环境样品前处理技术及其进展（二）

在前文中讨论了环境样品的制备、前处理的概况，以及超临界流体萃取法。本文将继续报导近年来环境样品制备与前处理领域中其他一些新技术和新方法，包括固相萃取（ＳＰＥ）、微波溶出（ＭＷＤ）和液膜萃取（ＳＬＭ）法，阐述了这些方法的基本原理、操作过程、各种实验参数的影响，及其在环境样品制备与前处理中的应用，并探讨了该领域的发展动向。     

多级硅胶／氧化名柱和GC／MS法测定焚烧炉固体排放物中的痕量PCBs

本文采用多段硅胶柱与碱性氧化铝柱提取纯化焚烧炉烟灰和炉灰中残留的多氯联苯（ＰＣＢｓ）。用１３Ｃ标记物测定了回收率，比较了固体样品的索氏提法和柱直接提取法，结果表明：柱提取方法是一种快速有效测定固体废物中ＰＣＢｓ的方法。应用ＨＲＧＣ／ＭＳ及ＧＣ／ＥＣＤ定量测定了焚烧炉固体排放物中ＰＣＢｓ总残留量及同系物含量。     

二甲基硫醚的真空紫外光电子谱

本文测定了二甲基硫醚（ＤＭＳ）的真空紫外光电子能谱（ＵＰＳ），实验测得的ＤＭＳ的各Ｉｖ（ｃＶ）值与Ｋｉｍｕｒａ的结果一致。８．７９，１１．２９ｅＶ峰指认为硫原子孤对电子ｎｇ，ｎｓ的电子电离，１２．６２ｅＶ峰相应于σｃｓ价电子电离，１４．０３－１５．４２ｅＶ的四个峰相应于πＣＨ３－，πＣＨ３＋电子电离，紫外光辐照影响ＤＭＳ的ＵＰＳ，显示在πＣＨ３有变化。微波放电时ＤＭＳ的ＵＰＳ有明显的影响，有许多新     

SPME-GC-MS联用快速检测赤潮海水中的有机物

本文用固相微萃取（ＳＰＭＥ）样品预处理技术,分离富集海水中的有机物,结合气相色谱－质谱（ＧＣ－ＭＳ）联用技术进行海水中有机物的快速检测,研究了赤潮发生时海水中有机物的种类及含量的变化规律,初步探讨了其变化原因,为研究赤潮的发生机理和赤潮预报提供了科学依据。     

NP型复合纳滤膜对豆腐废水处理的应用

本文对ＮＰ型复合纳滤膜的分离性能进行了初步实验并在此基础上采用纳滤膜平板过滤装置对豆腐加工过程中产生的废水进行处理,以降低废水中的ＣＯＤ含量,实验结果表明,ＮＰ型复合纳滤膜对０．２％ＭｇＳＯ４溶液的截留率（Ｒ）高于９０％,相应秀量约为２０Ｌｍ＾－２．ｈ＾－１（０．４ＭＰａ）,豆腐废水ＣＯＤ的去除率大于９０％     

转化血型用蕃茄α—D—半乳糖苷酶的分离,纯化及理化性质

成熟蕃茄匀浆后，经硫酸铵盐析，ＤＥＡＥ－ＳｅｐｈａｄｅｘＡ－５０离子交换层析，ＳｅｐａｄｅｘＧ－１００凝胶过滤和Ｍｅｌｉｂｉｏｓｅ－Ａｇａｒｏｓｅ亲和层析，获得了α－Ｄ－半乳糖苷酶（Ｃ．Ｅ．３．２．１．１１）。酶制剂经ＰＡＧＥ检测为一条带；ＳＤＳ－Ｇ－ＰＡＧＥ测得酶Ｍ，为３４０００；比活力５２．９Ｕ／ｍｇ．；提纯倍数为５２９０；产率为４５％。酶专一催化以α－Ｄ－半乳糖为末端ａ－（１，３）连接的糖苷     

