| 1. |
- Blachucki, Wojciech, et al.
(författare)
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A laboratory-based double X-ray spectrometer for simultaneous X-ray emission and X-ray absorption studies
- 2019
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Ingår i: Journal of Analytical Atomic Spectrometry. - : Royal Society of Chemistry. - 0267-9477 .- 1364-5544. ; 34:7, s. 1409-1415
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Tidskriftsartikel (refereegranskat)abstract
- X-ray spectroscopy studies are usually performed using synchrotron radiation sources, which offer bright, coherent, energy-tuneable and monochromatic light. However, the application of synchrotron-based Xray emission spectroscopy (XES) and X-ray absorption spectroscopy (XAS) is directly constrained by the limited, infrequent access to central facilities. With the advent of new technological solutions in the field of X-ray sources, optics and detectors, the development of efficient and compact laboratory X-ray spectroscopy systems is possible. A permanent laboratory-based setup offers the advantages of low cost and easy accessibility and, therefore, more flexibility in the preparation and scheduling of measurements. Herein, we report a laboratory X-ray setup allowing simultaneous XES and XAS measurements. The double von Hamos spectrometer performances are demonstrated by concurrent K beta XES and K-edge XAS measurements done for 3d elements.
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| 2. |
- Dowlatshahi Pour, Masoumeh, 1976, et al.
(författare)
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Mass spectrometry imaging as a novel approach to measure hippocampal zinc
- 2019
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Ingår i: Journal of Analytical Atomic Spectrometry. - : Royal Society of Chemistry (RSC). - 0267-9477 .- 1364-5544. ; 34:8, s. 1581-1587
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Tidskriftsartikel (refereegranskat)abstract
- Zinc (Zn2+) is an essential trace element that plays crucial roles in the functioning of hundreds of enzymes and DNA binding transcription factors. Zinc is also an essential neuromodulator and can act as a potent neurotoxin in excitotoxic brain injury after seizures, strokes, and brain trauma where high levels of Zn2+ can cause irreparable brain damage in certain brain regions. However, the mechanism of neurotoxicity has not been fully understood yet and is still under debate. In the present study, we have developed a time of flight secondary ion mass spectrometry (ToF-SIMS) imaging method to investigate the distribution of zinc in the rat brain. The zinc distribution in hippocampus sections from healthy rats and rats exposed to traumatic brain injury was imaged and the results were compared to those from conventional zinc-probe based fluorescence microscopy. Two related zinc species, ZnOH3 + and ZnO2H+, can successfully be visualized by ToF-SIMS in the rat hippocampus. Statistical data analysis of the image data demonstrated a substantial increase of both ZnOH3 + and ZnO2H+ in the zinc related species in the acute brain injury tissue. Our findings positively support the fact that toxic vesicular zinc accumulation might not be the sole source for neuronal degeneration following traumatic brain injuries. Also, we could successfully apply ToF-SIMS imaging for the first time to visualize the zinc content and distribution across hippocampus sections. Consequently, ToF-SIMS is a powerful method to further investigate biological phenomena such as seizures, ischemia, and strokes and also other forms of cellular damage in the central nervous system.
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| 3. |
- Grasse, Patricia, et al.
(författare)
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GEOTRACES inter-calibration of the stable silicon isotope composition of dissolved silicic acid in seawater
- 2017
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Ingår i: Journal of Analytical Atomic Spectrometry. - : Royal Society of Chemistry (RSC). - 0267-9477 .- 1364-5544. ; 32:3, s. 562-578
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Tidskriftsartikel (refereegranskat)abstract
- The first inter-calibration study of the stable silicon isotope composition of dissolved silicic acid in seawater, delta Si-30(OH)(4), is presented as a contribution to the international GEOTRACES program. Eleven laboratories from seven countries analyzed two seawater samples from the North Pacific subtropical gyre (Station ALOHA) collected at 300 m and at 1000 m water depth. Sampling depths were chosen to obtain samples with a relatively low (9 mmol L-1, 300 m) and a relatively high (113 mmol L-1, 1000 m) silicic acid concentration as sample preparation differs for low- and highconcentration samples. Data for the 1000 m water sample were not normally distributed so the median is used to represent the central tendency for the two samples. Median delta Si-30(OH)(4) values of +1.66& for the low-concentration sample and +1.25& for the high-concentration sample were obtained. Agreement among laboratories is overall considered very good; however, small but statistically significant differences among the mean isotope values obtained by different laboratories were detected, likely reflecting inter-laboratory differences in chemical preparation including pre-concentration and purification methods together with different volumes of seawater analyzed, and the use of different mass spectrometers including the Neptune MC-ICP-MS (Thermo Fisher (TM), Germany), the Nu Plasma MC-ICP-MS (Nu Instruments (TM), Wrexham, UK), and the Finnigan (TM) (now Thermo Fisher (TM), Germany) MAT 252 IRMS. Future studies analyzing delta Si-30(OH)(4) in seawater should also analyze and report values for these same two reference waters in order to facilitate comparison of data generated among and within laboratories over time.
