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Inductively Coupled Plasma Atomic Emission Spectrometry: Exploring the Limits of Different Sample Preparation Strategies
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry, Analytical Chemistry. (Ultratrace Elemental Analysis)
2011 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

This thesis describes two different sample preparation strategies for inductively coupled plasma atomic emission spectrometry (ICP-AES), and their ability regarding multi element quantification in complex samples. Sensitivity, repeatability, reproducibility and accuracy were investigated. The aim was to increase the over all efficiency, the speed of analysis, and/or the sensitivity of the analytical method. The intention was to measure analytes with concentrations ranging from ng/g to mg/g simultaneously. The aim was additionally to study chemical and physical processes occurring during the sample preparation, the sample transport to the plasma, and the atomization therein.

In the first sample preparation strategy, a hydrophilic highly cross-linked iminodiacetate-agarose adsorbent, IDA-Novarose, was used for preconcentration of metal ions, and matrix elimination in natural water samples. The sorbent was synthesized with different binding capacities. The effect of the capacity on preconcentration, matrix elimination, and uptake capability at high flow rates was studied. For a high capacity IDA-Novarose (≥ 45 µmole/ml) quantitative uptake was seen even at high flow rates (100 ml/min) for Cu2+ with a high affinity to the adsorbent, and for Cd2+ with a moderate affinity. For lower capacities the uptake of Cd2+ was affected by the sample matrix and the flow rate. A method based on the determination of the conditional stability constant of the metal sorbent complex was suggested for the prediction of the sorbent capacity needed to obtain quantitative recovery and optimal matrix elimination. The sorbent was used in a flow system with online buffering for the analysis of a certified riverine water (SLRS-3), tap water and lake water. With few exceptions the results obtained by ICP-AES after preconcentration agreed well with the certified concentrations and results obtained by ICP-MS.

The other sample preparation strategy discussed is a method for non digested biological samples from different animal organs for the multi element analysis by ICP-AES. This “mix and measure method” consists of a simple homogenization of the sample with a mixing rod in a small amount of neutral media, followed by dilution and direct measurement with ICP-AES. The total time of analysis is only a few minutes. The ability of this fast method to accurately quantify some elements of toxic, environmental, and/or physiological concern with the lowest possible sample dilution and the highest possible plasma load was evaluated. In 10 % liver slurry Cd, Co, and Sr, at concentration levels around 0.05 µg/g were quantified simultaneously with P and K around 2000 µg/g and with several other elements in between (Al, Ca, Cu, Fe, Mg, Mn, Pb, and Zn). The relative standard deviation of repeated measurements of samples was around 5 - 6 % for regardless of the concentration of the element. The method was also used for fast screening of the elemental distribution in mice organs (brain, heart, kidney, liver, lung and spleen).

Place, publisher, year, edition, pages
Uppsala: Acta Universitatis Upsaliensis , 2011. , 59 p.
Series
Digital Comprehensive Summaries of Uppsala Dissertations from the Faculty of Science and Technology, ISSN 1651-6214 ; 821
Keyword [en]
multi element analysis, trace element, ICP-AES, inductively coupled plasma atomic emission spectromtery, water analysis, liver analysis, non digested samples, medical samples, biological samples, samples from biopsies and autopsies, mice organ, fast analysis, internal standard, preconcentration, matrix elimination, Cu, Zn, Mn, Co, Pb, Cd, Mg, Ca, Fe, Ni, Cr, S, P, K, Al
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
URN: urn:nbn:se:uu:diva-150861ISBN: 978-91-554-8063-9OAI: oai:DiVA.org:uu-150861DiVA: diva2:409033
Public defence
2011-05-20, B22, Uppsala Biomedical Center, BMC, Husargatan 3, Uppsala, 10:15 (English)
Opponent
Supervisors
Available from: 2011-04-29 Created: 2011-04-06 Last updated: 2011-05-05Bibliographically approved
List of papers
1. Effects of capacity on the preconcentration of trace metals and matrix elimination by an iminodiacetate chelating adsorbent
Open this publication in new window or tab >>Effects of capacity on the preconcentration of trace metals and matrix elimination by an iminodiacetate chelating adsorbent
1998 (English)In: Talanta, ISSN 0039-9140, Vol. 46, no 5, 1051-1063 p.Article in journal (Refereed) Published
Abstract [en]

