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1.
The performance of a novel prototype instrument in determining solvents and solvent mixtures permeating through samples of chemical protective clothing (CPC) materials was evaluated. The instrument contains a mini-preconcentrator and an array of three polymer-coated surface-acoustic-wave (SAW) microsensors whose collective response patterns are used to discriminate among multiple permeants. Permeation tests were performed with a 2.54 cm diameter test cell in an open-loop configuration on samples of common glove materials challenged with four individual solvents, three binary mixtures, and two ternary mixtures. Breakthrough times, defined as the times required for the permeation rate to reach a value of 1 microg cm(-2) min(-1), determined by the instrument were within 3 min of those determined in parallel by manual sampling and gas chromatographic analysis. Permeating solvents were recognized (identified) from their response patterns in 59 out of 64 measurements (92%) and their vapor concentrations were quantified to an accuracy of +/- 31% (typically +/- 10%). These results demonstrate the potential for such instrumentation to provide semi-automated field or bench-top screening of CPC permeation resistance.  相似文献   

2.
Systems for the preparation and administration of drugs are designed to ensure that the drug is not contaminated. They do not necessarily consider the work environment for the medical staff and new techniques are therefore desirable. The aim of this work is to compare a new closed system for the preparation and administration of drugs with the traditional technique with regard to airborne emission and surface spillage of drugs. Platinum, determined using adsorptive voltammetry, was used as the tracer for airborne emission. Air samples were collected during the preparation and administration, and the collected platinum on the filters was determined by adsorptive voltammetry. For determination of spills and leakage onto surfaces the radioisotope 99m-technetium was used as a tracer. The radiation from the isotope was determined on protective gloves and bench covers after preparation and administration. The mean airborne emission was 6 ng m(-3) with the closed system and 15 ng m(-3) with the traditional pump technique. The average surface spillage using the closed technique was 0.005 microL. This is significantly smaller than with the traditional technique, which resulted in an average spillage of 64 microL. Our results also show that the dominant part of the leakage is surface spillage. Inexperienced nurses could also adequately handle the closed system.  相似文献   

3.
建立了生物介质内22种多溴联苯(PBBs)和27种多溴联苯醚(PBDEs)的净化和分析方法。通过分析不同时间段凝胶渗透色谱(GPC)洗脱液中49种化合物含量,得出不同化合物凝胶色谱洗脱曲线。样品经过凝胶渗透色谱-混合硅胶柱净化后,再使用GC-(NCI)/MS对样品进行检测。实验结果表明,PBBs和PBDEs检出限分别为0.02~0.88 pg/g和0.01~74.00 pg/g。对实验过程进行验证发现,样品不同浓度加标回收率为80%~120%,相对标准偏差小于20%。该方法具有良好的净化效果、准确度和精密度,拥有良好的线性范围及检出限,满足生物介质中溴代阻燃剂的检测分析实际要求。  相似文献   

4.
Tris(chloro-isopropyl)phosphate (TCPP) was identified by GC-MS by comparing mass spectra and retention times to original standards. The concentrations in wastewater of a sewage treatment plant's influent and effluent were analysed (520 ng l(-1) and 380 ng l(-1), respectively (mean values). The concentrations of TCPP in the wastewater inflow exhibited a high variability. The elimination of this compound in the sewage treatment plant also exhibits a high variability but is low. Additionally the concentrations in sewage sludge of the same plant were determined (mean value 5100 ng g(-1) dry weight; 1700 ng g(-1) wet weight, respectively). For a comparison sludge samples from twenty other plants were analysed. In these samples concentrations ranging from 1000-20000 ng g(-1)(dry weight) were determined. Thus sorption to sludge does occur to some extent.  相似文献   

