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1.
P. Quevauviller M. Lachica E. Barahona A. Gomez G. Rauret A. Ure H. Muntau 《Fresenius' Journal of Analytical Chemistry》1998,360(5):505-511
Single extraction tests are commonly used to study the eco-toxicity and mobility of metals in soils, e.g. to assess the bioavailable
metal fraction (and thus to estimate the related phyto-toxic and nutritional deficiency effects) and the environmentally accessible
trace metals upon disposal of e.g. sediment on to a soil (e.g. contamination of ground waters). However, the lack of uniformity
in the different procedures does not allow the results to be compared worldwide nor the procedures to be validated. This paper
describes the interlaboratory testing of EDTA- and DTPA-extraction procedures for soil analysis, followed by the preparation
of a calcareous soil reference material (CRM 600), the homogeneity and stability studies and the analytical work performed
for the certification of the EDTA- and DTPA- extractable contents of some trace metals (following the standardized extraction
procedures).
Received: 21 May 1997 / Revised: 4 July 1997 / Accepted: 9 July 1997 相似文献
2.
P. Quevauviller G. Rauret R. Rubio J.-F. López-Sánchez A. Ure J. Bacon H. Muntau 《Analytical and bioanalytical chemistry》1997,357(6):611-618
The ecotoxicity and mobility of trace elements in soils are often evaluated through analytical results resulting from operationally-defined
determinations (single and sequential extractions), e.g. based on EDTA, acetic acid etc. extractions. The significance and
comparability of these results is highly dependent on the procedures used (standardized protocols or standards adopted by
international bodies) and their quality control relies on the availability of reference materials certified following these
strictly applied procedures. Recognizing the need to harmonize some of the extraction schemes currently used for soil analysis,
the Measurements and Testing Programme (formerly BCR) has organized a series of interlaboratory studies, the first aim of
which was to evaluate EDTA- and acetic acid-extraction procedures and the second objective was to certify reference materials
for their extractable trace element contents. Two sewage amended soils have been prepared for this purpose, originating respectively
from Scotland and Catalonia. This paper describes the preparation, homogeneity and stability studies, and gives an overview
of the certification campaign.
Received: 6 May 1996/Revised: 14 June 1996/Accepted: 27 June 1996 相似文献
3.
Ph. Quevauviller G. Rauret B. Griepink 《International journal of environmental analytical chemistry》2013,93(1-4):231-235
Abstract The determination of extractable trace metal contents in soils and sediments is currently performed in many laboratories to assess the bioavailable metal fraction (and related potential phyto-toxic effects) and the importance and possibility of mobilization of trace metals from polluted soil, sludge and sediment upon landfill application. Single and sequential extraction schemes are used for the assessment of the different “forms” of trace metals (e.g. “mobile/bioavailable”, “carbonate-bound” etc.). The lack of uniformity in the different extraction procedures used throughout the world does not allow the results to be compared or the procedures to be validated which has led to many criticisms in the past few years. Moreover, the lack of suitable reference materials for this type of operationally defined determinations did not enable the quality of the measurements to be controlled. Owing to the need for establishing common schemes for single and sequential extractions as well as for the improvement of the quality of extractable trace metal determinations in soil and sediments, the Community Bureau of Reference (BCR) has organised a project which results along with the state of the art of extractable trace metal determinations, use and applicability of extraction schemes and analytical limitations were decided to be thoroughly discussed in a workshop. This paper presents its main conclusions. 相似文献
4.