中国自然保护区管理决策支持系统（NRMDSS）的若干问题探讨

本文回顾了我国自然保护区建设发展状况，对自然保护区管理中存在的一些问题进行了分析，并论述中国自然保护区管理决策支持系统（ＮＲＭＤＳＳ）在自然保护区管理中的地位、作用和意义，探讨ＮＲＭＤＳＳ的系统结构、功能。     

游蛇科4种的核型比较

以骨髓细胞直接制备染色体标本，分析了游蛇属（Ｎａｏｔｒｉｘ）３种和链蛇属（Ｄｉｎｏｄｏｎ）１种蛇的核型．草游蛇（Ｎ．ｓｔｏｌａｔａ）２ｎ＝３６，１８（１５Ｍ＋１ＳＴ＋２Ｔ）·１８ｍ（♀）．渔游蛇（Ｎ．Ｐｉｓｃａｔｏｒ）２ｎ＝４０，１６（１０Ｍ＋１ＳＭ＋３ＳＴ＋２Ｔ）·２４ｍ（♀）．乌游蛇（Ｎ．ｐ．ｐｅｒｃａｒｉｎａｔａ）２ｎ＝４０，１８（８Ｍ十２ＳＭ＋８Ｔ）·２２ｍ（♂）．赤链蛇（Ｄ．ｒｕｆｏｚｏｎａｔｕｍ）２ｎ＝４６，２０（１Ｍ＋３ＳＭ＋１６Ｔ）·２６ｍ（♀）．草游蛇和渔游蛇的Ｎｏｓ，赤链蛇的Ｎｏ３为ＺＺ／ＺＷ型性染色体．草游蛇Ｚ染色体为Ｍ型，Ｗ染色体为ＳＴ型；渔游蛇Ｚ为ＳＭ型，Ｗ也是ＳＴ型；赤链蛇Ｚ为Ｍ型，Ｗ为ＳＭ型．三者Ｚ均略大于Ｗ．草游蛇和渔游蛇Ｎｏ４长臂末端有时可见随体．对游蛇属、链蛇属以及游蛇亚科（Ｃｏｌｕｂｒｉｎａｅ）已知各属种的核型进行了比较和讨论．     

化学质量平衡受体模型新技术的应用──TEDA大气颗粒物来源解析实例

本文结合实例介绍了大气颗粒物来源解析最常用的模型－化学质量平衡（ＣＭＢ）的原理、有效方差最小二乘解法及诊断检验技术，并用ＭＰＩＮ矩阵检验了拟合元素对拟合源的灵敏度，奇异值分解法（ＳＶＤ）鉴别了共线源，得出天津市经济技术开发区（ＴＥＤＡ）的ＴＳＰ主要来源为风沙、扬尘，其次为燃煤飞灰和木灰。     

转化血型用蕃茄α－D－半乳糖苷酶的分离、纯化及理化性质

成熟蕃茄匀浆后，经硫酸铵盐析，ＤＥＡＥ－ＳｅｐｈａｄｅｘＡ－５０离子交换层析，ＳｅｐａｄｅｘＧ－１００凝胶过滤和Ｍｅｌｉｂｉｏｓｅ－Ａｇａｒｏｓｅ亲和层析，获得了α－Ｄ－半乳糖苷酶（Ｃ．Ｅ．３．２．１．１１）。酶制剂经ＰＡＧＥ检测为一条带；ＳＤＳ－Ｇ－ＰＡＧＥ测得酶Ｍｒ为３４０００；比活力５２．９Ｕ／ｍｇ·；提纯倍数为５２９０１产率为４５％．酶专－催化以α－Ｄ－半乳糖为末端ａ－（１，３）连接的糖苷键，以ＰＮＰＧ（对硝基苯－α－Ｄ－半乳糖昔）为废物，酶催化反应的Ｋｍ＝０．１１ｍｍｏｌ／Ｌ，Ｖｍａｘ为６７μｍｏｌ·ｍｇ１－·ｍｉｎ－１．ｔ稳定范是０～３５℃；ＰＨ稳定范围是４．０～７．０．最适ｐＨ为５．１．半乳糖是酶的竞争性抑制剂；Ｃｕ２＋、Ｚｎ２＋、Ｍｎ２＋、Ｆｅ３＋、Ａｇ＋和ＥＤＴＡ对酶活性无影响．纯酶制剂可作为Ｂ型血向Ｏ型血转化的工具酶液．     

