气相色谱法测定土壤中37种有机磷农药残留

采用气相色谱法测定土壤中37种有机磷农药,当取样量为10 g时,37种有机磷农药方法检出限为0. 002～0. 015 mg/kg,测定下限为0. 008～0. 060 mg/kg。低含量加标样品中有机磷农药的加标回收率为72. 8%～104%,相对标准偏差为4. 2%～13. 8%;中含量加标样品中有机磷农药的加标回收率为71. 5%～101%,相对标准偏差为4. 3%～13. 5%;高含量加标样品中有机磷农药的加标回收率为74. 6%～109%,相对标准偏差为6. 8%～14. 6%。该方法灵敏度高、分离效果好、重现性好,能够满足土壤中37种有机磷农药残留检测的要求。     

A conceptual approach to model sand–gravel extraction from rivers based on a game theory perspective

Sand–gravel mining is a significant parameter of economic development and social welfare function in modern societies. As demand for aggregate increases in construction industry, conflicts for the availability of the resource and environmental impacts become more intense. The present paper describes the contested status quo in riverbed sand–gravel mining activities with an example from Greece, as a case study. The scope is to propose a methodology about good governance of the mining sector that promotes a sustainable sharing of aggregate resource by securing environment and safekeeping revenues in the mining trade market.     

萃取法分离回收不锈钢酸洗污泥硫酸浸出液中的重金属

采用非皂化P204和皂化P204萃取剂对不锈钢酸洗污泥的硫酸浸出液进行萃取。在浸出液pH为0.80、非皂化P204体积分数为25%、萃取剂与浸出液体积比为1∶2、萃取时间为5 min的条件下,Fe~(3+)萃取率达99.64%,Cr~(3+)和Ni~(2+)萃取率为3.98%和6.99%,一次萃余液pH为0.64。采用皂化P204对除Fe~(3+)后的一次萃余液进行萃取,在P204体积分数为25%、萃取剂与浸出液体积比为1∶2、萃取剂皂化率为60%、一次萃余液pH为1.50、萃取时间为5 min的条件下,Ni~(2+)萃取率为93.12%,Cr~(3+)萃取率为20.69%,二次萃余液pH为2.63。     

Variability of pesticide residues in cauliflower units collected from a field trial and market places in Greece

To estimate the variability of pesticide residue levels present in cauliflower units, a total of 142 samples were collected from a field trial of a cooperative farmer, and 120 samples were collected from different market places in Thessaloniki, Greece. The collected samples were extracted using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction technique, and the residues were determined by liquid chromatography–tandem mass spectrometry. The developed method was validated by evaluating the accuracy, precision, linearity, limit of detection (LOD), and limit of quantification (LOQ). The average recoveries for all the analytes, derived from the data of control samples fortified at 0.01, 0.05, 0.1, and 0.2 mg/kg, ranged from 74 to 110% with a relative standard deviation of ≤8%. The correlation coefficient (R²) was ≥0.997 for all the analytes using matrix-matched calibration standards. The LOD values ranged from 0.001 to 0.003 mg/kg, and the LOQ was determined at 0.01 mg/kg for all the sought analytes. The matrix effect was found to be at a considerable level, especially for cypermethrin and deltamethrin, amounting to +90% and +145%, respectively. For the field samples, the unit-to-unit variability factors (VFs) calculated for cypermethrin and deltamethrin were 2.38 and 2.32, respectively, while the average VF for the market basket samples was 5.11. In the market basket samples, residues of cypermethrin, deltamethrin, chlorpyrifos, and indoxacarb were found at levels ≥LOQ and their respective VFs were 7.12, 5.67, 5.28, and 2.40.     

