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1.
Perchlorate originates as a contaminant in the environment from its use in solid rocket fuels and munitions. The current US EPA methods for perchlorate determination via ion chromatography using conductivity detection do not include recommendations for the extraction of perchlorate from soil. This study evaluated and identified appropriate conditions for the extraction of perchlorate from clay loam, loamy sand, and sandy soils. Based on the results of this evaluation, soils should be extracted in a dry, ground (mortar and pestle) state with Milli-Q water in a 1 ratio 1 soil ratio water ratio and diluted no more than 5-fold before analysis. When sandy soils were extracted in this manner, the calculated method detection limit was 3.5 microg kg(-1). The findings of this study have aided in the establishment of a standardized extraction method for perchlorate in soil.  相似文献   

2.
The extensive use of the broad range of pesticides employed to maintain golf courses has prompted serious environmental concerns in Japan since courses tend to be located in mountainous regions, often in close proximity to virgin water sources. Since older empirical methods are not appropriate for substance identification and determination of substance concentrations on the ppb order, gas chromatographyquadrupole mass spectrometry (GC/QPMS) can be employed. A simple extraction of 500 ml of drainage pond water gives a sample which allows identification of pesticides with quantitation on the ppb order using selected ion monitoring (SIM). A sample of drainage pond water from a golf course revealed fenitrothion, funitrothion, chlorothalonil and isoprothiolane in concentrations of 120.1, 20.7, 45.6 and 130.5 ppb, respectively.  相似文献   

3.
The native distribution of As(III) and As(v) in drinking water supplies can influence the treatment removal strategy. The stability of As(III) and As(v) in iron-rich drinking waters can be affected by the formation of Fe precipitates (Fe oxides and/or hydroxides designated by "FeOOH"). These precipitates (ppts) can form during the transport of the sample to the laboratory for arsenic speciation analysis. The analysis of the ppt indicates considerable loss of the aqueous arsenic species (As(aq)) to the solid phase "FeOOH" ppt. Studies of laboratory reagent water containing both As(III) and Fe(III) indicate that the resulting "FeOOH" ppt contained a mixture of As(III) and As(v) with near quantitative removal of the As(aq) in 18 hr. The corresponding aqueous fraction after filtration through a 0.45 microm filter was composed primarily of As(v). The formation of "FeOOH" ppt and the loss of As(aq) to the ppt can be virtually eliminated by the use of EDTA, which sequesters the FeIII). Reagent water fortified with Fe(III), As(III) and EDTA produced less than a 1 ppb change in the As(III)aq concentration over 16 d. The EDTA treatment was also tested on three well waters with different native As(III )/As(v) ratios. The native distribution of As(III)/As(v) was stabilized over a period of 10 d with a worst case conversion of As(III) to As(v) of 2 ppb over a 30 d period. All well waters not treated with EDTA had dramatic losses (a factor of 2-5) of As(aq) in less than 1 d. These results indicated that EDTA preservation treatment can be used to preserve As(aq) in waters where the predominant species is the reduced form [As(III)] or in waters which the predominant species is the oxidized form [As(v)]. This preliminary investigation of EDTA to preserve As species in Fe-rich waters indicates stability can be achieved for greater than 14 d.  相似文献   

4.
Perchlorate contamination was investigated in groundwater and surface water from Sivakasi and Madurai in the Tamil Nadu State of South India. Sensitive determination of perchlorate (LOQ?=?0.005 μg/L) was achieved by large-volume (500 μL) injection ion chromatography coupled with tandem mass spectrometry. Concentrations of perchlorate were <0.005–7,690 μg/L in groundwater (n?=?60), <0.005–30.2 μg/L in surface water (n?=?11), and 0.063–0.393 μg/L in tap water (n?=?3). Levels in groundwater were significantly higher in the fireworks factory area than in the other locations, indicating that the fireworks and safety match industries are principal sources of perchlorate pollution. This is the first study that reports the contamination status of perchlorate in this area and reveals firework manufacture to be the pollution source. Since perchlorate levels in 17 out of 57 groundwater samples from Sivakasi, and none from Madurai, exceeded the drinking water guideline level proposed by USEPA (15 μg/L), further investigation on human health is warranted.  相似文献   

