并联式双梯度反相离子对液相色谱法快速检测土壤中芳磺酸

通过阀切换并联式双系统,建立了一套测定土壤样品中7种芳磺酸的反相离子对液相色谱法。该方法采用2根色谱柱,一根色谱柱分析的同时,另一根色谱柱通过阀切换实现平衡,节约了38.5%的分析时间。方法使用Dikma Diamonsil C18(150 mm×4.6 mm×5μm)色谱柱,以离子对试剂(四丁基硫酸氢铵)和乙腈为流动相,检测波长为226、235、258 nm。各组分线性关系良好,线性相关系数均在0.999 9以上。随机抽取样品进行重新提取、检测,得到各组分的相对标准偏差均小于7%,且定量限最高不超过0.181 2μg/g,重复性和定量限均能满足实验要求。     

气溶胶脉冲实时在线测量装置的研制

介绍的气溶胶实时在线测量装置借鉴了色谱分析原理和实验方法，采用六通阀切换脉冲进样，以毛细管为扩散池，以TSI公司的3076型气溶胶发生器产生气溶胶，以TSI公司的3022A型凝结核计数器为在线探测器，采用AX5216为数据采集卡，能够同时测定气溶胶在扩散池中的穿透率和保留时间，适合于气溶胶脉冲在管道中扩散行为和传输机制的研究．     

气相色谱法测定非甲烷总烃

本文采用《空气和废气监测分析方法(第四版)》P585~P587总烃和非甲烷总烃测定方法一(B)利用六通阀定量环进样来测定环境空气以及废气中的非甲烷总烃浓度,对仪器条件进行优化,方法的检出限为0.13 mg/m3,标样总烃相对标准偏差为0.4%,甲烷的相对标准偏差为1.2%,总烃的加标回收率为100.9%~101.6%,甲烷的加标回收率为102.4%~102.6%,该方法操作简单,分析速度快,实验结果满意。     

在线固相萃取-液相色谱-串联质谱法直接测定水中15种全氟烷基化合物

通过优化样品保存、前处理、分析条件,建立了水中15种典型全氟烷基化合物(PFASs)在线固相萃取-液相色谱-串联质谱分析方法,并对饮用水水源地和末梢水中PFASs进行定量检测。水样过膜后,准确移取700 μL水样、300 μL甲醇至1.5 mL聚丙烯进样瓶,并加入同位素内标后直接进样800 μL至在线固相萃取流路,进行萃取富集,再通过十通阀切换将洗脱的PFASs转移至分析流路进行分离,质谱检测,内标法定量。方法分析总时长22 min,15种全氟烷基化合物的方法检出限为0.31~1.20 ng/L,纯水高、中、低浓度加标样品回收率为70%~115%,相对标准偏差为0.2%~14.0%(n=6)。经实际样品验证,该方法与传统手动固相萃取方法分析结果基本一致。结果表明,该方法操作简单、自动化程度高、有机试剂用量少、灵敏度高、方法稳定,可满足地表水和末梢水中PFASs的快速测定。     

基于顺序注射分析技术的总氮在线分析仪

针对环境监测领域,研制了一种基于顺序注射分析技术的总氮在线分析仪。该分析仪以注射泵为分析过程的液体驱动定量单元,以多通道选向阀为流路切换单元,以发光二极管和硅光电管为检测单元。在该分析平台上,含氮化合物在高温高压条件下经过硫酸钾氧化成硝酸根,硝酸根被还原为亚硝酸根后与N-(1-萘基)乙二胺盐酸盐生成偶氮染料,再由光电检测单元测定吸光度值,经计算得到总氮含量。与现有的总氮在线分析技术相比,该分析仪具有检测单元简单、生产成本低、测量精度高、试剂消耗和废液产生量少等优点,适合于环境监测等领域的长时间在线分析。     

TH- 600B型智能烟气采样分析器采样系统气路的改进

ＴＨ - 60 0Ｂ型智能烟气采样分析器采用直接碘量法原理 ,根据ＳＯ2 混合吸收液中的碘与淀粉指示剂显色的特征 ,通过光电转换器中的光接收管接收来自反应瓶对侧的光信号 ,自动检测指示终点 ,由单片机控制的电磁三通阀 ,自动停止采样 ,直接由微电脑处理和显示ＳＯ2 测量结果。用该分析器采集分析ＳＯ2 时 ,常常会出现电磁三通阀自动转换装置启动失灵。一种情况是按仪器说明书 ,启动仪器进入工作状态 ,当换气时间结束时 ,电磁三通阀装置中的自动阀不能自动将仪器从换气状态切换到采样状态 ,洗涤瓶支路不能被自动阀关闭 ,仪器仍处于换气状态 ,…     

胶束增敏光度法测定微量氰化物的研究

根据CN^-对丁二酮肟-Ni-曲通X-100体系的增色作用，建立了一种测定微量氰化物的新方法。方法选择性好，操作简便，不需要蒸馏和萃取。CN-含量在0-0．32mg／L内符合比耳定律，用于环境水中氰化物的测定，结果满意。     

