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1.
An optimized procedure based on gas chromatography-mass spectrometry (GC-MS) combined with accelerated solvent extraction (ASE) is developed for the analysis of six phthalic acid esters (PAEs), which are priority soil pollutants nominated by United States Environmental Protection Agency (USEPA). Quantification of PAEs in soil employs ultrasonic extraction (UE) (USEPA 3550) and ASE (USEPA 3545), followed by clean up procedures involving three different chromatography columns and two combined elution methods. GC-MS conditions under selected ion monitoring (SIM) mode are described and quality assurance and quality control (QA/QC) criteria with high accuracy and sensitivity for target analytes were achieved. Method reliability is assured with the use of an isotopically labeled PAE, di-n-butyl phthalate-d4 (DnBP-D4), as a surrogate, and benzyl benzoate (BB) as an internal standard, and with the analysis of certified reference materials (CRM). QA/QC for the developed procedure was tested in four PAE-spiked soils and one PAE-contaminated soil. The four spiked soils were originated from typical Chinese agricultural fields and the contaminated soil was obtained from an electronic waste dismantling area. Instrument detection limits (IDLs) for the six PAEs ranged 0.10–0.31 μg·L-1 and method detection limits (MDLs) of the four spiked soils varied from a range of 20–70 μg·kg-1 to a range of 90– 290 μg·kg-1. Linearity of response between 20 μg·L-1 and 2 mg·L-1 was also established and the correlation coefficients (R) were all>0.998. Spiked soil matrix showed relative recovery rates between 75 and 120% for the six target compounds and about 93% for the surrogate substance. The developed procedure is anticipated to be highly applicable for field surveys of soil PAE pollution in China.  相似文献   

2.
The residues of tetracycline antibiotics in water have attracted many concerns due to their harmful impact to human health. This paper reports an electrochemical sensor for the determination of tetracycline (TC) by the microelectrode, which was fabricated by electrodeposited gold colloids on tungsten tip. Cyclic voltammerty was used to study the electrochemical behavior of TC on the microelectrode. Well anodic wave was obtained at about 1.5 V in acidic solutions. Electrochemical determination of tetracycline was investigated using microelectrode by cyclic voltammetry. Under optimized conditions, the calibration curves for TC were obtained. The oxidation peak currents were linearly related to TC concentrations in the range of 1–10 mg·L-1 and 10–100 mg·L-1, respectively. The detection limit was 0.09 mg·L-1 (S/N = 3).  相似文献   

3.
本文使用岛津ICPMS-2030电感耦合等离子体质谱仪,采用微波消解法对锰结核样品进行前处理,测定了锰结核样品中32种元素含量.实验结果表明,各元素在1.0—100μg·L-1范围内线性关系良好,相关系数均大于0.9998,检出限低,各元素检出限都在0.00004—0.73μg·g-1之间.该方法操作简便、快速,测试结果准确,使用锰结核标准物质GBW07296进行验证,测定值与标准值基本吻合,该方法可适用于锰结核样品中多元素含量的测定.  相似文献   

4.
以乙二胺和抗坏血酸为原料,通过一步水热法制备了水溶性的氮掺杂碳量子点(N-CQDs).研究了N-CQDs的形貌特征、光学性能和应用分析.表征结果说明,N-CQDs形态为均匀分散的球形,有明显的晶格条纹,抗光漂白性能良好,表面富有含氧官能团,具有良好的水溶性.此外发现N-CQDs还具有优良的荧光性能和荧光稳定性,量子产率可以高达12.29%.分析得出,Hg2+对N-CQDs在1.0—120μmol·L-1范围内有一定的猝灭效应,可作为Hg2+的荧光探针,检出限达230 nmol·L-1.  相似文献   

