固载化瓜环的制备及其对磺胺间甲氧嘧啶的吸附性能研究

在微波无极灯下将烯氧基瓜环固载到巯基硅胶(MSG)上,制得固载化瓜环(ACB[6]-SG).通过红外光谱表征固载产物,并研究固载化瓜环对磺胺间甲氧嘧啶(SMM)的吸附性能.结果表明,SMM在固载化瓜环上的吸附基本在2 min内即可达到平衡;Henry方程和Freundlich方程均能较好地拟合SMM在固载化瓜环和巯基硅胶上的等温吸附曲线,但是SMM在固载化瓜环上的吸附主要是在瓜环中的分配,而SMM在巯基硅胶上的吸附则主要是多分子层的表面吸附作用;SMM在固载化瓜环上的平衡吸附量远大于在巯基硅胶上的平衡吸附量;SMM在两者上的吸附过程是一个放热过程,温度越低吸附效果越好.     

氟虫双酰胺在水稻和稻田中的残留动态研究

采用超高效液相色谱法(UPLC)测定了氟虫双酰胺19.8%悬浮剂(SC)在水稻及稻田环境中的残留动态.结果表明,当氟虫双酰胺及其代谢产物NNI-des-iodo的添加量为0.05～1.0 mg·kg-1时,其在水稻田土壤、田水、稻秆、稻米和稻壳中的平均回收率为78.2%～104.8%,变异系数为1.1%～4.4%.氟虫双酰胺在2011年三地(福建福州、天津、江苏南京)的稻田水中的降解半衰期为9.8～17.3 d,土壤中10.8～22.4 d,植株中7.6～17.3 d,其在稻田水样品中检出了代谢产物NNI-des-iodo,而在土壤和植株样品中未检出.在推荐使用剂量下,于末次施药10 d后,氟虫双酰胺在水稻稻米中的残留量均低于美国规定的在稻谷上的最大残留允许量(0.5 mg·kg-1).     

Application of comprehensive two-dimensional gas chromatography with mass spectrometric detection for the analysis of selected drug residues in wastewater and surface water

Pharmaceutical residues have become tightly controlled environmental contaminants in recent years, due to their increasing concentration in environmental components. This is mainly caused by their high level of production and everyday consumption. Therefore there is a need to apply new and sufficiently sensitive analytical methods, which can detect the presence of these contaminants even in very low concentrations. This study is focused on the application of a reliable analytical method for the analysis of 10 selected drug residues, mainly from the group of non-steroidal anti-inflammatory drugs (salicylic acid, acetylsalicylic acid, clofibric acid, ibuprofen, acetaminophen, caffeine, naproxen, mefenamic acid, ketoprofen, and dicofenac), in wastewaters and surface waters. This analytical method is based on solid phase extraction, derivatization by N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) and finally analysis by comprehensive two-dimensional gas chromatography with Time-of-Flight mass spectrometric detection (GC×GC- TOF MS). Detection limits ranged from 0.18 to 5 ng/L depending on the compound and selected matrix. The method was successfully applied for detection of the presence of selected pharmaceuticals in the Svratka River and in wastewater from the wastewater treatment plant in Brno-Modrice, Czech Republic. The concentration of pharmaceuticals varied from one to several hundreds of ng/L in surface water and from one to several tens of μg/L in wastewater.     

Simultaneous preconcentration of cadmium and lead in water samples with silica gel and determination by flame atomic absorption spectrometry

A new method that utilizes pretreated silica gel as an adsorbent has been developed for simultaneous preconcentration of trace Cd(II) and Pb(II) prior to the measurement by flame atomic absorption spectrometry. The effects of pH, the shaking time, the elution condition and the coexisting ions on the separation/preconcentration conditions of analytes were investigated. Under optimized conditions, the static adsorption capacity of Cd(II) and Pb(II) were 45.5 and 27.1mg/g, the relative standard deviations were 3.2% and 1.7% (for n = 11), and the limits of detection obtained were 4.25 and 0.60 ng/mL, respectively. The method was validated by analyzing the certified reference materials GBW 07304a (stream sediment) and successfully applied to the analysis of various treated wastewater samples with satisfactory results.     

顶空气相色谱法同时测定空气中甲醇和乙醇

顶空气相色谱测定空气中甲醇和乙醇含量,以蒸馏水吸收空气中甲醇和乙醇,顶空进样经DB-624毛细管柱分离,氢火焰离子化检测器检测。实际操作证明,该法能满足工业废气和空气中的甲醇和乙醇的监测。     

离子色谱法测定环境空气中丁酸

建立了用离子色谱法测定环境空气中丁酸的新方法。对实际样品进行分析,丁酸的回收率为94．5％-103．8％,当采样体积为60L时环境空气中丁酸的检出限为0．003mg／m^3。本方法分析速度快,所需样品量少,且无需复杂的前处理,简便、灵敏、可靠。     

气相色谱法测定大气中乙酸乙酯和甲基丙烯酸甲酯

建立了用气相色谱法测定大气中乙酸乙酯和甲基丙烯酸甲酯的方法。大气中乙酸乙酯和甲基丙烯酸甲酯活性炭吸附,二硫化碳解吸,DB-200毛细管柱分离,直接进样分析,氢火焰离子化检测器检测,时间定性,峰面积定量。本方法前处理简便,分离度好,分析灵敏度高,满足环境分析要求。     

离子色谱法测定废气中硫酸雾实验研究

文章建立了离子色谱法测定废气中硫酸雾的分析方法,制备好的样品经0．45um微孔滤膜抽滤,采用AS14A阴离子交换色谱柱分离,电导检测器检测,以0．8mmol／L碳酸钠和0．1mmol／L碳酸氢钠混合溶液为流动相,流速为0．5ml／min进行测定,以保留时间定性,峰面积进行定量,方法的适用范围为0．50～50mg／m3。与铬酸钡分光光度法进行比对试验,无显著性差异。该方法操作简便、灵敏度高、准确度好,实用性强,适用于大批量环境样品的分析。     

热脱附-气相色谱-质谱法测定环境空气中5种挥发性卤代烃

建立热脱附-气相色谱-质谱联用测定环境空气中三氯甲烷、四氯化碳、三氯乙烯、四氯乙烯、溴仿等5种挥发性卤代烃的分析方法。该方法在一定浓度范围内工作曲线线性良好,相关系数均在0．9990～0．9998之间,加标回收率在94．0％～106．6％之间,RSD为2．18％-7．62％,检出限为0．22μg／m3～0．30μg／m3。该方法具有操作简单、分析快速、准确度高、灵敏高的特点,用热脱附-气相色谱-质谱联用测定环境空气中5种挥发性卤代烃,结果令人满意。     

在线气相色谱测定园区中特征污染因子研究

近两年来,随着科学技术的不断发展,在线气相色谱分析仪已逐步在国内监测实际中得到应用,在线气相色谱的应用使挥发性有机物的实时、连续监测成了可能,有效改善了实验室监测数据的滞后性,减少了样品采集、储存、运输过程中产生的误差,结合常州市某化工园区大气特征污染因子预警系统的建设情况,简单介绍了在线气相色谱的工作原理和过程。通过特征污染因子标准曲线的建立和比对试验,说明了在线气相色谱环境监测应用的可行性。