Low capacity adsorbents, based on iminodiacetic acid and a crosslinked agarose, Novarose(TM), have been synthesised for the enrichment of metal ions. Test ions Cu2+ with high, and Cd2+ with a moderate affinity for the sorbent were selected. The study includes the effect of specific capacity and matrix composition on the rate of uptake and recovery of these ions. Using a column packed with 0.25 ml of a sorbent and a sample volume of 100 ml, Cu2+ is quantitatively accumulated from all of the matrices studied even at a capacity of 6 mu mol ml(-1) of adsorbent and a flow rate as high as 100 ml min(-1). The enrichment of Cd2+ is affected by the matrix and for quantitative recovery the flow rate and capacity must be properly adjusted. In the presence of 0.01 M Ca2+, a specific capacity of 45 mu mol ml(-1) is needed for quantitative retainment and a flow rate of 100 ml min(-1), whereas a capacity of 10 mu mol ml(-1) suffices at 10 ml min(-1). The advantage of low specific capacity on the removal of matrix elements has been demonstrated. A method based on the determination of conditional stability constants of the metal sorbent complex is suggested for predicting the sorbent capacity needed to acquire quantitative recovery and optimal matrix elimination.

Keyword
iminodiacetate adsorbent; low capacity; preconcentration; matrix elimination; PLASMA-MASS SPECTROMETRY; NATURAL-WATERS; SEPARATION; SYSTEM; ELEMENTS; RESIN
Identifiers
urn:nbn:se:uu:diva-84759 (URN)
Available from: 2005-04-04 Created: 2005-04-04 Last updated: 2011-05-05
2. Properties of a high capacity iminodiacetate-agarose adsorbent and its application in a flow system with on-line buffering of acidified samples for accumulation of metal ions in natural waters
Open this publication in new window or tab >>Properties of a high capacity iminodiacetate-agarose adsorbent and its application in a flow system with on-line buffering of acidified samples for accumulation of metal ions in natural waters
1999 (English)In: TALANTA, Vol. 49, no 4, 825-835 p.Other (Other scientific)
Abstract [en]

Adsorption properties of a fast iminodiacetate-agarose adsorbent, IDA-Novarose, with a capacity of 120-140 mu mol/ml were studied for preconcentration of eight transition elements. A FIA-ICP-PLES system was used in the study. It was shown that 0.3 ml of

Place, publisher, year, edition, pages
ELSEVIER SCIENCE BV, 1999. 825-835 p.
Keyword
iminodiacetate adsorbent; preconcentration; ICP-AES; natural waters; ATOMIC-ABSORPTION SPECTROMETRY; PLASMA-MASS SPECTROMETRY; ONLINE PRECONCENTRATION; EMISSION-SPECTROMETRY; TRACE-METALS; SEA-WATER; COLUMN PRECONCENTRATION; MATRIX ELIMINATION; CHELATIN
Identifiers
urn:nbn:se:uu:diva-84854 (URN)
Note
Addresses: Olin A, Univ Uppsala, Dept Analyt Chem, POB 531, S-75121 Uppsala, Sweden. Univ Uppsala, Dept Analyt Chem, S-75121 Uppsala, Sweden.Available from: 2008-10-17 Created: 2008-10-17 Last updated: 2011-05-05
3. Fast multi-element screening of non-digested biological materials by slurry introduction to ICP-AES.
Open this publication in new window or tab >>Fast multi-element screening of non-digested biological materials by slurry introduction to ICP-AES.
2010 (English)In: Talanta: The International Journal of Pure and Applied Analytical Chemistry, ISSN 0039-9140, E-ISSN 1873-3573, Vol. 80, no 5, 2068-2075 p.Article in journal (Refereed) Published
Abstract [en]