Evaluation of a sequential extraction procedure for the determination of extractable trace metal contents in sediments 总被引:11,自引:0,他引:11
P. Quevauviller G. Rauret H. Muntau A. M. Ure R. Rubio J. F. López-Sánchez H. D. Fiedler B. Griepink 《Fresenius' Journal of Analytical Chemistry》1994,349(12):808-814
The determination of extractable trace metals in sediments using sequential extraction procedures has been performed in many laboratories within the last ten years in order to study environmental pathways (e.g. mobility of metals, bounding states). However, the results obtained by different laboratories could hardly be compared due to lack of harmonized schemes. Owing to the need for standardization and subsequent validation of extraction schemes for sediment analysis, the Measurements and Testing Programme (formerly BCR Programme) of the European Commission has organized a project to adopt a sequential extraction procedure that could be used as a mean of comparison of data of extractable trace metals in sediments. A scheme was designed after a series of investigations on existing schemes and tested in interlaboratory studies. This paper presents the results of two round-robin exercises on extractable trace metals using this sequential extraction protocol and describes the final version of the extraction procedure amended according to the most recent improvements. 相似文献
5.
Philippe Quevauviller Gemma Rauret Allan Ure Roser Rubio José-Fírmin López-Sánchez Haidé Fiedler Herbert Muntau 《Mikrochimica acta》1995,120(1-4):289-300
The determination of extractable trace metal contents in soil using single extraction procedures is currently performed in many laboratories to assess the bioavailable metal fraction (and related phytotoxic effects) and the accessability to the environment (e.g. contamination of ground waters). Owing to the need for validation of the extraction schemes used and of the analytical techniques, the EC Measurements and Testing Programme (formerly BCR) has organized a project for improving the quality of determination of extractable trace metal contents in soil, the first step being an interlaboratory study to adopt common extraction procedures and the second being a certification campaign to certify two soils for their extractable trace element contents following these procedures. This paper gives a brief overview of the project organisation and describes the preparation, homogeneity and stability studies of two soil candidate reference materials (sewage sludge-amended and terra rossa soils). 相似文献
6.
A review with 159 references is presented on the applications of adsorptive stripping voltammetry (AdSV) for determining
trace metal ions in different environmental samples (e.g. water, soil, plant, biological fluids). The analytical applications
of AdSV to biologically active organic compounds (e.g. pharmaceuticals, pesticides, biomolecules) are also discussed.
Received: 18 December 1995/Revised: 8 January 1997/Accepted: 12 January 1997 相似文献
7.
A review with 159 references is presented on the applications of adsorptive stripping voltammetry (AdSV) for determining
trace metal ions in different environmental samples (e.g. water, soil, plant, biological fluids). The analytical applications
of AdSV to biologically active organic compounds (e.g. pharmaceuticals, pesticides, biomolecules) are also discussed.
Received: 18 December 1995/Revised: 8 January 1997/Accepted: 12 January 1997 相似文献
8.
Ph Quevauviller 《Trends in analytical chemistry : TRAC》1998,17(10):104
Single or sequential extraction procedures are often used for soil and sediment studies to determine forms or phases of elements (e.g. `bioavailable' forms of elements). The significance of the analytical results is highly dependent on the extraction procedures used, owing to the `operationally defined' character of these schemes which requires the adoption of standardized protocols. The first part of the present review discusses the aspects of standardization of leaching and extraction schemes as applied to environmental analysis. This second part focuses on the validation aspects of such procedures and describes the preparation and certification of soil and sediment reference materials certified for their extractable trace element contents, following standardized single and sequential extraction procedures. 相似文献
9.
Ph. Quevauviller 《Trends in analytical chemistry : TRAC》1998,17(10):632-642
Single or sequential extraction procedures are often used for soil and sediment studies to determine forms or phases of elements (e.g. ‘bioavailable' forms of elements). The significance of the analytical results is highly dependent on the extraction procedures used, owing to the ‘operationally defined' character of these schemes which requires the adoption of standardized protocols. The first part of the present review discusses the aspects of standardization of leaching and extraction schemes as applied to environmental analysis. This second part focuses on the validation aspects of such procedures and describes the preparation and certification of soil and sediment reference materials certified for their extractable trace element contents, following standardized single and sequential extraction procedures. 相似文献
10.