5.
The successful determination of mutagenic/carcinogenic heterocyclic amines (HCAs) in trace amounts (ng/g, ppb levels) in commercial foods depends largely on the detection sensitivity and selectivity, as well as the quality of clean-up of complex food matrices. In the present study, UV and fluorescence detection in series with gradient elution HPLC was used for the separation and determination of eight HCAs present in a local delicacy, satay. The identification of peaks was carried out by UV diode-array spectrophotometry. The most common HCA found in all types of satay (chicken, mutton, pork) cooked under Chinese and Malay styles was 2-amino-9H-pyrido[2,3-b]indole (AC) (1.3-12 ppb) while 3-amino-1-methyl-5H-pyrido[4,3-b]indole (Trp-P-2) was found at comparatively high levels (78 ppb) in both Chinese-style pork and Malay-style chicken satay. Other major HCAs included 3-amino-1,4-dimethyl-5H-pyrido[4,3-b]indole (Trp-P-1) (non-detectable (ND) to 31 ppb), 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP) (ND-12 ppb) and 2-aminodipyrido[1,2-a:3,2-d]-imidazole (Glu-P-2) (ND-25 ppb). Comutagen norharman (NH) was also detected at levels up to 84 ppb, while harman (H) was only detected in one sample (Chinese-style pork satay), at a level of 25 ppb. The differences in the type and level of HCAs in satay samples may be attributed to the variation in raw foodstuffs cooked under different styles by Chinese or Malay vendors, and the ingredients added during cooking.  相似文献   

6.
Samples of river water and treated drinking water were obtained from eight sites along the Potomac River between western Maryland and Washington DC. Samples were collected each month from October 2007 to September 2008 and analyzed for perchlorate by ion chromatography/mass spectrometry. Data on anions were also collected for seven of the twelve months. Data were analyzed to identify spatial and temporal patterns for the occurrence of perchlorate in the Potomac. Over the year of sampling, the largest monthly increase occurred from June to July, with levels then decreasing from July to September. Samples from the period between December and May had lower perchlorate concentrations, relative to the remainder of the study year. Spatially, higher levels of perchlorate were found at sites located in west-central Maryland, the eastern panhandle of West Virginia, and central northern Virginia, with levels decreasing slightly as the Potomac approaches Washington DC. Within the sampling boundaries, river (untreated) water perchlorate concentrations ranged from 0.03 μg L(-1) to 7.63 μg L(-1), averaged 0.67 ± 0.97 μg L(-1) over the year-long period and had a median value of 0.37 μg L(-1). There was no evidence that any of the existing drinking water treatment technologies at the sampling sites were effective in removing perchlorate. There were no correlations found between the presence of perchlorate and any of the anions or water quality parameters examined in the source water with the exception of a weak positive correlation with water temperature. Results from the summer (June-August) and fall (September-November) months sampled in this study were generally higher than from the winter and spring months (December-May). All but one of the locations had annual average perchlorate levels below 1 μg L(-1); however, 7 of the 8 sites sampled had river water perchlorate detections over 1 μg L(-1) and 5 of the 8 sites had treated water detections over this level.  相似文献   

