土壤中挥发酚的测定及质量控制

采用分光光度法测定土壤中的挥发酚，详细介绍了样品预处理方法，分析过程中的质量控制及土壤中有机物、矿物油对测定干扰的消除方法。分析结果表明：平行双样的相对偏差都低于其最大允许值，加标回收率在78.6％～81．7％范围内，测定结果具有较好的精密度和准确度。     

GC／MS外标法测定水中22种挥发性有机物的探究

以外标法定量,通过吹扫捕集-气相色谱质谱对22种挥发性有机物进行检测,建立了相应的分析方法。方法将单次分析时间控制样品在50min,连续进样分析时间在38min。并对样品的检测数据进行分析,样品回收率在84．9％～124．9％之间,相对标准偏差均小于10％,且加标回收率在半年内能稳定在81．5％～129．7％之间。结果表明,在采用自动进样器进样条件下,外标法在精准度上满足实验需求,且分析时间较短,节省了加入内标物所带来的成本负担。     

分光光度法测定地表水中总氮的监测质量控制指标研究

运用碱性过硫酸钾-紫外分光光度法对总氮的标准样品及实际样品进行研究分析,通过全国多家实验室的大量监测数据,得出了当前常用的精密度及准确度方面质量控制指标的建议值。研究表明：标准样品在0.5~3.5mg/L浓度范围内,相对标准偏差RSD≤5.0%;室间相对标准偏差RSD′≤10%;相对误差RE≤±10%;实际样品在0.07~10mg/L浓度范围内时,相对偏差RD≤10.0%;加标回收率范围为90%~110%。     

高锰酸盐指数加标回收率的探究

高锰酸盐指数的测定采用容量法,传统的容量法采用手工操作进行加标人为因素引起误差很大.本研究利用智能机器人分析系统测定高锰酸盐指数,对质控样、实际水样以及空白样进行加标测定,加标量控制在待测样的0.5～2.0倍.通过多组平行测定,得到很好的精密性和准确性,加标回收率的范围在85％～122％之间,满足质量控制要求.实验表明...     

气质联用法测定土壤中多环芳烃及其适用性研究

依据标准方法建立了真空冷冻干燥、加压流体萃取、固相萃取净化、气相色谱—质谱法联合测定土壤中15种多环芳烃的测定方法,对部分操作流程和仪器条件进行细化与优化,并对方法适用性进行研究。结果显示,该法检出限为0.03～0.06 mg/kg,低、中、高3个含量空白加标和实际样品加标的相对标准偏差分别为5.2%～8.4%,14%～19%,13%～16%和14%～20%,平均加标回收率分别为76.0%～88.0%,68.0%～74.0%,67.0%～77.0%和67.0%～77.4%,精密度和正确度良好,满足土壤环境质量监测要求。     

UPLC-MS/MS和HPLC测定水中氨基甲酸酯类农药的对比

应用超高效液相色谱-三重四级杆质谱（UPLC-MS/MS）法和高效液相色谱（HPLC）法分别建立了测定水中三种氨基甲酸酯类农药甲萘威、涕灭威和克百威的方法。对比了两者直接进样和固相萃取测定的正确度、精密度、检出限等指标。结果,HPLC直接进样法和固相萃取法对应三种组分的加标回收率范围分别为96.0%～109.0%、75.0%～90.0%,相对标准偏差（RSD）范围分别为1.9%～4.4%、1.9%～5.1%,方法检出限范围分别为1.63～2.85μg/L、0.03～0.04μg/L;UPLC-MS/MS直接进样法和固相萃取法对应三种组分的加标回收率范围分别为85.5%～100.0%、78.0%～89.0%,RSD范围分别为2.5%～6.6%、3.8%～7.9%,方法检出限范围分别为0.02～0.03μg/L、0.0003～0.0004μg/L。结论：相较于HPLC法,UPLC-MS/MS法操作简便,样品保留时间更短,无论是直接进样法还是固相萃取法,其方法检出限均低于HPLC法,可作为甲萘威、涕灭威和克百威检测的推荐方法。     