丹江口水库表层沉积物不同形态氮的赋存特征及其生物有效性

为了揭示丹江口水库沉积物氮空间分布特征及其生物有效性,采用连续分级提取法研究了表层沉积物中可交换态氮(Exchangeable nitrogen,EN)、酸解态氮(Acid hydrolysable nitrogen,HN)及残渣态氮(Residue nitrogen,RN)的赋存特征,同时结合生物可利用态氮的含量,探讨了各形态氮对生物可利用态氮的贡献。结果表明,丹江口水库沉积物中总氮(Total nitrogen,TN)在425~5796 mg/kg之间,平均为1 319.32 mg/kg,其中EN、HN和RN的平均值相对比例为2.15∶1.95∶1,且各形态氮含量的空间分布呈入库河流大于库区开阔区域的特征,尤其在丹江、老灌河以及犟河-堵河入库口的含量较大。潜在矿化氮(Potential mineralized nitrogen,PMN)含量在40.20~1 468.95 mg/kg之间,平均为275.06 mg/kg,其中EN对丹江口水库沉积物PMN的贡献较大,比例在19.85%~90.80%之间,平均为63.47%。各形态氮在不同的水环境条件下发生迁移转化,保持着水-沉积物界面氮的动态平衡。     

盐效萃取法从电子产品清洗废液中回收异丙醇

用盐效萃取法从电子产品清洗废液中回收片丙醇,考察了碳酸钾水溶液与该清洗废液的质量比对脱水率的影响,测定了异丙醇-水-碳酸钾体系存40℃时的液液相平衡数据,用Pitzer理论和NRTL方程对液液相平衡数据进行了理论计算。结果表明：当质量分数为60．00％的碳酸钾水溶液与该废液的质晕比为2．00时,脱水率高达90．00％;将有机相进行精馏可得到质量分数为99．50％的异丙醇;计算值与实测值接近,水相和有机相的绝对平均偏差分别为0．62％和0．46％。     

Aquafluor藻细胞活体分析法在三峡库区次级河流回水区Chla测定中的校准及应用

从三峡库区次级河流大宁河、小江、汤溪河及梅溪河139m回水区中段采集水样,经实验室培养后,用丙酮萃取分光光度法和Aquafluor藻细胞活体分析法测定Chla浓度.通过对Chla萃取值(y)和活体值(x)进行回归分析,得到其回归方程为y=4.15x 2.48,t检验显示回归方程具有线性.在库区次级河流139m回水区富营养化监测中,Chla模拟值与萃取值基本吻合,相对误差＜±7%,故可以采用Chla模拟值对水体富营养化程度进行评价.     

微波辐照热解废印刷电路板产物的分析研究

为了减少电子废弃物对环境的危害,实现其资源化回收利用,研究了微波辐照热解废印刷电路板的效果,并采用红外光谱、气相色谱质谱和X荧光光谱等方法对热解产物的组成及性质进行了分析.结果显示:微波热解得到的气体、液体、固体的产率分别为7%～33%、26%～45%、31%～51%,其中气体主要由CO、CO2、H2及有机烃类组成,可燃性气体占70%(体积分数)左右,可作为燃料气加以利用;液体分为水相及油相,经常压蒸馏后得到的120～250 ℃馏分主要为单酚化合物,苯酚高达50%(质量分数)左右,甲基苯酚和邻甲基苯酚为25%(质量分数)以上,是良好的化工原料;固体中除炭外,还含有许多金属如铅、锡和铜等,可以回收利用.说明微波热解技术处理电子废弃物可实现资源化回收利用.     

固相萃取和高效液相色谱联用测定污水中的五氯苯酚

采用固相萃取和高效液相色谱相结合的方法对污水中五氯苯酚的含量进行定量检测。结果表明,污水的pH值为4,流速控制在4mL/L以内,C18固相萃取柱对五氯苯酚有良好的吸附保留性能,以2mL的甲醇洗脱,洗脱效率在85%~95%之间。与传统的液液萃取相比,固相萃取的优势在于操作时间缩短、有机溶剂的使用量减少。     

微波联合消解流动注射光度法测定水中总氮和总磷

利用微波联合消解水样,采用流动注射分析技术,建立了在线测定水中总氮和总磷的快速分析方法.优化了试验条件,在线性范围内,总氮和总磷的工作曲线线性关系良好,检出限分别为0.03 mg/L和0.01 mg/L,相对标准偏差分别为1.5%和1.2%,加标回收率分别为96.7%～103%和98.8%～102%.