固相萃取-高效液相色谱法测定生活污水中壬基酚聚氧乙烯醚及其降解产物

比较了液-液萃取和固相萃取浓缩富集水体中壬基酚聚氧乙烯醚(NPnEO,n为聚合度)及其小分子代谢产物的效率,建立了复杂基体水样中壬基酚聚氧乙烯醚及其小分子代谢产物多成分同时测定的高分辨高灵敏的固相萃取(SPE)-正相高效液相色谱(NP-HPLC)-荧光检测(FL)方法。优化了影响SPE回收率的条件,洗脱溶剂和样品过柱的速度。SPE对NPnEO的回收率大于82%;使用1L水样,方法的检测限对壬基酚(NP)、NP1EO为0.01μgL,NP2EO、NP3EO为0.02μgL,NP4EO～NP12EO为0.05μgL。应用本方法测定了生活污水水样,检测到了NPnEO(n=1～12)及其小分子降解产物NP、NP1EO、NP2EO。     

高效液相色谱-串联质谱法测定废水中5种喹诺酮类抗生素

建立高浓度有机废水中5种喹诺酮类抗生素的高效液相色谱-串联质谱测定方法。水样经HLB固相萃取小柱富集净化,12 ml甲醇洗脱、浓缩并加入内标溶液后,定容至1 mL待测。以C18柱为分离柱,含0.01%甲酸的甲醇-含0.01%甲酸的水溶液为流动相,目标物质在10 min内分离。在0.25~1 250 ng/mL范围内,目标物质线性关系良好(R20.99)。基质加标试验结果表明,纯水中的回收率为61.40%~91.92%,废水中的回收率为54.92%~101.87%,检出限为0.25~2.5 ng/L,方法定量限为0.36~3.99 ng/L。应用该方法对21家猪场的64份废水样品进行分析,5种喹诺酮类抗生素的检出频率为47%~95%,平均检出浓度为980~5 734 ng/L。该方法快速、准确,适用于高浓度有机废水中喹诺酮类抗生素的同时测定。     

太湖沉积物铁形态分布特征及磷铁相关性分析

通过对太湖藻型湖区、草藻过渡型湖区、草型湖区柱状沉积物进行铁的形态分级分析沉积物中不同提取态磷铁含量,获得不同形态铁的空间分布特征.结果表明:沉积物总铁含量藻型湖区31.57mg/g(SD=8.51) >过渡型湖区30.34mg/g(SD=11.97) >草型湖区25.25mg/g(SD=4.59),不同湖区沉积物中铁形态的含量依次为可还原(晶型)铁氧化物Fe_ox2 >碳酸盐铁Fe_carb >易还原(无定形)铁氧化物Fe_ox1 >低活性硅酸铁Fe_prs >磁铁矿Fe_mag >可吸附性Fe(Ⅱ),Fe_carb、Fe_ox1、Fe_ox2,3种铁形态属于高活性铁Fe(Ⅲ),含量为7.79,6.16,8.18mg/g,分别占总铁含量的28.56%,21.54%,29.53%,表明高活性铁(Ⅲ)是沉积物中最主要的铁形态;沉积物中各提取态磷含量大小比较为NH₂OH·HCl-P >MgCl₂-P >NaAc-P >Na₂S₂O₄-P >浓HCl-P >(NH₄)₂C₂O₄-P,含量较高的MgCl₂-P(0.067mg/g)、NaAc-P(0.061mg/g)、NH₂OH·HCl-P(0.068mg/g),分别占总提取磷的35.28%、31.97%和22.55%,是沉积物铁分级提取态磷中最主要的形态.磷-铁相关性分析表明,二者之间呈显著的正相关(P<0.05),进一步从铁形态分级角度证实铁是沉积物內源磷释放的关键因子.     

几种化学浸提剂对底泥重金属生物有效部分浸提效果的比较

采用微生态系统生物长期暴露试验,比较５种化学浸提剂对底泥重金属生物有部分的浸提效果。结果表明,０．００５ｍｏｌ／ＬＤＴＰＡ＋０．１ｍｏｌ／Ｌ ＴＥＡ＋０．０１ｍｏＬ ＣａＣｌ２,ｐＨ７．３０是一种适合于食腐屑底栖动物的底泥重金属生物有效部分浸提剂;而０．００５ｍｏｌ／ＬＤＴＰＡ＋１ｍｏｌ／Ｌ ＮＨ４ＨＣＯ３．ｐＨ７．６８则一种适合于滤食性动物和水生根系植物底泥重金属生物有效部分浸提剂。     

