离子交换树脂吸附Cd(Ⅱ)和Pb(Ⅱ)的研究

采用静态法和动态法对阳离子交换树脂吸附Cd(Ⅱ)、Pb(Ⅱ)的行为进行了研究。考察了pH值、流速、吸附时间等条件对吸附效果的影响,优化了树脂洗脱再生的最佳条件。实验结果表明,732型强酸阳离子交换树脂能够有效地吸附废水中的Cd(Ⅱ)和Pb(Ⅱ)。对比两种交换方式,动态法具有操作简单、效率高、可连续运行等特点,具有较高的实用价值。     

GC／MS法定量测定工业废水中半挥发性有机物

采用ＧＣ／ＭＳ方法定量测定工业废水中半挥发性有机物。研究了试样预富集方法，采用不同的预富集方法，对茶，二氢苊及苯并（ａ）芘等７种物质进行富集的结果表明，采用Ｎ２吹与Ｋ－Ｄ浓缩相结合的方法，优于其他方法，其回收率与美国ＥＰＡ－６２５方法的数据相近，回收率在９２％以上，研究了定量测定条件，以２，２′－二氟联苯为内标物质，测定不同浓度的半挥发性ＥＰＡ标准样品的响应因子Ｄ≤２５％。测定了上海焦化厂工业放心     

土壤中铅的平台石墨炉原子吸收法测定

采用悬浮液进样,以平台石墨炉原子吸收法直接测定土壤中的铅。通过180目筛孔的土壤样,可均匀、稳定地悬浮于0.2％(W/V)琼脂液中。方法的相对标准偏差为1.2％～5％;回收率为93％～110％;进样10μl ,检出限为21.4pg。与火焰原子吸收法对照,两者测定结果相吻合。     

土壤样品中铅和镉的微波消解法研究

利用微机控制的微波－聚四氟乙烯高压溶出装置，对土壤样品中的铅和镉两种重金属的消解进行了研究，结果表明，微波消解法具有较为满意的准确度与精密度，制样效率大大提高。     

石墨炉原子吸收光谱法测定海水中的三丁基锡

本文采用石墨炉原子吸收光谱法（ＧＦＡＡＳ）测定海水甲苯抽提液中的三丁基锡。文中考察了１４种基体改进剂对灵敏度的影响，选出了能显著提高测定灵敏度的Ｃａ－Ｃｒ基体改进剂，以０．５／０．１ｍｇ／ｍｌ的浓度比例对８个实样进行了测定，其相对标准偏差（ＲＳＤ）为３％，其特征浓度为７ｐｇ，回收率在８８％￣１０４％之间，成功地应用于近海沉积物对三丁基锡吸附规律的研究。     

基于超高效液相色谱串联质谱法的番茄果实和土壤中氟吡菌胺残留测定

建立了番茄果实和土壤中氟吡菌胺残留的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。用乙腈水溶液提取样品中的氟毗菌胺,以C_(18)柱为分析柱、乙腈-甲酸水溶液为流动相,采用超高效液相色谱-串联质谱多反应监测、电喷雾正离子源、外标法定量。氟吡菌胺在0.05~1.00 mg/L范围内与峰面积呈良好的线性关系,线性方程为y=6964.10x-143.28,决定系数为0.996 8。向对照番茄果实、对照土壤中分别添加氟吡菌胺标样,使其添加量分别为0.10 mg/kg、0.40 mg/kg和2.00 mg/kg,平均回收率分别为92.43%~103.32%和92.75%~104.46%,相对标准偏差分别为3.8%~4.9%和3.4%~4.4%。番茄果实和土壤中氟吡菌胺的定量限分别为1.0μg/kg和1.7μg/kg,检出限分别为0.3μg/kg和0.5μg/kg。     

Oxidation state specific analysis of arsenic species in tissues of wild-type and arsenic (+ 3 oxidation state) methyltransferase-knockout mice

Arsenic methyltransferase(As3mt) catalyzes the conversion of inorganic arsenic(i As) to its methylated metabolites, including toxic methylarsonite(MAs~Ⅲ) and dimethylarsinite(DMAs~Ⅲ). Knockout(KO) of As3 mt was shown to reduce the capacity to methylate i As in mice. However, no data are available on the oxidation states of As species in tissues of these mice. Here, we compare the oxidation states of As species in tissues of male C57BL/6 As3mt-KO and wild-type(WT) mice exposed to arsenite(iA s~Ⅲ) in drinking water. WT mice were exposed to50 mg/L As and As3mt-KO mice that cannot tolerate 50 mg/L As were exposed to 0, 15, 20, 25 or30 mg/L As. iA s~Ⅲaccounted for 53% to 74% of total As in liver, pancreas, adipose, lung, heart, and kidney of As3mt-KO mice; tri- and pentavalent methylated arsenicals did not exceed 10% of total As. Tissues of WT mice retained iA s and methylated arsenicals: iA s~Ⅲ, MAs~Ⅲand DMAs~Ⅲ represented 55%‐68% of the total As in the liver, pancreas, and brain. High levels of methylated species, particularly MAs~Ⅲ, were found in the intestine of WT, but not As3mt-KO mice,suggesting that intestinal bacteria are not a major source of methylated As. Blood of WT mice contained significantly higher levels of As than blood of As3mt-KO mice. This study is the first to determine oxidation states of As species in tissues of As3mt-KO mice. Results will help to design studies using WT and As3mt-KO mice to examine the role of iA s methylation in adverse effects of iA s exposure.     