5.
This study reports the feasibility of applying directly suspended liquid-phase microextraction (DSLPME)-gas chromatography detection for the pre-concentration and determination of low levels of eight polychlorinated biphenyls (PCBs) in aqueous samples. The technique requires minimal sample preparation, analysis time and solvent consumption and represents significant advantages over conventional analytical methods. The experimental parameters such as salt content, sample temperature, stirring rate, extraction time, micro-drop volume and breakthrough volume were investigated and found to have significant influences on DSLPME. Under the optimal experimental conditions, the enrichment factor ranged from 578 to 729, and the recovery was above 93 %. Calibration curves possessed good linearity (R 2?>?0.99) over a wide concentration range of 0.1–10.0 μg L?1 with limits of detection ranging from 0.01 to 0.07 μg L?1. The relative standard deviations for 1.0 μg L?1 of PCBs in water by using internal standard were in the range 2–14 % (n?=?3). The proposed simple, accurate and sensitive analytical method was applied successfully to the determination of trace amounts of PCBs in water samples.  相似文献   

6.
The occurrence and fate of fourteen androgens, four estrogens, five glucocorticoids and five progestagens were investigated in two different types of wastewater treatment plants (Plant A: activated sludge with chlorination, and Plant B: oxidation ditch with UV) of Guangdong province, China. 14, 14, and 10 of 28 target compounds were detected in the influent, effluent and dewatered sludge samples with the concentrations ranging from below 1.2 ± 0.0 ng L(-1) (stanozolol) to 1368 ± 283 ng L(-1) (epi-androsterone), below 1.0 ± 0.0 ng L(-1) (progesterone) to 23.1 ± 1.0 ng L(-1) (5α-dihydrotestosterone), 1.0 ± 0.1 ng g(-1) (estrone) to 460 ± 4.4 ng g(-1) (5α-dihydrotestosterone), respectively. The concentrations of total androgens (1554-1778 ng L(-1) in influent, 13.3-47.8 ng L(-1) in effluent, 377-923 ng g(-1) in dewatered sludge) were much higher than those of total estrogens (41.5-60.2 ng L(-1) in influent, 5.6-13.5 ng L(-1) in effluent, 13.9-57.8 ng g(-1) in dewatered sludge), glucocorticoids (171-192 ng L(-1) in influent, 2.2-6.3 ng L(-1) in effluent, N.D.-4.4 ng g(-1) in dewatered sludge), and progestagens (39.6-40.5 ng L(-1) in influent, 6.9-12.1 ng L(-1) in effluent, N.D. in dewatered sludge) in these two WWTPs. According to mass balance analysis, the removal rates of most target steroids in Plant A had exceeded 90%, while those in Plant B for nearly half of detected target steroids were lower than 80%. It is obvious that the treatment capacity of the activated sludge system (Plant A) is superior to the oxidation ditch (Plant B) in the degradation of steroids in sewage treatment systems. Androgens, estrogens and progestagens were mainly removed by sorption and degradation, while the reduction of glucocorticoids was primarily due to degradation.  相似文献   

7.
A new sensitive analytical procedure has been developed for the determination of residues of endosulfan in human blood samples. The method involves the extraction of residues of endosulfan from blood samples by the addition of 60% sulfuric acid at 10 degrees C, liquid/liquid partitioning by using hexane and acetone mixture (9:1) and quantification by using GC-ECD. Residues of endosulfan in blood samples were quantified as the sum of alpha-endosulfan, beta-endosulfan, endosulfan sulfate and endosulfandiol. The influence of temperature during the extraction has been studied. Recovery experiments were conducted over the concentration range 1.0-50 ng ml(-1) and the relative standard deviation calculated. The method was found to be sufficiently sensitive to quantify the residue of total endosulfan up to the 1.0 ng ml(-1) level. The recovery was 92% with a calculated relative standard deviation of 1.96%. Conversion of endosulfan to endosulfandiol is found to be less than 0.5% under the defined conditions. The method was applied to the analysis of residue contents of endosulfan and its metabolites in blood samples collected from the exposed population. The data obtained has been confirmed by GC-MS-EI in selective ion monitoring (SIM) mode.  相似文献   

