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利用超高效液相色谱-串联质谱,建立土壤和沉积物中痕量氨基甲酸酯农药的分析方法。该方法用体积比1:1的二氯甲烷/甲醇对土壤和沉积物样品进行加速溶剂萃取,GCB/PSA固相萃取小柱对萃取液进行净化,内标法定量,用超高效液相色谱-串联质谱法分析土壤和沉积物中20种氨基甲酸酯农药。20种氨基甲酸酯农药在0.02~1.0 μg/mL范围内线性良好(r≥0.99),检测限为0.20~0.60 ng/g。沉积物加标样品(20ng/g)和土壤加标样品(20ng/g)的回收率分别为33.2%~101.9%、38.8%~120.5%,相对标准偏差为6.1%~28.0%、2.3%~16.0%。沉积物加标样品(2.0 ng/g)回收率为43.0%~100.0%,相对标准偏差为2.1%~11.3%。 相似文献
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固相微萃取-气相色谱法测定水中酞酸酯类化合物 总被引:1,自引:1,他引:0
建立了固相微萃取(SPME)-气相色谱(GC)法分析环境水样中痕量酞酸酯类化合物(PAEs)的方法。选用65 μm PDMS/CVB萃取纤维,在磁力搅拌转速为700 r/min、萃取温度为60℃条件下,对水样中的PAEs萃取富集50 min,然后直接注入GC进样口,在 250℃ 温度下解吸1.5 min后进行分析测定,6种PAEs能得到充分提取和分离。方法的检出限为0.010 8~0.029 3 μg/L。对水样进行3个质量浓度水平(0.025、0.125、0.25 μg/L)的加标实验,加标回收率为41.79%~132.80%,RSD为6.53%~18.74%(n=7),用该法测定了某制药厂的实际水样,测得DBP含量为0.018 6 μg/L,DEHP、 DMP、DEP、DOP、BBP均未检测到。 相似文献
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建立了直接进样-超高效液相色谱分离-紫外吸收测定地表水中丁基黄原酸的分析方法。通过对流动相的优化,确定最佳分析条件:0.050 mol/L超纯水乙酸铵溶液(pH约为9.5):乙腈=80:20等度洗脱,Waters ACQUITY UPLC BEH C18色谱柱(50 mm×2.1 mm,1.7 μm)分离,流速0.30 mL/min,进样体积10.0 μL,302 nm紫外吸收。结果显示,0.5~20.0 μg/L范围线性良好,R=0.9998; 2.0、10.0、20.0 μg/L重复测定,变异系数小于5%,精密度良好;实际水样加标回收率为95.5%~101.6%;以3倍信噪比计算得出检出限为0.80 μg/L。该方法分析速度快,2 min内可完成,满足环境质量监测要求。 相似文献
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超高效液相色谱-串联质谱法同时检测溴代阻燃剂 总被引:1,自引:0,他引:1
采用Acquity BEH C18色谱柱,以甲醇-乙腈混合液和水为流动相,辅以电喷雾正离子模式多反应监测(MRM)进行定性定量分析,建立了一种同位素稀释超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测四溴双酚A(TBBPA)、三-(2,3-二溴丙基)异氰脲酸酯(TBC)和3种六溴环十二烷(HBCD)异构体的方法。水样通过固相萃取进行净化,回收率达到85.3%~96.1%。土壤和底泥样品经加速溶剂萃取后,采用酸性硅胶和中性硅胶柱进行净化,回收率达到81.5%~102.7%。该方法对TBBPA、TBC、α-HBCD、β-HBCD、γ-HBCD在水和土壤中的检测限分别为1.0、1.2、2.0、0.8、1.2 ng/L和0.10、0.12、0.20、0.08、0.12 ng/g。 相似文献
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建立了气相色谱法(GC)和高效液相色谱法(HPLC)测定水中苦味酸的分析方法,并对2种方法进行比较。GC法检出限为0.000 4 mg/L,线性范围为0.0~0.050 mg/L,加标回收率为92.3%~94.1%,相对标准偏差为4.6%~8.9%。HPLC法检出限为0.02 mg/L,线性范围为0.10~5.00 mg/L,加标回收率为93.7%~96.5%,相对标准偏差为1.3%~2.0%。2种方法相比,GC法灵敏度较高,可用于痕量分析,但操作烦琐,不能有效地将苦味酸与硝基酚类干扰物分离;而HPLC法虽然灵敏度较差些,但简单、快速、稳定性好、准确度高,可有效地将苦味酸与硝基酚类干扰物分离。 相似文献
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建立电子制冷预浓缩仪-气相色谱-质谱法测定空气中10种含硫化合物的方法。经考察不同采样容器、优化预处理条件、研究样品保存等获得了最佳实验条件,并通过实际样品的测定,考察了方法的适用性。结果表明:硫化氢、甲硫醇和乙硫醇3种高活性含硫化合物校准曲线线性回归系数在0.990以上,另外7种含硫化合物在0.995以上;高、中、低空白加标样品相对标准偏差均为9.5%以内,乙硫醇由于具有高活性和吸附性,低浓度空白加标回收率为63%,其余组分回收率范围为83%~110%;当进样体积为400 mL时,各目标化合物的方法检出限为0.2×10-3~1.1×10-3 mg/m3。分析污水处理厂无组织排放监控点的空气结果显示,该方法具有较低的检出限及较强的抗干扰能力,能较好地满足目前监测工作的要求。 相似文献
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二氯甲烷萃取与气相色谱—质谱结合新方法测定饮用水源地水中的苦味酸 总被引:2,自引:0,他引:2
为建立饮用水源地中苦味酸分析测定的新方法,将10 ml水样中的苦味酸氯化后,以二氯甲烷萃取,用气相色谱—质谱法(GC—MSD)测定水中苦味酸的含量,采用保留时间定性,外标法定量。结果表明,最佳萃取时间为4 min,最佳萃取剂用量为1.5 ml,该法能快速而有效的提取并测定水中苦味酸,检出限低(0.4μg/L)、精密度(RSD=1.8%)和准确度高(加标回收率93.16%)、标准曲线线性(r=0.999)较好,能满足饮用水源地水中苦味酸的测定要求。 相似文献
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为测定被污染土壤中的低浓度苦味酸和联苯胺,研究建立了一种基于高效液相色谱-串联三重四级杆质谱检测技术的分析方法,实现了超声波乙酸乙酯溶剂萃取后直接进样的高效定性和定量检测。研究表明,在0.5~100.0μg/L质量浓度范围内,目标化合物的线性关系良好(r0.999 9),苦味酸、联苯胺的检出限分别为0.16、0.30μg/kg,精密度相对标准偏差为1.5%~5.8%,加标回收率范围为70.1%~111.0%。该方法灵敏度高、前处理步骤简便,适用于低含量苦味酸和联苯胺的土壤测定。实验表明,以碱性木素为原料,采用热解法在氮气氛围下600℃煅烧得到的生物质炭,对土壤中联苯胺的去除率高达98.2%,对苦味酸的去除率超过50%,可有效实现污染土壤的修复。 相似文献
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城市饮用水源地水质直接关系到人民群众的健康和经济发展与社会稳定的大局.根据监测资料,采用国家有关标准,本文对伊犁州县市饮用水源地(河流、水库、地下水)的水质状况进行了分析评价,并提出了相应的保护措施和建议. 相似文献
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末梢水与其水源水的数据“倒挂”现象是影响居民饮水健康的安全隐患。基于末梢水数据“倒挂”现象在新闻报道、政府信息公开及相关调查研究中的表现形式,分析了引起末梢水数据“倒挂”的原因主要包括:监测采样、分析偏差,物理因素和化学、生物反应以及综合因素造成的污染等。提出,在饮用水水源方面,加强规范化管理,保持水源水水质合格并长期稳定;在水处理阶段,选择适宜且安全高效的水处理方式;在水管输送阶段,选择健康的管道材质并合理规划设计、维护输水管网体系;在饮用水使用阶段,加强用水宣传,让居民养成良好的健康用水习惯。从而逐渐消除末梢水数据“倒挂”现象,保障居民的饮水安全。 相似文献
