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Author |
Margui, E.; Hidalgo, M.; Queralt, I.; van Meel, K.; Fontas, C. |
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Title  |
Analytical capabilities of laboratory, benchtop and handheld X-ray fluorescence systems for detection of metals in aqueous samples pre-concentrated with solid-phase extraction disks |
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A1 Journal article |
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Year |
2012 |
Publication |
Spectrochimica acta: part B : atomic spectroscopy |
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Volume |
67 |
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Pages |
17-23 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Abstract |
We aimed to achieve improved instrumental sensitivity and detection limits for the analysis of several elements (Cu, Ni, Zn, Pb and Cd) in aqueous samples with energy dispersive X-ray fluorescence spectrometry (EDXRF). The metals were pre-concentrated from aqueous solutions using commercially available organic-based solid-phase extraction (SPE) disks functionalized with iminodiacetate groups. These thin-layer organic materials provide an ideal support for XRF analysis. The elements were collected on the SPE extraction disks using a simple filtration procedure (starting with 1 L of aqueous sample) that allows direct XRF measurements to be performed in the field (in situ). We evaluated the analytical possibilities and drawbacks of using this pre-concentration procedure in combination with the following XRF configurations: a handheld unit, a benchtop EDXRF system and a high-energy polarized-beam EDXRF instrument (HE-P-EDXRF). Using the HE-P-EDXRF system, the detection limits for all metals were more than one order of magnitude lower than those attained using handheld and benchtop EDXRF instrumentation. For the detection of metal concentrations higher than similar to 20 mu g/L, however, handheld or benchtop systems remain a very good option due to their extreme simplicity of operation and low-cost, compact design. We demonstrate the application of these methodologies, using the three equipment systems, to the analysis of trace concentrations of metals in different types of aqueous samples, including tap water and waste water. (C) 2011 Elsevier B.V. All rights reserved. |
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Wos |
000302757200003 |
Publication Date |
2011-12-19 |
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0584-8547; 1873-3565 |
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UA library record; WoS full record; WoS citing articles |
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Call Number |
UA @ admin @ c:irua:98338 |
Serial |
7454 |
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Author |
van Meel, K.; Fontàs, C.; Van Grieken, R.; Queralt, I.; Hidalgo, M.; Marguí, E. |
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Title |
Application of high-energy polarised beam energy dispersive X-ray fluorescence spectrometry to cadmium determination in saline solutions |
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A1 Journal article |
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Year |
2008 |
Publication |
Journal of analytical atomic spectrometry |
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Volume |
23 |
Issue |
7 |
Pages |
1034-1037 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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000257146000017 |
Publication Date |
2008-04-22 |
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ISSN |
0267-9477 |
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UA library record; WoS full record; WoS citing articles |
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Call Number |
UA @ admin @ c:irua:69424 |
Serial |
7476 |
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Author |
Marguí, E.; Padilla, R.; Hidalgo, M.; Queralt, I.; Van Grieken, R. |
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Title |
High-energy polarized-beam EDXRF for trace metal analysis of vegetation samples in environmental studies |
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A1 Journal article |
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Year |
2006 |
Publication |
X-ray spectrometry |
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Volume |
35 |
Issue |
3 |
Pages |
169-177 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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000237818300005 |
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2006-03-23 |
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ISSN |
0049-8246 |
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UA library record; WoS full record; WoS citing articles |
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Call Number |
UA @ admin @ c:irua:57751 |
Serial |
8031 |
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Author |
Marguí, E.; Fontàs, C.; van Meel, K.; Van Grieken, R.; Queralt, I.; Hidalgo, M. |
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Title |
High-energy polarized-beam energy-dispersive X-ray fluorescence analysis combined with activated thin layers for cadmium determination at trace levels in complex environmental liquid samples |
Type |
A1 Journal article |
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Year |
2008 |
Publication |
Analytical chemistry |
Abbreviated Journal |
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Volume |
80 |
Issue |
7 |
Pages |
2357-2364 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Wos |
000254593500015 |
Publication Date |
2008-03-08 |
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ISSN |
0003-2700; 5206-882x |
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UA library record; WoS full record; WoS citing articles |