7.
Interest in possible sources of perchlorate (ClO4) that could lead to environmental release has been heightened since the Environmental Protection Agency placed this anion on its Contaminant Candidate List for drinking water. Although recent investigations have suggested that fertilizers are minor contributors to environmental perchlorate contamination overall, there is still interest in screening commercial products for possible contamination and quantitating perchlorate when it is found. Ion chromatography (IC) has been used for this application owing to its speed, low detection limits, widespread availability, and moderate ruggedness relative to other techniques. However, fertilizer matrixes complicate the IC analysis relative to potable water matrixes. In this study, the performance of poly(vinyl alcohol) gel resin IC columns (100 mm and 150 mm) was evaluated for fertilizer matrixes using method EPA/600/R-01/026. The NaOH eluent included an organic salt, sodium 4-cyanophenoxide. Detection was by suppressed conductivity. A set of 55 different field samples representing 48 products and previously used by the EPA to assess occurrence of perchlorate in fertilizers (EPA/600/R-01/049) was reanalyzed on the 150 mm column. The 100 mm column was used to further investigate the positive hits. Both columns gave satisfactory performance in fertilizer matrixes, with spike recoveries (+/- 15%), assured reporting levels (0.5-225 microg g(-1) except for one at 1,000 microg g(-1)), accuracy (relative error < 30% always and most < 15%), and precision [injection-to-injection reproducibility < 3% relative standard deviation (RSD)] comparable to those reported in other studies. Performance did not vary substantially between column lengths. Lastly, the results of this investigation provided further evidence in support of the conclusions that had been reached previously by the EPA on the occurrence of perchlorate in fertilizers.  相似文献   

8.
A new extraction-spectrophotometric method for the determination of indium at ppb level in zinc effluent is described. It is based on quantitative extraction (51.2–99.2%) of the tetrabromoindate complex with toluene solution of N,N-diphenylbenzamidine and its nine analogous from sulphuric acid solutions, which allowed the extract to react with basic dye (i.e. brilliant green, malachite green, crystal violet) solution in sequence. Among the basic dyes tested, brilliant green gave the most sensitive colour reaction. The value of molar absorptivity of the amidine bromoindate extracts with brilliant green lie in the range of (0.53–1.03)×105 l mole-1 cm-1 at absorption maximum, 630–640. With the most sensitive compound, N-(2-methyl-phenyl)-N-phenylbenzamidine(APPBA), the detection limit of the method is 13 ppb. The method is free from interferences of almost all ions associated with indium. The method has been applied for the determination of indium to zinc-effluent.  相似文献   

9.
Previous studies have shown that tobacco plants are tolerant of perchlorate and will accumulate perchlorate in plant tissues. This research determined the uptake, translocation, and accumulation of perchlorate in tobacco plants. Three hydroponics growth studies were completed under greenhouse conditions. Depletion of perchlorate in the hydroponics nutrient solution and accumulation of perchlorate in plant tissues were determined at two-day intervals using ion chromatography. Perchlorate primarily accumulated in tobacco leaves, yielding a substantial storage capacity for perchlorate. Mass balance results show that perchlorate degradation was negligible in plants. Tobacco plants were shown to effectively accumulate perchlorate over a wide range of initial concentrations (10 ppb to 100 ppm) from the hydroponics solution. Results suggest that plants are potential plants for the phytoremediation of perchlorate. A mathematical model was developed to describe the distribution of perchlorate in tobacco plants under rapid growth conditions. The Plant Kinetic (PK) model defined a plant as a set of compartments, described by mass balance differential equations and plant-specific physiological parameters. Data obtained from a separate hydroponics growth study with multiple solution perchlorate concentrations were used to validate predicted root, stem, and leaf concentrations. There was good agreement between model predictions and measured concentrations in the plant. The model, once adequately validated, can be applied to other terrestrial plants and inorganic chemicals currently used for both phytoremediation and ecological risk assessment.  相似文献   

10.
Groundwater is the primary source of drinking water for more than 95% of the population in Punjab. The world health organization and US Environment Protection Agency recently established a new maximum contaminant level of 10 ppb for arsenic in drinking water. The arsenic concentration of deep water tube wells located in Amritsar city used for domestic supply for urban population ranged from 3.8 to 19.1 ppb with mean value of 9.8 ppb. Arsenic content in hand pump water varied from 9 to 85 ppb with a mean value of 29.5 ppb. According to the safe limit of As, 54% and 97%, water samples collected from deep water tube wells and hand pumps, respectively, were not fit for human consumption. Arsenic content in canal water varied from 0.3 to 8.8 ppb with a mean value of 2.89 ppb. Canal water has got higher oxidation potential followed by deep tube well and hand pump water. The present study suggests the regular monitoring of arsenic content in deep tube well and shallow hand pump waters by water testing laboratories. The consumption of water having elevated concentration of As above the safe limit must be discouraged. In south-western districts of Punjab, it recommends the use of canal water for drinking purposes and domestic use by rural and urban populations than ground water sources.  相似文献   