高脂肪样品中PCBs和OCPs分离方法研究

研究开发了用于分离高脂肪样品中21种多氯联苯（PCBs）和22种有机氯农药（OCPs）的分离柱填料,以及利用该填料分离含脂肪的动物组织样品中PCBs或OCPs的方法。该填料按质量百分比由硅胶-弗罗里硅土混合物30%-35%、酸性改性硅胶50%-60%和无水硫酸钠10%-15%组成,并使用自主研发的四通道色谱分离仪对样品进行分离和净化。利用本方法的填料分离PCBs或OCPs,分离方法高效、快速、工艺简单,可在成本较低的条件下达到显著的分离效果。PCBs化合物柱回收率可达96.4%-119%,对鱼脂肪组织加标回收率可达74.4%-100%;OCPs化合物柱回收率可达78.4%-103%,对鱼脂肪组织加标回收率可达78.3%-102%。结果表明该填料可用于分离PCBs或OCPs,色谱分离效果良好,可以满足高脂肪样品中OCPs和PCBs的监测分离需要。     

超声水浴-原子荧光光谱法同时测定土壤和沉积物中汞和砷

建立了改进HJ 680-2013方法,采用超声水浴-原子荧光光谱法同时测定土壤和沉积物样品中汞与砷元素。探讨了15种消解体系对不同类型标准物质测定结果的影响,筛选得到采用盐酸-硝酸-硫酸-过氧化氢(体积比为3∶1∶0.5∶0.5)消解体系为最佳消解条件。超声水浴法为样品前处理方法,消解时间为0.5h。汞和砷元素的质量浓度范围在0.10～10.0μg/L具良好线性,线性相关系数大于0.999,检出限为0.002～0.006mg/kg,检测下限为0.006～0.018 mg/kg,测定结果的相对标准偏差为1.96%～2.97%,样品加标回收率范围为89.9%～104%。经标准物质和实际环境样品验证该方法,能满足当前环境分析检测工作,一次处理同时测定的高效,解决了环境检测行业精确测定的大量工作需求。     

火焰原子吸收光谱法测定模拟尘铅中铅的前处理方法探讨

分别用酸煮法和索氏提取法对模拟尘铅样品进行前处理,采用火焰原子吸收光谱法测定,方法线性范围0.08~1.50 mg/L,检出限为0.025 mg/L。对两种前处理效果作了比较,结果表明,采用酸煮法,6次重复测量的相对标准偏差小于2%,加标回收率为90.0%~102%;索氏提取法受装置影响,提取效率不稳定,6次重复测量的相对标准偏差小于11%,加标回收率为81.5%~82.6%,酸煮法的效果优于索氏提取法。     

快速溶剂萃取-水浴氮吹-高效液相色谱法检测土壤16种多环芳烃

建立了快速溶剂萃取-水浴氮吹-高效液相色谱法检测土壤样品中16种多环芳烃(PAHs)的方法。分别对比了快速溶剂萃取与索式抽提、旋转蒸发浓缩与水浴氮吹浓缩、硅酸镁固相萃取柱与硅胶固相萃取柱净化的预处理效果,经实验对比后,确认优化预处理条件为：快速溶剂萃取温度120℃,静态萃取时间16 min,萃取次数两次,水浴氮吹浓缩,氮吹温度40℃,浓缩液经硅酸镁固相萃取柱净化。方法检出限和测定下限分别为0.21～0.47μg/kg和0.84～1.88μg/kg。在优化条件下,加标水平为0.5 mg/kg时,目标物加标回收率为72.66%～113.90%,替代物加标回收率为69.25%,108.63%,相对标准偏差(n=7)为0.69%～11.8%,适合实际土壤样品中PAHs的检测。     

