固相萃取/气相色谱-质谱法对土壤中有机氯农药的分析及基质效应研究

建立了一种固相萃取/气相色谱-质谱法同时测定土壤中23种有机氯农药的方法,并研究了不同基质效应补偿方式。土壤样品经正己烷∶丙酮(体积比1∶1)提取,弗罗里土小柱净化,采用气相色谱-质谱仪检测。结果发现7种有机氯存在中/强程度的基质效应;在10 mL二氯甲烷∶正己烷(体积比1∶9)+10 mL丙酮∶正己烷(体积比1∶9)为固相萃取的洗脱剂,且脉冲压力为275.8 kPa条件下,可将23种有机氯的基质效应均控制在20%以内。23种有机氯农药在0.4～10μg·mL~(-1)质量浓度范围内线性良好,相关系数(r~2)均不小于0.999 2,检出限为1.0～8.6μg·kg~(-1),定量下限为4.0～34.4μg·kg~(-1);在20、60、100μg·kg~(-1)3个加标水平下空白土壤中的平均回收率为46.3%～127%,相对标准偏差(n=6)为0.68%～15%。采用该方法在某土壤样品中检出α-六六六、γ-六六六、p,p′-DDE、异狄氏剂醛、p,p′-DDT 5种有机氯农药。     

高效液相色谱–串联质谱法同时测定土壤中8种杀菌剂残留

建立高效液相色谱-串联质谱法同时测定土壤中戊唑醇、腈菌唑、腈苯唑、氟硅唑、三唑酮、丙环唑、烯唑醇、苯醚甲环唑8种杀菌剂残留量的方法。采用QuEChERS样品前处理方法对土壤样品进行提取、净化和富集,用电喷雾离子源、正负离子扫描,以多反应监测(MRM)模式进行定性和定量分析。在优化的实验条件下,8种杀菌剂的质量浓度在0.01~0.50 mg/L范围内与色谱峰面积均成良好的线性关系,相关系数均大于0.995,方法检出限为0.005~0.010 mg/kg。样品平均加标回收率为85.6%~102.2%,测定结果的相对标准偏差为4.6%~13.2%(n=5)。该方法操作简便,灵敏度和准确度高,满足土壤中戊唑醇等8种杀菌剂残留量的测定要求。     

Enantioselective separation and dissipation of pydiflumetofen enantiomers in grape and soil by supercritical fluid chromatography–tandem mass spectrometry

Pydiflumetofen is registered in many countries and is widely used in crop production in the racemate form. However, the environmental behavior of the enantiomers has not been studied. An effective and sensitive chiral analytical method was first established for analyzing the pydiflumetofen enantiomers by supercritical fluid chromatography with tandem triple quadrupole mass spectrometry. The enantiomers could be separated and detected using the Chiralcel OD‐3 column in less than 3 min. The separation conditions were as follows: mobile phase, CO₂/methanol (80:20); flow rate, 1.0 mL/min; column temperature, 30°C, auto back‐pressure regulator pressure, 2000 psi with modified quick, easy, cheap, effective, rugged, and safe sample treatment method. The average recoveries of analytes from both matrices at three spiking levels were in the range of 84.1–103.0%. The limit of quantitation for each enantiomer was 0.005 mg/kg with a baseline resolution of approximately 1.64. The method was applied to monitor the enantioselective dissipation of pydiflumetofen in grape and soil. In grapes, (?)‐pydiflumetofen was degraded more rapidly than (+)‐pydiflumetofen. In soil, (+)‐pydiflumetofen was preferentially degraded. The data provided useful references for the risk assessment and rational use of pydiflumetofen in agriculture.     

激光烧蚀脉冲放电激发的土壤等离子体电子数密度和温度的研究

以激光烧蚀快脉冲放电激发土壤为例,研究了激光烧蚀快脉冲放电等离子体技术产生的土壤等离子体的电子数密度和温度。根据实验测得的Si原子和离子谱线的强度和萨哈玻尔兹曼方程,计算了等离子体的电子温度,并从分析Si I 250.69nm谱线的斯塔克展宽中导出了等离子体的电子数密度。与使用同样激光能量激发的激光等离子体相比,激光烧蚀快脉冲放电激发等离子体的电子数密度和温度都明显增加,与观察到的光谱信号强度是一致的。     