Interactions Among the Copper Species and Forms in Sea Water/Sediments and Copper Bioaccumulation in Oysters

Abstract

Earlier papers indicated that the first incident of green discoloration in oysters (Crassostrea gigas) and the mass mortality observed in 1986 along the Taiwan Erhjin Chi coastal area were caused by the higher contents of total copper and copper species (mainly bioavailable and free ion) in sea water. the copper in sea water would be sorbed by suspended matter and transferred to sediments, and the copper in the sediments would also be desorbed to sea water. Processes of copper adsorption and desorption are the major factors influencing the contents of total copper and copper species in sea water and sediments. in this study, the Erhjin Chi sediments were mixed with sea water by a shaker technique. When the mixture was shaken for one hour, analogous to tidal mixing in estuaries, only copper desorption from sediments was observed. If the shaking time is increased for more than 3 hours, the copper released from the sediments was resorbed to the remaining solid phases. the higher the contents of mud (91.71%) and total copper (701 mg kg^?1) in sediments, the higher the copper desorption rate (1.86 ppm hr^?1) and copper adsorption rate (0.50 ppm hr^?1) were observed. in sediments containing lower mud (0.80%) and lower copper (43.5 mg kg^?1), the copper desorption and adsorption rates were 0.83 ppm hr^?1 and 0.22 ppm hr^?1, respectively. the interactions among the total copper and copper species in sea water and sediments, chemical and ecological parameters, and copper bioaccumulation in oysters in the Erhjin Chi estuarine and coastal area are also discussed.     

Interactions Among the Copper Species and Forms in Sea Water/Sediments and Copper Bioaccumulation in Oysters

Earlier papers indicated that the first incident of green discoloration in oysters (Crassostrea gigas) and the mass mortality observed in 1986 along the Taiwan Erhjin Chi coastal area were caused by the higher contents of total copper and copper species (mainly bioavailable and free ion) in sea water. the copper in sea water would be sorbed by suspended matter and transferred to sediments, and the copper in the sediments would also be desorbed to sea water. Processes of copper adsorption and desorption are the major factors influencing the contents of total copper and copper species in sea water and sediments. in this study, the Erhjin Chi sediments were mixed with sea water by a shaker technique. When the mixture was shaken for one hour, analogous to tidal mixing in estuaries, only copper desorption from sediments was observed. If the shaking time is increased for more than 3 hours, the copper released from the sediments was resorbed to the remaining solid phases. the higher the contents of mud (91.71%) and total copper (701 mg kg^-1) in sediments, the higher the copper desorption rate (1.86 ppm hr^-1) and copper adsorption rate (0.50 ppm hr^-1) were observed. in sediments containing lower mud (0.80%) and lower copper (43.5 mg kg^-1), the copper desorption and adsorption rates were 0.83 ppm hr^-1 and 0.22 ppm hr^-1, respectively. the interactions among the total copper and copper species in sea water and sediments, chemical and ecological parameters, and copper bioaccumulation in oysters in the Erhjin Chi estuarine and coastal area are also discussed.     

Dimethylsulfide,algal pigments and light in an Antarctic Phaeocystis sp. bloom

Dimethylsulfide (DMS) concentrations in sea water were found to be high (0.19 to 390 nM) in an Antarctic bloom of Phaeocystis sp. during October and November 1990. DMS concentrations were positively correlated with algal pigments, particularly 19-hexanoyloxyfucoxanthin, a prymnesiophyte pigment. Concentrations of DMS varied diurnally, possibly due to effects of sunlight, although the exact mechanism is unknown. Since oceanic DMS production has been linked to the global albedo through the formation of cloud condensation nuclei, light-mediated changes in DMS concentrations may affect the global climate. The flux of DMS from this bloom into the atmosphere is calculated to be 67±55 mol m^-2 d^-1.     

