An optimised sequential extraction scheme for the evaluation of vanadium mobility in soils

Reviewing the current state of knowledge about sequential extraction applied for soil vanadium(V) fractionation, we identified an urgent requirement of an sequential extraction(SE) specified for V. Namely, almost all previous SE extracted only 8.4%–48% of total V in soils(excluding residue). Thus, we proposed an eight-step SE for V fractionation in soils according to the knowledge gained from literature and our own dissolution experiments with model minerals. After extracting the mobilisable and adsorbed V with de-ionised water and 5 mmol/L phosphate, 1 mol/L pyrophosphate was applied to gather organic matter bound V which minimised the artefact dissolving Al and Fe(hydr)oxides occurred when using HNO_3–H_2O_2for extraction. Extraction with 0.4 mol/L NH_2OH·HCl was highly selective toward manganese oxides. Fractionation of different crystalline Al and Fe(hydr)oxides associated V with 1 mol/L HCl, 0.2 mol/L oxalate buffer and 4 mol/L HCl at 95°C especially improved the extractability of V incorporated with crystalline phase associated V. The suitability of our new SE scheme was confirmed by its higher selectivity against the target phases and higher extraction efficiencies(55%–77% of total V) with model minerals and 6 soils of different properties than previous SE.     

土壤中总石油烃预处理方法研究

采用了索氏提取法、超声波萃取法和加速溶剂萃取对土壤中的总石油烃预处理进行了研究分析,方法在0 mg/L~500 mg/L范围内均有良好的线性.采用索氏提取法时,总石油烃的方法检出限均在0.001 mg/kg~0.016 mg/kg范围内,回收率在65%~80%之间,相对标准偏差均在6.8%~12%之间;采用超声波萃取法时,总石油烃的方法检出限均在0.002 mg/kg~0.023 mg/kg范围内,回收率在60%~88%之间,相对标准偏差均在8.6%~15%之间;采用加速溶剂萃取时,总石油烃的方法检出限均在0.001 mg/kg~0.009 mg/kg范围内,回收率在70%~95%之间,相对标准偏差均在2.5%~8.8%之间.实验表明三种方法均可以作为土壤中总石油烃的预处理分析方法,但加速溶剂萃取更加快捷方便,更适合实际样品的分析.     

低分子量有机酸提取土壤中部分重金属的拟合模型研究

为研究不同浓度低分子量有机酸与提取的土壤重金属含量之间的关系,本文以采自安徽省安庆市某铜矿区及其周围的土壤为例,通过浸提法,研究了不同浓度苹果酸、甲酸对采样点土壤中重金属Cu、Mn、Zn、Pb提取能力的影响并进行模型拟合.结果表明:不同浓度苹果酸和甲酸对采样点土壤中重金属的提取量不同,两种有机酸对低pH、高重金属含量采样点及其周围土壤中的重金属提取量较大,两种低分子量有机酸对S6采样点的重金属Mn的提取量最大,分别为322.5 mg·kg~(-1)和193.58 mg·kg~(-1),提取率达70.02%和42.03%,Zn、Pb次之,Cu最低;随着苹果酸、甲酸浓度的升高,土壤中重金属Cu、Mn、Zn、Pb的提取量增加,苹果酸对土壤中重金属的提取能力大于甲酸;拟合模型对于两种低分子量有机酸与其提取的土壤中部分重金属含量之间的关系,具有较好的拟合性,其决定系数R~2在0.8293～0.9990之间,都具有显著性(p0.05),该模型可以定量表征低分子量有机酸对土壤重金属的提取能力,此研究结果为土壤中重金属的固定化和增强植物修复受重金属污染的土壤提供了理论支持.     

固相微萃取和固相萃取评价多环芳烃降解过程中的生物有效性变化

为了揭示多环芳烃(PAHs)降解过程中的生物有效性变化规律,应用PAHs降解菌剂对PAHs污染焦化厂土壤进行微生物修复,采用固相微萃取及固相萃取方法提取评价PAHs的生物有效性,分析降解率和生物有效性变化的差异及相关关系.结果表明,该焦化厂土壤中PAHs总量以低环PAH为主,微生物菌剂对土壤总PAHs降解率为68.3%;微生物作用后,孔隙水中PAHs的降低以3、4环为主,孔隙水中PAHs变化率普遍低于土壤中的降解率;Tenax-TA提取降解前后土壤中的PAHs,降解后3、4环PAHs的快速解吸组分降低,5、6环的快速解吸组分变化不大;土壤中PAHs降解量分别与PAHs孔隙水浓度和Tenax-TA快速提取量存在相关关系.以上结果表明可用PAHs孔隙水浓度以及Tenax-TA快速提取量预测微生物对土壤PAHs的降解,这为焦化厂土壤PAHs污染的修复提供了理论依据.     

