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Suitable techniques have been developed for the extraction of arsenic species in a variety of biological and environmental samples from the Pak Pa-Nang Estuary and catchment, located in Southern Thailand, and for their determination using HPLC directly coupled with ICP-MS. The estuary catchment comprises a tin mining area and inhabitants of the region can suffer from various stages of arsenic poisoning. The important arsenic species, AsB, DMA, MMA, and inorganic arsenic (As III and V) have been determined in fish and crustacean samples to provide toxicological information on those fauna which contribute to the local diet. A Hamilton PRP-X100 anion-exchange HPLC system employing a step elution has been used successfully to achieve separation of the arsenic species. A nitric acid microwave digestion procedure, followed by carrier gas nitrogen addition- (N2)-ICP-MS analysis was used to measure total arsenic in sample digests and extracts. The arsenic speciation of the biological samples was preserved using a Trypsin enzymatic extraction procedure. Extraction efficiencies were high, with values of 82-102%(As) for fish and crustacean samples. Validation for these procedures was carried out using certified reference materials. Fish and crustacean samples from the Pak Pa-Nang Estuary showed a range for total arsenic concentration, up to 17 microg g(-1) dry mass. The major species of arsenic in all fauna samples taken was AsB, together with smaller quantities of DMA and, more importantly, inorganic As. For sediment samples, arsenic species were determined following phosphoric acid (1 M H3PO4) extraction in an open focused microwave system. A phosphate-based eluant, pH 6-7.5, with anion exchange HPLC coupled with ICP-MS was used for separation and detection of AsIII, AsV, MMA and DMA. The optimum conditions, identified using an estuarine sediment reference material (LGC), were achieved using 45 W power and a 20 minute heating period for extraction of 0.5 g sediment. The stability and recovery of arsenic species under the extraction conditions were also determined by a spiking procedure which included the estuarine sediment reference material. The results show good stability for all species after extraction with a variability of less than 10%. Total concentrations of arsenic in the sediments from the Pak Pa-Nang river catchment and the estuary covered the ranges 7-269 microg g(-1)and 4-20 [micro sign]g g(-1)(dry weight), respectively. AsV was the major species found in all the sediment samples with smaller quantities of AsIII. The presence of the more toxic inorganic forms of arsenic in both sediments and biota samples has implications for human health, particularly as they are readily 'available'.  相似文献   

3.
The presence of heavy metals/metalloids in the ecosystem has been an increasing ecological and global public health concern due to their potential to cause adverse health effects. For this reason, the accumulation of some heavy metals such as Cr, Mn, Ni, Cu, As, Cd, Pb was assessed by way of ICP-MS in water, sediment and fish (Cyprinus carpio) sampled from Gonyeli Lake, North Cyprus. The results showed that these metals/metalloids are found widespread throughout the study area. In water, most concentrated element was manganese with 92.1 ppb and least concentrated was lead with 0.914 ppb. In sediment, copper had the highest concentration with 613 ppm, and cadmium the lowest with 1.57 ppm. In fish tissues (muscle and gills), the most concentrated element was manganese with 12.5 ppm and the least concentrated cadmium with 0.017 ppm. These results indicate that future remediation efforts are indispensable for the rehabilitation of the lake.  相似文献   

4.
Inductively coupled plasma mass spectrometry (ICP-MS) is becoming more widely used for trace elemental analysis in the occupational hygiene field, and consequently new ICP-MS international standard procedures have been promulgated by ASTM International and ISO. However, there is a dearth of interlaboratory performance data for this analytical methodology. In an effort to fill this data void, an interlaboratory evaluation of ICP-MS for determining trace elements in workplace air samples was conducted, towards fulfillment of method validation requirements for international voluntary consensus standard test methods. The study was performed in accordance with applicable statistical procedures for investigating interlaboratory precision. The evaluation was carried out using certified 37-mm diameter mixed-cellulose ester (MCE) filters that were fortified with 21 elements of concern in occupational hygiene. Elements were spiked at levels ranging from 0.025 to 10 μg filter(-1), with three different filter loadings denoted "Low", "Medium" and "High". Participating laboratories were recruited from a pool of over fifty invitees; ultimately twenty laboratories from Europe, North America and Asia submitted results. Triplicates of each certified filter with elemental contents at three different levels, plus media blanks spiked with reagent, were conveyed to each volunteer laboratory. Each participant was also provided a copy of the test method which each participant was asked to follow; spiking levels were unknown to the participants. The laboratories were requested to prepare the filters by one of three sample preparation procedures, i.e., hotplate digestion, microwave digestion or hot block extraction, which were described in the test method. Participants were then asked to analyze aliquots of the prepared samples by ICP-MS, and to report their data in units of μg filter(-1). Most interlaboratory precision estimates were acceptable for medium- and high-level spikes (RSD <25%), but generally yielded greater uncertainties than were anticipated at the outset of the study.  相似文献   