8.
This study focused on investigation of treatment alternativesfor COD wastewater from academic laboratories, using a number oftechnologies including chemical reduction/precipitation, ion exchange and adsorption by chitosan. Results showed that highconcentrations of 375 mg l-1 chromium, 1,740 mg l-1mercury and 993 mg l-1 silver in COD wastewater can be reduced to 2.34 mg l-1, 3.65 mg l-1 and 1.89 mg l-1 respectively, by the chemical reduction/precipitationprocess. Results from ion exchange at a flowrate of 20 ml min-1 showed breakthrough effluent concentrations obtainedat 0.59 mg l-1 chromium, 3.92 g l-1 mercury and 0.65 mg l-1 silver corresponding to 75.6 l at 63 hr, 40.8 l at 34 hr and 33.6 l at 28 hr respectively. Kinetic and isotherm studies revealed that chitosan can adsorb Cr6+, Hg2+ and Ag+ ions most effectively at a flowrate of 20 ml min-1 and the optimum pH for feed solution is 4. Chitosan column experiments indicated that average effluent concentrations at breakthrough point for chromium, mercury andsilver are 0.76 mg l-1, 6.04 mg l-1 and 0.51 mg l-1 respectively with throughput volumes and retention times of 120 l at 100 hr, 60 l at 50 hr and 48 l at 40 hr. Results of solidification experiments for chemical sludge and residual chitosan based on compressive strength and metal leachabilitytests showed, that the acceptable ranges of the solidificationparameters were: sludge/cement = 0.1–1.0 (weight/weight), water/cement = 0.5–0.6 (weight/weight) and sand/cement = 0.5–3.0 (weight/weight). Operating cost per litre of COD wastewater treated, based on the current prices in Thailand wasfound to be Baht 19.95 for the chemical reduction/precipitationprocess, Baht 96.35 for ion exchange treatment and Baht 18.29 forchitosan adsorption.  相似文献   

9.
In this work we present the results of extensive characterization and optimization of the Ambient Ion Monitor-Ion Chromatograph (AIM-IC) system, an instrument developed by URG Corp. and Dionex Inc. for simultaneous hourly measurements of the water-soluble chemical composition of atmospheric fine particulate matter (PM(2.5)) and associated precursor gases. The sampling assembly of the AIM-IC consists of an inertial particle size-selection assembly, a parallel-plate wet denuder (PPWD) for the collection of soluble gases, and a particle supersaturation chamber (PSSC) for collection of particles, in series. The analytical assembly of the AIM-IC consists of anion and cation IC units. The system detection limits were determined to be 41 ppt, 5 ppt, and 65 ppt for gas phase NH(3(g)), SO(2(g)), and HNO(3(g)) and 29 ng m(-3), 3 ng m(-3), and 45 ng m(-3) for particle phase NH(4)(+), SO(4)(2-), and NO(3)(-) respectively. From external trace gas calibrations with permeation sources, we determined that the AIM-IC is biased low for NH(3(g)) (11%), SO(2(g)) (19%), and HNO(3(g)) (12%). The collection efficiency of SO(2(g)) was found to strongly depend on the composition of the denuder solution and was found to be the most quantitative with 5 mM H(2)O(2) solution for mixing ratios as high as 107 ppb. Using a cellulose membrane in the PPWD, the system responded to changes in SO(2(g)) and HNO(3(g)) within an hour, however for NH(3(g)), the timescale can be closer to 20 h. With a nylon membrane, the instrument response time for NH(3(g)) was significantly improved, becoming comparable to the responses for SO(2(g)) and HNO(3(g)). Performance of the AIM-IC for collection and analysis of PM(2.5) was evaluated by generating known number concentrations of ammonium sulfate and ammonium nitrate particles (with an aerodynamic diameter of 300 nm) under laboratory conditions and by comparing AIM-IC measurements to measurements from a collocated Aerosol Mass Spectrometer (AMS) during a field-sampling campaign. On average, the AIM-IC and AMS measurements agreed well and captured rapid ambient concentration changes at the same time. In this work we also present a novel inlet configuration and plumbing for the AIM-IC which minimizes sampling inlet losses, reduces peak smearing due to sample carryover, and allows for tower-height sampling from the base of a research tower.  相似文献   