超声波辅助化学萃取对某工业场地铅污染土壤修复效果研究

以某铅蓄电池厂污染场地5个铅污染区域(WS、A、B、C及BZ)的土壤为研究对象,对土壤中铅全量及各形态含量进行分析.在0.1 mol.L-1EDTA,30 min,25℃相同条件下,使用超声波辅助化学洗脱(ultrasonic-assisted chemical extraction,UCE)与传统化学洗脱(conventional chemical extraction,CCE)两种不同的作用方式,对铅的去除效率进行比较,并对两种不同清洗方式后铅的形态变化进行了探讨.结果表明,UCE对铅的去除效率显著优于CCE.在CCE作用下,5份污染土壤WS、A、B、C、BZ铅的去除效率依次为10.06%、48.29%、48.69%、53.28%及36.26%,而UCE作用下铅的去除效率依次为22.42%、69.31%、71.00%、74.49%及71.58%,平均效率高出22%.通过对比两种清洗方式后土壤中的铅形态发现,酸可提取态在UCE作用后持平或有所降低,但CCE后使酸溶态有增高的趋势;对于铁锰氧化态,UCE对其有着极好的去除能力,可达98%左右,同时对有机物及硫化物结合态、残渣态也具有较好的去除能力.因此,UCE在化学萃取中的应用具有一定的可行性,是一种简单、极快速去除污染场地中重金属铅的增效手段.     

Screening of factors influencing Cu(II) extraction by soybean oil-based organic solvents using fractional factorial design

This study aimed to identify the significant factors that give large effects on the efficiency of Cu(II) extraction from aqueous solutions by soybean oil-based organic solvents using fractional factorial design. Six factors (mixing time (t), di-2-ethylhexylphosphoric acid concentration ([D2EHPA]), organic to aqueous phase ratio (O:A), sodium sulfate concentration ([Na(2)SO(4)]), equilibrium pH (pH(eq)) and tributylphosphate concentration ([TBP])) affecting the percentage extraction (%E) of Cu(II) were investigated. A 2(6-1) fractional factorial design was applied and the results were analyzed statistically. The results show that only [D2EHPA], pH(eq) and their second-order interaction ([D2EHPA] × pH(eq)) influenced the %E significantly. Regression models for %E were developed and the adequacy of the reduced model was examined. The results of this study indicate that fractional factorial design is a useful tool for screening a large number of variables and reducing the number of experiments.     

Metal and oxalate contamination in a suburban watershed in the greater Toronto area: the benefits of combining acid leach and selective extraction procedures

Environmentally available concentrations of Fe, Mn, Zn, Cu, Pb, Cr and Ni in soils and sediments from a small suburban catchment, obtained using an acid leach procedure, are compared to the Ontario Ministry of the Environment lowest effect level (LEL) and severe effect levels (SEL) and to Provincial sediment quality guidelines (PSQG's). These data are then compared to the bioavailability, potential bioavailability and non-bioavailability of the same metals, plus oxalate concentration, identified using a selective extraction procedure. This combination of techniques enhanced analytical interpretation with respect to metal mobility and potential metal contamination. Selective extraction highlighted the presence of oxalate as a potential contaminant, especially in poorly drained valley floor deposits (33,633 mg kg(-1) and 26,284 mg kg(-1)) and lakeshore sediments (27,095 mg kg(-1) and 13,729 mg kg(-1)). These levels are considerably in excess of those previously documented in a similar study from Rio de Janeiro, where contamination of urban sediment by sewage is a recognised environmental problem, and could possibly be used both as an indicator of similar contamination and the identification of those areas that warrant further investigation.     

高效液相色谱串联质谱检测地表水中五种生物胺

采用固相萃取及高效液相色谱串联质谱技术,建立了地表水中5种生物胺（腐胺、尸胺、2-苯乙胺、酪胺、色胺）的测定方法。水样中2-苯乙胺、酪胺和色胺可直接进样测定,腐胺和尸胺经HLB固相萃取柱富集,乙腈洗脱,氮吹浓缩至1.0mL后进样液相色谱串联质谱分析,以选择离子监测（SRM）模式定量分析。在本实验条件下,加标回收率在89.4%～122%之间,相对标准偏差2.15%～11.9%（n=7）,检出限在0.05～5μg/L。     

基于DEA- Benchmarking模型的资源开采企业绩效评价与发展研究

通过固定资产净额等4个输入指标和净利润等3个输出指标,利用DEA方法对全国19家上市资源开采企业的绩效水平进行测度,同时利用Benchmarkirg方法在众多企业中找到标杆企业和待改进企业.待改进企业通过向标杆企业学习得到不断发展,从而促进行业的整体效率的提高.     

长梗黄精主根与须根多糖的提取工艺研究

对长梗黄精主根与须根多糖的提取工艺进行了研究.在对乙醇浓度、浸提温度、浸提时间和粉碎粒度等进行单因素试验的基础上,通过正交试验确定了长梗黄精主根与须根多糖提取的最佳工艺条件,即对长梗黄精主根多糖的提取最佳条件为乙醇浓度80％、浸提温度80℃、浸提时间50min、颗粒大小40目,此时多糖提取率为18.754％;而对长梗黄精须根多糖的提取最佳条件为乙醇浓度70％、浸提温度60℃、浸提时间30min、颗粒大小80目,此时多糖提取率为16.652％.须根多糖含量与主根含量差异性不显著,故须根的利用价值也很高,有待开发利用.