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1.
An ICP–MS instrument fitted with an octopole reaction system (ORS) was used to directly measure the inorganic contents of
several biofuel materials. Following sample preparation by simple dilution in kerosene, the biofuels were analysed directly.
The ORS effectively removed matrix- and plasma-based spectral interferences to enable measurement of all important analytes,
including sulfur, at levels below those possible by ICP–OES. A range of commonly produced biofuels was analysed, and spike
recovery and long-term stability data was acquired. Suitably configured ICP–MS has been shown to be a fast and very sensitive
technique for the elemental analysis of biofuels. 相似文献
2.
Konstantina Pasvanka Alexandros Tzachristas Marios Kostakis Nikolaos Thomaidis 《Analytical letters》2019,52(17):2741-2750
AbstractStudying wine mineral profile has been proven as a valuable tool in geographical origin discrimination and authenticity for both producers and consumers. Adulteration of wines, in terms of geographical origin or variety, is considered a major topic of extensive research. Traceability and authenticity of wines have been previously studied on the basis of typical mineral element patterns by means of chemometric methods. In this context, analytical methods were developed for the determination of mineral elements in wines by inductively coupled plasma–mass spectrometry. This study aimed at classifying selected varietal Greek wines from various regions by employing instrumental analysis. Preliminary data of wine mineral content enabled for the classification of samples according to geographical origin and variety. However, further work is required in order to draw more valid conclusions and to obtain a detailed map of the mineral element content of Greek wines according to their geographical origin and/or variety. 相似文献
3.
For analysis of uranium in urine determination of the isotope ratio and quantification were investigated by high-resolution inductively coupled plasma mass spectrometry (HR ICP-MS). The instrument used (ThermoFinniganMAT ELEMENT2) is a single-collector MS and, therefore, a stable sample-introduction system was chosen. The methodical set-up was optimized to achieve the best precision for both the isotope ratio and the total uranium concentration in the urine matrix.Three spiked urine samples from an European interlaboratory comparison were analyzed to determine the (235)U/(238)U isotope ratio. The ratio was found to be in the range 0.002116 to 0.007222, the latter being the natural uranium isotope ratio. The first ratio indicates the abundance of depleted uranium.The effect of storage conditions and the stability for the matrix urine were investigated by using "real-life" urine samples from unexposed persons in the Netherlands. For samples stored under refrigeration and acidified the results (range 0.8 to 5.3 ng L(-1) U) were in the normal fluctuation range whereas a decrease in uranium concentration was observed for samples stored at room temperature without acidification. 相似文献
4.
Elżbieta Lipiec Grzegorz Siara Katarzyna Bierla Laurent Ouerdane Joanna Szpunar 《Analytical and bioanalytical chemistry》2010,397(2):731-741
A method for the simultaneous determination of selenomethionine (SeMet), selenocysteine (SeCys), and selenite [Se(IV)] in
chicken eggs was developed. A sample preparation protocol including defatting, protein denaturation, and carbamidomethylation
was optimized in order to achieve complete protein digestion and to avoid SeCys losses. Quantification was carried out by
reversed-phase HPLC–inductively coupled plasma mass spectrometry (ICP MS) after quantitative isolation of the selenium-containing
fraction by size-exclusion liquid chromatography. The detection limits were 0.06, 0.003, and 0.01 μg g−1 (dry weight) for SeCys, Se(IV) and SeMet, respectively, and the precision was 5–10%. The end products of carbamidomethylation
of the different selenium species were identified for the first time by electrospray QTOF MS after custom-designed 2D HPLC
purification. Differences in selenium speciation in egg yolk and white were highlighted, the yolk containing more SeCys and
the white more SeMet. An insight into selenium bioaccessibility in eggs was obtained by digestion with simulated gastric and
gastrointestinal juices and size-exclusion HPLC-ICP MS. 相似文献
5.
