搅拌棒萃取-热脱附/气质联用法测定水中2-MIB和土臭素

采用搅拌棒萃取-热脱附/气质联用法测定水中2-甲基异莰醇和土臭素，优化了搅拌棒萃取和热脱附进样的条件。试验表明：两种目标化合物在1．00 ng/L～200 ng/L范围内线性良好，2-甲基异莰醇的相关系数为0．9993，土臭素的相关系数为0．9997，方法检出限分别为0．31 ng/L和0．15 ng/L；空白和实际样品的加标回收率为82．4％～116％，测定结果的RSD＜10％。     

太湖东岸饮用水主要异味物质年变化规律及来源分析

于2015年对苏州市太湖东岸饮用水主要异味物质进行了调查。结果表明,主要异味物质为土臭素、2-甲基异莰醇、β-环柠檬醛、β-紫罗兰酮等,检出率分别50.0%,66.7%,70.8%和66.7%,其中2-甲基异莰醇年均值是其嗅觉阈值的2.31倍,其他异味物质年均值未超过其阈值,水体主要表现为土霉味。异味问题爆发时间为夏季(5—9月),土臭素、2-甲基异莰醇、β-环柠檬醛、β-紫罗兰酮检出最高值分别为13.8,170,170和29.6 ng/L。分析了异味物质与环境因子的相关性,初步推断太湖主要异味物质为水中蓝藻的某些种类所致。     

HS/SPME-GC/MS/MS法测定水中痕量2-甲基异莰醇和土臭素

建立了测定水中痕量2-甲基异莰醇(2-MIB)和土臭素(GSM)的顶空固相微萃取-气相色谱/二级质谱联用法(HS/SPME-GC/MS/MS),并对HS/SPME条件进行优化。优化后的方法 2-MIB和GSM在1.00~50.0 ng/L范围内,线性良好(r≥0.999 4),RSD分别为7.36%和7.75%,方法检出限分别为0.226和0.239 ng/L,加标回收率分别为87.0%~97.0%和85.2%~112%。结果表明,所建立的方法操作简便、准确度高、重现性好、灵敏度高,无需有机溶剂,适用于水中痕量2-MIB和GSM的测定。     

吹扫捕集-气相色谱联用同时测定水中致嗅挥发性有机硫化物

建立了一种利用吹扫捕集(PT)-气相色谱(GC)/火焰光度检测器(FPD)同时测定水中16种致嗅类有机硫化物的分析方法。研究并优化了捕集阱类型、吹扫温度、吹扫时间,解吸温度以及解吸时间对PT的影响。实验表明:大部分硫醚类和硫醇类化合物分别在1~100 ng/L和3~300 ng/L范围内线性良好,线性相关系数大于0.99;相对标准偏差小于9.47%(n=6);加标回收率为81.68%~115.18%。定量下限(10倍信噪比)范围从0.19 ng/L(二乙基二硫醚)到2.67 ng/L(2-甲基-1-丙硫醇)。采用此方法对北京市3条河流水样进行了检测,除1-丙基二硫醚和2-甲基-2-丙硫醇外,其他14种有机硫化物都有检出,质量浓度为1.95~1 282.35 ng/L。     

固相萃取-气质联机测定水中嗅味物质2-甲基异茨醇和土霉素

分别利用固相萃取剂XAD-2树脂和C18SEP柱富集,二氯甲烷洗脱,固相萃取装置浓缩,通过气质联机(GC/MS)测定了水中土霉化合物MIB和Geosmin。该方法重现性好,相对标准偏差5.4%~7.0%,回收率80%~92%,MIB和Geosmin检出限分别为5ng/L和2ng/L。两种固相萃取剂对MIB和Geosmin吸附效率相当,吸附效率不受嗅味物质浓度影响,但当水溶液中其它有机质增多时,C18SPE的回收率明显下降。利用该方法对不同培养时间的放线菌代谢产物进行了测定,培养25天后代谢产物MIB和Geosmin的浓度达到200ng/L和130ng/L。     