5.
The present study deals with the ground water quality assessment in Kahuta Industrial Triangle Islamabad, Pakistan. The objective of the study was to assess ground water quality against the drinking water standards for various toxic inorganic elements. Representative groundwater samples were collected and analyzed in the Water Quality Laboratory of Pakistan Council of Research in Water Resources (PCRWR) at Islamabad, Pakistan. The samples were run on ICP-MS (Inductively coupled plasma mass spectrometry), which has the capability to separate and quantify 70 elements at a time. One of the finding of study is that ICP-MS is a very good tool to analyze broad range of toxic inorganic elements to the level of parts per billion (ppb). World Health Organization drinking water standards shows that these toxic inorganic elements such as heavy metals even at this concentration level (ppb) are injurious to human health. This analysis indicated pollution of various toxic elements including Selenium. Vertical leachate through industrial waste septic tanks is identified as major cause of groundwater pollution in the Industrial Triangle. Monitoring of the septic tanks and groundwater quality in study area is suggested along with remedial measures.  相似文献   

6.
An analytical procedure has been proposed for the determination of (226)Ra at the low femtogram per ml concentration level in mineral water samples using double focusing sector field ICP-MS (ICP-SFMS). For the pre-concentration and separation of radium from the matrix elements in water a tandem of a laboratory-prepared filter, based on MnO(2), and Eichrom "Sr-specific" resin was used. The recovery of the method was determined to be 70.5%. The limit of detection for (226)Ra determination was 0.02 fg ml(-1), including a pre-concentration factor of 10. In addition, uranium concentration and uranium isotope ratios were measured by ICP-SFMS. In several mineral water samples with a relatively high uranium content, (226)Ra concentrations were found between 0.7-15 fg ml(-1). The effective dose of the contribution was calculated using the radionuclide concentration and dose conversion factors from the World Health Organization, WHO (1993). Assuming a mineral water consumption of 2 l d(-1), a slightly higher calculated dose than the suggested limit for drinking water (0.1 mSv y(-1)) was found in some samples.  相似文献   

7.
Flow field flow fractionation (FlFFF) in combination with inductively coupled plasma mass spectrometry (ICP-MS) was used to study the chemical speciation of U and trace metals in depleted uranium (DU) contaminated soils. A chemical extraction procedure using sodium pyrophosphate, followed by isolation of humic and fulvic substances was applied to two dissimilar DU contaminated sample types (a sandy soil and a clay-rich soil), in addition to a control soil. The sodium pyrophosphate fractions of the firing range soils (Eskmeals and Kirkcudbright) were found to contain over 50% of the total U (measured after aqua regia digestion), compared to approximately 10% for the control soil. This implies that the soils from the contaminated sites contained a large proportion of the U within more easily mobile soil fractions. Humic and fulvic acid fractions each gave characteristic peak maxima for analytes of interest (Mn, Fe, Cu, Zn, Pb and U), with the fulvic acid fraction eluting at a smaller diameter (approximately 2.1 nm on average) than the humic fraction (approximately 2.4 nm on average). DU in the fulvic acid fraction gave a bimodal peak, not apparent for other trace elements investigated, including natural U. This implies that DU interacts with the fulvic acid fraction in a different way to all other elements studied.  相似文献   