10.
三重四极杆质谱技术测定固体废弃物中多氯联苯   总被引:1,自引:0,他引:1  
以二氯甲烷为萃取剂,采用快速溶剂萃取、凝胶渗透色谱净化、三重四极杆质谱技术测定固体废弃物中7种多氯联苯单体,选择十氯联苯为内标物,2,4,5,6-四氯间二甲苯为替代物。质谱采用MRM扫描,优化了目标物质保留时间、母离子和子离子质量数及碰撞能量等参数。方法在0.050 mg/L~2.00 mg/L范围内线性良好,7种多氯联苯单体的检出限为0.194 ng/g~0.355 ng/g(以称取30 g样品、定容至2.0 mL计),标准样品回收率多在60%~105%之间,空白加标样品测定值的相对标准偏差在8.6%~13.0%之间。  相似文献   

11.
The development of easy-to-use and rapid-monitoring immunoassay methods for organic environmental pollutants in a class-selective manner is a topic of considerable environmental interest. In this work, a heterologous competitive indirect enzyme-linked immunosorbent assay (ciELISA) based on a monoclonal antibody (MAb) with broad-specificity for organophosphorus pesticides (OPs) was applied to the detection of O,O-diethyl and O,O-dimethyl OPs in water samples. The ciELISA conditions were carefully optimized to obtain a three to five-fold improvement of sensitivity for most OPs, and thirteen OPs were determined at concentrations ranging from 0.017 to 30 ng mL(-1). The determination of spiked environmental water samples showed average recoveries from 81.5% to 115.1%, with the coefficient of variation (CV) ranging from 6.1% to 20.9%, which showed satisfactory reproducibility of the developed ciELISA. To overcome the negative aspect of broad-specificity immunoassays not providing qualitative and quantitative analysis of individual OPs in blind samples, we used "percent inhibition rate" to make the developed ciELISA a semi-quantitative method, which allows the monitoring of positive samples from hundreds of negative samples. The determination of OPs in blind water samples by the developed ELISA with confirmation by HPLC-MS/MS analysis demonstrated that the assay is ideally suited as a screening method for OP residues prior to chromatographic analysis.  相似文献   

12.
This paper presents the results of the determination of arsenic, antimony and selenium concentrations of inorganic speciation in surface water samples from Gniezno city (western Poland) and its neighborhood. The concentration of elements were up to 1.85 ng/ml for arsenic, 1.61 ng/ml for antimony and 0.45 ng/ml for selenium (detection limits: 0.04 ng/ml for As and Sb and 0.03 ng/ml for Se). A variety of concentrations for the determined elements has been obtained in waters from Gniezno city’s neighborhood and in water from down-town reservoirs which are under strong anthropogenic pressure.  相似文献   

13.
The in vitro estrogen receptor (ER) agonist potency and C1 to C9 alkyl substituted phenol content of offshore produced water effluents collected from the UK sector of the North Sea were determined using a combination of bio-analytical and chemical analysis techniques. An in vitro reporter gene assay was used to determine ER agonist potency, whilst gas chromatography coupled to mass spectrometry (GC-MS) was used to quantify the concentration of alkylphenols. The in vitro ER agonist potency was highly variable and ranged from less than the limit of detection (theoretically 0.03 ng 17beta-estradiol (E2) l(-1)) to 91 ng E2 l(-1). C1 to C5 alkylphenol concentrations were also highly variable ranging from 5 to 1600 microg l(-1) with a median concentration of 206 microg l(-1). These data reflect the highly variable composition of produced water discharges from different fields. The observed poor correlation of the alkylphenol isomer content and ER agonist activity suggests that other compounds present in the produced water discharges may be responsible for the ER agonist activity observed. It is recommended that further work be performed to characterise the full range of ER agonists present in offshore produced water discharges.  相似文献   

