高效液相色谱法测定土壤中多环芳烃的条件优化

研究了加速溶剂萃取(ASE)、固相萃取柱净化(SPE)、高效液相色谱仪(HPLC)联合测定土壤中16种多环芳烃(PAHs)的分析方法,选择以正己烷/丙酮(1+1,V/V)作为ASE提取溶剂,提取液经SPE硅胶小柱净化,正己烷/二氯甲烷(1+1,V/V)进行洗脱,洗脱体积为10 m L,洗脱液经旋转蒸发浓缩至近干,过0.22μm有机滤膜,用乙腈定容至1 m L,最后用HPLC-紫外检测器对提取液中16种PAHs进行定量分析。土壤中16种PAHs的方法检出限为2.8~4.9μg/kg,加标回收率为81.9%~102%,相对标准偏差为2.5%~6.2%,完全满足土壤中PAHs分析的质量控制要求,该法稳定性好、准确度高、可操作性强,适合于土壤样品中16种PAHs的准确测定。     

固相微萃取—气相色谱法测定水中痕量硝基苯类化合物

建立了固相微萃取种类与气相色谱联用测定地下水中12种硝基苯类化合物的分析方法,对萃取头种类、萃取时间、萃取温度、进样口衬管种类等分析条件进行了优化。实验结果表明,该方法的检出限为0.001~0.050 μg/L,线性范围0.005~500 μg/L（相关系数大于0.997）,加标回收率为72.1%~122.0%,相对标准偏差为3.65%~12.60%。应用该方法对地下水及地表水样品进行分析,结果表明该方法具有环保、灵敏、快速、简便等特点,适用于水中痕量硝基苯、硝基甲苯类化合物和硝基氯苯类化合物的测定。     

离子色谱法测定化工废水中有机醇胺类化合物

采用固相萃取-离子色谱法同时测定化工废水中乙醇胺、二乙醇胺、三乙醇胺、N-甲基二乙醇胺和N-丁基二乙醇胺等5种有机醇胺类化合物。通过试验,对固相萃取、离子色谱条件进行优化,优选C_(18)为固相萃取填料,使方法在1.10 mg/L～26.0 mg/L范围内线性良好,方法的检出限为0.72 mg/L～1.02 mg/L。废水样品3个质量浓度水平的加标回收率为84.0%～101%,测定6次结果的RSD为1.7%～12.0%。将该方法用于医药化工企业废水的测定,结果部分醇胺类化合物检出。     

SVD在串联故障电弧检测及选相中的应用*

煤矿井下发生串联故障电弧易引发火灾等安全事故,为了预防电气火灾、指导线路维修,利用三相电动机及变频器负载开展不同线路、不同电流条件下的串联故障电弧实验,研究三相串联故障电弧的检测及选相方法。首先,对单相电流进行一阶差分处理后,建立改进的吸引子轨迹矩阵作为故障特征矩阵;其次,对故障特征矩阵进行奇异值分解,采用特征矩阵的奇异值构建串联故障电弧检测及选相的特征向量;最后,利用极限学习机建立故障电弧检测及选相模型,并测试检测及选相准确率。研究结果表明:提出的SVD方法可以利用单相电流实现三相电动机及变频器负载回路中的串联故障电弧检测及选相。     

SO42-/SnO2 -Fe2O3-硅藻土固体酸催化剂的制备及其对染料废水的催化处理

以硅藻土为载体,采用溶胶-凝胶法引入金属氧化物SnO₂和Fe₂O₃,制备了二元氧化物复合型SO₄^2-/SnO₂-Fe₂O₃-硅藻土固体酸催化剂。利用该催化剂与H₂O₂构成非均相类Fenton试剂氧化体系,催化H₂O₂产生氧化能力极强的·OH,用于处理实际翠蓝废水和模拟亚甲基蓝废水。催化剂的最佳制备条件为：H₂SO₄溶液的浓度3 mol/L,浸渍时间2.0 h,焙烧温度550 ℃,焙烧时间3.5 h,焙烧方式为随炉升降温。实验结果表明：采用在最佳工艺条件下制得的催化剂,处理实际翠蓝废水COD去除率可达79.5%、脱色率达99.6%;处理模拟亚甲基蓝废水COD去除率可达83.1%、脱色率达99.6%。     