5.
When bromide/iodide is present in source water, hypobromous acid/hypoiodous acid will be formed with addition of chlorine, chloramine, or other disinfectants. Hypobromous acid/hypoiodous acid undergoes reactions with natural organic matter in source water to form numerous brominated/iodinated disinfection byproducts (DBPs). In this study, tap water samples were collected from eight cities in China. With the aid of electrospray ionization-triple quadrupole mass spectrometry by setting precursor ion scans of m/z 35, m/z 81, and m/z 126.9, whole pictures of polar chlorinated, brominated, and iodinated DBPs in the tap water samples were revealed for the first time. Numerous polar halogenated DBPs were detected, including haloacetic acids, newly identified halogenated phenols, and many new/unknown halogenated compounds. Total organic chlorine, total organic bromine, and total organic iodine were also measured to indicate the total levels of all chlorinated, brominated, and iodinated DBPs in the tap water samples. The total organic chlorine concentrations ranged from 26.8 to 194.0 μg·L–1 as Cl, with an average of 109.2 μg·L–1 as Cl; the total organic bromine concentrations ranged from below detection limit to 113.3 μg·L–1 as Br, with an average of 34.7 μg·L–1 as Br; the total organic iodine concentrations ranged from below detection limit to 16.4 μg·L–1 as I, with an average of 9.1 μg·L–1 as I; the total organic halogen concentrations ranged from 31.3 to 220.4 μg·L–1 as Cl, with an average of 127.2 μg·L–1 as Cl.  相似文献   

6.
The purpose of this study was to give a worldwide overview of the concentrations of typical estrogenic endocrine disrupting chemicals (EDCs) in the effluent of sewage plants and then compare the concentra- tion distribution of the estrogenic EDCs in ten countries based on the survey data of the estrogenic EDCs research. The concentrations of three main categories (totally eight kinds) of estrogenic EDCs including steroidal estrogens (estrone (El), estradiol (E2), estriol (E3) and 17a- ethynylestradiol (EE2)), phenolic compounds (nonylphe- nol (NP) and bisphenol A (BPA)) and phthalate esters (dibutyl phthalate (DBP) and dibutyl phthalate (2- ethylhexyl) phthalate (DEHP)) in the effluents of sewage plants reported in major international journals over the past decade were collected. The statistics showed that the concentration distributions of eight kinds of EDCs were in the range of ng·L^-1 to μg·L^-1. The concentrations of steroidal estrogens mainly ranged within 50.00 ng. L-1, and the median concentrations of El, E2, E3 and EE2 were 11.00, 3.68, 4.90 and 1.00 ng·L^-1, respectively. Phenolic compounds and phthalate esters were found at pg. L-1 level (some individual values were at the high level of 40.00 μg·L^-1). The median concentrations of BPA, NP, DBP and DEHP were 0.06, 0.55, 0.07 and 0.88 μg·L^-1, respectively. The concentrations of phenolic compounds and phthalate esters in the effluents were higher than that of steroids estrogens. The analysis of the concentration in various ten countries showed that steroids estrogens, phenolic compounds and phthalate esters in sewage plant effluents were detected with high concentration in Canada, Spain and China, respectively.  相似文献   

7.
The objective of this study is to investigate the occurrence of haloacetic acids (HAAs), a group of disinfection byproducts, in swimming pool and spa water. The samples were collected from six indoor pools, six outdoor pools and three spas in Pennsylvania, the United States, and from five outdoor pools and nine indoor pools in Beijing, China. Five HAAs (HAA5), including monochloroacetic acid, dichloroacetic acid, trichloroacetic acid, monobromoacetic acid, and dibromoacetic acid were analyzed. Total chlorine, pH and total organic carbon concentration were analyzed as well. Results indicated that the levels of HAA5 in swimming pools and spas in the United States ranged from 70 to 3980μg·L^-1, with an arithmetic average at 1440μg·L^-1 and a median level at 1150μg·L^-1. These levels are much higher than the levels reported in chlorinated drinking water and are likely due to organic matters released from swimmers' bodies. The levels of HAA5 in swimming pools in China ranged from 13 to 332μg·L^-1, with an arithmetic average at 117μg·L^-1 and a median level at 114μg·L^-1. The lower HAA levels in swimming pools in China were due to the lower chlorine residuals. Results from this study can help water professionals to better understand the formation and stability of HAAs in chlorinated water and assess risks associated with exposures to HAAs in swimming pools and spas.  相似文献   