J. W. Einax O. Kampe D. Truckenbrodt 《Fresenius' Journal of Analytical Chemistry》1998,361(2):149-154
Partial least squares regression (PLS) as a method for multivariate data analysis has been applied to environmental data
of the German rivers Saale, Ilm and Unstrut. Main aspects of the study are to describe the relationships of the distribution
of metals between river water and river sediment using PLS. A simulation of the distribution of metals between the liquid
and solid phase by variation of some parameters (e.g. conductivity, DOC, dissolved oxygen, pH, phosphate and suspended matter)
is presented and compared with experimental results.
Received: 15 July 1997 / Revised: 6 November 1997 / Accepted: 7 November 1997 相似文献
11.
Comparison of three sequential extraction procedures used to study trace metal distribution in an acidic sandy soil 总被引:1,自引:0,他引:1
Parat C Lévêque J Dousset S Chaussod R Andreux F 《Analytical and bioanalytical chemistry》2003,376(2):243-247
On an acid sandy soil contaminated with trace metals (Fe, Mn, Cu, Pb and Zn), three sequential extraction procedures were compared to determine the efficiency of the reagents used and the effects of the step order on the fractionation of metal species. In all cases, a magnesium nitrate solution (MgNIT) was previously used to extract exchangeable forms. In the first procedure (I), the next extraction step was performed with sodium acetate buffer (NaOAc), as used on calcareous soils, to dissolve active calcium carbonate. Then trace metals bound to different forms of oxi-hydroxides (NH(2)OH, TAMOx and TAMAs fractions) were extracted before organic matter/sulfide oxidation with hydrogen peroxide at pH 2.0 in nitric acid medium (OMHyd). Finally, residual bound metals (RESID) in each procedure were extracted with a nitric-hydrofluoric-perchloric acid mixture. The second procedure (II) was the same as I, but without the NaOAc step, because of the absence of carbonate in the study soil. In procedure III, the NaOAc step was omitted and the oxidizable organic/sulfide fraction was extracted with sodium hypochlorite at pH 8.5 (OMOCl) before the reducible fractions. This study first showed that NaOAc may remove considerable amounts of metals (especially Mn and Zn) in other forms than exchangeable ones. Procedures II and III give similar results for Fe, Mn and Zn forms, which were mainly found in fractions of inorganic soil components, but not for Cu and Pb. Copper distribution was affected by the position of the oxidation step in the sequence. In procedure II, where the oxidation step (OMHyd) ended the sequence, Cu was mainly recovered in the TAMOx fraction. However, in procedure III, where the oxidation step (OMOCl) preceded the NH(2)OH, TAMOx and TAMAs steps, Cu was found in both OMOCl and TAMOx fractions. Lead distribution varied with oxidation reagent: it was partly removed in the OMHyd fraction of procedures I and II, and to a much lower extent in the OMOCl fraction of procedure III, probably due to the alkaline pH of the reagent in the latter case. 相似文献
12.
13.
A method based on solid phase extraction was developed for the determination of the herbicide triallate and its metabolite
2,3,3-trichloro-prop-2-en-sulfonic acid (TCPSA). Soil samples were extracted with methanol and diluted with water to yield
a methanol/water ratio of 1 : 4. Triallate was adsorbed on C18 cartridges while TCPSA was enriched on quaternary amine anion exchange resins. Cartridges were eluted with methanol/ethyl
acetate and methanol/sulfuric acid mixture, respectively. TCPSA methyl ester was formed using trimethyl orthoformate and subsequently
analyzed by GC/ECD. Determination limits of both target compounds were 5 μg/kg soil with recoveries of 100 ± 12% for triallate
and 57 ± 5% for TCPSA. In water analysis, determination limits were 0.05 μg/L with recoveries of 84 ± 14% for triallate and
100 ± 22% for TCPSA. In laboratory batch experiments, concentration of triallate decreased from 2690 to 1550 μg/kg soil within
59 days. 14 days after triallate application, TCPSA was determined to be 14 μg/kg which increased to 98 μg/kg soil at the
end of the incubation period. Soil/water distribution coefficients in loamy sand soil were 102 for triallate and 0.02 for
TCPSA which indicated a higher leaching tendency of the polar metabolite.