太湖水源水主要异味物质变化规律及来源初探

采用顶空固相微萃取-气相色谱/质谱联用测定技术,以太湖某饮用水源地水体中甲基异莰醇-2和土臭素为主要研究对象,通过环境因子相关性分析,对异味物质的变化规律和来源作初步分析。研究结果表明,该水源地2013年的主要异味物质为甲基异莰醇-2,超标时段主要集中在夏秋高温季节(5—9月);水体中的硅藻可能是异味物质的重要产生者,底泥中的藻类和微生物次生代谢活动可能是水体产生异味的主要原因。     

阳澄湖水源中典型嗅味物质测定与来源分析

以阳澄湖水源为研究对象,采用固相微萃取-气质联用法测定水中2-甲基异莰醇(2-MIB)、土臭素(GSM)、2,4,6-三氯苯甲醚(2,4,6-TAC)、2,3,4-三氯苯甲醚(2,3,4-TAC)、2,3,6-三氯苯甲醚(2,3,6-TAC)、2-异丙基-3甲氧基吡嗪(IPMP)、2-异丁基-3甲氧基吡嗪(IBMP)、β-环柠檬醛、β-紫罗兰酮、异氟尔酮等10种典型嗅味物质,并分析可能的来源藻类.以2018年1月-12月阳澄湖水源中优势藻种为基础,建立以上述嗅味物质为变量的多元线性回归模型.结果表明,水源中2-MIB、GSM、β-环柠檬醛、β-紫罗兰酮、异氟尔酮5种嗅味物质与直链藻、针杆藻、鱼腥藻、色球藻、颤藻、微囊藻、束丝藻7种藻类有较强的相关性.     

固相萃取-气相色谱质谱联用法测定地表水中藻致嗅味物质

选用HLB固相萃取小柱进行富集,用二氯甲烷进行洗脱,优化了固相萃取过程,建立了固相萃取-气相色谱质谱法测定地表水中7种藻致嗅味物质的方法,浓度在0.004~0.1 mg/L范围内线性关系良好,具有较高的灵敏度和精密度,方法检出限为1×10-6~2×10-6mg/L,加标回收率为85.9%~108.6%,适用于地表水中嗅味物质的检测。     

固相萃取-高效液相色谱-质谱联用法测痕量双酚A的方法优化

通过优化固相萃取和液相色谱条件,建立了固相萃取-高效液相色谱-质谱法测定水中双酚A的检测方法。水样经C_(18)固相萃取柱净化并富集双酚A后,采用C_(18)反相色谱柱XR-ODS(2.0 mm×100 mm,2.2μm)分离,MRM负离子模式测定。结果表明:BPA浓度为5～200 ng/L范围内线性关系良好(相关系数为0.999 9),取样量500 mL,浓缩500倍时,方法检出限(LOD)和定量下限(LOQ)分别为2.0、8.0 ng/L。实际水样加标量为5、20 ng水平时,BPA的相对标准偏差(RSD,n=8)分别为8%和7%,回收率范围分别为82%～103%和90%～111%。     

在线固相萃取-高效液相色谱-串联质谱法测定饮用水中10种磺胺类化合物

采用在线固相萃取-高效液相色谱-串联质谱法测定饮用水中磺胺噻唑、磺胺吡啶、磺胺甲基嘧啶、磺胺二甲嘧啶、磺胺间二甲氧嘧啶、磺胺喹噁啉、磺胺间甲氧嘧啶、磺胺邻二甲氧嘧啶、磺胺对甲氧嘧啶、三甲氧苄氨嘧啶共10种磺胺类化合物。当进样体积为1.0mL时,方法的检出限为0.649～17.3ng/L,测定下限为2.60～69.2ng/L。     

Seasonal change and correlation with environmental parameters for 2-MIB in Feng-Shen Reservoir, Taiwan