8.
Arsenobetaine, two arsenosugars, dimethylarsinate and several unidentified arsenic species were detected in extracts of the haemolymph of the Dungeness crab, Cancer magister, by using HPLC-ICP-MS. This is the first report of the presence of arsenosugars in the haemolymph/blood of marine animals. Total, extractable and residual arsenic concentrations were determined by ICP-MS. The concentration of total arsenic was in the range of 1.4-3.8 [micro sign]g ml(-1). Nearly all (98%) the arsenic was found to be extractable, and accounted for primarily by arsenobetaine, two arsenosugars and dimethylarsinate. The results demonstrate that arsenic compounds present in the diet of crabs are not fully metabolized in the gut. They are, at least partly, taken up into the haemolymph. The concurrence of arsenobetaine and arsenosugars suggests that the use of repeated haemolymph sampling in crustaceans could facilitate investigations into the kinetics of the biotransformation pathways of arsenic compounds. Finally, the present study clearly demonstrates the unique capabilities of HPLC-ICP-MS for the detection and identification of minor arsenic components amongst the predominant arsenobetaine.  相似文献   

9.
Evidence for the occurrence of Ni(CO)4 in addition to Mo(CO)6 and W(CO)6 in fermentation gases from a municipal sewage treatment plant is presented for the first time. The gases were sampled at the top of the sewage sludge digester using Tedlar bags, and were analysed using cryotrapping followed by gas chromatography coupled with inductively coupled mass spectrometry (GC-ICP-MS). The use of an ICP-MS as an element-specific detector gives sufficiently low detection limits for metals and was coupled to a packed column gas chromatograph. This method provides information about the speciation of volatile transition metals in contrast to previously used methods for the determination of Ni(CO)4 in gas samples. The element-specific detection of three different isotopes (m/z 58, 60, 62) and the correspondence of the samples' retention times with those of the standard provided convincing evidence that Ni(CO)4 is present in the fermentation gas. The concentrations found were in the sub-ppb level, which is at least one order of magnitude lower than the threshold level of 1 ppb (v/v). In addition, Mo(CO)6 and W(CO)6 were also measured in the sub-ppb range in contrast to the absence of Fe(CO)5. The stabilities of Ni(CO)4, Fe(CO)5, and Mo(CO)6 were tested in a carbon monoxide atmosphere. In the presence of distilled water, the following order of stability was found after 11 weeks: Fe(CO)5 < Ni(CO)4 < Mo(CO)6. In the presence of an aqueous solution containing nickel, molybdenum, tungsten and iron, however, only Fe(CO)5 was significantly decomposed (< 0.3% recovery); Ni(CO)4 and Mo(CO)6 were stable after 11 weeks. No W(CO)6 was formed. The low stability of Fe(CO)5 in the presence of water could be the reason why no volatile iron compound was found in sewage gas. This study showed that GC-ICP-MS can be employed to identify species-specific traces of metal carbonyls in process gases such as sewage gas.  相似文献   

10.
The tanning industry is one of the largest environmental polluters due to high generation waste in all production processes, but the tanning is particularly worrisome due to the use of significant amounts of chromium. Cr is an element potentially toxic to both health and the environment, depending on the concentration and the oxidation state. Cr(VI) can come in contact with human skin when using leather goods, which can cause allergies and dermatitis, besides being carcinogenic. Considering that approximately 90% of the world production of leather is performed with Cr salts, the determination of this element in leather is necessary to avoid exposure to the risks that the element can provide. The main goal of this study was the development of an alternative analytical method for the determination of Cr in leathers (ovine and bovine leather tanned with Cr and vegetable tannin) using wavelength dispersive X-ray fluorescence (WDXRF) for direct solid analysis. Besides performing analysis of the chemical composition and determination of Al, As, Ba, Ca, Cd, Cr, Cu, Fe, Mg, Ni, Pb, Sb, Sr, Ti, and Zn in leather by inductively coupled plasma optical emission spectrometry (ICP OES). Principal component analysis (PCA) was also used in the evaluation of the WDXRF and ICP OES data sets. WDXRF calibration models for Cr presented satisfactory figures of merit and the analysis of the leathers revealed an alarming concentration of total Cr in the samples reaching 21,353 mg kg?1.  相似文献   