Received: 2 July 1997 / Revised: 15 September 1997 / Accepted: 25 September 1997 相似文献
14.
Determination of persistent organochlorine compounds in blood by solid phase micro extraction and GC-ECD 总被引:2,自引:0,他引:2
Lars R?hrig Michael Püttmann H.-U. Meisch 《Fresenius' Journal of Analytical Chemistry》1998,361(2):192-196
Biomonitoring of persistent organochlorine compounds in blood using the solid phase microextraction technique (SPME) and
gas chromatography with electron capture detection (GC-ECD) is described. Polar substances as tri-, tetra- and penta-chlorophenols
are analyzed simultaneously with less polar compounds such as hexachlorobenzene (HCB), α-, β-, and γ-hexachlorocyclohexane
(HCH), dichlorodiphenyltrichloroethane (DDT) and its derivatives and with some important congeners of the polychlorinated
biphenyls (PCB). No derivatization is needed for the determination of the phenolic compounds. The results show a good reproducibility
down to the lower μg/L-region. The method is very fast and of low cost compared to the classic extraction and determination
procedures.
Received: 7 July 1997 / Revised: 6 October 1997 / Accepted: 21 October 1997 相似文献
15.
Oan Muhammad Sahito Hassan Imran Afridi Jameel Ahmed Baig 《International journal of environmental analytical chemistry》2015,95(11):1066-1079
In the present study, three-step Community Bureau of Reference sequential extraction scheme (BCR-SES) and single extraction methods were performed to assess the mobility and availability of heavy metals (Cd, Cu, Pb, Fe and Zn) in an agricultural soil before and after amendment with poultry waste (PW).The PW samples were collected from poultry farms, situated in Hyderabad Sindh, Pakistan. The extractable heavy metals were measured by flame and electrothermal atomic absorption spectrometry. The validation of the method was carried out by analysis of a certified reference material of soil amended with sewage sludge (BCR-483). The single extractions using calcium chloride and EDTA, separately, while BCR-SESs were developed to evaluate the available heavy metals to plants and their environmental accessibility for control soil (CS), PW and soil amended with PW (SPW).The pH of the PW and SPW were found to be < 6.0, which may enhance the leaching of heavy metals to agricultural soil. The results from the partitioning study indicated that easily mobilised forms (acid exchangeable) of Cd were higher than other heavy metals. The oxidisable fractions of all heavy metals were dominant in PW and SPW as compared to found in CS samples. The EDTA- and CaCl2-extractable heavy metals correspond to 5.0 to 10 and 0.5 to 3.0%, respectively of total contents in all three solid samples. Contamination factors revealed that the retention of Pb and Zn were higher compared with Cu, Cd and Fe in CS, PW and SPW samples. 相似文献
16.
Optimized experimental procedures including time of extraction, extraction solvent in Soxhlet extraction technique were sought for detection of trace ethion residues in soil. The largest recoveries over 96% were achieved with a 1:1 mixture of methanol and acetone as extraction solvent for three hours. In comparing EI, CI, EI-CAD, and PCI-CAD modes of a four sector mass spectrometry for detection ethion, it was shown the best monitoring mode to be EI monitoring of the M+ of ethion, m/z 384, which fragments to give the m/z 231 product ion. The limit of detection obtained was 170 pg/g in soil. 相似文献
17.
A new method for the preconcentration and determination of trace amounts of lead at the μg/L level in natural waters has
been established based on the formation of the thenoyltrifluoroacetone (TTA) complex with dibenzo-18-crown-6 (DB18C6) by means
of synergistic extraction and back-extraction combined with atomic absorption spectrometry (AAS). The effect of various factors
(synergism with TTA and DB18C6, shaking time, preconcentration factor, composition of the extracted species, and foreign ions
etc.) on the extraction and back-extraction of lead has been investigated in detail. The lead-TTA chelate in o-dichlorobenzene forms a stable adduct with DB18C6 as Pb(TTA)2 DB18C6. The stability constant (β) of the adduct determined by curve fitting method was log β = 4.2. The amount of lead in
natural waters such as tap water (Kanazawa University) and Kakehashi river (Komatsu City) determined by the present method
was found to be 0.64 ± 0.02 μg/L and 5.10 ± 0.03 μg/L, respectively.