Rodushkin I Engström E Stenberg A Baxter DC 《Analytical and bioanalytical chemistry》2004,380(2):247-257
A procedure is described for the determination of Y, Zr, Nb, Ru, Rh, Pd, Ag, Sb, Te, Hf, Ta, W, Re, Os, Ir, Pt, Au, Tl, Bi, and U in human urine and serum at concentrations relevant to the occupationally unexposed population. Sample preparation was limited to tenfold dilution with 2% HCl. A combination of a sample-introduction system designed to provide enhanced sensitivity and the use of water and acids of high-purity has resulted in limits of quantification (LOQ) in the sub-nanogram per liter range for 13 analytes. Instrumental background caused by release of analytes (Y, Zr, Ag, Sb, Au, Tl, Bi, U) from different parts of the sample-introduction system was found to be the major limitation in obtaining even better LOQ. Nevertheless, detection capabilities of the proposed procedure were adequate for all elements except Ru, Pd, and Rh. Despite of the use of high-resolution mode for these analytes some unresolved spectral interferences might still be present. For 13 elements an external accuracy assessment was accomplished by participation in proficiency testing and inter-comparison programs. Results obtained for pooled urine and serum were compared with concentrations reported for occupationally unexposed populations in recent publications. 相似文献
6.
James Sommers Marcos Jimenez Mary Adamic Jeffrey Giglio Kevin Carney 《Journal of Radioanalytical and Nuclear Chemistry》2009,282(3):929-932
Two Americium–Beryllium neutron sources were dismantled, sampled (sub-sampled) and analyzed via inductively coupled plasma
mass spectrometry (ICP-MS). Characteristics such as “age” since purification, actinide content, trace metal content and inter
and intra source composition were determined. The “age” since purification of the two sources was determined to be 25.0 and
25.4 years, respectively. The systematic uncertainties in the “age” determination were ±4% 2σ. The amount and isotopic composition
of U and Pu varied substantially between the sub-samples of Source 2 (n = 8). This may be due to the physical means of sub-sampling or the way the source was manufactured. Source 1 was much more
consistent in terms of content and isotopic composition (n = 3 sub-samples). The Be–Am ratio varied greatly between the two sources. Source 1 had an Am–Be ratio of 6.3 ± 52% (1σ).
Source 2 had an Am–Be ratio of 9.81 ± 3.5% (1σ). In addition, the trace element content between the samples varied greatly.
Significant differences were determined between Sources 1 and 2 for Sc, Sr, Y, Zr, Mo, Ba and W. 相似文献
7.
Schaumlöffel D Prange A Marx G Heumann KG Brätter P 《Analytical and bioanalytical chemistry》2002,372(1):155-163
In a new approach to the characterization and quantification of metallothionein isoforms an on-line isotope-dilution method in combination with the coupling of capillary electrophoresis (CE) to an inductively coupled plasma-sector field mass spectrometer (ICP-SFMS) is reported. Metallothionein (MT) isoforms are separated by CE and the elements Cu, Zn, Cd, and S are detected simultaneously by use of ICP-SFMS in the medium resolution mode. On-line isotope dilution is performed by continuous introduction of an isotopically enriched, species-unspecific spike solution after the separation step. MT from rabbit liver and a further purified MT-1 isoform were quantified by determination of sulfur, and the stoichiometric compositions of the metalloprotein complexes are characterized by determination of their sulfur-to-metal ratios. 相似文献
8.
The application of inductively coupled plasma – time-of-flight mass spectrometry for the speciation analysis of organolead compounds in environmental waters is described. Construction of the transfer line was achieved by means of a relatively simple and rapid coupling procedure. Derivatization of the ionic lead species was achieved by in-situ propylation with sodium tetrapropylborate; simultaneous extraction of the derivatized compounds in hexane was followed by separation and detection by capillary gas chromatography hyphenated to inductively coupled plasma–time-of-flight mass spectrometry. Detection limits for the different organolead species ranged from 10 to 15 fg (as Pb), corresponding to procedural detection limits between 50 and 75 ng L–1, on the basis of a 50 mL snow sample, extraction with 200 μL hexane, and subsequent injection of 1 μL of the organic extract on to the column. The accuracy of the system was confirmed by additional analysis of the water samples by capillary gas chromatography coupled with microwave-induced plasma–atomic-emission spectrometry and the analysis of a standard reference material CRM 605 (road dust) with a certified content of trimethyllead. 相似文献
9.
