水中苯胺类化合物分析的难点

结合实验研究了水中苯胺类化合物的测定难点和影响因素，包括样品保存和水样中悬浮物的影响。苯胺类化合物易被氧化，样品不易保存且受悬浮物的影响。研究结果表明：样品中未加入抗氧化剂进行保存时，部分苯胺类化合物迅速降解；当样品中加入80 mg/L硫代硫酸钠进行保存时，部分苯胺类化合物的保存时间可以延迟2~3 d后降解。样品中悬浮物对联苯胺萃取影响较大，回收率偏低，可以通过调节样品pH至酸性后过滤，再将滤液调至中性后进行萃取，回收率明显提高。笔者同时讨论了消除与补偿基质干扰的方法，包括色谱分离条件和检测器条件的选择、优化，内标法、空白基质匹配标准校正法和工作曲线法等定量方法的选择。     

地表水中丁基黄原酸的保存条件研究

通过对不同基质地表水样中丁基黄原酸在p H值、温度、光照、保存时间等条件下进行保存研究,确定对其保存效果的影响为:保存时间保存温度样品中丁基黄原酸浓度光照强度p H值。建议地表水样品使用棕色玻璃瓶盛装,于4℃下避光保存原水。高浓度样品,保存时间不超过5 d;低浓度样品,保存时间不超过1 d,最好采样后立即分析。     

富集在GDX树脂上的酚类污染物的贮存条件研究

本文研究ＴＧＤＸ树脂富集柱富集酚后，在各种保存剂中室温柱上贮存的适宜条件．实验表明，被富集的酚在水溶液中贮存的效果均优于在有机溶剂中．而水溶液保存剂中，又以Ｎａ２Ｓ２Ｏ３·５Ｈ２Ｏ（１ｇ／Ｌ）－Ｎａ２ＣＯ３（０．１ｇ／Ｌ）水溶液的贮存效果最佳，富集后的９种一元酚在该保存剂中室温密封蔽光贮存８天后，总酚损失仅约１５％，大大优于现行含酚水样的保存方法。     

PT-GC-CVAFS法测定沉积物中甲基汞的影响因素及应用

研究了碱提取吹扫捕集气相色谱冷原子荧光光谱法测定沉积物中甲基汞的影响因素，包括载气流速、柱温、衍生化试剂、样品称取量、前处理时碱性提取液加入量和反应瓶中提取液加入量的影响，分析了提取液加入量对Tenax管的影响、提取液保存的影响因素、沉积物样品保存的影响因素以及样品中Hg²⁺的干扰影响。根据影响情况确定最佳测定条件，应用于广西龙江河流域上9个代表性监测断面的底泥样品中甲基汞的测定，采用污染指数法对该流域甲基汞的污染现状进行评价。结果表明，最佳载气流速范围为22～27 mL/min,最佳柱温为46℃。衍生化试剂选择四乙基硼化钠和四丙基硼化钠均能达到较好的回收率。样品称取量选择0.50 g时回收率好。前处理时碱性提取液的加入量对甲基汞的提取效率没有显著影响。为保证水相衍生反应体系最终pH在5左右，乙酸-乙酸钠缓冲溶液的加入量随提取液加入量的增加而增加。当缓冲溶液为300μL时，提取液小于150μL不会影响Tenax管性能。避光与否对提取液的保存和样品的保存影响都不大，提取液保存3 d后、样品保存15 d后，甲基汞回收率将低于80%。衍生化前定量体积提取液中Hg     

气体样品的保存及其成分的变化

介绍了气体样品的各种保存方法及其在保存过程中成分变化的特点，以降低气体保存过程中的损失，提高监测管理水平。     

氰化钾标准中间液保存时间试验

在《水和废水监测分析方法》（第四版）异烟酸-吡唑啉酮光度法测定总氰化物中，需将10mg／L氰化钾标准中间液在临用前再稀释10倍，配成1．0mg／L标准使用液。该方法没有对氰化钾标准中间液保存时间作明确要求，为保证分析结果的准确性，也为提高工作效率，对氰化钾标准中间液在2℃-4℃时的保存时间作试验，测定结果见表1。     