11.
Arsenic in the soil and water of eastern districts of Uttar Pradesh (Ballia and Ghazipur) was estimated. Survey results revealed that arsenic in soil samples ranged from 5.40 to 15.43 parts per million (ppm). In water samples, it ranged from 43.75 to 620.75 parts per billion (ppb) which far exceeded the permissible limit of 10 ppb as recommended by the World Health Organization. Maximum concentration of arsenic in water was found in Haldi village of Ballia (620.75 ppb). However, mean arsenic concentration in water followed the order: Karkatpur (257.21 ppb) < Haldi (310.15 ppb) < Sohaon (346.94 ppb) < Dharmarpur (401.75 ppb). In case of soil, maximum arsenic was detected in soil of Sohaon (15.43 ppm). Mean arsenic levels in soils followed the order: Karkatpur (9.24 ppm) < Haldi (9.82 ppm) < Dharmarpur (11.32 ppm) < Sohaon (14.08 ppm). Arsenic levels were higher in soils collected from 15–30 cm depth than 0–15 cm from the soil surface.  相似文献   

12.
Fluoride Deposition in Central India   总被引:1,自引:0,他引:1  
Fluoride is a volatile element emitted from natural and anthropogenic sources into the atmoshere and scavenged from the atmosphere by rain water. We collected 444 rain water and 36 dust samples on an event basis at 13 sites and on the bulk basis (monthly) at 3 sites, respectively, in central India (extending over 17°N to 24°N latitude and 80° 17 to 84°11E longitude). The level of F- in the atmospheric samples was determined by automating the conventional Zr(IV)-SPADNS [Sodium 2- (parasulfophenylazo)-1, 8-dihydroxy-3, 6-naphthalene disulfonate] method in the presence of surfactant, i.e. TX–100 [Triton x- 100]. The detection limit of the method is 10.0 ppb F- with a sample throughput of 70 samples/h. The F- deposited with rain water (in 13 sites) and with dust (three sites) were ranged between 54.8 to 483.0, and 105.0 to 503.3 kg/km2/year, respectively. The level of F- in atmospheric samples, seasonal and spatial variation in deposition and sources of F- are discussed.  相似文献   

13.
Styrene-7,8-oxide (SO) is generated at low concentrations from the oxidation of styrene during the processing of reinforced plastics. Since exposure to SO has important health implications, we developed air sampling and analytical methods to measure low levels of airborne SO in the presence of styrene and its other oxidation products, namely phenylacetaldehyde (PAA) and acetophenone (AP). Both active and passive air monitors were used. The active sampling method, which employed adsorption on Tenax, was suitable for measuring SO, PAA and AP but had limited capacity for styrene due to breakthrough. The passive monitor employed a carbon adsorbent and was suitable for measurement of styrene and SO but not PAA and AP due to poor recovery. After sampling, the analytes were extracted from the adsorbents with ethyl acetate and measured by gas chromatography with flame ionization detection or mass spectrometry. By maintaining the injection port at 70 degrees C, the thermal rearrangement of SO to PAA was minimized. Recovery of styrene and SO from the passive monitor depended upon loading and was corrected by linearization of the Freundlich isotherm. The limits of detection for SO, PAA, and AP were 0.2 ppb using the active monitor, and for SO was 1 ppb using the passive monitor. The sampling precision for SO (RSD from personal measurements) was 5.0% for the passive monitor and was 13.4% for the active monitor over a range of exposures from 5-150 ppb. The corresponding precision for styrene was 5.3% for the passive monitor for levels ranging from 1.2 to 104 ppm. Measurements of 235 personal exposures with the active monitor in 12 facilities manufacturing fiberglass-reinforced plastics (FRP) showed that levels of AP and PAA were below 7.8 ppb and 5 ppb, respectively. In contrast, SO averaged 30.4 ppb (SE=2.4) in these FRP facilities, ranging from below 0.2 ppb to 190 ppb. The active monitor was also used to detect airborne SO at levels of approximately equals 1 ppb in one facility manufacturing styrene butadiene rubber, suggesting that SO is generally present during the polymerization of styrene. Personal passive monitoring in the 12 FRP facilities (n = 657) revealed mean concentrations of styrene ranging between 1.8 and 55.4 ppm, and for SO between 1.7 and 62.6 ppb. The ratio of the mean styrene level to the mean SO level varied between 449:1 and 1,635:1 among the 12 FRP facilities.  相似文献   