基于PSTN的环境监测设备远程控制系统

针对目前环境空气质量自动监测系统中经常遇到的各种监测设备掉电需人工手动重启等问题，提出了一种基于固定电话网的远程控制系统。此系统以单片机为主控部件，实现了振铃检测、摘挂机检测、双音频解码等功能，并采用语音录放芯片实现语音提示功能，增强了人机交互性，同时还具有密码验证、外部噪音隔离、防雷击等保护功能。利用电话线进行监测设备的远程通断可避免对设备的人工复位，且方便、经济，具有实用价值。     

过硫酸钾氧化-紫外分光光度法测定水中总氮的几点体会

目前在碱性过硫酸钾 -紫外分光光度法测定总氮过程中 ,由于受到某些因素的影响 ,往往使测定结果的精密度及准确度有一定的差异 ,今对如何保证测定的准确性 ,谈几点看法。1　过硫酸钾试剂的质量直接影响测试结果含氮化合物量过高、质量差的过硫酸钾不仅会引起空白值增大 (吸光值 >1 ) ,甚至会导致无法比色。因此 ,必须选用符合国家标准分析纯的、且在有效期内的过硫酸钾试剂 ,必要时要进行提纯处理 ,主要是去除溶液中的氨氮类化合物。在碱性过硫酸钾溶液中通入氩气 ,可去除其中的ＮＨ 4,降低空白值 ,去除效果见图 1。图 1　氩气通入时间与Ｎ…     

不明水质污染事故排查案例分析

南京市六合区通江河发生大面积水质变浑浊现象，污染来源不明，直接进入长江，威胁下游饮用水安全。通过不断调整污染筛查方案，最终锁定污染因子及污染源头，为有效应对措施提供了科学准确的监测数据。通过此次事故得到启示，因为环境事故的复杂性，对监测人员的综合分析判断能力提出了新的更高的要求。     

Water quality assessment by means of HFNI valvometry and high-frequency data modeling

The high-frequency measurements of valve activity in bivalves (e.g., valvometry) over a long period of time and in various environmental conditions allow a very accurate study of their behaviors as well as a global analysis of possible perturbations due to the environment. Valvometry uses the bivalve's ability to close its shell when exposed to a contaminant or other abnormal environmental conditions as an alarm to indicate possible perturbations in the environment. The modeling of such high-frequency serial valvometry data is statistically challenging, and here, a nonparametric approach based on kernel estimation is proposed. This method has the advantage of summarizing complex data into a simple density profile obtained from each animal at every 24-h period to ultimately make inference about time effect and external conditions on this profile. The statistical properties of the estimator are presented. Through an application to a sample of 16 oysters living in the Bay of Arcachon (France), we demonstrate that this method can be used to first estimate the normal biological rhythms of permanently immersed oysters and second to detect perturbations of these rhythms due to changes in their environment. We anticipate that this approach could have an important contribution to the survey of aquatic systems.     

Online detection of waterborne bioavailable copper by valve daily rhythms in freshwater clam Corbicula fluminea

Freshwater clam Corbicula fluminea, a surrogate species in metal toxicity testing, is a promising bioindicator of impairment in aquatic ecosystems. Little is known, however, about the relationship between clam valve daily rhythmic response and metal bioavailability related to a metal biological early warning system (BEWS) design. The purpose of this study was to link biotic ligand model (BLM)-based bioavailability and valve daily rhythm in C. fluminea to design a biomonitoring system for online in situ detection of waterborne copper (Cu). We integrated the Hill-based dose-time-response function and the fitted daily rhythm function of valve closure into a constructed programmatic mechanism. The functional presentation of the present dynamic system was completely demonstrated by employing a LabVIEW graphic control program in a personal computer. We used site-specific effect concentration causing 10% of total valve closure response (EC10) as the detection threshold to implement the proposed C. fluminea-based Cu BEWS. Here our results show that the proposed C. fluminea-based BEWS could be deliberately synthesized to online in situ transmit rapidly the information on waterborne bioavailable Cu levels under various aquatic environmental conditions through monitoring the valve daily rhythmic changes. We suggested that the developed C. fluminea-based dynamic biomonitoring system could assist in developing technically defensible site-specific water quality criteria to promote more efficient uses in water resources for protection of species health in aquatic environments.     

Dynamic extreme values modeling and monitoring by means of sea shores water quality biomarkers and valvometry

Water quality can be evaluated using biomarkers such as tissular enzymatic activities of endemic species. Measurement of molluscs bivalves activity at high frequency (e.g., valvometry) during a long time period is another way to record the animal behavior and to evaluate perturbations of the water quality in real time. As the pollution affects the activity of oysters, we consider the valves opening and closing velocities to monitor the water quality assessment. We propose to model the huge volume of velocity data collected in the framework of valvometry using a new nonparametric extreme values statistical model. The objective is to estimate the tail probabilities and the extreme quantiles of the distribution of valve closing velocity. The tail of the distribution function of valve closing velocity is modeled by a Pareto distribution with parameter ??_t,τ, beyond a threshold τ according to the time t of the experiment. Our modeling approach reveals the dependence between the specific activity of two enzymatic biomarkers (Glutathione-S-transferase and acetylcholinesterase) and the continuous recording of oyster valve velocity, proving the suitability of this tool for water quality assessment. Thus, valvometry allows in real-time in situ analysis of the bivalves behavior and appears as an effective early warning tool in ecological risk assessment and marine environment monitoring.     