Persistent organochlorine pesticides in internal organs of coypu,Myocastor coypus

A highly selective and sensitive method based on gas chromatography-tandem mass spectrometry (GC-MS/MS) to identify and quantify persistent organochlorine pesticides, (18 compounds including primary compounds and metabolites), in animal internal organs (kidneys, liver, and brain) has been developed. Tandem mass spectrometric conditions were individually optimized for each target compound in Multiple Reaction Monitoring (MRM) mode to obtain maximum sensitivity. Prior to instrumental analysis, a sample preparation method based on matrix solid phase dispersion (MSPD) followed by acidic digestion with sulfuric acid to reduce matrix co-extractives was employed. Analyses of real samples were carried out on coypus (Myocastor coypus) from the autumn slaughter of 19 animals. In the analyzed samples, three of the target compounds, namely DDE-pp′ (DDT metabolite), HCB and lindane, were detected. Their concentration levels fell in the ranges of 0.003–0.007, 0.003–0.025, and 0.003–0.021 mg kg^?1 (0.005, 0.010, and 0.010 mg kg^?1 on average) in the case of DDE-pp′, HCB and lindane, respectively. Although low quantities of organochlorine pesticides do not pose an immediate danger to consumers' health, they should be of public health concern considering long-term, low-dose exposure.     

Decomposition of Al13 promoted by salicylic acid under acidic condition: Mechanism study by differential mass spectrometry method and DFT calculation

Decomposition of the polycation Al₁₃O₄(OH)₂₄(H₂O)₁₂⁷⁺ (Al₁₃) promoted by ligand is a vital subject to advance our understanding of natural and artificial occurrence and evolution of aluminum ions, especially in the case of acidic condition that dissolved Al³⁺ species can be released from the Al-bearing substances. However, the microscopic pathway of synchronous proton-promoted and ligand-promoted decomposition process for Al₁₃ is still in the status of ambiguity. Herein, we applied differential mass spectrometry method and DFT calculation to study the initial detailed process of Al₁₃ decomposition under the presence of proton and salicylic acid (H₂Sal). Mass results showed that the mononuclear Al³⁺-H₂Sal complexes dominated the resulting Al species, whereas the monodentate complex Al₁₃HSal⁶⁺ was not observed in the spectra. The difference of decomposition levels between the ligand/Al ratio 0.2 and 0.5 cases revealed that proton and ligand performed synergistic effect in initial Al₁₃ decomposition process, and the proton transfer determined the ring closure efficiency. The ring closure reaction is the prerequisite for the collapse of Al₁₃ structure and detachment of the mononuclear complex. DFT calculations reveal that hydrogen bond plays an important role in inducing the formation of chelated complex accompanying proton transfer. Attachment of protons at the bridging OH⁻ can elongate and weaken the critical bond between targeted Al³⁺ and µ₄-O^2- resulting from delocalization of electron pairs in the oxygen atom. These results demonstrate the detailed mechanism of Al₁₃ composition promoted by ligand and proton, and provide significant understanding for further application and control of Al₁₃.     

浑河-大辽河水系水体与沉积物中典型全氟化合物的污染水平及生态风险评价

采用超高效液相色谱串联质谱(UPLC-ESI-MS/MS)分析了水体和沉积物中全氟化合物(PFCs)浓度水平,结果表明,浑河-大辽河的干流水中,PFCs总浓度范围为1.80~13.0 ng·L-1,其中,PFHx A、PFHp A、PFOA、PFOS和PFDA是主要污染物;沈阳细河中PFCs的总浓度为27.0~50.0 ng·L-1,其主要污染物为PFPA、PFOA、PFOS和PFDA.在浑河-大辽河沉积物中,PFHx A是唯一的检出物,其含量为0.130~0.490 ng·g-1干重;除了PFHx A,PFOS也是细河中的主要污染物,其浓度水平分别为0.070~0.220 ng·g-1和0.180~0.830 ng·g-1干重.采用实测的水和沉积物中PFOA和PFOS的暴露浓度以及预测的无效应浓度(PNEC),运用商值法对浑河-大辽河干流及沈阳细河水体和沉积物中PFOA和PFOS的生态风险进行评价.结果表明水体和沉积物中PFOA和PFOS的浓度均未达到对生态环境具有风险的水平.