8.
The efficient removal of phosphorous from water is an important but challenging task. In this study, we validated the applicability of a new commercially available nanocomposite adsorbent, i.e., a polymer-based hydrated ferric oxide nanocomposite (HFO-201), for the further removal of phosphorous from the bioeffluent discharged from a municipal wastewater treatment plant, and the operating parameters such as the flow rate, temperature and composition of the regenerants were optimized. Laboratory-scale results indicate that phosphorous in real bioeffluent can be effectively removed from 0.92 mg·L-1 to<0.5 mg·L-1 (or even<0.1 mg·L-1 as desired) by the new adsorbent at a flow rate of 50 bed volume (BV) per hour and treatable volume of 3500–4000 BV per run. Phosphorous removal is independent of the ambient temperature in the range of 15°C–40°C. Moreover, the exhausted HFO-201 can be regenerated by a 2% NaOH+ 5% NaCl binary solution for repeated use without significant capacity loss. A scaled-up study further indicated that even though the initial total phosphorus (TP) was as high as 2 mg·L-1, it could be reduced to<0.5 mg·L-1, with a working capacity of 4.4–4.8 g·L-1 HFO-201. In general, HFO-201 adsorption is a choice method for the efficient removal of phosphate from biotreated waste effluent.  相似文献   

9.
The adsorption of direct fast black onto acid-thermal modified sepiolite was investigated. Batch adsorption experiments were performed to evaluate the influences of experimental parameters such as initial dye concentration, initial solution pH and adsorbent dosage on the adsorption process. The three-factor and three-level Box-Behnken response surface methodology (RSM) was utilized for modeling and optimization of the adsorption conditions for direct fast black onto the acid-thermal modified sepiolite. The raw sepiolite was converted to acid-thermal modified sepiolite, and changes in the fourier transform infrared spectrum (FTIR) adsorption bands of the sample were noted at 3435 cm-1 and 1427 cm-1. The zeolitic water disappeared and the purity of sepiolite was improved by acid-thermal modification. The decolorization rate of direct fast black adsorbed increased from 68.2% to 98.9% on acid-thermal modified sepiolite as the initial solution pH decreased from 10 to 2. When the adsorbent dosage reached to 2.5 g·L-1, 2.0 g·L-1, 1.5 g·L-1 and 1.0 g·L-1, the decolorization rate was 90.3%, 86.7%, 61.0% and 29.8%, respectively. When initial dye concentration increased from 25 to 200 mg·L-1, the decolorization rate decreased from 91.9% to 60.0%. The RSM results showed that the interaction between adsorbent dosage and pH to be a significant factor. The optimum conditions were as follows: the adsorbent dosage 1.99 g·L-1, pH 4.22, and reaction time 5.2 h. Under these conditions, the decolorization rate was 95.1%. The three dimensional fluorescence spectra of direct fast black before and after treatment showed that the direct fast black was almost all adsorbed by the acid-thermal modified sepiolite.  相似文献   

10.
建立了食品工业废水中8种合成色素残留的固相萃取-液相色谱测定方法.水样经固相萃取柱富集,氮吹浓缩定容后直接进样.采用C18色谱柱分离,以甲醇-乙酸铵(0.01mol·L-1)溶液为流动相,进行梯度洗脱,最后利用二极管阵列检测器(DAD)进行可变波长分析,外标法定量.结果表明,8种合成色素在1.0—50mg·L-1的浓度范围内线性良好,相关系数均大于0.999,定量限为1.6—2.4μg·L-1.以实际废水样品为加标对象,分别考察了低、中、高三个浓度水平的加标回收率和精密度,平均加标回收率在82.3%—95.9%之间,精密度均小于5.45%.该方法准确可靠,灵敏度高,可用于食品工业废水中痕量色素残留的测定.  相似文献   