Two common drinking water earthy/musty odorants, 2-methyl-isoborneol (2-MIB) and trans-1,10-dimethyl-trans-9-decalol (geosmin), were monitored and analyzed for their correlation with environmental conditions in Feng-Shen Reservoir (FSR), Taiwan. Long-term monitoring results, from December 2000 to July 2003, indicated that 2-MIB was present in the reservoir at concentrations between 10 and 200 ng L(-1), and those of geosmin were always smaller than 10 ng L(-1). The 2-MIB concentrations followed a trend of higher concentrations during the warm seasons. After being analyzed with 10 water quality and three meteorological parameters, 2-MIB concentration was found to correlate with corresponding air and water temperatures. An analysis of air temperature history versus 2-MIB concentration in FSR suggested that 2-MIB concentration was best correlated with the mean of average daily temperature from 1 to 9 days before sampling, with R (2) = 0.90. This correlation was further employed to predict the 2-MIB concentration observed during another sampling period in FSR. A similar degree of fit was observed between predictions and experimental data, suggesting the potential applicability of the approach. In addition to the effect of temperature, heavy rainfalls that occurred before the sampling time may also reduce the 2-MIB concentration in the reservoir. A short-term continuous monitoring of the odorants for 32 h showed that both geosmin and 2-MIB concentrations in the reservoir remained almost constant, with only about a 10% difference during the sampling period. This may suggest that the odorants were uniformly distributed in the water near the sampling location in the reservoir.     

苏州市太湖饮用水源地异味物质种类及其与环境因子相关性分析

于2013年每月测定了苏州太湖饮用水源地9种异味物质含量及TP、TN、水温、藻密度等指标,结果表明,苏州太湖饮用水源地主要检出的异味物质有2-甲基异崁醇、土臭素、β-环柠檬醛和β-紫罗兰酮等4种。2-甲基异崁醇年均值是其嗅觉阈值的2.9倍,水体主要表现为土霉味。根据异味物质与环境因子相关性分析结果及相关文献讨论,水温是影响异味物质含量的重要因素。微囊藻等藻类对β-环柠檬醛和β-紫罗兰酮有明显贡献。     

Use of fuzzy logic models for prediction of taste and odor compounds in algal bloom-affected inland water bodies

Mechanistic modeling of how algal species produce metabolites (e.g., taste and odor compounds geosmin and 2-methyl isoborneol (2-MIB)) as a biological response is currently not well understood. However, water managers and water utilities using these reservoirs often need methods for predicting metabolite production, so that appropriate water treatment procedures can be implemented. In this research, a heuristic approach using Adaptive Network-based Fuzzy Inference System (ANFIS) was developed to determine the underlying nonlinear and uncertain quantitative relationship between observed cyanobacterial metabolites (2-MIB and geosmin), various algal species, and physical and chemical variables. The model is proposed to be used in conjunction with numerical water quality models that can predict spatial–temporal distribution of flows, velocities, water quality parameters, and algal functional groups. The coupling of the proposed metabolite model with the numerical water quality models would assist various utilities which use mechanistic water quality models to also be able to predict distribution of taste and odor metabolites, especially when monitoring of metabolites is limited. The proposed metabolite model was developed and tested for the Eagle Creek Reservoir in Indiana (USA) using observations over a 3-year period (2008–2010). Results show that the developed models performed well for geosmin (R ²?=?0.83 for all training data and R ²?=?0.78 for validation of all 10 data points in the validation dataset) and reasonably well for the 2-MIB (R ²?=?0.82 for all training data and R ²?=?0.70 for 7 out of 10 data points in the validation dataset).     

Analysis of BTEX and other substituted benzenes in water using headspace SPME-GC-FID: method validation