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| 4. |
- Hogmalm, Johan, 1979, et al.
(författare)
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In situ Rb-Sr and K-Ca dating by LA-ICP-MS/MS: an evaluation of N2O and SF6 as reaction gases
- 2017
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Ingår i: Journal of Analytical Atomic Spectrometry. - : Royal Society of Chemistry (RSC). - 0267-9477 .- 1364-5544. ; 32:2, s. 305-313
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Tidskriftsartikel (refereegranskat)abstract
- In situ dating of K-rich minerals, e.g. micas and K-feldspar, by the Rb–Sr isotopic system is a new development made possible by the ICP-MS/MS technique. Online chemical separation of Rb and Sr is possible in an O2-filled reaction cell, wherein a portion of the Sr reacts to SrO+ while simultaneously no RbO+ is formed. O2 reactions provide stable analytical conditions sufficient for precise and accurate determination of Rb/Sr and Sr/Sr isotopic ratios using 80 micron laser ablation spots. However, to date <10% of the Sr reacts with O2 as reaction gas, leaving room for improvement using more potent reaction gases. With a more efficient reactive transfer, it should be possible to obtain similar results with a smaller laser spot size, hence gaining higher spatial resolution. In this study, we have evaluated N2O and SF6 as reaction gases since they have previously been shown to react strongly with Sr+, without affecting Rb+. Analytical conditions, including cell parameters and reaction gas flow rate were optimized while ablating NIST SRM 610. The main reaction product is SrO+ for N2O reaction and SrF+ for SF6 reaction. Both gases show significantly higher reaction product formation compared to O2 with >85% of Sr reacting with N2O and >70% Sr reacting with SF6; Rb does not react with either gas. As a result, the sensitivity for Sr reaction products is ∼10 times higher with N2O and ∼8 times higher with SF6 compared to O2. With these more reactive gases, the error of mica isochron ages, calibrated against a newly developed nano-particulate pressed powder tablet of mica–Mg, is ∼1% using a 50 μm laser spot. Our tests show that both N2O and SF6 form interfering reaction products, e.g., SrOH (N2O), SiF3 and TiF3 (SF6) that are difficult to handle using single mass spectrometer instruments, but which can be overcome using MS/MS. Using SF6 combined with H2, it is possible to measure 40Ca+ as 40Ca19F+, free from interference of 40Ar+ and 40K+. This facilitates the dating of micas by the K–Ca isotopic system; we present the first in situ K–Ca age determination.
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| 5. |
- Hogmalm, Johan K., et al.
