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1.
High resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) was applied for multielement-determination in high-purity
copper (approx. 99.99%). The samples were introduced into the instrument by three different introduction systems, which were
studied with respect to high accuracy, low detection limits and fast analysis: continuous nebulization (CN), flow injection
analysis (FIA) and laser ablation (LA). The trueness of the applied method was checked by the analysis of high-purity copper
reference material (BCR Cu074). All values obtained for this CRM using CN were in the range of the stated uncertainty for
the 9 elements determined: Ag, As, Bi, Cr, Fe, Ni, Pb, Sb, and Sn with contents in the range of 0.5–13 μg/g. Another approach
for checking the trueness of the method was to compare the results obtained by this method characterizing the purity of a
4N (99.99% copper content) copper material with those obtained by application of electrothermal atomic absorption spectrometry
(ET-AAS) and inductively coupled plasma optical emission spectrometry (ICP-OES). For further characterizing, the concentrations
of 49 elements were found in this material below detection limits of HR-ICP-MS in the range of low μg/kg and sub μg/kg. The
combination of HR-ICP-MS and a flow injection analysis system (FIAS) improved the robustness of the system in regard to high
matrix concentrations. Therefore, matrix concentrations up to 4 g/L could be used for liquid analysis and detection limits
were lowered by a factor of 2–5. A calibration method for bulk analysis with laser ablation was developed with doped copper
powder as pressed pellets for calibration standards. This method proved to be an excellent fast semi-quantitative method,
which was less time consuming in comparison with the analysis of liquids. After application of correction factors the deviation
between the results obtained by laser ablation and by analysis of liquids was ≈ 15% for most elements. The method offered
the possibility to check for potential losses of analytes occurring during the wet chemical operations.
Received: 23 November 1998 / Revised: 25 February 1999 / Accepted: 2 March 1999 相似文献
2.
Laser-ablation inductively coupled plasma mass spectrometry (LA–ICP–MS) has been established as a very efficient and sensitive
technique for the direct analysis of solids. In this work the capability of LA–ICP–MS was investigated for determination of
trace elements in high-purity graphite. Synthetic laboratory standards with a graphite matrix were prepared for the purpose
of quantifying the analytical results. Doped trace elements, concentration 0.5 μg g–1, in a laboratory standard were determined with an accuracy of 1% to ± 7% and a relative standard deviation (RSD) of 2–13%.
Solution-based calibration was also used for quantitative analysis of high-purity graphite. It was found that such calibration
led to analytical results for trace-element determination in graphite with accuracy similar to that obtained by use of synthetic
laboratory standards for quantification of analytical results. Results from quantitative determination of trace impurities
in a real reactor-graphite sample, using both quantification approaches, were in good agreement. Detection limits for all
elements of interest were determined in the low ng g–1 concentration range. Improvement of detection limits by a factor of 10 was achieved for analyses of high-purity graphite
with LA–ICP–MS under wet plasma conditions, because the lower background signal and increased element sensitivity.
Received: 4 January 2001 / Revised: 27 March 2001 / Accepted: 28 March 2001 相似文献
3.
Trace amounts of gold and silver in high-purity iron or steel were preconcentrated by reductive coprecipitation with palladium
using ascorbic acid, and determined by electrothermal atomic absorption spectrometry (ET-AAS). Both gold and silver could
be simultaneously separated and sensitively determined in 10 metals (aluminum, cobalt, chromium, copper, iron, manganese,
molybdenum, nickel, vanadium and zinc). Comparable values were obtained for gold and silver in reference materials (low alloy
steel) by the proposed method and a non-separation method; good agreement was found between the analytical values by both
methods and the certified values. The proposed method is easy, simple and not dependent on sample composition and content.
Moreover, gold and silver in metal samples could be simultaneously separated together with selenium and tellurium. The detection
limits for gold and silver (3 σ) are 0.003 μg g–1 and 0.002 μg g–1, respectively.
Received: 3 February 2000 / Revised: 11 April 2000 / Accepted: 16 April 2000 相似文献
4.