11.
通过优化固相萃取条件和高效液相色谱-串联质谱参数,建立了可以同时检测地表水和地下水中26种典型药物及个人护理品(pharmaceuticals and personal care products,PPCPs),包括磺胺类、大环内酯类、喹诺酮类、酰胺醇类、精神类、消炎止痛类以及个人护理品的检测方法.通过将水样pH值调节至7,利用HLB固相萃取柱对水样中PPCPs进行富集,以甲醇和含0.005%甲酸的水溶液作为正离子模式流动相,甲醇和含0.5 mmol·L-1乙酸铵的水溶液作为负离子模式流动相进行梯度洗脱,采用多反应监测的质谱扫描模式(MRM)分析测定.26种PPCPs的检出限为0.007—1.78 ng·L-1,定量限为0.02—5.68 ng·L-1,回收率为52.28%—115.24%.利用该方法检测北京潮白河地表水和地下水中PPCPs的浓度,结果表明,地表水中PPCPs的含量普遍高于地下水,磺胺甲恶唑、舒必利、咖啡因、卡马西平和布洛芬在地表水和地下水中的含量相对较高,检测浓度分别高达147.83、52.48、78.35、166.58、30.63 ng·L-1.  相似文献   

12.
Effluents from wastewater treatment plant (WWTP) have been reported to have a broad spectrum of endocrine disrupting compounds (EDCs). The majority of studies have focused on the occurrence of estrogenic activity, while ignoring nuclear hormone receptors (NRs) pathways. In the present study, a battery of in vitro yeast bioassays and a cell bioassay, including antagonistic and agonistic effects on estrogen receptor (ER), androgen receptor (AR), progesterone receptor (PR), estrogen- related receptor (ERR) and aryl hydrocarbon receptor (AHR), were conducted to evaluate the removal efficien- cies of EDCs by different treatment processes of a WWTP located in Beijing. Estrogenic, anti-estrogenic, anti- androgenic, anti-progesteronic, anti-ERR and the activa- tion of AHR activities were detected in samples from all treatment processes and the receiving water. The concen- tration of estrogenic contaminants with estradiol (E2) equivalent concentrations ranged from 0.82 x 10-9 to 3.54 x 10 9g Ee_EQ.L-1. The concentration of anti-estrogenic contaminants with 4-hydroxytamoxifen (4-OHT) equiva- lent concentrations ranged from 1.24 × 10-6 to 2.36 x 10-6 g 4-OHT-EQ.L-1. The concentration of anti-androgenic contaminants ranged from 2.21 x 10-s to 3.52 × 10-6g flutamide-EQ. L-1. The concentration of anti-progesteronic contaminants ranged from 3.15 x 10^-5 to 2.71 x 10^-4g RU486-EQ. L-1. The concentration of anti-ERR contami- nants ranged from 7.09 x 10-5 to 6.50 x 104 g 4-OHT-EQ × L^-10. The concentration of AHR activators ranged from 1.7 × 10-10 to 3.4 × 10^-10g TCDD-EQ-L-1. These processes including secondary clarifier, coagulation, as well as coal and sand filtration could eliminated 67.2% of estrogenic contaminants, 47.0% of anti-estrogenic contaminants, 98.3% of anti-androgenic contaminants, 88.4% of anti- progesteronic contaminants, 65.4% of anti-ERR contami- nants and 46.9% of AHR activators. WWTP effluents contain multiple receptor disruptors may have very complex adverse effects on exposed organisms.  相似文献   

13.
Polycyclic musks are widely used for cosmetics and other personal care and household cleaning products. The occurrence and removal of two representative polycyclic musks, galaxolide (HHCB) and tonalide (AHTN) were investigated in three different processes of two sewage treatment plants (STPs) in Xi’an, China. The samples were preconcentrated by solid phase extraction procedure and analyzed using a gas chromatography mass spectrometry (GC/MS) by a modified procedure. The HHCB was in the range of 82.8 to 182.5 ng·L-1 in the influents and 22.6 to 103.9 ng·L-1 in the effluents. The AHTN ranged from 11.0 to 19.3 ng·L-1 in the influents and 2.2 to 8.8 ng·L-1 in the effluents. The removal efficiency of the two musks varied in the ranges of 43.1%–70.4% for HHCB and 54.2%–84.4% for AHTN. Concentrations of the two musks in aqueous phase of three processes slightly increased along the primary process, and significantly removed during the biologic treatment processes, revealing that the selected musks could be remarkably removed in varied activated sludge processes. Advanced processes of activated sludge did not show a significant superiority on selected musk removal compared to the conventional process. The selected musk removal mainly resulted from the adsorption function of activated sludge. There was no significant change of HHCB/AHTN ratios along the treatment flow, indicating that each sewage treatment structure had a similar removal efficiency for the two musks.  相似文献   