SMBR内气液两相流三维CFD模拟

应用CFD软件Fluent对浸没式膜生物反应器(submerged membrane bioreactor,SMBR)内气液两相流进行数值模拟研究,重点考查曝气系统的改变对气液两相流态的影响,并结合PIV实验验证模拟结果,从而为反应器的优化设计及膜污染的控制提供理论依据。模拟结果表明,SMBR内曝气强化了气液两相紊动,膜表面液相速度沿反应器高度增加且形成循环流动,有利于膜面污染物的脱落;反应器内气含率分布不均匀,出现死区,不利于微生物的生长;经实验验证,模拟结果吻合良好。     

Analysis of Organophosphorus Pesticides in Whole Milk by Solid Phase Microextraction Gas Chromatography Method

Solid phase microextraction (SPME) was used for the extraction of residual coumaphos and dichlorvos in whole milk. The residues were analyzed by capillary gas chromatography equipped with nitrogen phosphorus detector (GC-NPD). A manual SPME holder with a 100-μm polyacrylate fiber was used. The optimized conditions for extraction by SPME method were: sample agitation, absorption temperature of 30°C, absorption time of 40 min, desorption time of 10 min, and sample volume was 16.0 mL in the vial. Under these conditions, the calibration graphs were linear in the range of 0.17 μgL^?1 to 1.75 μgL^?1 for coumaphos and 0.69 μgL^?1 to 6.90 μgL^?1 for dichlorvos. Precision was good with RSD values of 13% for coumaphos and 14% for dichlorvos. The detection limits (LOD) were 0.060 μgL^?1 for dichlorvos and 0.052 for coumaphos. The quantification limits (LOQ) were 0.086 μgL^?1 for dichlorvos and 0.066 μgL^?1 for coumaphos. The results obtained in this study suggest that SPME is a suitable technique for residual pesticide analysis of milk. The data demonstrate that particular OP pesticides used in dairy farming in the region of Minas Gerais were found to contaminate cow whole milk, and the residues are not removed by treating the milk by boiling.     

Book Reviews

Books reviewed:
Rutherford H., Platt et al. Disasters and Democracy: The Politics of Extreme Natural Events
S., Suri Orissa Disaster: Agony of the Living     

The Accuracy of Mortality Reporting in Displaced Persons Camps During the Post-emergency Phase

For humanitarian organisations, accurate data are essential to identify emerging health problems and determine programme needs. We visited 45 post-emergency phase displaced persons camps and collected three months' mortality data which we compared with organisations' routine mortality reports. Organisations reported 612 deaths and we identified 741 deaths, for a mortality-reporting ratio, defined as the number of organisation-reported deaths divided by the number of investigator-identified deaths, of 83 per cent. For the majority of camps which under-reported deaths, mortality reporting ratios were significantly higher for women than men, and for camps with central mortality registers rather than those without. In the few camps which over-reported deaths, these occurred primarily among children younger than five years of age, probably due to the inclusion of abortions and stillbirths. Despite the overall under-reporting of deaths by humanitarian organisations, the existing health information systems appear to estimate mortality rates adequately in these post-emergency camps. However, organisations should improve the precision and completeness with which they report the characteristics of deaths in order to provide valuable data to target their programmes at the most vulnerable people.     

自制固相微萃取涂层用于自来水中五氯酚的测定

采用石英毛细管作为模具,甲基丙烯酸和乙二醇二甲基丙烯酸酯在石英纤维表面原位聚合得到聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)作为固相微萃取涂层,并以五氯酚为研究对象,采用顶空SPME-GC-ECD法对该涂层的萃取性能进行评价。使用正交试验优化萃取温度、萃取时间、盐浓度、pH和搅拌速度。在最优条件下,建立了水样中五氯酚的分析方法,方法检出限为1ng/L,线性范围为2～5000ng/L,线性相关系数为0.9999,相对标准偏差(RSD,n=5)为8.9%,加标回收率为110.8%。