我国大气细颗粒物污染防治目标和控制措施研究

我国面临着严重的细颗粒物(PM2.5)污染问题,PM2.5对人体健康、能见度、气候变化、生态系统等均产生了不良影响。本文旨在提出我国PM2.5污染防治目标和控制措施,为从根本上改善空气质量提供科学依据。首先,本文提出了2020年和2030年我国PM2.5污染防治目标。其次,采用能源和污染排放技术模型,分情景预测了我国未来一次大气污染物排放量的变化趋势。基于情景预测结果和此前研究建立的一次污染物排放与PM2.5浓度间的非线性关系,确定了2020年—2030年与PM2.5浓度改善相适应的全国和重点区域大气污染物减排目标。最后,利用能源和污染排放技术模型,提出了实现大气污染物减排的技术措施和对策建议。研究表明,2030年全国二氧化硫、氮氧化物、一次PM2.5和挥发性有机物的排放量应分别比2012年至少削减51%、64%、53%和36%,氨排放量也要略有下降。对于污染严重的重点区域,必须采取更严格的控制力度。要实现上述减排,应加快能源结构调整,推进煤炭清洁高效集中可持续利用,建立"车-油-路"一体的移动源控制体系,并强化多源多污染物的末端控制。     

臭氧-活性炭工艺在炼化循环排污水处理中的应用＊

针对炼化企业循环排污水中有机污染物浓度不能满足脱盐处理工艺进水水质要求的问题,开展了臭氧氧化-活性炭吸附工艺去除循环排污水中有机污染物的研究。通过对两种处理工艺进行不同组合的实验结果得知:当反应时间控制在最佳值,臭氧氧化和活性炭吸附单独处理循环排污水时,COD去除率分别约为27%和20%,处理效率偏低;当两种工艺组合后,在臭氧浓度为12 mg/L、氧化时间20 min、吸附时间为10 min时,COD去除率则达到52%,组合工艺协同作用效果明显。     

火焰原子吸收法测定水中铁的质量控制指标研究

本文研究了火焰原子吸收法测定水中铁的质量控制指标,全国共12个省份的46家实验室参加测定工作,提供了具有全国性指导意义的工作参考数据.研究结果为:标准样品在0.2～4.0mg/L浓度范围内的RSD≤3.0%,RSD'≤10.0%,室间标准偏差≤0.10mg/L;浓度≤2.0mg/L时,RE≤±10.0%,2.0～4.0...     

对饮用水中有机污染物的控制

以保护饮用水的水质为出发点，控制饮用水中有机污染物为目的，本文介绍了有机污染物对饮用水水质的影响，着重从治理污染源和加强饮用水的深度处理等方面讨论了对饮用水中有机污染物的控制。     

嘉陵江C市段源水中有机污染物定性研究

采用XAD-2树脂富集水中有机物，用GC＼MS进行定性分析。对嘉陵江C市段水源水中有机污染物进行分析，共检出有机污染物13种，其中以多环芳烃，邻苯二甲酸酯类为主，并且有3种物质为中国环境优先控制污染物，分别是邻苯二甲酸二辛酯，邻苯二甲酸二丁酯、荧蒽。     