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Organochlorine insecticide residues in drinking and ground water in and around Delhi 总被引:4,自引:0,他引:4
A multiresidue method was developed for the estimation of 15organochlorine pesticides in water. 50 samples of drinking watersupplied by the Municipal Corporation to the residential areasof Delhi and 20 ground water samples from nearby villages usedfor irrigation were monitored for the presence of organochlorineinsecticides by the method developed. Although, organochlorinepesticides were detected in the ground water and irrigationwater samples, the levels of pesticides were below the MaximumContaminant Level as prescribed by WHO. No organochlorineinsecticides were detected in any of the drinking water samples. 相似文献
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Jurdi M Korfali SI Karahagopian Y Davies BE 《Environmental monitoring and assessment》2002,77(1):11-30
The increased demand on water resources in Lebanon as a resultof: progressive urbanization, socio-economic growth, agriculturalactivities and development of industries is, according to the national authorities, a major critical factor by the year 2010.Political difficulties in earlier years imply a dearth of pertinent data. The objective of this study was to evaluate water quality of the Qaraaoun Reservoir of the Litani River andassess its feasibility for multi-purpose usage as one of the solutions to the aggravated water problems in Lebanon. Sampleswere collected from 18 sampling sites at several dates duringthe dry season. Parameters analysed were, pH, electrical conductivity, TDS, turbidity, alkalinity, Ca, Mg, TH, Cl-, SO4
2-, NH3, NO3
-,PO4
3-, Fe, Al, Na, Zn, Cr, Cu and As. The reported data were in compliancewith WHO guidelines, USEPA regulation and EEC directives. Statistical analysis of the data defined three distinct environmental zones and water quality in the central, main zone satisfied most criteria. It is concluded that the reservoir water is fit for multipurpose uses, namely, drinking, domestic,recreational activities, irrigation, fisheries, livestock and industrial, and should be properly managed accordingly. 相似文献
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Spatial and seasonal differences in water quality of drainage water and unconfined shallow groundwater were related to irrigation in Samandağ, a Mediterranean coastal region. Eighteen wells, seven drainage points and Orontes River were monitored bimonthly for one year for analyses of electrical conductivity (EC), total dissolved solids (TDS), sodium adsorption ratio (SAR), cations (Na, K, Ca + Mg) and anions (CO3, HCO3, Cl and SO4). Agricultural irrigation using saline groundwater decreased water quality of Orontes River during the irrigation season (May to September) more than during the non-irrigation season (October to April). Seasonal fluctuations in water quality of shallow groundwater were greater during the irrigation season than the non-irrigation season in the study area. Excessive use of groundwater resulted in a decline in the water table levels in the irrigation season. Water table level rose up to the soil surface in areas where there was a lack of drainage or poor drainage, due to the impact of precipitation in the winter. SAR and pH values of drainage water increased in the irrigation season, while the other properties of drainage water decreased. Irrigation water quality of Orontes River was classified as C3S1 in both seasons. Irrigation water quality of shallow groundwater and drainage water varied from C2S1 to C4S2 in one year. Drainage and well waters were found to be different on yearly basis in terms of Na, SAR (p<0.01) and Ca + Mg concentrations (p<0.001). Ca + Mg concentrations for both sources were different for all sampling dates (p<0.001). 相似文献