14.
采用固相萃取-高效液相色谱-串联质谱法(SPE-HPLC-MS/MS)建立了地表水中25种抗生素类药物和8种非抗生素类药物的分析方法。通过重点优化质谱参数、色谱条件、样品pH、洗脱溶剂组成及用量等确定了最佳分析条件。水样经过滤、固相萃取柱富集净化后,选择Shim-pack XR-ODS为色谱柱,以乙腈和0.2%甲酸-2 mmol/L乙酸铵-水溶液为流动相进行梯度洗脱,采用电喷雾电离源,在多反应监测模式下(MRM)分析测定,内标法定量。33种药物的仪器定量限为0.012~4.68 ng/L,方法检出限为0.011~7.60 ng/L,地表水加标回收率为53.7%~122%,相对标准偏差为1.22%~32.1%(n=6)。方法成功应用于北京市凉水河12个地表水样分析,共检出32种药物,检出质量浓度为未检出~239 ng/L。利托那韦(RTV)作为新型冠状病毒诊疗方案中推荐的药物在凉水河检出率为100%。  相似文献   

15.
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   

16.
A simple and sensitive solid phase extraction (SPE) method on multiwalled carbon nanotubes (MWCNTs) is presented for the determination of cadmium, lead, nickel, copper, and zinc at trace levels combined with flame atomic absorption spectrometry. The effects of parameters like pH, sample volume, sample and eluent flow rates, eluent concentration, and volume and type of eluent on the recovery of trace elements was examined. The metals retained on the nanotube at pH 6.5 as α-benzoin oxime complexes were eluted by 10 mL 2 M HNO3 in acetone. The influence of matrix ions on the developed method was also evaluated. The preconcentration factor of the method was found to be 50. The detection limits for Cd(II), Pb(II), Ni(II), Cu(II), and Zn(II) were found as 1.7, 5.5, 6.0, 2.3, and 2.4 μg L?1, respectively. To test the accuracy of the method, the method was applied to TMDA-70 fortified lake water and Spinach 1570A standard reference materials. Addition recovery studies were applied to tap water and cracked wheat samples, and determination of the analyte elements was carried out in some food samples with good results.  相似文献   

17.
In this paper, the applicability of a Long-Path Differential Optical Absorption Spectroscopy (LP-DOAS) system was checked for the feasibility of the simultaneous measurement of trace gases (such as O3, NO2, SO2, and HCHO) and atmospheric visibility (light extinction by aerosols) in Asian urban areas. Field studies show that an LP-DOAS system can simultaneously measure the key pollutants (such as O3, NO2, SO2, and HCHO) at detection limits in the ppb/sub-ppb range as well as the Mie extinction coefficient with an uncertainty of 0.1 km–1 at time resolution of a few minutes. It is thus concluded that the use of LP-DOAS system is feasible for simultaneous measurement of gaseous pollutants as well as an atmospheric extinction coefficient which is tightly bound to fine particulate concentration.  相似文献   

18.
An Ion Chromatography-Mass Spectrometry (IC-MS) method was developed for the simultaneous quantification of 14 volatile amines in air. The method includes collection of compounds into two midget impingers in a row filled with 15 ml of ultrapure water. The analytical performances with mass spectrometry detection were compared to those obtained with classical conductivity detection. The use of mass spectrometry detection (in SIM mode) overcomes most of the coelutions encountered with conductivity detection. Although the linearity domain of calibrations is reduced for the MS detection as compared with the CD detection, the detection limits in MS detection are highly lowered allowing the quantification of amines at the levels of μg m(-3) in air with a good accuracy for most compounds (RSD of less than 10%). This method was successfully applied to the analysis of amines released from polyurethane foams. Seven amines were identified and some in high concentrations, like dimethylaminoethanol, NIAX and TEDA.  相似文献   