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Call Number |
UA @ admin @ c:irua:68425 |
Serial |
8032 |
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Author |
Marguí, E.; van Meel, K.; Van Grieken, R.; Buendía, A.; Fontás, C.; Hidalgo, M.; Queralt, I. |
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Title |
Method for the determination of Pd-catalyst residues in active pharmaceutical ingredients by means of high-energy polarized-beam energy dispersive X-ray fluorescence |
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A1 Journal article |
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Year |
2009 |
Publication |
Analytical chemistry |
Abbreviated Journal |
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Volume |
81 |
Issue |
4 |
Pages |
1404-1410 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Abstract |
In medicinal chemistry, Pd is perhaps the most-widely utilized precious metal, as catalyst in reactions which represent key transformations toward the synthesis of new active pharmaceutical ingredients (APIs). The disadvantage of this metal-catalyzed chemistry is that expensive and toxic metal residues are invariably left bound to the desired product. Thus, stringent regulatory guidelines exist for the amount of residual Pd that a drug candidate is allowed to contain. In this work, a rapid and simple method for the determination of Pd in API samples by high-energy polarized-beam energy dispersive X-ray fluorescence spectrometry has been developed and validated according to the specification limits of current legislation (10 mg kg−1 Pd) and the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH guidelines). Sample and calibration standards preparation includes a first step of homogenization and then, in a second step, the pressing of the powdered material into pellets without any chemical treatment. The use of several synthetic calibration standards made of cellulose to simulate the API matrix appears to be an effective means to obtain reliable calibration curves with a good spread of data points over the working range. With the use of the best measuring conditions, the limit of detection (0.11 mg kg−1 Pd) as well as the limit of quantitation (0.37 mg kg−1 Pd) achieved meet rigorous requirements. The repeatability of the XRF measurement appeared to be less than 2%, while the precision of the whole method was around 7%. Trueness was evaluated by analyzing spiked API samples at the level of the specification limit and calculating the recovery factor, which was better than 95%. To study the applicability of the developed methodology for the intended purpose, three batches of the studied API were analyzed for their Pd content, and the attained results were comparable to those obtained by the daily routine method (acid digestion plus atomic spectroscopy) used in most pharmaceutical laboratories. |
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Wos |
000263319000015 |
Publication Date |
2009-01-22 |
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ISSN |
0003-2700; 5206-882x |
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UA library record; WoS full record; WoS citing articles |
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Call Number |
UA @ admin @ c:irua:74340 |
Serial |
8220 |
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Author |
Marguí, E.; Van Grieken, R.; Fontàs, C.; Hidalgo, M.; Queralt, I. |
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Title |
Preconcentration methods for the analysis of liquid samples by X-ray fluorescence techniques |
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A1 Journal article |
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Year |
2010 |
Publication |
Applied spectroscopy reviews |
Abbreviated Journal |
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Volume |
45 |
Issue |
3 |
Pages |
179-205 |
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Keywords |
A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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Abstract |
This article gives an overview of the state-of-the-art of multi-element and single-element preconcentration procedures prior to X-ray fluorescence (XRF) analysis of liquid samples. Many of these preconcentration methods were developed long ago and the purpose of this review is to present some new efficient variations of these methods and new techniques extending the possibilities of XRF for liquid solutions analysis. In addition, trends and future perspectives in this domain are also commented on and discussed in the last section of the review. |
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000277705800002 |
Publication Date |
2010-01-28 |
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ISSN |
0066-5541 |
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UA library record; WoS full record; WoS citing articles |
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Call Number |
UA @ admin @ c:irua:82557 |
Serial |
8400 |
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Author |
Margu'i', E.; Queralt, I.; Van Grieken, R. |
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Title |
X-ray fluorescence analysis, sample preparation for |
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H1 Book chapter |
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2009 |
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Abbreviated Journal |
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Pages |
1-20
T2 - Sncyclopedia of analytical chemistry / M |
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Keywords |
H1 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation) |
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978-0-471-97670-7 |
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Call Number |
UA @ admin @ c:irua:81641 |
Serial |
8765 |
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