development of the LC method and allowed screening and quantification of P compounds. The presented LC-ESI-MS/MS technique was able to identify several sediment organic P compounds.

National Category
Analytical Chemistry
Identifiers
urn:nbn:se:uu:diva-97626 (URN)10.1021/ac8006335 (DOI)000258865300034 ()
Available from: 2008-10-15 Created: 2008-10-15 Last updated: 2017-12-14Bibliographically approved
5. Analysis of non-dissolved organic materials by ICP-AES and ICP-TOF-MS
Open this publication in new window or tab >>Analysis of non-dissolved organic materials by ICP-AES and ICP-TOF-MS
Manuscript (Other academic)
Identifiers
urn:nbn:se:uu:diva-96100 (URN)
Available from: 2007-09-04 Created: 2007-09-04 Last updated: 2010-01-13Bibliographically approved

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