(författare)
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In situ Rb–Sr and K–Ca dating by LA-ICP-MS/MS: an evaluation of N2O and SF6 as reaction gases
- 2017
-
Ingår i: Journal of Analytical Atomic Spectrometry. - 0267-9477 .- 1364-5544. ; 32, s. 305-313
-
Tidskriftsartikel (refereegranskat)abstract
- In situ dating of K-rich minerals, e.g. micas and K-feldspar, by the Rb–Sr isotopic system is a new development made possible by the ICP-MS/MS technique. Online chemical separation of Rb and Sr is possible in an O2-filled reaction cell, wherein a portion of the Sr reacts to SrO+ while simultaneously no RbO+ is formed. O2 reactions provide stable analytical conditions sufficient for precise and accurate determination of Rb/Sr and Sr/Sr isotopic ratios using 80 micron laser ablation spots. However, to date <10% of the Sr reacts with O2 as reaction gas, leaving room for improvement using more potent reaction gases. With a more efficient reactive transfer, it should be possible to obtain similar results with a smaller laser spot size, hence gaining higher spatial resolution. In this study, we have evaluated N2O and SF6 as reaction gases since they have previously been shown to react strongly with Sr+, without affecting Rb+. Analytical conditions, including cell parameters and reaction gas flow rate were optimized while ablating NIST SRM 610. The main reaction product is SrO+ for N2O reaction and SrF+ for SF6 reaction. Both gases show significantly higher reaction product formation compared to O2 with >85% of Sr reacting with N2O and >70% Sr reacting with SF6; Rb does not react with either gas. As a result, the sensitivity for Sr reaction products is ∼10 times higher with N2O and ∼8 times higher with SF6 compared to O2. With these more reactive gases, the error of mica isochron ages, calibrated against a newly developed nano-particulate pressed powder tablet of mica–Mg, is ∼1% using a 50 μm laser spot. Our tests show that both N2O and SF6 form interfering reaction products, e.g., SrOH (N2O), SiF3 and TiF3 (SF6) that are difficult to handle using single mass spectrometer instruments, but which can be overcome using MS/MS. Using SF6 combined with H2, it is possible to measure 40Ca+ as 40Ca19F+, free from interference of 40Ar+ and 40K+. This facilitates the dating of micas by the K–Ca isotopic system; we present the first in situ K–Ca age determination.
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| 6. |
- Korvela, Marcus, et al.
(författare)
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Internal standards in inductively coupled plasma mass spectrometry using kinetic energy discrimination and dynamic reaction cells
- 2018
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Ingår i: Journal of Analytical Atomic Spectrometry. - : ROYAL SOC CHEMISTRY. - 0267-9477 .- 1364-5544. ; 33:10, s. 1770-1776
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Tidskriftsartikel (refereegranskat)abstract
- ICP-MS is a sensitive element analysis technique used for analyzing several different sample types. This can result in difficult matrixes which can affect both physical parameters and create overlaps of analyte elements. Some of the possible overlaps can be reduced by the use of reaction and/or collision cells, while the use of internal standards can help with reducing the physical interferences caused by a matrix. While both internal standardization and the use of cells have been studied separately, their effects on each other have not been investigated earlier. In this study ICP-MS was used to analyze Mg-24, Al-27, Ti-47, Ti-49, V-51, Cr-52, Cr-53, Mn-55, Fe-57, Co-59, Ni-60, Ni-61, Ni-62, Cu-63, Cu-65, Zn-66, Zn-67, As-75, Se-78, Se-82, Cd-111, and Pb-208 with Be-9, Y-89, Ga-69, Rh-103, In-115, Ir-193, and Tl-205 as internal standards with high concentrations of either HNO3, PBS-buffer, or Triton X-100 as the matrix, in reaction-, collision- and standard-cell modes. This was done to investigate which internal standards would compensate matrix effects in different cell modes. All internal standards, except Be, compensated fairly well (relative sensitivity RSD < 10%) even for severe matrix effects for most elements regardless of similarity in mass in the different cell modes. For Zn, As and Se no proper internal standard could be found, of the ones investigated.
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| 7. |
- Pontér, Simon, et al.
(författare)
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Chromium isotope ratio measurements in environmental matrices by MC-ICP-MS
- 2016
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Ingår i: Journal of Analytical Atomic Spectrometry. - 0267-9477 .- 1364-5544. ; 31:7, s. 1464-1471
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Tidskriftsartikel (refereegranskat)abstract
- An analytical procedure consisting of high pressure/temperature acid digestion using an UltraCLAVE system and a one pass, single column matrix separation using DOWEX AG 1X8 anion exchange resin was applied to the determination of Cr concentrations and δ53Cr in chromites, soils, and biological matrices (epiphytic lichens and mosses) using a combination of ICP-SFMS and MC-ICP-MS. The overall reproducibility of the method was assessed by replicate preparation and Cr isotope ratio measurements performed by different operators in multiple analytical sessions over a few months and was found to be 0.11‰ (2σ). The accuracy was evaluated using commercially available reference materials for which measured data were compared with certified values (for Cr concentrations) and previously published results (for isotope data). The results demonstrate a uniform Cr isotope composition in soil depth profiles sampled in different urban environments. A strong negative correlation between δ53Cr and Cr concentrations in lichens and mosses indicates that airborne Cr from local anthropogenic source(s) is depleted in heavy isotopes.
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| 8. |
- Pontér, Simon, et al.