Trace amounts of gold and silver in high-purity iron or steel were preconcentrated by reductive coprecipitation with palladium
using ascorbic acid, and determined by electrothermal atomic absorption spectrometry (ET-AAS). Both gold and silver could
be simultaneously separated and sensitively determined in 10 metals (aluminum, cobalt, chromium, copper, iron, manganese,
molybdenum, nickel, vanadium and zinc). Comparable values were obtained for gold and silver in reference materials (low alloy
steel) by the proposed method and a non-separation method; good agreement was found between the analytical values by both
methods and the certified values. The proposed method is easy, simple and not dependent on sample composition and content.
Moreover, gold and silver in metal samples could be simultaneously separated together with selenium and tellurium. The detection
limits for gold and silver (3 σ) are 0.003 μg g–1 and 0.002 μg g–1, respectively.
Received: 3 February 2000 / Revised: 11 April 2000 / Accepted: 16 April 2000 相似文献
5.
C. Pickhardt I. B. Brenner J. S. Becker H.-J. Dietze 《Analytical and bioanalytical chemistry》2000,368(1):79-87
Laser ablation inductively coupled plasma mass spectrometry using a quadrupole-based mass spectrometer (LA-ICP-QMS) was applied
for the analysis of powdered zeolites (microporous aluminosilicates) used for clean-up procedures. For the quantitative determination
of trace element concentrations three geological reference materials, granite NIM-G, lujavrite NIM-L and syenite NIM-S, from
the National Institute for Metallurgy (South Africa) with a matrix composition corresponding to the zeolites were employed.
Both the zeolites and reference materials were fused with a lithium borate mixture to increase the homogeneity and to eliminate
mineralogical effects. In order to compare two different approaches for the quantification of analytical results in LA-ICP-MS
relative sensitivity coefficients (RSCs) of chemical elements and calibration curves were measured using the geostandards.
The experimentally obtained RSCs are in the range of 0.2-6 for all elements of interest. Calibration curves for trace elements
were measured without and with Li or Ti as internal standard element. With a few exceptions the regression coefficients of
the calibration curves are better than 0.993 with internal standardization. NIM-G granite reference material was employed
to evaluate the accuracy of the technique. Therefore, the measured concentrations were corrected with RSCs which were determined
using lujavrite reference material NIM-L. This quantification method provided analytical results with deviations of 1–11%
from the recommended and proposed values in granite reference material NIM-G, except for Co, Cs, La and Tb. The relative standard
deviation (RSD) of the determination of the trace element concentration (n = 5) is about 1% to 6% using Ti as internal standard
element. Detection limits of LA-ICP-QMS in the lower μg/g range (from 0.03 μg/g for Lu, Ta and Th to 7.3 μg/g for Cu, with
the exception of La) have been achieved for all elements of interest. Under the laser ablation conditions employed (λ: 266
nm, repetition frequency: 10 Hz, pulse energy: 10 mJ, laser power density: 6 × 109 W/cm2) fractionation effects of the determined elements relative to the internal standard element Ti were not observed.
Received: 7 April 2000 / Revised: 25 May 2000 / Accepted: 31 May 2000 相似文献
6.
Slurry sampling followed by electrothermal vaporization was used as sample introduction technique for digestion-free analysis
of aluminium nitride and aluminium oxide by inductively coupled plasma atomic emission spectrometry. The vaporizer consisted
of a tungsten coil in a quartz chamber. Spectral interferences and background emission caused by tungsten ablation from the
coil were reduced by coating it with tungsten carbide. Different approaches for background correction techniques were considered.
The analytes Ca, Cd, Co, Cr, Cu, Fe, Mg, Ni and Zn were determined simultaneously, whereas Mn and Na were determined in the
sequential mode. Calibration was performed using the standard additions method. The accuracy was checked by comparison of
the results with those of independent methods. Detection limits between 0.01 (Mg) and 8.5 μg/g (Co) were achieved.
Received: 21 September 1998 / Revised: 30 October 1998 / Accepted: 3 November 1998 相似文献
7.
Davide Bleiner Kathrin Hametner D. Günther 《Analytical and bioanalytical chemistry》2000,368(1):37-44
Simultaneous ion sampling and sequential detection offered by inductively coupled plasma ‘time of flight’ mass spectrometry (ICP-TOFMS) provides advantages for the analysis of short transient concentration-variable signals as produced in laser ablation. In
order to investigate the capabilities of ICP-TOFMS in combination with an excimer laser ablation system, ablation studies
on reference materials and geological samples were carried out. Various ICP-TOFMS parameters were optimized for laser-induced
aerosols. Transverse rejection ion pulse was used to extend the dynamic range in concentration. A reduced volume ablation
cell was designed and used in order to increase the sample density in the ICP. Results for 63 simultaneously measured isotopes
(SRM 610 from NIST) lead to limits of detection in the 1–100 μg/g range for a 80 μm crater diameter (10 Hz, 1.2 mJ pulse energy).