Cmelík J Machát J Niedobová E Otruba V Kanický V 《Analytical and bioanalytical chemistry》2005,383(3):483-488
Sulfur dioxide (SO2) is used as a preservative and stabilizer in wine production to prevent undesired biochemical processes in the must and the
final product. The concentration of SO2 is restricted by national regulations. There are two main forms of SO2 in wine—free (inorganic forms) and bound (fixed to organic compounds, e.g. aldehydes). Iodometric titration is commonly employed
for determination of SO2 concentration (either by direct titration or after pre-separation by distillation); other techniques are also used. In this
work inductively coupled plasma–optical-emission spectrometry with vapour generation was used for determination of free and
total SO2 in wine. Gaseous SO2 is released from the sample by addition of acid and swept into the ICP by an argon stream. The intensity of the sulfur atomic
emission lines is measured in the vacuum UV region. Determination of total SO2 is performed after hydrolysis of bound forms with sodium hydroxide (NaOH). Concentrations of acid for vapour generation and
NaOH for hydrolysis were optimised. The method was used for determination of free and total SO2 in red and white wine samples and results were compared with those from iodometric titration. 相似文献
10.
Conventional figures of merit such as limits of detection, signal to background ratio or repeatability, are used to determine the performance of pneumatic and ultrasonic sample introduction systems in an ultra-clean environment with an axially viewed inductively coupled plasma-atomic emission spectrometry and multichannel detection. We observed that the ultrasonic nebuliser offered a large improvement of signal intensity (10-133 greater) compared to a cyclone chamber coupled with a pneumatic Meinhard nebuliser. This improvement is associated with an average increase of signal to background ratio by a factor 86 and an average decrease of detection limits by a factor 6. The improvement factors generally depend on the element and for the same element on spectral lines. Typically, the observed values of detection limits in this work are lower than those published and obtained in non-ultra-clean conditions. The results emphasize that the environmental conditions of cleaning and analysis are essential to avoid and control cross contamination of the samples and hence to obtain low detection limits. 相似文献
11.
《Trends in analytical chemistry : TRAC》1986,5(5):110-114
The use of electrothermal vaporization for sample introduction to the inductively coupled plasma for emission spectrometric determination of elements in complex samples is discussed. The advantages and disadvantages, analytical performance characteristics, and ease of operation as compared to conventional pneumatic nebulization and other sample introduction techniques, are described. 相似文献
12.
G. C. Turk L. L. Yu Marc L. Salit William F. Guthrie 《Analytical and bioanalytical chemistry》2001,370(2-3):259-263
Multielement analyses of environmental reference materials have been performed using existing certified reference materials (CRMs) as calibration standards for inductively coupled plasma–mass spectrometry. The analyses have been performed using a high-performance methodology that results in comparison measurement uncertainties that are significantly less than the uncertainties of the certified values of the calibration CRM. Consequently, the determined values have uncertainties that are very nearly equivalent to the uncertainties of the calibration CRM. Several uses of this calibration transfer are proposed, including, re-certification measurements of replacement CRMs, establishing traceability of one CRM to another, and demonstrating the equivalence of two CRMs. RM 8704, a river sediment, was analyzed using SRM 2704, Buffalo River Sediment, as the calibration standard. SRM 1632c, Trace Elements in Bituminous Coal, which is a replacement for SRM 1632b, was analyzed using SRM 1632b as the standard. SRM 1635, Trace Elements in Subbituminous Coal, was also analyzed using SRM 1632b as the standard. 相似文献
13.
A study was conducted to develop a microwave-enhanced extraction method for the determination of arsenic species in prenatal and children's dietary supplements prepared from plant materials. The method was optimized by evaluating the efficiency of various solutions previously used to extract arsenic from the types of plant materials used in the dietary supplement formulations. A multivitamin standard reference material (NIST SRM 3280) and a prenatal supplement sample were analyzed in the method optimization. The identified optimum conditions were 0.25 g of sample, 5 mL of 0.3 mol L−1 orthophosphoric acid (H3PO4) and microwave heating at 90 °C for 30 min. The extracted arsenic was speciated by cation exchange ion chromatography–inductively coupled plasma mass spectrometry (IC–ICP-MS). The method detection limit (MDL) for the arsenic species was in the range 2–8 ng g−1. Ten widely consumed prenatal and children's dietary supplements were analyzed using the optimized protocol. The supplements were found to have total arsenic in the concentration range 59–531 ng g−1. The extraction procedure recovered 61–92% of the arsenic from the supplements. All the supplementary products were found to contain arsenite (As3+) and dimethylarsinic acid (DMA). Arsenate (As5+) was found in two of the supplements, and an unknown specie of arsenic was detected in one product. The results of the analysis were validated using mass balance by comparing the sum of the extracted and non-extracted arsenic with the total concentration of the element in the corresponding samples. 相似文献
14.