Predicting bioavailability and bioaccumulation of arsenic by freshwater clam Corbicula fluminea using valve daily activity

There are many bioindicators. However, it remains largely unknown which metal–bioindicator systems will give the reasonable detection ranges of bioavailable metals in the aquatic ecosystem. Various experimental data make the demonstration of biomonitoring processes challenging. Ingested inorganic arsenic is strongly associated with a wide spectrum of adverse health outcomes. Freshwater clam Corbicula fluminea, one of the most commonly used freshwater biomomitoring organisms, presents daily activity in valve movement and demonstrates biotic uptake potential to accumulate arsenic. Here, a systematical way was provided to dynamically link valve daily activity in C. fluminea and arsenic bioavailability and toxicokinetics to predict affinity at arsenic-binding site in gills and arsenic body burden. Using computational ecotoxicology methods, a valve daily rhythm model can be tuned mathematically to the responsive ranges of valve daily activity system in response to varied bioavailable arsenic concentration. The patterned response then can be used to predict the site-specific bioavailable arsenic concentration at the specific measuring time window. This approach can yield predictive data of results from toxicity studies of specific bioindicators that can assist in prediction of risk for aquatic animals and humans.     

Shell disturbances and butyltins burden in commercial bivalves collected from the Bizerta lagoon (northern Tunisia)

Shell disturbances and soft tissues butyltin burden were investigated in commercial bivalves Lithophaga lithophaga, Mytilus galloprovincialis, Solen marginatus and Crassostrea gigas from the Bizerta lagoon. Shell disturbances were found in all bivalves, being scarce in S. marginatus. In the internal valve of L. lithophaga, burrowing annelids and sipunculids living inside galleries were observed, while in the external valve, brown-blackish or white stains were found. In M. galloprovincialis, a yellowish mass located at the shell anterior side was found fixed firmly to the pearly layer by a hard brownish structure covering some annelid elliptic eggs. In the internal shell layer of some specimens collected in April, embryos belonging to tubiculous annelids at various developmental stages were observed. In C. gigas, shell thickening was revealed in some specimens corresponding to white doughy deposits at the internal valve and between shell layers. In S. marginatus, only one specimen showing a cavity at the posterior site was found. Total butyltin concentrations in the studied bivalves varied between 30 and 245?ng/g dry weight with tributyltin (TBT) being the predominant compound. The highest concentration was recorded in L. lithophaga collected from the Bizerta Bay and the lowest concentration in S. marginatus from Maghraoua. This study provided baseline data that could serve for long-term monitoring of TBT pollution in Tunisia, since legislation to reduce the use of TBT-based antifouling paints has not been introduced yet.     

物元分析法在水质监测优化布点中的应用

物元分析法是处理不相容问题的一种有效方法。以竺山湾2010年7月水质监测数据为例，利用物元分析法分析太湖竺山湾水质监测点位分布情况，并将分析结果与系统聚类法的分析结果相比较，发现物元分析法的分析结果是准确、可信的。综合使用物元分析法和系统聚类法，最终确定水质监测点位可由14个优化至11个。     

标准加入法在原子吸收光度法中的应用

介绍了原子吸收光度法中的光谱干扰和非光谱干扰，指出标准加入法和分析校准曲线法是消除和减少某些干扰最简单、快速的校准方法。在标准加入法中，当分析曲线呈线性时，表明分析结果可信，当分析曲线不呈线性，表明方法灵敏度随质量浓度变化而变化，分析结果的准确性有问题。以改变基体的质量浓度和在同一质量浓度的基体溶液中加入不同量的标准两个实验可以验证标准加入法在原子吸收光度法中的适用性。     

X射线荧光分析法及其在环境监测中的应用

综述了X射线荧光分析法在水质分析和大气颗粒物分析中的应用，介绍了粉状固态物、液体、气体等环境试样的制备方法，以及标准曲线法、标准加入法、内标法、散射线监控法、稀释法等定量分析方法，指出X射线荧光分析法前处理简单，分析精度高，操作简便、快速．在环境监测领域具有广阔的发展前景。     

流动注射分光光度法测定水中六价铬的研究

研究建立了测定水中六价铬的流动注射光度分析方法,探讨了利用抗坏血酸的还原性扣除水样中轻度色度或浊度干扰的可行性.本方法线性关系好,检出限低,精密度和准确度高,对地表水、地下水、生活污水、工业废水等实样的测定获得了令人满意的结果.与传统的二苯基碳酰二肼分光光度法相比,具有方法简单、灵敏度高、分析速度快等优点,适用于环境监测的分析工作.