A fast method for direct multi-element analysis of non-digested biological samples is presented. The only sample preparation needed is 1 min homogenization with a Polytron mixer in a small volume of neutral phosphate buffer saline solution (PBS). The total time for analysis (sample preparation and measurement) is 4 min only. This "mix and measure" method can handle large sample loads of biological samples and thus minimize dilution of trace elements. For example 100% whole blood was introduced without any clogging of the introduction system or extinguishing of the plasma. In 70% (v/v) whole blood reference material 14 of 16 analytes were quantified within ±10% (Al, B, Ba, Ca, Cu, Fe, Mg, Mn, P, Pb, S, Sr, Ti and Zn) and two semi-quantified within ±20% (Cd and K). Fresh bovine liver was also analyzed with the same method and 7 of 9 analytes were quantified in 5% (w/v) liver slurry. Three different nebulizers were tested, Glass Expansion Concentric (GEC) of Meinhard type, Cross Flow and Burgener T2100 and they performed roughly equally well in giving quantitative results for the slurries but the sensitivity was better with the GEC. The stability of the plasma was studied by evaluating the ratio of Mg 280.270 nm and Mg 285.213 nm lines. When increasing the sample load from 20 to 100% (v/v) of whole blood and from 0.5 to 10% (w/v) of bovine liver the Mg ratio was constant within a few percent for all of the nebulizer tested. The ratio of the sensitivity between GEC and Burgener T2100 was studied and the ratio increased with the energy sum for atomic and ionic lines separately.

Keyword
External calibration, ICP-AES, internal standards, liver, slurry, whole blood
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:uu:diva-122404 (URN)10.1016/j.talanta.2009.11.007 (DOI)000275612500073 ()20152454 (PubMedID)
Available from: 2010-04-12 Created: 2010-04-12 Last updated: 2011-05-06Bibliographically approved
4. Application of a fast multi element screening method using ICP-AES on liver samples and mice organs
Open this publication in new window or tab >>Application of a fast multi element screening method using ICP-AES on liver samples and mice organs
2011 (English)In: Journal of Trace Elements in Medicine and Biology, ISSN 0946-672XArticle in journal (Other academic) Submitted
Abstract [en]

A fast mix and measure method for direct multi element analysis of non digested biological samples was used for the simultaneous determination of low, medium, and high concentrations elements in liver samples from domestic and wild animals. The method was also used for screening several elements in different organs from five mice. Brain (cerebrum, left and right cerebellum), heart, kidney, liver, lung, spleen, and blood samples were analysed. The total time for sample preparation and measurement is four minutes only for each sample (dissection not included). Quantitative results within ± 10 % are presented in the liver samples for Al, Cd, Pb, Mn, Sr, P, K, and semi quantitative within ± 20 % for Ca, Co, Cu, Fe, Mg, and Zn. The overall reproducibility was around 5 % for most elements, slightly higher for elements close to the detection limit, which meets well with the 2-3 % obtained for the acid digestion method used for comparison. A bovine liver sample was spiked with low amounts of Al, Cd, Co, and Pb to outline the possibilities of the slurry method to quantify concentrations close to the estimated limit of quantification. The recoveries were 103, 104, 97 and 103 % respectively.

Place, publisher, year, edition, pages
Elsevier, 2011
Keyword
multi element, screening, medical samples, biological samples, ICP-AES, inductively coupled plasma atomic emission spectrometry, liver, mice
National Category
Analytical Chemistry
Research subject
Analytical Chemistry
Identifiers
urn:nbn:se:uu:diva-150837 (URN)
Available from: 2011-04-06 Created: 2011-04-06 Last updated: 2011-05-05Bibliographically approved

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