大气颗粒物中重金属元素在不同粒径上的形态分布

采用DFJ 1型五段分级采样器 ,对衡阳市区冬、夏两季空气中不同粒径颗粒物中重金属元素的组成和化学形态进行了分析。应用ICP AES法测定了各形态中元素的含量 ,计算了元素在各种形态中的分配比例。结果表明 ,衡阳市大气环境中多数重金属元素的含量冬季明显高于夏季。对人体危害较大的金属元素主要富集在小于 2 0 μm的细颗粒上 ,Mn、Zn、Cu和Co主要分布在氧化态、水可溶态、碳酸盐态和有机态中 ,Pb和V主要分布在不溶态中     

乳状液膜提取废汞触媒浸出液中的汞及 乳状液破乳

采用乳状液膜法分离提取废汞触媒浸出液中的Hg~(2+)。考察了影响乳状液膜体系分离富集汞的主要因素,并对分离提取后的乳液相进行了破乳研究。分离提取实验结果表明:乳状液膜体系的最佳配方为流动载体磷酸三丁酯体积分数10%、表面活性剂失水山梨糖醇脂肪酸酯体积分数4%、膜溶剂磺化煤油体积分数86%、内水相HCl溶液浓度0.10mol/L、油相与内水相的体积比1∶1;在乳状液与外水相的体积比为1∶10的条件下Hg~(2+)提取率达78.50%。破乳实验结果表明:加热破乳、离心破乳、加热离心联合破乳3种方法的破乳率分别为29.0%,54.0%,85.7%;采用加热离心联合法破乳后,Hg~(2+)富集倍数达8.5。     

反胶团萃取技术的影响因素与应用

反胶团是一种新型提取分离技术,具有防止生物大分子失活、变性等优良特性.综述了反胶团的原理、含水率、pH、表面活性剂、助表面活性剂、离子浓度、萃取时间等因素对反胶团萃取的影响及反胶团的应用.     

Heavy metal content and distribution in surface sediments of the Seyhan River, Turkey

Chemical fractionation of seven heavy metals (Cd, Cr, Cu, Mn, Ni, Pb and Zn) was studied using a modified three-step sequential procedure to assess their impacts in the sediments of the Seyhan River, Turkey. Samples were collected from six representative stations in two campaigns in October 2009 and June 2010, which correspond to the wet and dry seasons, respectively. The total metal concentrations in the sediments demonstrated different distribution patterns at the various stations. Cadmium was the only metal that was below detection at all stations during both sampling periods. Metal fractionation showed that, except for Mn and Pb, the majority of metals were found in the residual fraction regardless of sampling time, indicating that these metals were strongly bound to the sediments. The potential mobility of the metals (non-residual fractions) is reflected in the following ranking: Pb > Mn > Zn > Cu > Ni > Cr in October 2009 and Mn > Pb > Zn > Cu > Ni > Cr in June 2010. The second highest proportion of metals was bound to organic matter/sulfides, originating primarily from anthropogenic activities. Non-residual metal fractions for all stations were highest in June 2010, which may be linked to higher organic matter concentrations in the sediment samples with 1.40% and 15.1% in October 2009 and June 2010, respectively. Potential sediment toxicity was evaluated using the Risk Assessment Code (RAC). Based on RAC classification, Cd and Cr pose no risk, Cu and Ni pose low risk, Pb and Zn were classified as medium risk metals, while the environmental risk from Mn was high. In addition, based on the sediment quality guidelines (SQG), the Seyhan River can be classified as a river with no, to moderate, toxicological risks, based on total metal concentrations.     

“热洗+助溶剂萃取”技术处理含油污泥的应用

为解决大量堆存的含油污泥可能造成的环境隐患问题,新疆油田公司针对含油污泥无害化、资源化技术进行探索研究。采用"热洗+助溶剂萃取"工艺技术处理,使含油污泥中矿物油含量从处理前的8%～30%降低至处理后的0.3%以下,满足GB 4284—84《农用污泥中污染物控制标准》的要求,有效回收了石油资源,减少环境污染,装置运行能耗成本为62.55元/t,具有运行费用低、操作简便的特点,为油田规模化、产业化处理含油污泥提供借鉴。     

海军某型飞机典型电连接器失效分析

目的分析得出电连接器失效的主要原因。方法以海军某型飞机三个型号典型电连接器插孔端为主要研究对象,对电连接器宏观形貌进行目视检查分析,并采用扫描电子显微镜进行微观形貌观察,采用能谱分析仪进行微观成分分析,研究壳体表面和插孔接触面的化学成分组成。结果腐蚀和磨损是外场电连接器失效的主要诱因,电连接器有一定程度的局部腐蚀,表面积聚的灰尘和海盐颗粒对腐蚀有较明显的促进作用。插拔不当造成的插针与插孔间同心度的偏差,与微动磨损共同作用加速了局部腐蚀。结论插拔不当、微振磨损与局部腐蚀是导致电连接器性能下降乃至失效的三大主要因素。