11.
The oxidation of sulphidic mine tailings and consequent acid generation poses challenges for the environment. Accurate and precise analysis of sulphur content is necessary for impact assessment and management of mine tailings. Here, the authors aim at developing a rapid and easy digestion procedure, which may analyse and measure the total amount of sulphur in mine tailings by using inductively coupled plasma. For evaluating effects of several variables, the researchers used a univariate (analysis of variance (ANOVA)) strategy and considered factors such as composition of the acid mixture, heating time, and refluxing device to optimize the performance. To do the experiment, the researchers have used two certified reference materials (KZK-1 and RTS-2) and samples of tailings from Musselwhite mine. ANOVA result shows that heating time is the most influencing factor on acid digestion of the reference materials whereas in case of a digestion of tailings sample, hydrochloric acid proved to be the most significant parameter. Satisfactory results between the measured and referenced values are found for all experiments. It is found that the aqua regia (1 ml HNO3 + 3 ml HCl) digestion of 0.1 g of samples after only 40 min of heating at 95°C produced fast, safe, and accurate analytical results with a recovery of 97% for the selected reference materials.  相似文献   

12.
The Fusaro Lagoon is a shallow lagoon, located in SW Italy, largely influenced in the last decades by several anthropic impacts. The study examined the pollution status of the lagoon, during year 2011–2012 at nine sampling stations with the aim to find out proper measurements of water lagoon restoration. Concentrations of heavy metals (HMs) (aluminium [Al], barium [Ba], cadmium [Cd], copper [Cu], iron [Fe], manganese [Mn], vanadium [V] and zinc [Zn]) were examined in water, sediments and specimens of the ascidian Ciona intestinalis sp. A. Low levels of dissolved oxygen concentration were detected at many stations, with mean values of 5.2–6.4 mg L?1. The redox potential of surface waters was also low, ?2.7 to 50.7 mV. Sediments possessed high organic matter content, 17.7–29.4 %. In sediments, the mean Zn level, 251.4 mg kg?1, was about sixfold higher than that recorded in year 2000 (38.5 mg kg?1) and considerably higher than that recorded in 2007 (191 mg kg?1). The mean levels of Cd were outstandingly high, with a mean value of 70.5 mg kg?1, about 30- and 50-fold higher than those determined in 2000 and 2007, respectively. Cadmium (Cd), Cu and nickel (Ni) appeared in excess with respect to most current guidelines, reaching significant pollution levels. C. intestinalis sp. A was detected only at few stations, with metals accumulated preferentially in the body in respect to the tunic, from 1.2 times for Zn (178 mg kg?1) to 4.0 times for V (304 mg kg?1). Data suggests the necessity of an immediate action of eco-compatible interventions for environmental restoration.  相似文献   

13.
A field study was carried out at six locations in the Lazio region (Central Italy) aimed at characterising atmospheric particulate matter (PM10 and PM2.5) from the point of view of the chemical composition and grain size distribution of the particles, the mixing properties of the atmosphere, the frequency and relevance of natural events. The combination of four different analytical techniques (ion chromatography, X-ray fluorescence and ICP for inorganic components, thermo-optical analysis for carbon compounds) yielded sound results in terms of characterisation of the air masses. During the first three months of the study (October-December 2004), many pollution events of natural (sea-salt or desert dust episodes) or anthropogenic nature were identified and characterised. More than 90% of the collected mass was identified by chemical analysis. The central role played by the mixing properties of the lower atmosphere when pollution events occurred was highlighted. The results show a major impact of primary anthropogenic pollutants on traffic stations and a homogeneous distribution of secondary pollutants over the regional area. An evaluation of the sources of PM and an identification of possible reliable tracers were obtained using a chemical fractionation procedure.  相似文献   