14.
A disposable biosensor was fabricated using single-walled carbon nanotubes, gold nanoparticles and tyrosinase (SWCNTs-AuNPs-Tyr) modified screen-printed electrodes. The prepared biosensor was applied to the rapid determination of phenolic contaminants within 15 minutes. The SWCNTs-AuNPs-Tyr bionanocomposite sensing layer was characterized with scanning electron microscopy, electrochemical impedance spectroscopy and cyclic voltammetry methods. The characterization results revealed that SWCNTs could lead to a high loading of tyrosinase (Tyr) with the large surface area and the porous morphology, while AuNPs could retain the bioactivity of Tyr and enhance the sensitivity. The detection conditions, including working potential, pH of supporting electrolyte and the amount of Tyr were optimumed. As an example, the biosensor for catechol determination displayed a linear range of 8.0 × 10-8 to 2.0 × 10-5 mol·L-1 with a detection limit of 4.5 × 10-8 mol·L-1 (S/N = 3). This method has a rapid response time within 10 s, and shows excellent repeatability and stability. Moreover, the resulting biosensor could be disposable, low-cost, reliable and easy to carry. This kind of new Tyr biosensor provides great potential for rapid, on-site and cost-effective analysis of phenolic contaminants in environmental water samples.  相似文献   

15.
建立了超高效液相色谱-串联质谱(UPLC-MS;MS)快速测定蔬菜中18种农药残留的方法.样品经乙腈提取后,经Oasis PRiME HLB固相萃取柱净化,采用ACQUITY UPLC HSS T3 C18(50 mm×2.1 mm,1.8μm)色谱柱进行分离,以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱.采用电喷雾电离源、正离子模式下以多反应监测(MRM)进行定性和定量分析.结果表明,18种农药在0.5—50μg·L-1范围内线性关系良好(r2>0.995),方法最低检出限为0.4—1.5μg·kg-1,最低定量限为1.4—5.0μg·kg-1.在韭菜、芹菜、番茄、白菜基质中,5、10、50μg·kg-1添加水平下的加标回收率为60.2%—126.9%,相对标准偏差(RSD)为0.4%—21.6%(n=3).  相似文献   

16.
Metabolites of algae such as geosmin, 2-methylisoborneol etc. are reported to induce pungent odors into drinking water and attract additional scientific attention. Recently, in China, taste and odor outbreaks in drinking water supply have become increasingly common. In source water affected by eutrophication, dimethyl trisulfide, speculated to be produced by decayed algae, was found to be the source of taste and odor issues and can be removed effectively by usual oxidation agents. In this experimental study, batch scale tests were carried out focusing on the removal of dimethyl trisulfide. Reaction kinetics of dimethyl trisulfide oxidized by potassium permanganate in water had been studied; influence factors such as pH, organic substrate, other existed taste, and odor contaminant in equivalent concentration were also discussed. Results showed that dimethyl trisulfide can be removed by potassium permanganate efficiently; the ratio can reach more than 70% with oxidant dosage of 4 mg·L-1 and contact time prolonged to 120 min. The dimethyl trisulfide decomposition followed a second-order kinetics pattern with a rate constant k = 0.00213 L·(min·mg)-1. Typically, the degradation rate of dimethyl trisulfide was increased with the increasing KMnO4 dosage, but dramatically dropped with the increasing levels of humic acid (1.8–4.5 mg·L-1) and other odor-causing compounds (e.g. β-cyclocitral, 0–1886.0 μg·L-1). Solution pH (5.2–9.0) and initial dimethyl trisulfide concentration did not significantly affected the degradation. This study demonstrates that KMnO4 oxidation is an effective option to remove dimethyl trisulfide from water.  相似文献   