The reproducibility of signal ratios was determined to be better than 2% RSD for transient signals using 102 ms integration
time. These optimized parameters were then used for the analysis of tin-rich fluid inclusions. Preliminary results of multielement
analysis and isotopic ratio determinations on individual fluid inclusions (63 isotopes, 102 ms integration time) demonstrate
the capabilities of ICP-TOFMS in combination with laser ablation.
Received: 6 March 2000 / Revised: 11 May 2000 / Accepted: 14 May 2000 相似文献
8.
Two different mass spectrometric methods, negative thermal ionization isotope dilution mass spectrometry (NTI-IDMS) and inductively
coupled plasma mass spectrometry (ICP-MS), off-line and on-line coupled with anion exchange chromatography, have been developed
for simultaneous bromide and bromate determinations in water samples. The detection limits of these methods are in the range
of 0.03–0.09 μg/L using a 50 mL sample.The results are independent of the content of other anions, which could be demonstrated
by the analyses of six mineral waters containing chloride and sulfate of up to 160 mg/L and 1500 mg/L, respectively. Bromide
has been analyzed by the NTI-IDMS method in the range of 10–500 μg/L and bromate in the range of 1–50 μg/L with relative standard
deviations of 0.3–1.2% and 0.4–6%. Quantification for the ICP-MS method was carried out by the standard addition technique,
which resulted in relative standard deviations of 5.5% for bromide at the 500 μg/L level and of 13% for bromate at the level
of about 3 μg/L. These results are compared with those described in the literature for ion chromatographic (IC) and other
methods and those obtained in this work by IC using UV detection, which allows high concentrations of chloride in the bromate
fraction. The detection limits of this IC method are 6 μg/L for bromide and 30 μg/L for bromate. NTI-IDMS and ICP-MS therefore
fit the recommendations of the European Union (detection limit<2.5 μg/L; precision and accuracy better than 25% at the 10 μg/L
level) for methods analyzing the carcinogenic bromate much better than IC and other methods applied up to now. As a definitive
but time consuming method, NTI-IDMS is preferably applicable as a calibration technique, whereas ICP-MS, with relatively short
analysis times, due to on-line coupling with chromatography, can be used as a sensitive and powerful routine method for trace
bromide and bromate species in water samples.
Received: 5 July 1996/Accepted: 7 August 1996 相似文献
9.
Solid-phase extraction (SPE) method for preconcentration and determination of Cd(II), Pb(II), Co(II), Ni(II), and Cu(II) aqueous
samples by inductively coupled plasma optical emission spectrometry is described. The preconcentration of analytes is accomplished
by retention of their chelates with 1.10-phenanthroline in aqueous solution on a solid phase containing carboxylic acid (COOH)
bonded to silica gel in a column. The limits of detection values (defined as “3s” where “s” is standard deviation of the blank
determination) are 3.6 μg/L for Cd(II), 17.5 μg/L for Pb(II), 3.1 μg/L for Co(II), 2.1 μg/L for Ni(II), and 4.4 μg/L for Cu(II)
and corresponding limit of quantification (6s) values are 7.2, 35, 6.2, 4.2 and 8.8 μg/L, respectively. As a result, a simple
method was elaborated for the group concentration and determination of the above mentioned metals in reference material and
in samples of plant material.
The article is published in the original. 相似文献
10.