(författare)
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Chromium isotope ratio measurements in environmental matrices by MC-ICP-MS
- 2016
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Ingår i: Journal of Analytical Atomic Spectrometry. - : Royal Society of Chemistry (RSC). - 0267-9477 .- 1364-5544. ; 31:7, s. 1464-1471
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Tidskriftsartikel (refereegranskat)abstract
- An analytical procedure consisting of high pressure/temperature acid digestion using an UltraCLAVE system and a one pass, single column matrix separation using DOWEX AG 1X8 anion exchange resin was applied to the determination of Cr concentrations and delta Cr-53 in chromites, soils, and biological matrices (epiphytic lichens and mosses) using a combination of ICP-SFMS and MC-ICP-MS. The overall reproducibility of the method was assessed by replicate preparation and Cr isotope ratio measurements performed by different operators in multiple analytical sessions over a few months and was found to be 0.11 parts per thousand (2 sigma). The accuracy was evaluated using commercially available reference materials for which measured data were compared with certified values (for Cr concentrations) and previously published results (for isotope data). The results demonstrate a uniform Cr isotope composition in soil depth profiles sampled in different urban environments. A strong negative correlation between delta Cr-53 and Cr concentrations in lichens and mosses indicates that airborne Cr from local anthropogenic source(s) is depleted in heavy isotopes.
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| 9. |
- Rodushkin, Ilia, et al.
(författare)
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Assessment of the natural variability of B, Cd, Cu, Fe, Pb, Sr, Tl and Zn concentrations and isotopic compositions in leaves, needles and mushrooms using single sample digestion and two-column matrix separation
- 2016
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Ingår i: Journal of Analytical Atomic Spectrometry. - 0267-9477 .- 1364-5544. ; 31:1, s. 220-233
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Tidskriftsartikel (refereegranskat)abstract
- An analytical procedure allowing multi-elemental analyses and isotope ratio measurements of eight of these (B, Cd, Cu, Fe, Pb, Sr, Tl and Zn) in matrices relevant for bio-monitoring using a single highpressure acid digestion was developed. Method blanks, separation efficiency of matrix elements, repeatability and reproducibility were evaluated using sets of preparation blanks, certified reference materials and duplicate samples prepared and analyzed over a period of several months. The method was used to assess the natural variability of concentrations and isotopic compositions in bio-indicators (tree leaves, needles and mushrooms, over 240 samples) collected mainly from a confined area in North-East Sweden. Ranges found from leaves and needles were compared with data obtained for limited numbers of samples collected in Spain, Italy, France, United Kingdom and Iceland.
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| 10. |
- Tharaud, M., et al.
(författare)
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TiO2 nanomaterial detection in calcium rich matrices by spICPMS. A matter of resolution and treatment
- 2017
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Ingår i: Journal of Analytical Atomic Spectrometry. - : Royal Society of Chemistry (RSC). - 0267-9477 .- 1364-5544. ; 32:7, s. 1400-1411
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Tidskriftsartikel (refereegranskat)abstract
- High Ca concentrations in complex matrices such as river waters often hamper the detection of titanium nanomaterials (TiO2 NPs) by single particle inductively coupled plasma mass spectrometry (spICPMS), because of isobaric interference of Ca-48 on the most abundant Ti isotope (Ti-48). Several approaches were used to reduce this interference while measuring TiO2 in solutions with different Ca concentrations up to 100 mg L-1. ICP-MS/MS was used with ammonia as the reaction ceLL gas and high resoLution (HR) ICP-MS was used under different resoLution settings. These approaches were compared by measuring different Ti isotopes (Ti-47 and Ti-49). spICPMS data were then treated with a deconvoLution method to filter out dissolved signals and identify the best approach to detect the Lowest possible corresponding spherical size of TiO2 NPs (D,in). ICP-MS/MS aLLowed for an important decrease of the theoretical D-min compared to standard quadrupole ICP-MS, down to 64 nm in uLtrapure water; however the sensitivity was reduced by the reaction gas and increasing Ca concentrations also increased the D-min. The comparably higher sensitivity of HR-ICP-MS aLLowed for theoretically measuring a D-min of 10 nm in uLtrapure water. Combined with the deconvoLution analysis, the highest resoLution mode in HR-ICP-MS Leads to the Lowest D-min at high Ca concentrations, even though significant broadening of the measured mass distributions occurred for TiO2 NPs at Ca concentrations up to 100 mg L-1.
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