GROUND AND SURFACE WATER QUALITY IMPACTS OF NORTH CAROLINA SANITARY LANDFILLS1

ABSTRACT: Ground and surface water quality monitoring data from 71 municipal sanitary landfills in North Carolina were analyzed to determine the nature and extent of current contamination problems and identify any common characteristics associated with this contamination. A total of 322 surface and 411 ground water quality records were analyzed using the SAS data system. Almost all the landfill records included inorganic and heavy metal analyses while approximately half of the records also included organic analyses by CC/MS. Our analysis indicates that landfills are having measurable impacts on ground and surface water quality, but these impacts may not be as severe as is commonly assumed. Statistically significant increases were detected in the average concentrations in ground water and downstream surface water samples when compared to upstream surface water samples. The largest percentage increases were observed for zinc, turbidity, total organic carbon, conductivity, total dissolved solids, and lead. Violations of ground water quality standards for heavy metals and hazardous organic compounds were detected at 53 percent of the landfills where adequate data existed. The moat common heavy metal violations were for lead (18 percent), chromium (18 percent), zinc (6 percent), cadmium (6 percent), and arsenic (6 percent) (percentage of landfills violating shown in parenthesis). The organic compounds that appear to pose the greatest threat to ground water are the chlorinated solvents (8 percent), petroleum derived hydrocarbons (8 percent), and pesticides (5 percent). A comparison of monitoring data from sanitary landfills and secondary wastewater treatment plants suggests that the concentrations of heavy metal and organic pollutants discharged to surface waters from these two sources are similar.     

三峡库区重庆段鲶鱼和鲤鱼体内持久性有机污染物分析

为了了解三峡库区重庆段水体中持久性有机污染物的生物富集情况,对该水体部分鱼类样品进行了分析。分析结果显示三峡库区重庆段水体中的部分持久性有机污染物已经在鲶鱼和鲤鱼体内形成富集,其检出浓度较之水体中对应浓度要高出2~4个数量级。     

WATER QUALITY BENEATH URBAN RUNOFF WATER MANAGEMENT BASINS1

ABSTRACT: The chemical impact of urban runoff water on water quality beneath five retention/recharge basins was investigated as part of the US EPA's Nationwide Urban Runoff Program in Fresno, California. Soil water percolating through alluvium soils and the ground water at the top of the water table were sampled with ceramic/Teflon vacuum water extractors at depths up to 26 m during the two-year investigation. Inorganic and organic pollutants are present in the runoff water delivered to the basins. No significant contamination of percolating soil water or ground water underlying any of the five retention/recharge basins has occurred for constituents monitored in the study. The oldest basins was constructed in 1962. The concentration of selected trace elements in the ground water samples was similar to the levels reported in the regional ground water. None of the pesticides or other organic priority pollutants, for which water samples were analyzed, was s̊ detected except diazinon which was found in trace amounts (0.3 μg/L or less) in only three soil water samples. These results are important to the continued conservation of storm water and the development of a best management practice for storm-water management using retention/recharge basins in a semi-arid climate.     

黄浦江上游原水强化处理选炭试验研究

以黄浦江上游水源为原水,通过煤质炭、竹质炭、椰壳炭等炭种筛选小试和中试试验,研究了黄浦江上游原水中有机污染物强化去除的最佳炭种及其最佳投加量。结果表明黄浦江上游原水中投加PAC能够改善处理后水质,提高原水中有机物的去除效果;并且随着PAC投加量的增加,原水中有机物去除效果增强;综合性价比、碳源等因素确定竹质炭较为经济合理;当竹质炭投加量为10～15mg/L时,处理后出水CODMn可达到3mg/L或以下。     

WATER QUALITY OF STORMWATER RUNOFF FROM TEN INDUSTRIAL SITES1

ABSTRACT: This study was to designed to determine concentrations of selected metals, organic compounds, pesticides, and conventional pollutants in stormwater runoff from two North Carolina businesses in each of the following five general industrial groups: auto salvage, metal fabrication, scrap and recycling, vehicle maintenance, and wood preserving facilities. The sampling procedure involved collecting a first flush sample of runoff from a single storm event and both first flush and composite samples of runoff from three consecutive storm events. Analysis of samples collected during the first flush indicated that zinc and copper were the most common of the 13 metals included in the analysis. Additional analysis documented that several volatile organic, semi-volatile organic, or pesticide compounds including acrolein, methylene chloride, xylenes, toluene, tetrachloroethylene, trichloroethylene, pentachlorophenol, and aldrin were also found in the first flush samples. Concentrations of aggregate organics, nitrogen, phosphorus, and sediment were determined in both first flush and three-hour composite samples. Concentrations of pollutants in first flush samples were similar to those in corresponding composite samples.