土壤重金属铬元素的激光诱导击穿光谱定量分析研究

利用Nd ∶YAG脉冲激光器(波长:1064 nm)作为光源,在实验室自然大气环境下诱导产生土壤激光等离子体,通过等离子体原子发射光谱法定量分析了国家标准土壤样品中元素Cr的含量.实验上研究了在最佳实验条件下土壤中Cr的LIBS分析谱线,测定了Cr元素的定标曲线.实验结果表明,Cr元素浓度在(60—400)×10^-6范围内,元素含量与光谱线强度之间有较好的线性关系;元素Cr浓度分析测量的相对标准偏差(RSD)为7.89%,定量分析结果与标准值的相对偏差为5.3%,Cr元素的检测限为1 关键词： 土壤污染 定量分析 激光诱导击穿光谱 定标曲线     

污染土壤的物化修复治理技术研究

污染土壤的修复治理过程中,物化技术以其快速高效的特点成为国内外研究的热点。本文通过对工程措施、玻璃化技术、热修复、电动力修复、光化学降解、化学淋洗、化学固定/稳定化、化学氧化以及联合修复等常见土壤物化治理技术进行了分析,探讨了各种工艺技术的性能及优缺点,旨在为我国土壤污染修复治理技术的选择提供参考。     

Determination of Prometryne in water and soil by HPLC-UV using cloud-point extraction

A CPE-HPLC (UV) method has been developed for the determination of Prometryne. In this method, non-ionic surfactant Triton X-114 was first used to extract and pre-concentrate Prometryne from water and soil samples. The separation and determination of Prometryne were then carried out in an HPLC-UV system with isocratic elution using a detector set at 254 nm wavelength. The parameters and variables that affected the extraction were also investigated and the optimal conditions were found to be 0.5% of Triton X-114 (w/v), 3% of NaCl (w/v) and heat-assisted at 50 °C for 30 min. Using these conditions, the recovery rates of Prometryne ranged from 92.84% to 99.23% in water and 85.48% to 93.67% in soil, respectively, with all the relative standard deviations less than 3.05%. Limit of detection (LOD) and limit of quantification (LOQ) were 3.5 μg L⁻¹ and 11.0 μg L⁻¹ in water and 4.0 μg kg⁻¹ and 13.0 μg kg⁻¹ in soil, respectively. Thus, we developed a method that has proven to be an efficient, green, rapid and inexpensive approach for extraction and determination of Prometryne from soil samples.     

ICP-OES法测成都市三环内表层土壤13种金属元素含量

采用电感耦合等离子体发射光谱(ICP-OES)法同时测定成都市三环内表层土壤13种金属元素含量与分布.研究显示,重金属元素As、Cr、Cu、Ni、Pb、Zn平均含量分别为24.3mg/kg,154.0 mg/kg,32.8 mg/kg,31.4 mg/kg,64.9 mg/kg,165.1 mg/kg.Mn、Mo、Fe平均含量分别为400.1 mg/kg,10.7 mg/kg,18911 mg/kg.Sr 74.0 mg/kg、Sb 4.9 mg/kg、Co 13.7 mg/kg、Sc 5.9 mg/kg.采用单项污染指数法和内梅罗综合污染指数法来评价土壤重金属污染程度,并针对表层土壤金属污染状况进行了讨论.     

快速溶剂萃取一气相色谱法测定土壤中多氯联苯Aroclor系列

建立了快速溶剂萃取、浓硫酸净化、气相色谱法测定土壤中多氯联苯Aroclor系列的方法.方法线性良好、灵敏度高、回收率在70%～110%之间、相对标准偏差RSD小于17%,并用于有证的标准土壤样品及环境实样的分析,结果满意.     

益智及其种植区土壤中汞含量研究

采用氢化物原子荧光法测定了益智种植区土壤与益智各部位中的痕量汞,比较了HNO3＋HF＋H2O2、HNO3＋HF、HNO3＋HClO43种混酸消解体系的消解效果。结果表明,HNO3＋HF＋H2O2为最佳消解体系;样品加标回收率为93．70％～102．25％;土壤及益智果实、根、茎、叶中汞含量分别为0．3583、0．1632、0．0950、0．0700、0．0747mg·kg^-1,土壤中汞在益智果实、根、茎、叶间的迁移率分别为45．55％、26．51％、19．52％、20．83％,土壤及益智各部位的汞含量均在国家规定标准以内。说明海南益智种植区地理环境良好,未受到汞污染。