Four different organic solvents: dimethylformamide, 1,4-dioxane, n-propanol and ethanol were evaluated as alternative organic modifiers to acetonitrile for liquid chromatography (LC) separations. The aim was to establish common sets of chromatographic conditions that could be applied for LC hyphenation to inductively coupled plasma mass spectrometry (ICPMS) as well as to electrospray ionization MS (ESIMS). The approach was to evaluate candidate solvents that, compared to acetonitrile, potentially could give improved analytical performance (low solvent vapor loading, maximized analyte sensitivity and minimized carbon depositions on instrumental parts) in ICPMS analysis while retaining chromatographic and ESIMS performances. The study showed that dimethylformamide, 1,4-dioxane, n-propanol and ethanol all can be advantageous chromatographic modifiers for LC–ICPMS analysis, giving superior performance compared to acetonitrile. For the combined use of LC–ICPMS and LC–ESIMS with a common set of chromatographic conditions, n-propanol gave the best overall performance. The 195Pt+ signal in ICPMS was continuously monitored during a 0–60% organic solvent gradient and at 25% of organic modifier, 100% of the signal obtained at the gradient start was preserved for n-propanol compared to only 35% of the signal when using acetonitrile. Platinum detection limits were 5–8 times lower using n-propanol compared with acetonitrile. Signal-to-noise ratio in continuous ESIMS signal measurements was 100, 90 and 110 for a 100 μg/ml solution of leucine–enkephaline using acetonitrile, ethanol and n-propanol, respectively. Chromatographic efficiency in reversed phase separations was preserved for n-propanol compared to acetonitrile for the analysis of the whole protein cytochrome C and the peptide bacitracin on a column with particle and pore sizes of 5 μm and 300 Å, but slightly deteriorated for the separation of the peptides leucine–enkephaline and bacitracin on a 3 μm and 90 Å column as the peak width at half height for both peptides increased by a factor of two. The performance on the smaller dimensioned column could however be improved by running the separations at 40 °C. 相似文献
15.
CMSX-4 is the second-generation nickel-based single crystal superalloy used widely in the world. The oxidation resistance and corrosion resistance of CMSX-4 alloy can be improved by adding trace lanthanum (La), cerium (Ce) and other rare earth elements. A method for the simultaneous determination of La and Ce in CMSX-4 nickel-based superalloy by wet dissolution-inductively coupled plasma mass spectrometry was established. The sample was heated and dissolved under normal pressure by aqua regia and hydrofluoric acid, and the interference of fluorine ion was eliminated by using perchloric acid. The amount of dissolved acid and the digestion conditions were optimized. The limits of detection were 0.23 μg/g for La and 0.85 μg/g for Ce under optimized conditions. The spiked recoveries were 95.0%–98.9% with the relative standard deviations of 1.3%–3.9%, which can meet the requirements of accurate and rapid determination of La and Ce in CMSX-4 nickel-based superalloy. © 2023, Youke Publishing Co.,Ltd. All rights reserved. 相似文献
16.
Determination of elemental fingerprint profile of 40 commercial beer samples was performed using inductively coupled plasma–mass
spectrometry combined with principal component analysis and receiver operating characteristic (ROC) analysis. Fourteen trace
elements, 51V, 52Cr, 59Co, 60Ni, 75As, 82Se, 95Mo, 111Cd, 115In, 121Sb, 133Cs, 208Pb, 209Bi, and 238U, were monitored. All 40 beer samples are distinguishable by using the proposed method. ROC analysis showed that individual
beer samples can be correctly identified via the magnitude of its correlation coefficient with respect to the other beers
with low false positive rate. The obtained results suggested that the elemental fingerprint technique is feasible for sample
differentiation and comparison. 相似文献
17.
Different sample treatment procedures were combined with inductively coupled plasma mass spectrometry (ICP-MS) and negative thermal ionisation mass spectrometry (NTI-MS) for the determination of ruthenium traces in photographic emulsions. Dissolution of the samples in concentrated ammonia solution was used in connection with ICP-MS by external calibration, which has the advantage of a simple sample preparation technique but introduces high amounts of the silver matrix into the mass spectrometer. On the other hand, isotope dilution mass spectrometry (IDMS) with an enriched 99Ru spike solution was applied for ICP-MS and NTI-MS measurements, respectively, in connection with a significant reduction of the matrix by AgCl precipitation. In these cases loss of ruthenium by the AgCl precipitate has no effect on the analytical result. The results of the different methods agreed usually well analysing ruthenium traces in the range of 0.1–10 μg per gram emulsion. The detection limits obtained were 4 ng/g for ICP-IDMS, 20 ng/g for NTI-IDMS, and 15 ng/g for ICP-MS with external calibration. Differences in the results between the different methods could mainly be attributed to sample inhomogeneities. ICP-IDMS with silver matrix reduction by AgCl precipitation is recommended as a routine method, NTI-IDMS with the corresponding sample treatment as a calibration method. 相似文献
18.