14.
Diffusive sampling of a mixture of 42 volatile organic compounds (VOCs) in humidified, purified air onto the solid adsorbent Carbopack X was evaluated under controlled laboratory conditions. The evaluation included variations in sample air temperature, relative humidity and ozone concentration. Linearity of samples with loading was examined both for a constant concentration with time varied up to 24 h and for different concentrations over 24 h. Reverse diffusion and its increase with accumulation of sample were determined for all compounds. Tubes were examined for blank levels, change of blanks with storage time, and variability of blanks. Method detection limits were determined based on seven replicate samples. Based on this evaluation, 27 VOCs were selected for quantitative monitoring in the concentration range from approximately 0.1 to 4 ppbv. Comparison results of active and diffusive samples taken over 24 h and under the same simulated ambient conditions at a constant 2 ppbv were interpreted to estimate the effective diffusive sampling rates (ml min(-1)) and their uncertainties and to calculate the corresponding diffusive uptake rates (ng ppmv(-1) min(-1)).  相似文献   

15.
A simple, sensitive and selective method by solvent extraction-first derivative spectrophotometry is described for the determination of microamounts of copper in water by means of its reaction and extraction at pH 8.0 with 3-(4-phenyl-2-pyridinyl-5-phenyl-1,2,4-triazine) (PPT) and picrate (2,4,6-trinitro-phenol) into 1,2-dichloroethane. Copper was thus determined in the range 7.5–350 ng/ml with a detection limits (3) of 2.3 ng/ml. The relative standard deviations were in all instances less than 2.0%. The proposed method was successfully applied for the determination of copper in several kinds of water.  相似文献   

16.
An atmospheric deposition sampler was validated with respect to polybrominated diphenyl ethers (PBDEs), a compound group that is widely used as flame retardants in many types of consumer products. The deposition sampler consists of an adsorption cartridge that is connected to a glass funnel. Extraction tests with spiked cartridges using soxhlet extraction with acetone revealed recoveries of >80% for all of the investigated PBDEs. Once adsorbed, PBDEs are stable, as proven by extractions of spiked cartridges that were stored outdoors and collected after different periods of time, up to 84 days. High recoveries indicate that degradation of adsorbed PBDEs does not play a role under realistic field conditions. Bulk deposition rates of PBDEs were determined in a field test with 3 replicates, and a possible breakthrough of target compounds was assessed in the field using a second adsorption cartridge in series. No breakthrough of target compounds could be observed within a sampling period of 61 days, and a bulk deposition rate of approximately 1 ng m(-2) day(-1) for the sum of all analysed PBDEs was measured. The highest deposition rates were measured for octa-brominated congeners, followed by BDEs 99, 183, 153, and 47. Overall, the sampler was successfully validated regarding the atmospheric deposition of PBDEs.  相似文献   

17.
One hundred and fourteen surface sediments were collected from the Maozhou River Watershed in Shenzhen, China from December 2009 to January 2010. Three individual chlorinated polycyclic aromatic hydrocarbons (ClPAHs), six individual brominated polycyclic aromatic hydrocarbons (BrPAHs), and five corresponding parent polycyclic aromatic hydrocarbons (PAHs) were determined. The concentration of 9-chlorophenanthrene was the highest ranging from 0.51-289 ng g(-1) (average, 16.5 ng g(-1)). For BrPAHs, the concentration of 2-bromofluorene was the highest ranging from 0.31-266 ng g(-1) (average, 35.3 ng g(-1)). No correlation was observed between the concentrations of ClPAHs and parent PAHs in surface sediments. In addition, there was no correlation between 1-bromopyrene, 7-bromobenz(a)anthracene and 9,10-dibromoanthracene, and corresponding parent PAHs. However, a significant correlation was found between 9-bromophenanthrene and phenanthrene (p < 0.01), between 9-bromoanthracene and anthracene (p < 0.05), and between 2-bromofluorene and fluorene (p < 0.05). Six fly ash samples collected from one of the municipal domestic waste incineration plants in Shenzhen were also analyzed for source identification. The concentration of 7-bromobenz(a)anthracene was the highest, ranging from 3.21-4.08 ng g(-1). In addition, 2-bromofluorene was not detected in all the fly ash samples. No correlation was found between the concentrations of Cl-/BrPAHs and corresponding parent PAHs in fly ashes. We also examined the relationship between the levels of Cl-/BrPAHs in surface sediments and the urbanization process. Our results suggested the levels of individual Cl-/BrPAHs congeners presented a similar increasing trend with the increasing urbanization level.  相似文献   