17.
新型溴系阻燃剂(NBFRs,novel brominated flame retardants)作为传统溴系阻燃剂的替代品已广泛应用于电子产品、纺织品、家具等商品中,随着这些商品的生产、使用和处置,NBFRs不可避免地释放到环境中,给环境和人体带来潜在的危害.部分NBFRs可通过摄食和呼吸作用进入人体对人体产生一定危害...  相似文献   

18.
To fulfill the requirements of Guidelines for approval of ballast water management system (G8), a set of onshore ballast water treatment equipment utilizing micro-pore ceramic filtration (MPCF) and UV radiation (MPCF&UV) system was designed and set up with a maximum flow rate of 80 m3·h-1. Technical feasibilities of MPCF&UV system were evaluated in three areas: removal efficiencies of indicator organism and oceanic bacteria, perdurability of a ceramic filter, and application on native seawater. The results showed that no indicator organism (Dunaliella) or oceanic bacteria was detected after treatment of 20 L MPCF and UV radiation at 1.3× 104 μW·s·cm-2. A 20 L ceramic filter can run continuously for 5.3 h at the flow rate of 15 m3·h-1 before its pressure drop up to 0.195 MPa. The removal percentage of total plankton amounts were 91.9% at a flow rate of 70 m3·h-1 by 80 L MPCF and UV radiation at 1.3× 104 μW·s·cm-2.  相似文献   

19.
Optimization of an integrated anaerobic-aerobic bioreactor (IAAB) treatment system for the reduction of organic matter (Chemical Oxygen Demand (COD), Biochemical Oxygen Demand (BOD) and Total Suspended Solids (TSS) concentrations) in Palm Oil Mill Effluent (POME) to legal standards with high methane yield was performed for the first time under thermophilic condition (50°C–55°C) by using response surface methodology (RSM). The experiments were conducted based on a central composite rotatable design (CCRD) with three independent operating variables, organic loading rates in anaerobic compartment (OLRan) and mixed liquor volatile suspended solids (MLVSS) concentration in anaerobic (MLVSSan) and aerobic compartments (MLVSSa). The optimum conditions for the POME treatment were determined as OLRan of 15.6 g COD·L-1·d-1, MLVSSan of 43100 mg·L-1, and MLVSSa of 18600 mg·L-1, where high aerobic COD, BOD and TSS removal efficiencies of 96.3%, 97.9%, and 98.5% were achieved with treated BOD of 56 mg·L-1 and TSS of 28 mg·L-1 meeting the discharge standard. This optimization study successfully achieved a reduction of 42% in the BOD concentrations of the final treated effluent at a 48% higher OLRan as compared to the previous works. Besides, thermophilic IAAB system scores better feasibility and higher effectiveness as compared to the optimized mesophilic system. This is due to its higher ability to handle high OLR with higher overall treatment efficiencies (more than 99.6%), methane yield (0.31 L CH4·g-1 CODremoved) and purity of methane (67.5%). Hence, these advantages ascertain the applicability of thermophilic IAAB in the POME treatment or even in other high-strength wastewaters treatment.  相似文献   

20.
Forward osmotic membrane bioreactor is an emerging technology that combines the advantages of forward osmosis and conventional membrane bioreactor. In this paper, bisphenol A removal by using a forward osmotic membrane bioreactor and a conventional membrane bioreactor that shared one biologic reactor was studied. The total removal rate of bisphenol A by the conventional membrane bioreactor and forward osmotic membrane bioreactor was as high as 93.9% and 98%, respectively. Biodegradation plays a dominant role in the total removal of bisphenol A in both processes. In comparison of membrane rejection, the forward osmosis membrane can remove approximately 70% bisphenol A from the feed, much higher than that of the microfiltration membrane (below 10%). Forward osmosis membrane bioreactor should be operated with its BPA loading rate under 0.08 mg·g-1·d-1 to guarantee the effluent bisphenol A concentration less than10 μg·L-1.  相似文献   

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