Received: 14 July 1997 / Revised: 3 November 1997 / Accepted: 20 January 1998 相似文献
18.
G. Meissner Kari Hartonen M.-L. Riekkola 《Fresenius' Journal of Analytical Chemistry》1998,360(5):618-621
A method is developed for the determination of β-blockers in serum and urine at levels of 0.5 μg/mL. The technique uses a
combination of solid phase extraction (SPE) with in situ derivatization and supercritical fluid extraction (SFE) with subsequent
gas chromatography mass spectrometry. The optimization of the SFE step shows that a static extraction period can be eliminated.
The method gives good linearity (r = 0.991–0.999) and repeatability in the concentration range of 0.5 to 5 μg/mL. Relative
standard deviations for oxprenolol, propanolol and metoprolol were less than 5% in serum and 5–11% in urine.
Received: 23 May 1997 / Revised: 28 July 1997 / Accepted: 5 August 1997 相似文献
19.
Ph. Quevauviller A. Ure H. Muntau B. Griepink 《International journal of environmental analytical chemistry》2013,93(1-4):129-134
Abstract The determination of extractable trace metal contents in soil and sediment, using respectively single and sequential extraction procedures, is currently performed in many laboratories to assess the bioavailable metal fraction (and related phyto-toxic effects) and the accessability to the environment (e.g. contamination of ground waters). Owing to the need for validation of the extraction schemes used and of the analytical techniques, the Community Bureau of Reference (BCR) decided to organize a project for the improvement of the quality of determinations of extractable trace metal contents in soil and sediment. The implementation of this project follows a stepwise approach involving feasibility studies, intercomparisons to detect and remove sources of errors in the application of the analytical methods, and the certification of the extractable compounds. This paper describes the organization of the work completed so far (feasibility studies and first intercomparison) and discusses its further development. 相似文献
20.
Determination of organophosphorus pesticides in soil by headspace solid-phase microextraction 总被引:1,自引:0,他引:1
W. F. Ng Mui Jun Karen Teo Hans-?ke Lakso 《Fresenius' Journal of Analytical Chemistry》1999,363(7):673-679
Headspace solid-phase microextraction (SPME) has been developed for the analysis of common organophosphorus pesticides in
soil. Factors such as adsorption-time, sampling temperature and matrix modification by addition of water were carefully considered
to optimize the extraction efficiency. This technique could achieve limits of detection of 143 ng/g for Malathion and Parathion,
and 28.6 ng/g for Phorate, Diazinon and Disulfoton in humic soil when the extracted sample was analyzed by gas chromatography-flame
ionization detector (GC-FID). Lower limits of detection of 28.6 ng/g for Malathion and Parathion, and 14.3 ng/g for Phorate,
Diazinon and Disulfoton can be achieved by analyzing the extracted sample with gas chromatography/mass spectrometric detector
(GC/MS). As the extraction efficiency was generally better when analyzing sandy soil, the limits of detection are envisaged
to be even better for such a matrix. The technique was found to be reliable with good precision of about 6.5% RSD for the
sandy soil and about 15% for the humic material. The poorer precision of extraction from the humic material is probably related
to the poorer homogeneity of this material. The linearity of extraction was good with linear calibration in the range of 0.143
to 28.6 μg/g. Finally, headspace SPME was compared to aqueous extraction of soil followed by SPME (LE-SPME). The recoveries
obtained by headspace SPME were comparable to those from liquid-liquid extraction of soil followed by SPME. However, the analysis
of headspace SPME has less background interference. Perhaps, the greatest advantage of this technique is its non-destructive
nature so that it is possible to perform further laboratory analysis of the samples after headspace SPME has been carried
out.
Received: 13 July 1998 / Revised: 10 November 1998 / Accepted: 17 November 1998 相似文献