Yu Min Park Ji Yeon Choi Eun Yeong Nho Cheong Mi Lee In Min Hwang Naeem Khan 《Analytical letters》2019,52(6):1018-1030
This study determined the concentration of eight macroelements (Na, K, Mg, P, S, Ca, Fe, Zn) and nineteen trace elements (Li, Be, Cr, Mn, Co, Ni, V, Cu, Ga, Se, Rb, Sr, In, Sn, Cs, Ba, Tl, Bi, U) in commonly consumed canned marine products from South Korea. The samples were wet-digested using nitric acid and hydrogen peroxide by a microwave system and analyzed for macroelements using inductively coupled plasma—optical emission spectrometry (ICP-OES) and for trace elements by inductively coupled plasma—mass spectrometry (ICP-MS). The analytical methods were validated by the correlation coefficients, limits of detection and quantification, correlation variance, spiking recovery tests, and analyzing a NIST 1566?b oyster tissue certified reference material. The concentrations of macro and trace elements varied among the canned marine products. The macroelements were present in the order of Na?>?K?>?P?>?S> Mg?>?Ca?>?Fe?>?Zn. In general, the concentrations of macro and trace elements were within the specified limits of Food and Nutrition Board, Joint Food and Agriculture Organization/World Health Organization Expert Committee on Food Additives, and Ministry of Food and Drug Safety, Korea. The results suggest that the analyzed canned marine products are safe in terms of the analyzed elements and their consumption therefore does not cause any threat to human health. 相似文献
19.
Gunda Koellensperger Stephan Hann Günter Prinz Gerhard Stingeder Michael Bujatti-Narbeshuber 《Analytical and bioanalytical chemistry》2001,370(5):559-565
Three different analytical strategies have been evaluated for the quantification of Ir in geological samples. Glassy rock samples from Köfels and reference material WGB-1 were analyzed directly by inductively coupled plasma sector field mass spectrometry (ICP–SFMS) at mass resolution 400 using membrane desolvation and at mass resolution 9500 without membrane desolvation. Matrix separation by anion-exchange pre-concentration was also investigated. The ultrasonic nebulizer USN6000AT+ (Cetac Technologies, Omaha, NE, USA) incorporating a membrane desolvation unit was used as the sample-introduction system. Sample preparation involved complete microwave-assisted acid digestion of the silicate matrix with HNO3–HCl–HF. The results obtained by the three methods of quantification were in good agreement, showing that oxide-type interferences were effectively eliminated solely by membrane desolvation. The limits of detection were 6 pg g–1 for low resolution measurement with use of the membrane, 15 pg g–1 at a mass resolution of 9500, and 59 pg g–1 for the ion-exchange procedure. The ultimate precision obtained for the Köfelsit Ir data was, however, compromised by the small sample intake (0.3 g), because of the inhomogeneous distribution of Ir in geological samples. 相似文献
20.
An inductively coupled plasma mass spectrometer (ICP-MS) with a rapid sample-preparative procedure was used for the determination of selenium in blood serum. Blood serum was prepared by dilution in an acidic solution consisting of nitric acid (1%), X-triton (0.1%) and 1-butanol (0.8%). A calibration curve was established for 1-40 microg mL(-1) (r(2)>0.99). The limit of detection was 0.5 microg mL(-1). Repeatability and intermediate precision were satisfactory with relative standard deviations (RSD) of 2.0% and 3.2%, respectively. This method was easily applied to reference materials with satisfactory accuracy. Good correlation (r(2)=0.96) was observed between ICP-MS and atomic absorption spectrometry (AAS) for the determination of (82)Se in blood serum from 23 patients. These results suggest that the sample preparative procedure coupled with ICP-MS can be used for the routine determination of (82)Se in human blood serum. 相似文献