Dimethylsulphide and ocean–atmosphere interactions

Dimethylsulphide (DMS) is a trace sulphur gas found in most atmospheric and surface water samples, which is derived from dimethylsulphonioproprionate (DMSP). Although it has been extensively studied over the last 50 years, its natural production, consumption and cycling are still not completely understood. Until recently, DMS was believed to originate mainly from marine waters, but later studies have shown that estuaries and lakes are also an important source of DMS. DMS also originates from terrestrial plants such as maize, wheat and lichen, but it is not fully understood why. DMS is believed to have an important impact on the global environment by influencing factors such as the acidity of the atmosphere, cloud condensation nuclei (CNN) and solar insolation. The impact that humans have on the cycling of DMS and on its environmental impact is not well understood either. DMS is affected by temporal and geographical factors, as well as physical factors such as salinity and wind speed, yet when studied under El Niño conditions which modify these physical factors in vivo, there was found to be no fluctuation in the concentration of DMS in the water column. This review outlines our current state of knowledge on DMS.     

饮用水中苯并（a）芘的毛细管气相色谱分析

本文叙述了应用毛细管气相色谱测定饮用水中苯并（ａ）芘含量的方法，二氯甲烷用做提取剂，萃取１Ｌ水样，提取液在微沸状态下蒸干并定容，以不分流方式注入色谱仪进样口，样品在５０Ｍ张的ＳＥ－５４毛细管色谱柱上分离，氢火焰离子化检测器检测后，进行定性定量分析，方法的检测下限达２．５ｎｇ／ｌ，不仅能满足生活饮用水，也可满足天然饮用矿泉水，湖水，河水等水体中苯并（ａ）芘的检测。     

Synthesis of 2,3-dihydroxynaphthalene-functionalized Amberlite XAD-4 resin: Applications for the separation and preconcentration of trace metal ions prior to their determination by inductively coupled plasma atomic emission spectrometry

A simple, sensitive column solid-phase extraction procedure for separation and preconcentration of Cu(II), Ni(II), Co(II), and Cd(II) in spiked and natural water samples using 2,3-dihydroxynaphthalene-functionalized Amberlite XAD-4 (XAD-4-DHN) chelating resin prior to their determination by inductively coupled plasma atomic emission spectrometry was discussed. The optimum experimental parameters such as pH, volume of sample and eluent, flow-rates of uptake and stripping, and sorption capacity of the chelating resin, were evaluated. The effect of the electrolytes and the cations on the preconcentration of metal ions was also investigated. The chelating resin could be reused for more than 20 cycles of sorption–desorption without any significant change (<1.0%). Recoveries obtained from this method range from 96 to 102% with R.S.D of 2.50 (n = 4). The detection limits for Cu(II), Ni(II), Co(II), and Cd(II) were found to be 1.9, 0.9, 1.2 µg, and 1.4 µg L^?1, respectively. The proposed method was applied for the determination of Cu(II), Ni(II), Co(II), and Cd(II) in spiked, tap water, and river water samples.     

钯卟啉室温磷光氧传感器的研究

1　IntrudctionOxygensensorsareofgreatimportanceinenvironmentalmonitoring (e g.,theamountofoxy gendissolvedinwaterisanindicatorofthequalityofwaterbecauseadecreaseinthisamountusual lyindicatesthepresentoforganicwaste) ,inindustrialprocesscontrol (e g.carefu…     

Enhanced desorption of fluoxetine from polyethylene terephthalate microplastics in gastric fluid and sea water