Beltrami D Calestani D Maffini M Suman M Melegari B Zappettini A Zanotti L Casellato U Careri M Mangia A 《Analytical and bioanalytical chemistry》2011,401(4):1401-1409
An integrated approach based on the use of inductively coupled plasma mass spectrometry (ICP-MS) and scanning electron microscopy
(SEM) for the qualitative and quantitative analyses of metal particles in foods was devised and validated. Different raw materials
and food products, like wheat, durum wheat, wheat flour, semolina, cookies, and pasta were considered. Attention was paid
to the development of sample treatment protocols for each type of sample to avoid potential artifacts such as aggregation
or agglomeration. The analytical protocols developed followed by ICP-MS and SEM investigations allowed us the quantitative
determination and the morphological and dimensional characterization of metal nano- and microparticles isolated from the raw
materials and finished food products considered. The ICP-MS method was validated in terms of linearity (0.8–80 μg/g and 0.09–9 μg/g
for Fe and Ti, respectively), quantification limits (0.73 μg/g for Fe and 0.09 μg/g for Ti), repeatability (relative standard
deviation (RSD) % equal to 10% for Fe and 20% in a wheat matrix as an example), and extraction recoveries (93 ± 2–101 ± 2%).
Validation of the scanning electron microscopy–energy dispersive X-ray spectroscopy (SEM-EDS) measurements was performed working
in a dimensional range from 1 to 100 μm with an estimated error in the size determination equal to 0.5 μm. ICP-MS data as
well as SEM measurements showed a decrease in the concentration of metal particles from wheat to flour and from durum wheat
to semolina samples, thus indicating an external contamination of grains by metal particles. These findings were confirmed
by environmental SEM analysis, which allowed investigation of particles of lower dimensions. Generally, the largest number
of particles was found in the case of iron and titanium, whereas particles of copper and zinc were only occasionally found
without any possibility of quantifying their number. 相似文献
11.
Two different mass spectrometric methods, negative thermal ionization isotope dilution mass spectrometry (NTI-IDMS) and inductively
coupled plasma mass spectrometry (ICP-MS), off-line and on-line coupled with anion exchange chromatography, have been developed
for simultaneous bromide and bromate determinations in water samples. The detection limits of these methods are in the range
of 0.03–0.09 μg/L using a 50 mL sample.The results are independent of the content of other anions, which could be demonstrated
by the analyses of six mineral waters containing chloride and sulfate of up to 160 mg/L and 1500 mg/L, respectively. Bromide
has been analyzed by the NTI-IDMS method in the range of 10–500 μg/L and bromate in the range of 1–50 μg/L with relative standard
deviations of 0.3–1.2% and 0.4–6%. Quantification for the ICP-MS method was carried out by the standard addition technique,
which resulted in relative standard deviations of 5.5% for bromide at the 500 μg/L level and of 13% for bromate at the level
of about 3 μg/L. These results are compared with those described in the literature for ion chromatographic (IC) and other
methods and those obtained in this work by IC using UV detection, which allows high concentrations of chloride in the bromate
fraction. The detection limits of this IC method are 6 μg/L for bromide and 30 μg/L for bromate. NTI-IDMS and ICP-MS therefore
fit the recommendations of the European Union (detection limit<2.5 μg/L; precision and accuracy better than 25% at the 10 μg/L
level) for methods analyzing the carcinogenic bromate much better than IC and other methods applied up to now. As a definitive
but time consuming method, NTI-IDMS is preferably applicable as a calibration technique, whereas ICP-MS, with relatively short
analysis times, due to on-line coupling with chromatography, can be used as a sensitive and powerful routine method for trace
bromide and bromate species in water samples.
Received: 5 July 1996/Accepted: 7 August 1996 相似文献
12.
S. T. Girousi G. C. Kaspentakis A. N. Voulgaropoulos J. A. Stratis 《Mikrochimica acta》2001,136(3-4):223-226
Adsorptive voltammetry was employed for the determination of copper and molybdenum in manganese compounds. As working electrode
the hanging mercury drop electrode (HMDE) was used. The method was applied in aqueous solutions of MnCl2 and Mn(NO3)2, as well as in pre-treated manganese dioxide and manganese ores. The detection limits are 3 μg/g for copper and 5 μg/g for
molybdenum in the sample. The RSDs at concentration level of 8 μg/g are 2.2 and 3.2% for copper and molybdenum, respectively. 相似文献
13.
J. W. Mitchell 《Journal of Radioanalytical and Nuclear Chemistry》1982,69(1-2):47-105
The detection limits of many nonnuclear methods for ultratrace (≤0.1 μg/g) elemental determinations lie well below the level
at which precise and accurate practical analysis can be executed routinely. Advances in analytical methodologies which are
rapidly eroding such disparities are reviewed. The applications of X-ray fluorescence, atomic absorption, stable isotope dilution
mass spectrometry, and laser intracavity absorption spectrophotometry to ultratrace analyses not amenable to solution by nuclear
methods are discussed. 相似文献
14.