水中痕量砷的富集测定方法

实验部分 一、巯基棉的制备方法:取硫代乙醇酸20ml、乙酸酐14ml,混匀后加入浓硫酸2滴,摇匀并冷却至室温,加脱脂棉4g浸湿,室温放置24小时以上。用蒸馏水洗至中性、挤干残存水,放入37～38℃烘箱中烘干后放入棕色磨口瓶中保存。在避光、密闭、较低温度下可保存一年以上。 二、冷原子荧光法间接测定痕量砷的方法: 分别加入0,0.4,0.8,1.2,1.5μg As于含100ml去离子水的砷化氢发生瓶中,再加入1:1硫酸13ml,20％碘化钾2ml,40％氯化亚锡5ml,摇匀后煮沸5min。冷却后加无砷锌粒4g,生成的砷化氢通过10％醋酸铅溶液     

紫外分光光度法在水中亚硝酸盐氮标样研制中的应用

1.主要仪器和试剂UV3000紫外/可见分光光度计和751型紫外可见分光光度计2.5mg/L亚硝酸盐氮标准物质:准确称取0.0246g亚硝酸钠,溶解定容于2000ml容量瓶中.混合均匀后定量封装于安瓿中,高温高压灭菌后室温下保存.     

水样中痕量六价铬的保存

建议用硬质玻璃瓶盛水样。水中含还原性无机物较多时,可用NaOH调pH为9～10,后加入2m12N醋酸锌(1升水),以保证六价铬不被还原。天然水样室温保存,工业废水样必须冰箱保存。     

降水中甲酸、乙酸和草酸的离子色谱法测定及样品保存研究

甲酸、乙酸和草酸是降水中有机酸的主要成分。研究选用离子色谱法同时测定降水中的甲酸、乙酸和草酸,并对降水样品中3种有机酸的保存条件进行了研究。优化后的色谱条件为4. 0 mmol/L Na_2CO_3和1. 2 mmol/L NaHCO_3混合淋洗液,淋洗液流速为1. 0 m L/min,进样体积为200μL,电导池温度为30℃,柱温为室温。甲酸、乙酸和草酸的检出限分别为0. 002、0. 005、0. 005 mg/L,实际降水样品测定时平行样的相对标准偏差为1. 4%～12%,加标回收率为95%～118%。样品采集后需尽快用0. 45μm聚醚砜微孔滤膜过滤,4℃以下冷藏密封保存,2 d内测定。若用氢氧化钠溶液调节p H至8～10,样品可保存7 d。     

绍兴市典型印染废水中重金属锑排放现状及排放源调查

分析和统计的86家印染工业企业当中,废水总排口中的总锑超标率为25.6%,质量浓度0.050 mg/L以下较低排放浓度所占比例最大,达62.8%。印染废水锑排放源主要有涤棉和涤纶化纤类布料的染色、印花工艺废水,碱减量工艺废水等,工业液碱、废酸以及硫酸铝污水处理剂等原料当中含锑浓度较高。印染废水经污水处理厂集中纳管深度处理后,锑排放浓度较低,锑去除效率最高达到88.0%,大大降低了环境地表水体锑污染的风险。     

Determination of antimony in human blood with inductively coupled plasma-mass spectrometry

A method is presented for the determination of antimony in whole human blood samples with an ICP-MS instrument using a quadrupole mass analyzer. A nitric acid/hydrogen peroxide open digestion procedure was employed for the blood sample treatment and preparation for analysis. The precision and accuracy of the method were evaluated by analyzing several Seronorm trace elements whole blood reference materials. The precision of the method at various antimony levels was better than 4% RSD and the recovery was greater than 92% at all levels. The detection limit, calculated as three times the standard deviation of the blank (3sigma, n= 12), was 0.03 microg L(-1). The method was successfully applied for the determination of antimony in blood samples from school children in rural areas of Kwazulu/Natal, South Africa and adults from Dearborn, Michigan. Blood antimony levels ranged from <0.03 to 3.82 microg L(-1) in children and 1.40 to 4.35 microg L(-1) for adults.     