There are concerns that microplastics act as a vector of pharmaceuticals in the aquatic environment. Most studies have focussed on pharmaceutical adsorption and have not investigated desorption in the various matrices that microplastics enter. Therefore we studied the desorption of the antidepressant drug fluoxetine from polyethylene terephthalate (PET) microplastics in river water, sea water, and simulated gastric and intestinal fluids. We found that most desorption occurred rapidly, within a few hours of exposure. Fluoxetine desorption fitted well to the Freundlich isotherm with r² values ranging from 0.97 to 0.99. Desorption decreased in the following order: gastric fluid at 20 °C and 37 °C; sea water at 20 °C; intestinal fluid at 20 °C and 37 °C; then river water at 20 °C. The little difference in desorption in gastrointestinal fluids at 20 °C and 37 °C suggests a similar exposure risk to cold- and warm-blooded organisms following PET microplastic ingestion. Total desorption following sequential incubation 2 h in gastric fluid then 4 h in intestinal fluid to mimic gastrointestinal digestion was 37% at 20 °C and 41% at 37 °C. Interestingly, higher desorption of 18–23% occurred in sea water compared to river water, of 4–11%. Under a worst-case scenario, more than 44 mg kg⁻¹ body weight d⁻¹ or more than 52 mg kg⁻¹ body weight d⁻¹ of PET microplastics from river water or sea water, respectively, need to be consumed to exceed the mammalian acceptable daily intake for fluoxetine. Further studies are needed on microplastic ingestion and the bioavailability of adsorbed pharmaceuticals to a range of exposed aquatic organisms.

     

固相微萃取-气相色谱/质谱联用法测定饮用水中苯类化合物

用固相微苹取(ＳＰＭＥ)－气相色谱/质谱联用法测定饮用水中苯类化合物,以１００μｍ ＰＤＭＳ(聚二甲基硅氧烷)萃取针提取、浓缩、分离与测定九种目标化合物．萃取时间经优化选定为８ｍｉｎ,而热解析时间设定为２ｍｉｎ． 本方法的相对标准偏差小于５%,线性范围宽(２０ｎｇ·ｍｌ－１－１００００ｎｇ·ｍｌ－１),多数化合物的检测限低于５μｇ·ｌ－１．饮用水样品检测显示,样品加标回收率范围在８４%至１１０%内．     

Reagenzienfreie Bestimmung von Quecksilberspuren in Wasserproben

A comprehensive ecological monitoring of hazardous substances is indispensable to preserve our health and environment. Therefore, fast and inexpensive techniques for routine analysis of pollutants are essential. However, in the measuring procedure itself often toxic reagents are used producing hazardous waste. Omitting environmentally hazardous substances in the analysis procedure is an important contribution to a more sustainable and green analytical chemistry. A reagent-free method for ultra-trace (pg to ng?L^-1) mercury determination in water samples was developed and validated. An active nanogold collector integrated in a fully automated flow injection system is the core of this new method. All mercury species dissolved in the water sample are adsorbed and preconcentrated on the nano-structured gold surface of the collector. After rinsing and drying of the collector, the enriched mercury is thermally desorbed and finally measured by atomic fluorescence spectrometry. This method was optimized and validated for the determination of mercury in natural waters. The influence of various water constituents was investigated and only high contents of dissolved organic carbon (DOC) showed interferences of mercury preconcentration due to the strong complexation of mercury by DOC. This restriction can be solved by UV-irradiation, i.?e. reagent-free digestion of DOC rich samples prior to the preconcentration procedure. Mercury concentration of several natural river and sea waters and water from the discharge of a waste water treatment plant were determined with this new analytical method. Accuracy and precision of the method were demonstrated by several recovery experiments in natural water samples (recoveries: 96–102?%) and by analysis of the certified reference material BCR-579 (Mercury in Coastal Sea Water; recovery: 101?±?1?%). With a detection limit of only 80?pg?Hg?L^–1 the proposed method is highly sensitive. Furthermore the method avoids potential contamination of the sample by reagent addition and is due to the reagent-free procedure environment-friendly. Hence this work is an important contribution to sustainable environmental analysis and at the same time improves accurate routine mercury trace analysis.