Yong-Jae Kim Chang-Kyu Kim Cheol-Su Kim Ju-Yong Yun Byung-Hwan Rho 《Journal of Radioanalytical and Nuclear Chemistry》1999,240(2):613-618
A time-saving and accurate technique for determining226Ra in groundwater and soil was examined, using high-resolution inductively coupled plasma-mass spectrometry (HR-ICP-MS). The
technique was applied to the determination of226Ra in groundwater and soil samples and compared with the conventional liquid scintillation counting method. This technique
was capable of completing226Ra counting within 3 minutes, without the in-growth period to allow radon and its progeny to achieve secular equilibrium with
the parent226Ra. The detection limits of HR-ICP-MS for226Ra in groundwater and soil were 0.19 mBq·1−1 and 0.75 Bq·kg−1, respectively, which were about 10 times lower than that of the liquid scintillation counter. The results obtained from HR-ICP-MS
in groundwater and soil were in accordance with those of LSC within a relative error of about 13%. 相似文献
15.
M. ?deg?rd S. H. Dundas B. Flem A. Grimstvedt 《Fresenius' Journal of Analytical Chemistry》1998,362(5):477-482
Results of the use of a double-focusing, magnetic sector inductively coupled plasma mass spectrometer (ICP-MS) with ultraviolet
(UV) laser ablation (LA) are presented for the bulk analysis of rare earth elements (REEs) in rocks fused with Li2B4O7. The sample preparation procedure used a sample to flux weight ratio of 1 : 7, and was identical with a procedure routinely
used for X-ray fluorescence (XRF) analyses of major and minor elements in geological materials. Calibration was based on a
total of 18 international standard reference materials (SRMs), and Ba was used as an internal standard element for all REEs.
The calibration curves were constructed using a weighted regression model. The use of internal standard, without exception,
improved the correlation coefficients significantly. The 3σ detection limits were established by a blank sample of SiO2 spiked with Ba, and were in the range from 0.003 μg g–1 (159Tb) to 0.051 μg g–1 (140Ce). The use of a large set of SRMs for calibration gave a good basis for the evaluation of analytical quality, and extensive
data for calculated analytical uncertainty are presented. Instrumental precision and the repeatability of the method were
studied separately, and no significant difference in these two sets of parameters were found, indicating that the spread of
results predominantly was connected to the instrumental measurements. Repeated ablations on the surface of a disk did not
influence subsequent measurements with XRF, showing that the fused disks can be stored for future use in XRF and/or LA-ICP-MS
analysis.
Received: 12 February 1998 / Revised: 6 April 1998 / Accepted: 17 April 1998 相似文献
16.
Elemental mapping and quantitative analysis of Cu, Zn, and Fe in rat brain sections by laser ablation ICP-MS 总被引:1,自引:0,他引:1
This report details the application of laser ablation quadrupole ICP-MS for the (multi)elemental mapping of 100-μm-thick sections
of rat brain. The laser spot size used was 60 μm, and the laser scan speed was 120 μm s−1. The analysis was relatively rapid, allowing mapping of a whole brain thin section (≈1 cm2) in about 2 h. Furthermore, the method was amenable to multi-element data collection including the physiologically important
elements P and S and afforded sub μg g−1 detection limits for the important trace elements Cu and Zn. Calibrations were performed with pressed pellets of biological
certified reference materials, and the elemental distributions and concentrations of Cu, Zn, and Fe were determined in whole
rat brain sections. The distributions and concentration ranges for these elements were consistent with previous studies and
demonstrate the utility of this technique for rapid mapping of brain thin sections. 相似文献
17.