Monitoring of copper,arsenic and antimony levels in agricultural soils impacted and non-impacted by mining activities,from three regions in Chile

This paper reports a comparative study of the concentration of three important environmental elements that are often found together in mineral deposits and then associated with mining activities; copper, arsenic and antimony. These elements were determined in 26 different agricultural soils from regions I, II and V in Chile, zones where the most important and biggest copper industries of this country are located. As background levels of these elements in soils have not been well established, in this study, both, impacted and non-impacted agricultural soils from different regions were considered. The relationships between the concentrations of these elements in soils were also examined. The concentration ranges for copper, arsenic and antimony were 11-530; 2.7-202 and 0.42-11 mg kg(-1) respectively. The copper concentrations in non-polluted soils from the north and central zone of Chile were similar. However, three sites from the north region have copper concentration as higher as 100 mg kg(-1), values that exceed the critical concentration for copper in soils. The concentration of arsenic and antimony in the north soils were higher than in non-impacted ones and, in the case of arsenic, greatly exceeded the world average concentration reported for this element in soils. The highest arsenic and antimony concentrations were found in Calama and Quillagua soils, two different sites in the Loa valley. The arsenic/antimony concentration ratio was higher in Quillagua soil. The high concentrations of three elements determined in impacted soils from region V (Puchuncaví and Catemu valleys) clearly shows the impact produced in this zone by the industrial and mining activities developed in their proximities. At Puchuncaví valley a clear decrease was observed in copper, arsenic and antimony concentrations in soils on the function of the distance from the industrial complex "Las Ventanas", and all concentrations exceeded the reported critical values for this matrix. Instead at Catemu valley, only the copper concentration was higher than this value. Statistically significant correlation was found for Cu-Sb in all soils; more significant Cu-As, Cu-Sb and Sb-As correlations were evaluated for soils from Puchuncaví and Catemu valleys, corroborating that high concentrations of copper, arsenic and antimony in these soils coming from the same pollution sources, the copper industry and the thermoelectric power plant.     

五日生化需氧量测定中稀释倍数的估算

假定样品经过培养后耗氧率达５５％；推导出ＢＯＤ５稀释倍数Ｋ＝ＢＯＤ５／４．４，由稀释程度规定推导出ＢＯＤ５稀释倍数Ｋ＝（ＢＯＤ５－１）／４．０两种方法Ｋ基本相同，标准样品，工业废水经上述方法稀释后，测定结果比较满意，尤其对工业废水测定，既缩短了分析时间，又降低了测定误差。     

用Excel制作环境监测声像报告

阐述了运用办公自动化应用软件电子表格Ｅｘｃｅｌ制作及播放新型声像片的方法，并以环境监测工作中的实例介绍了具体的制作过程。     

生物监测技术在工业废水监测领域的应用研究

生物监测可以系统反映污染物对生物生长的影响及其在生物体内的转化和迁移,在水环境监测与生态健康管理中的重要性日益突出。伴随着工业化的快速发展,中国水环境污染问题依然严峻,工业废水治理和排放问题仍旧突出。为进一步保障工业废水出水及受纳水体水质安全,迫切需要在工业废水监测中引入生物监测技术。对传统微生物群落监测法、水生生物毒性监测法和基于分子生物学技术的微生群落监测法等在工业废水监测领域的研究及应用进行了综述,并对存在的问题进行了总结。建议后续进一步完善工业废水生物监测体系时,参考国外成熟经验,制定出符合国内需求及特征的工业废水生物监测方法与评价标准,以便更好地掌握工业区整体环境健康及污染状况。     

Antimony speciation in terrestrial plants. Comparative studies on extraction methods