14.
A field study was carried out at six locations in the Lazio region (Central Italy) aimed at characterising atmospheric particulate matter (PM10 and PM2.5) from the point of view of the chemical composition and grain size distribution of the particles, the mixing properties of the atmosphere, the frequency and relevance of natural events. The combination of four different analytical techniques (ion chromatography, X-ray fluorescence and ICP for inorganic components, thermo-optical analysis for carbon compounds) yielded sound results in terms of characterisation of the air masses. During the first three months of the study (October–December 2004), many pollution events of natural (sea-salt or desert dust episodes) or anthropogenic nature were identified and characterised. More than 90% of the collected mass was identified by chemical analysis. The central role played by the mixing properties of the lower atmosphere when pollution events occurred was highlighted. The results show a major impact of primary anthropogenic pollutants on traffic stations and a homogeneous distribution of secondary pollutants over the regional area. An evaluation of the sources of PM and an identification of possible reliable tracers were obtained using a chemical fractionation procedure.  相似文献   

15.
The slurry sampling technique has been applied for the determination of arsenic, cadmium and lead in sidestream cigarette smoke condensate (SS CSC) by inductively coupled plasma mass spectrometry (ICP-MS). The smoke collection system consists of a "fishtail" chimney in conjunction with an impaction trap and a mixed cellulose ester (MCE) backup filter for the SS CSC collection. The smoke condensates, collected at three different regions of the system (i.e. the inner wall of the chimney, the impaction trap and the MCE filter), were individually prepared and analyzed and showed that about 70 and 20% of Cd and Pb, respectively, were trapped by the impaction trap and the MCE filter with less than 5% trapped by the chimney. In contrast, about 60% of As was trapped by the impactor and a relatively high percentage of As, about 30%, was deposited onto the inner wall of the chimney. The uneven distribution of trace metals at each collection stage strongly suggested that the composition of smoke aerosol and the associated physical form of the analytes may be different. The yields of As, Cd and Pb for the sidestream cigarette smoke of the 1R4F reference cigarette were 29.5 +/- 2.4, 421 +/- 6.6 and 46.4 +/- 0.9 ng cigarette(-1)(n= 3) respectively, when the cigarette was smoked according to the smoking regime: 45 mL puff volume of 2-s puff duration at an interval of 30 s with 50% ventilation holes covered. The analytical results for the slurry sampling technique were also compared with other sample preparation techniques and show good agreement.  相似文献   

16.
自然水体中Th和U的浓度极低,尤其Th的浓度单位仅为ng/L,定量测试非常困难。该研究建立了一种NOBIAS PA1螯合树脂萃取结合电感耦合等离子体质谱(ICP-MS)同时测定自然水体中痕量Th和U的分析方法。该方法首先使用UV/H2O2法消解水样30 min,去除水体中的有机物,然后在pH=3.00±0.05条件下,将水样以2 mL/min流速通过树脂对Th和U进行富集,使用NH4AC-HAC溶液去除树脂上吸附的盐类,最后用1 mol/L超纯硝酸对样品进行洗脱,用ICP-MS测试。分析结果显示:Th和U的流程空白值分别为0.47、0.22 ng/L,检出限分别为2.9、2.3 ng/L,测定下限分别为11.46、9.11 ng/L。将该方法应用于不同有机物浓度的咸水和淡水中,结果显示:Th和U的回收率分别为97%~104%和98%~103%,相对标准偏差分别为3%~6%和1%~3%。说明该方法具有较高的回收率、精密度和准确度,适用于自然界各种不同水体中Th和U的定量分析。  相似文献   

17.
The presence of emerging contaminants (ECs) in different aquatic systems may contribute to hazardous effects on aquatic organisms and subsequently on human health. In the present work, liquid chromatography coupled to a quadrupole time of flight mass spectrometer (LC-Q-ToF-MS) was used to identify and quantify a series of ECs in Periyar River in Aluva region, Kerala, India. The water samples were pre concentrated using solid-phase extraction (SPE) prior to analysis. The compounds were probed in both positive and negative ionization mode using electro spray ionization (ESI). Method validations were performed for linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision (intraday and inter day). The ECs were quantified using standard calibration curve. The identified nine ECs include pharmaceuticals, personal care products, steroids, surfactants, and phthalate. A relatively high concentration was observed in the case of 2-dodecyl benzene sulfonic acid (1012 ng/l) and low concentration was observed for lignocaine (4.3 ng/l; since this is below LOQ, the value is only approximate). In addition, we have identified another 28 organic compounds using the technique of non-target analysis out of which seven compounds fall in the category of surfactants. Being the first report on ECs in Periyar River, the data is very important as this river is one of the biggest and important rivers of Kerala having several purification units for drinking water in the province.  相似文献   