Bechstein K Michels J Vogt J Schwartze GC Vogt C 《Analytical and bioanalytical chemistry》2011,399(1):501-508
Previous studies have revealed silica formation in the teeth of mandibular gnathobases of copepods while significant amounts
of zinc and copper are present, which might improve mechanical stability of the teeth and represent an adaptation to compact
food particles. The present study aimed at analysing the distribution and concentration of trace elements in the mandibular
gnathobases of females of the Antarctic copepod species Calanoides acutus. Because of the low overall masses of few micrograms per specimen the application of a combination of position-resolved micro-beam
techniques was necessary and micro-particle-induced X-ray emission spectrometry and laser ablation inductively coupled plasma
mass spectrometry were used to determine Ba, Br, Ca, Cl, Cu, Fe, K, Mg, Na, Ni, P, S, Si and Zn in the samples with μm to
sub-μm resolution. Calibration strategies were optimised to fit for the carbonate matrix. The analyses revealed a distinct
enrichment of Br, Ca, Fe, K, S, Si and Zn in the teeth of the gnathobases. 相似文献
18.
K. Janssens L. Vincze B. Vekemans C. T. Williams M. Radtke M. Haller A. Kn?chel 《Fresenius' Journal of Analytical Chemistry》1999,363(4):413-420
The sensitivity and applicability of the synchrotron radiation induced X-ray microfluorescence (μ-SRXRF) spectrometer at
the Hamburg synchrotron laboratory Hasylab for the determination of the distribution of trace concentrations of rare-earth
elements (REE) in fossilized bone are discussed and critically compared to those of other trace analytical methods such as
instrumental neutron activation analysis (INAA) and LAMP-ICPMS (laser ablation microprobe inductively-coupled plasma mass
spectrometry). Measurements were carried out on two bone samples from contrasting terrestrial depositional environments at
Olduvai Gorge (Tanzania). Results indicate that the microdistribution of the REE in these biological materials is not homogeneous
and that the relative abundance of these elements can provide information on the palaeoenvironment during the fossilization
process. The heterogeneous distribution of the REE can be determined in a quantitative and completely non-destructive manner
provided the concentrations of individual REE are above 10 μg/g.
Received: 18 January 1998 / Revised: 6 October 1998 / Accepted: 10 October 1998 相似文献
19.
Determination of trace elements in residual oil by high-resolution inductively coupled plasma mass spectrometry 总被引:2,自引:0,他引:2
Hualin Xie Kelong Huang Jinchun Liu Xidu Nie Liang Fu 《Analytical and bioanalytical chemistry》2009,393(8):2075-2080
An analytical method using high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous
determination of 20 elements, including Na, Mg, Al, Ca, Ti, V, Mn, Fe, Co, Ni, Cu, Zn, Ga, As, Mo, Cd, Sn, Sb, Ba, and Pb
elements, in residual oil was described. The sample was dissolved in HNO3 by microwave digestion, and then the above 20 elements in the solution were analyzed directly by HR-ICP-MS. Most of the spectral
interferences could be avoided by measuring in the high-resolution mode. The matrix effect caused by the sample-digesting
solution and corrected by Sc, Rh, and Bi as the internal standard elements was studied in detail. The optimum condition of
the determination was also tested and discussed. The result showed that the detection limits of the method were in the range
of 0.014 to 11.6 μg L−1; the relative standard deviation was less than 3.8% and recoveries in the samples were in the range of 88.4% to 108.0%. This
method can be used to determine the trace elements in residual oil with the features of accurate, rapid, and convenient determination. 相似文献
20.
An on-line solid phase extraction method, linked to inductively coupled plasma optical emission spectrometry (ICP-OES), has been examined using octadecyl-bonded silica cartridge for determination of low levels of uranium and thorium in aqueous
samples. 2,3-dihydro-9,10-dihydroxy-1,4-anthracenedion forms a hydrophobic complex with cations and the resulted complex was
retained on SPE. The retained complex was eluted using an acidic solution and introduced into ICP for determination. Various
effective parameters and chemical variables such as sample pH, amount of ligand (as a complexing agent), sampling and eluting
flow rates and concentration of the eluent were optimized. Under optimal conditions, calibration curves with dynamic linear
ranges of 1–200 μg/L (r
2 = 0.9999) and 1–500 μg/L (r
2 = 0.9994) for U and Th were obtained, respectively. Detection limits based on three times of standard deviations of blank
by 6 replicates were 0.69 μg/L and 0.84 μg/L for U and Th, respectively. Sample throughput was 10 samples/h. The interference
effects of several metal ions on percentage of recovery of U and Th were also studied. The method was applied to the recovery
and sequential determination of these actinide elements in different water samples. 相似文献