The analysis of BTEX and other substituted benzenes in water samples using solid phase microextraction (SPME) and quantification by gas chromatography with flame ionization detection (GC-FID) was validated. The best analytical conditions were obtained using PDMS/DVB/CAR fibre using headspace extraction (HS-SPME) at 50 [degree]C for 20 min without stirring. The linear range for each compound by HS-SPME with GC/FID was defined. The detection limits for these compounds obtained with PDMS/DVB/CAR fibre and GC/FID were: benzene (15 ng L(-1)), toluene (160 ng L(-1)), monochlorobenzene (54 ng L(-1)), ethylbenzene (32 ng L(-1)), m-xylene (56 ng L(-1)), p-xylene (69 ng L(-1)), styrene (35 ng L(-1)), o-xylene (42 ng L(-1)), m-dichlorobenzene (180 ng L(-1)), p-dichlorobenzene (230 ng L(-1)), o-dichlorobenzene (250 ng L(-1)) and trichlorobenzene (260 ng L(-1)). This headspace SPME-GC-FID method was compared with a previously validated method of analysis using closed-loop-stripping analysis (CLSA). The headspace SPME-GC-FID method is suitable for monitoring the production and distribution of potable water and was used, in field trials, for the analysis of samples from main intakes of water (surface or underground) and from the water supply system of a large area (Lisbon and neighbouring municipalities).     

Determination of organophosphorus fire retardants and plasticizers in wastewater samples using MAE-SPME with GC-ICPMS and GC-TOFMS detection

Determination of organophosphorus fire retardants and plasticizers at trace levels in wastewater is described. In this work, microwave assisted extraction (MAE) and solid-phase microextraction (SPME) are used for sample preparation to extract and preconcentrate the analytes, followed by analysis by gas chromatography coupled to inductively coupled plasma mass spectrometry (GC-ICP-MS) for phosphorus-specific detection. Gas chromatography coupled to time of flight mass spectrometry (GC-TOF-MS) was used to confirm the organphosphorus fire retardants in wastewater. The detection limits of organophosphorus fire retardants (OPFRs) were 29 ng L(-1) for tri-n-butyl phosphate (TnBP), 45 ng for L(-1) for tris(2-butoxyethyl)phosphate (TBEP), and 50 ng L(-1) for tris(2-ethylhexyl)phosphate (TEHP). Optimized extraction conditions were performed at 65 degrees C for 30 min and with 10% NaCl. Application of MAE during the sample preparation prior to the SPME allowed the detection of tris(2-ethylhexyl) phosphate, which has been difficult to determine in previous work. Application of the method to wastewater samples resulted in detecting 3.1 microg L(-1) P from TnBP, 5.0 microg L(-1) P from TBEP, and 4.0 microg L(-1) P from TEHP. The presence of these compounds were also confirmed by SPME-GC-TOF-MS.     

Feasibility of detection and quantification of gas-phase carbonyls in indoor environments using PFBHA derivatization and solid-phase microextraction (SPME)

Solid-phase microextraction (SPME) was evaluated for the detection and quantification of the gas-phase carbonyls: citronellal, glyoxal, methylglyoxal, and beta-ionone. Prepared air samples containing the carbonyl compounds were collected at a flow rate of 2.8 L min(-1) in an impinger containing a 25% reagent water/75% methanol collection liquid. The aqueous samples were then derivatized with O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride (PFBHA), extracted with a PDMS/DVB coated SPME fiber, and analyzed by GC-MS. Detection limits with a sample air volume of 76 L were calculated to be 0.03 ppbv, 0.34 ppbv, 0.12 ppbv, and 0.28 ppbv for citronellal, glyoxal, methylglyoxal, and beta-ionone, respectively.     

SPE-GC-MS/MS法测定水源水中多种有机氯EDCs

采用C 18柱固相萃取(SPE)-三重四级杆气相色谱-质谱法同时测定水中18种含有机氯的环境内分泌干扰物,方法在0.500μg/L^100μg/L范围内线性良好,方法检出限为0.04 ng/L^0.8 ng/L,空白水样的加标回收率为61.3%~108%,6次测定结果的RSD为3.8%~18.0%。将该方法用于饮用水源水监测,18种目标化合物的测定值为未检出~1.5 ng/L,平均加标回收率为71.9%~109%,平行测定结果的RSD<15%。     

顶空固相微萃取-气相色谱法测定水中四乙基铅

建立了水中四乙基铅的测定方法——顶空固相微萃取-气相色谱法,探讨了影响水中四乙基铅萃取效率的温度、转速和萃取时间等因素。实验结果表明,在0.08～10μg/L范围内线性关系良好,方法检出限为0.02μg/L,实际水样加标回收率为96.2%～98.3%。