19.
Adsorption and release of perchlorate in a variety of soils, minerals, and other media were studied when the solid media were exposed to low and high aqueous solutions of perchlorate salts. Low level ClO4- exposure was investigated by subjecting triplicate 5.0 g portions of a solid medium (38 different soils, minerals, or dusts) to 25 mL of an aqueous ammonium perchlorate (NH4ClO4) solution containing 670 ng mL(-1) (6.8 microM) perchlorate. This corresponds to a perchlorate-to-soil ratio of 3.4 microg g(-1) (34 nmol g(-1)). At this level of exposure, more than 90% of the perchlorate was recovered in the aqueous phase, as determined by ion chromatography. In some cases, more than 99% of the perchlorate remained in the aqueous phase. In some cases, the apparent loss of aqueous perchlorate was not clearly distinguishable from the variation due to experimental error. The forced perchlorate anion exchange capacities (PAECs) were studied by soaking triplicate 5.0 g portions of the solid media in 250 mL of 0.20 M sodium perchlorate (NaClO4) followed by repeated deionized water rinses (overnight soaks with mixing) until perchlorate concentrations fell below 20 ng mL(-1) in the rinse solutions. The dried residua were leached with 15.0 mL of 0.10 M sodium hydroxide. The leachates were analyzed by ion chromatography and the perchlorate concentrations thus found were subsequently used to calculate the PAECs. The measurable PAECs of the insoluble and settleable residua ranged from 4 to 150 nmol g(-1) (micromol kg(-1)), with most in the 20-50 nmol g(-1) range. In some soils or minerals, no sorption was detectable. The mineral bentonite was problematic, however. Overall, the findings support the widely accepted idea that perchlorate does not appreciably sorb to soils and that its mobility and fate are largely influenced by hydrologic and biologic factors. They also generally support the idea that intrasoil perchlorate content is depositional rather than sorptive. On the other hand, sorption (anion replacement) of perchlorate appears to occur in some soils. Therefore, the measurement of perchlorate in soils requires accounting for ion exchange phenomena; leaching with water alone may give inaccurate results. If perchlorate anion exchange is confirmed to be negligible, then leaching procedures may be simplified accordingly.  相似文献   

20.
Perchlorate is known to competitively interfere with iodide uptake by the thyroid gland and thereby human exposure to perchlorate is a public health concern. Prevalence of perchlorate in dairy milk is documented; nevertheless, co-occurrence of perchlorate with other thyroid-binding monovalent ions such as iodide and nitrate is not well understood. In this study, we analyzed perchlorate, iodide, and nitrate-N in dairy milk, water and other dairy-related samples collected from Japan and Sri Lanka. Concentrations of perchlorate in Japanese dairy milk samples ranged from 1.03 to 14.1 ng ml(-1); the corresponding concentrations in dairy milk and powdered milk from Sri Lanka were 1.14-38.5 ng ml(-1). Perchlorate concentrations in commercial milk were significantly higher in Japan than in Sri Lanka, while iodide and nitrate levels in milk between the two countries were comparable. All three ions were ubiquitously found in water samples from Japan and Sri Lanka. Analysis of colostrum and raw milk collected from cows fed with the same feed for over 30 days showed no significant temporal variations in perchlorate, iodide and nitrate-N concentrations. A significant positive correlation was found between the concentrations of perchlorate and iodide in Japanese commercial milk. The concentrations of perchlorate and nitrate-N in water samples analyzed from both countries also showed a significant positive correlation. The exposure estimation revealed that dairy milk provides a greater source for perchlorate and iodide, while water predominantly contributes nitrate-N intake for all age groups in both counties. Infants and children demonstrated the highest estimated perchlorate, iodide and nitrate-N intake on a body weight basis in comparison to other age groups. Therefore, further studies of risk associated with perchlorate may need to reconsider co-existence of iodine and other iodide transport inhibitors in food.  相似文献   

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