18.
A four-step chemical sequential extraction procedure was used to evaluate the distribution of Al, As, Cr, Cu, Fe, Mn, Ni, Pb, Ti, V and Zn in airborne particulate matter collected on glass fibre filters using a high-volume sampler. Two sets of samples were collected in 2001 (winter and summer campaigns) in representative zones of an industrial city of Argentina. The leaching scheme was applied to PM-10 particles and consisted in extracting the elements in four fractions, namely soluble and exchangeable elements; carbonates, oxides and reducible elements; bound to organic matter and sulfidic metals; and residual elements. Metals and metalloids at microg g(-1) level were determined in each fraction by inductively coupled plasma optical emission spectrometry (ICP OES). Analyte concentration varied from 14 microg g(-1) (equivalent to 1.0 ng m(-3)) for As to 11.8 mg g(-1) (equivalent to 2,089 ng m(-3)) for Al. Seven elements, namely Al, Cr, Fe, Mn, Pb, Ti and Zn showed similar distributions in both seasons while As was distributed in a significantly different manner in each season. The results exhibited low As contents in the first and second fractions that could be associated with routine coal combustion and a high content in the third and fourth fractions of the summer samples that could be linked to the use of pesticides. Aluminium, As, Cu, Mn, Ni, Ti, V and Zn were found in different percentages in the more bioavailable aqueous fraction with As, Mn, V and Zn exhibiting solubilities greater than 1% while Cr and Pb being insoluble. The content of Al, Cr, Cu, Fe, Ni, Pb, and Zn in the residual fraction was, in average, higher than 50%. A comparative assessment of the use of the underlying information available from fractionation studies compared to that obtained from total element content was done for Fe and Mn. It showed that the results obtained using chemical sequential extraction procedures allowed further discrimination of the potential air pollution sources.  相似文献   

19.
Capillary microextractor (CME) in combination with a gas chromatograph-mass spectrometer (GC-MS) was employed for the determination of trace priority hazardous substances in water. Three groups of semivolatile organic compounds (SVOCs), i.e., chlorinated hydrocarbons, pesticides and polycyclic aromatic hydrocarbons (PAHs), were simultaneously determined. SVOCs were extracted from 7 mL of water samples on a 100 cm commercial gas chromatographic column (0.32 mm id x film thickness 0.25 microm, HP-5 capillary column) and eluted with only 3 microL of acetonitrile. The extractant was analyzed by GC-MS in the selected ion monitoring mode. The method showed good linearity over the concentration range 10 ng L(-1) to 3.0 mg L(-1) with correlation coefficients (r) greater than 0.99 and low limits of detection ranged from 10 ng L(-1) to 1.0 mg L(-1). High recovery (more than 80%) was obtained with relative standard deviation less than 10%. The method was successfully applied for trace level analyses of SVOCs in water samples.  相似文献   

20.
Total suspended particulates (TSP) were collected with a high volume sampler from the indoor work environment of 23 industries in Al-Rusayl Industrial Estate in Muscat, Oman. The values measured ranged from 39 microg m(-3) to 1033 microg m(-3). TSP in the ambient air of the area was found to have an average value of 1802 microg m(-3). TSP were analyzed for Pb, Cu, Ni, Zn and Cr. Compared to other metals, Pb emission was high with values ranging from 3 to 15 109 ng m(-3) with the mean value being 1 293 ng m(-3); Cu concentration varied from 3 to 2600 ng m(-3) with a mean value of 131 ng m(-3); Ni concentration ranged from 6 to 46 ng m(-3) with a mean value of 17 ng m(-3); Cr concentration ranged from 1 to 133 ng m(-3) with a mean value of 23 ng m(-3) while that of Zn varied from 0.01 to 1 978 ng m(-3) with the mean value being 464 ng m(-3). The concentrations of Pb, Ni, Cu, Cr, and Zn in the ambient air were also measured and found to have the following values: 122, 18, 16, 5 and 0.01 ng m(-3), respectively. These values indicate that the industries in the area do not contribute significantly to heavy metal air pollution.  相似文献   

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