18.
Benzotriazole UV stabilizers (BUVSs), such as UV-328 and UV-327, were identified in the blubbers of finless porpoises (Neophocaena phocaenoides) collected from the Ariake Sea, western Japan, by gas chromatography-high resolution mass spectrometry (GC-HRMS). The mean concentrations and standard deviations of UV-328 and UV-327 in five blubber samples were 38 ± 28 ng g(-1) (lipid wt) and 19 ± 19 ng g(-1), respectively. The bioconcentration factor (BCF) of UV-327 between water and finless porpoises was estimated to be 33?300, which is approximately one order of magnitude higher than that found for small fish inhabiting the same regions. The BCF of UV-327 in finless porpoises was similar to that of persistent organochlorine pesticide, hexachlorocyclohexane (HCH: 37?000) in marine mammals from the western North Pacific Ocean. These results suggest that BUVSs appear to be persistent and bioaccumulative in the aquatic food chain. Further investigations on temporal trends, and regional and global monitoring of BUVSs are needed to understand their environmental profiles and potential risks to wildlife and human.  相似文献   

19.
Feathers, eggs, and excreta of Gentoo penguin (Pygoscelis papua ellsworthii), adults, from Livingston Island (South Shetlands), chosen as bioindicators, were used to test the quality of the Antarctic environment. Sex was not examined. The bioaccumulations of toxic trace elements (Cd, Pb, Al, and As), essential trace elements (Fe, Cu, Zn, Mn, Cr, V, Ni, and Sr), and major essential elements (Na, K, Mg, Ca, P, and S) were established. For the first time data about the element contents in Gentoo eggs is provided. Two hypotheses were tested: (1) there are differences in the metal levels among eggs and feathers; and (2) the element concentrations are highest in the excreta. The hypotheses were confirmed at 0.01-0.05 confidence levels. The concentrations of almost all trace elements were significantly higher in the feathers compared to those in the eggs. The following values of the concentrations ratio Fe/Zn were obtained: in the embryo, Fe/Zn = 1.5, and in the feathers, Fe/Zn = 0.5. The concentration of Pb in the embryo and excreta was below 0.4 μg/g, and Cd and As in eggs were below 0.05 and 0.3 μg/g, respectively. This indicates that there is no toxic risk for penguin offspring. Arsenic could be considered as a potential pollutant for Antarctic soil due to its relative high concentration in excreta, 5.13 μg/g. The present data (year 2007) were compared to the data for years 2002 and 2003. No trend of toxic element contamination was established. The concentrations of Pb, Cd, and As in representatives from the top of the food chain in the Antarctic (the present study) and Arctic (literature data) were compared. The data supports the hypothesis that there is an abnormality in cadmium levels in polar marine areas. Regarding Pb, the South Shetlands displayed 3-fold lower level compared to the Aleutians.  相似文献   

20.
The purpose of this study was to examine the levels of trace elements and to discuss the origin and mobility of these contaminants in the canal sediments (alluvial formation of the Danube River). The most significant fractions binding all of the studied elements were oxides and silicates. The high proportion of elements in the residual fraction and the generally low contents of extractable elements reflected the background geochemical conditions. The contents of trace elements (except Hg and As) were dominantly controlled by the presence of Fe and Mn oxides as well as by the grain size and the geochemical composition of the sediment. The studied alluvial sediments were not heavily contaminated; there were only few sites where an anthropogenic influence on the concentrations of some metals (Cu, Cd, Zn, and Pb) was noticed. The results from this study show that impact of Pan?evo industrial zone on the quality of the Danube River and its contamination with trace element is minor.  相似文献   

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