A suitable method for the extraction of antimony species from plant materials prior to IC-HG-AFS analysis is presented. The extraction efficiency with different extraction systems using various aqueous and aqueous/solvent mixtures was initially evaluated by analysing the Virginia Tobacco Leaves Certified Reference Material. The concentration of antimony extracted was compared with the total antimony content in the plant material measured by HG-AFS after focused microwave-acidic digestion using HNO3 and H2O2. The proposed extraction procedures were applied to antimony speciation in several plants from a natural terrestrial environment impacted by mining activities. End-over-end agitation (4 h) followed by sonication (1 h) extraction using 0.1 mol l(-1) citric acid was found to provide the best extraction efficiency while also giving reliable speciation information. Both inorganic and methylantimony species were found in the extractable portion of some terrestrial plants.     

Comparison of fecal coliform bacteria before and after wastewater treatment plant in the Izmir Bay (Eastern Aegean Sea)

The distribution of fecal coliforms was investigated and determined in Izmir Bay from 1996 to 2005. Izmir Bay severely was polluted from industrial and domestic discharges during decades. In early 2000, a wastewater treatment plant began to treat domestic and industrial wastes. This plant treats the wastes about 80% capacity after 2001. The sampling periods cover before and after treatment plant. Assessment method for determining the number of fecal coliform has evolved membrane filtrations. Maximum surface fecal coliform concentration was 4.9 × 10⁵ cfu 100 ml^???1 in 1996–2000 period. Following the opening treatment system, fecal coliform density decreased 2.1 × 10⁴ cfu 100 ml^???1 during 2001–2005. A continuous improvement can be sustained in the water quality if direct inflow of untreated wastewater is prevented.     

液相色谱-串联质谱法同时测定污水中10种精神活性物质

建立了采用液相色谱-串联质谱法(LC-MS/MS)同时测定污水中10种精神活性物质的分析方法。污水样品经甲酸与甲酸铵调节pH后,加入氘代内标混匀,离心并过滤膜后可直接上样分析。研究表明,在1~250 ng/L的线性范围内,10种精神活性物质的线性相关系数均大于0.992,定量限均低于0.5 ng/L。在3个加标水平下,10种精神活性物质的加标回收率为87.2%~114%,相对标准偏差为0.53%~3.60%(n=3)。将该方法应用于某区域10份生活污水样品的检测,在3份水样中检出吗啡、甲基苯丙胺、氯胺酮等精神活性物质,对应的质量浓度范围分别为3.41~9.55、0.90~1.63、1.06~1.78 ng/L。与经固相萃取前处理后的分析方法相比,该方法可在10 min内完成分离和检测的全过程,具有简单、快速、节约的优点,可用于污水样品中10种痕量水平精神活性物质的定量分析。     

Determination of total Cr in wastewaters of Cr electroplating factories in the I.organize industry region (Kayseri, Turkey) by ICP-AES

The wastewater pollution in industrial areas is one of the most important environmental problems. Heavy metal pollution, especially chromium pollution in the wastewater sources from electroplating, dyeing, and tannery, has affected the life on earth. This pollution can affect on all ecosystems and human health directly or by food chain. Therefore, the determination of total chromium in this study is of great importance. In this study, accurate, rapid, sensitive, selective, simple, and low-cost technique for the direct determination of total Cr in wastewater samples collected from the some Cr electroplating factories in March 2008 by inductively coupled plasma-atomic emission spectrometry has been developed. The analysis of a given sample is completed in about 15 min by this technique applied. As the result of the chromium analysis, the limit of quantification for the total Cr were founded to be over the limit value (0.05 mg L^???1; WHO, EPA, TSE 266, and inland water quality classification) as 1,898.78 ± 0.34 mg/L at station 1 and 3,189.02 ± 0.56 mg/L at station 2. The found concentration of total Cr has been determined to be IV class quality water according to the inland water classification. In order to validate the applied method, recovery studies were performed.