废弃等离子显示屏玻璃中重金属化学形态分布

通过BCR3步和BCR4步连续提取法,对等离子体显示屏玻璃中重金属的化学形态进行研究。结果表明,BCR3步连续提取法对废弃等离子体显示屏玻璃中重金属的提取比BCR4步连续提取法更稳定。废弃等离子体显示屏玻璃中Zn、Cu和Ag化学形态分布存在差异。BCR3步和BCR4步连续提取法均认为Ag以残渣态为主要赋存形态,对环境影响比较小;Cu的可交换与弱酸可溶态或交换态和碳酸盐结合态含量较少,潜在的环境风险也比较小;BCR3步和BCR4步连续提取法对Zn的形态分布结果评价不一致,BCR3步连续提取法表明Zn主要以可交换与弱酸可溶态为主,对环境影响较大,而BCR4步连续提取法结果认为Zn是以铁锰氧化态为主要存在形态。     

A rapid method for screening of the Stockholm Convention POPs in small amounts of human plasma using SPE and HRGC/HRMS

A rapid analytical screening method allowing simultaneous analysis of 23 persistent organic pollutants (POPs) in human plasma was developed. Sample preparation based on solid-phase extraction (SPE) with additional clean-up using small multilayer silica gel columns. SPE was performed using a custom made polystyrene-divinylbenzene sorbent for the extraction of chlorinated and brominated POPs. Special efforts to reduce sample volume and improve speed and efficiency of the analytical procedure were made. Determination of 16 polychlorinated biphenyls (PCBs), 5 organochlorine (OC) pesticides, octachlorinated dibenzo-p-dioxin (OCDD) and polybrominated diphenyl ether (BDE #47) in 0.5 mL human plasma was performed by using high resolution gas chromatography coupled to high resolution mass spectrometry (HRGC/HRMS). Recovery of POPs ranged between 46% and 110%, and reproducibility was below 25% relative standard deviation (RSD) for all target compounds, except for trans-nonachlor and OCDD, which were present only at low levels. Limits of detection (LOD) were for the PCBs between 0.8 and 117.7 pg mL⁻¹ plasma and for the OC pesticides between 5.9 and 89.1 pg mL⁻¹ plasma. The LOD for OCDD and BDE #47 were 1.4 pg mL⁻¹ plasma, and 9.2 pg mL⁻¹ plasma, respectively. The presented method was successfully applied to 1016 human plasma samples from an epidemiological study on cardiovascular disease.     

萃取净化废水中镉的动力学研究简

采用恒界面池研究了二壬基萘磺酸（简称DNNSA或HD）-煤油体系萃取废水中镉离子的动力学。考察了搅拌转速、二壬基萘磺酸浓度、镉离子浓度和温度对萃取速率的影响，并得到了DNNSA萃取废水中镉离子的萃取动力学方程。实验结果表明，镉离子的萃取速率在200 r/min时出现与搅拌强度无关的化学反应动力学“坪区”，FT-IR结果表明，反应产物为磺酸盐；在动力学“坪区”，镉离子萃取速率随着萃取剂浓度、水相中的镉离子浓度增加而增加；随着温度升高，萃取速率增加，萃取活化能为11.8 kJ/mol。     

Simultaneous determination of organochlorine and pyrethriod pesticide residues in the Chinese patent medicines by gas chromatography-tandem mass spectrometry

A simple, sensitive, reliable method was developed for the simultaneous determination of organochlorine and pyrethriod pesticide residues in Chinese patent medicines Six ingredient rehmannia pills and Xiaoyao pills. These pesticides were extracted by ethyl acetate. The extraction time and volume of ethyl acetate were optimized. Cleanup of extracts was performed with dispersive-solid phase extraction using graphitized carbon black as the sorbent. The determination of pesticides in the final extracts was carried out by gas chromatography–tandem mass spectrometry in multiple reaction monitoring mode (GC-MS/MS, MRM). The linearity of the calibration curves is good in matrix-matched standard and yields the coefficients of determination (R²) ≥0.99 for all of the target analytes. Under optimized conditions, the average recoveries (five replicates) for most pesticides range from 75.5% to 114.6%, and RSDs are less than 10.0%. The LODs of 18 pesticides in Six ingredient rehmannia pill and Xiaoyao pills are in the range of 0.01–8.82 μg kg^?1. The developed method meets the requirements of pesticide residue analysis and could be effectively used for routine analysis of the organochlorine and pyrethriod pesticide residues in Six ingredient rehmannia pills and Xiaoyao pills.     

固体废物氰化物总量和浸出毒性测定方法的比较

中国现行的固体废物氰化物总量和氰化物浸出毒性的分析方法存在缺陷，不便于广泛指导监测工作，笔者优化了固体废物氰化物测定的前处理方法，明确了固体废物氰化物总量、氰化物浸出毒性测定时的样品粒径、浸提方法和消解方法，建立了容量法、分光光度法、流动注射法测定固体废物氰化物总量和浸出毒性的方法，并与标准方法（离子色谱法）进行比较。实验结果表明：容量法、分光光度法、流动注射法测定结果与离子色谱法无显著差异，3种方法测定固体废物氰化物总量加标回收率为80.5%~102%，平行样测定相对标准偏差为3.0%~6.9%，3种方法测定固体废物氰化物浸出毒性加标回收率为80.1%~107%，平行样测定相对标准偏差为7.8%~9.5%，3种方法测定结果精密度和准确度良好，均能够满足固体废物氰化物总量和氰化物浸出毒性的测定要求。其中容量法、分光光度法由于其仪器设备简单、操作简便，可用于突发环境事件应急监测等情况下固体废物氰化物的测定。但容量法检出限较高，不能满足评价标准较低的分析测试工作要求，离子色谱法、分光光度法和流动注射法检出限均能满足一般分析测试要求。     

离子色谱法同时测定大气PM2.5中水溶性有机酸和无机阴离子的研究

建立超声提取-离子色谱法55 min内同时测定大气PM_(2.5)中13种水溶性低分子有机酸和无机阴离子的方法,经不同样品膜空白值考察、预处理条件优化、样品保存实验研究等获得了最佳的实验条件。研究发现,无机阴离子线性回归系数均为0.999以上,有机酸均为0.993以上;样品膜中各离子的相对标准偏差为3.2%~9.8%,样品提取液中各离子的加标回收率为90.6%~108%;当采样体积为24 m~3时,各目标化合物的方法检出限为0.003~0.032μg/m~3。分别于2015年1、6月采集了PM_(2.5)实际样品,1月各离子浓度之和为31.9μg/m~3,范围为0.04~15.0μg/m~3;6月各离子浓度之和为22.3μg/m3,范围为0.01~12.7μg/m~3。两个采样期间,氯离子、硝酸根、硫酸根在13种化合物中占绝对优势,均占总量的95%以上;乙酸、甲酸、甲烷磺酸和乙二酸为其他低含量离子中的主要组分。     

Alamine336对低浓度模拟含硝酸废水的萃取分离

以模拟低浓度含硝酸废水为研究对象,以煤油为稀释剂,考察了工艺条件对硝酸萃取和反萃效果的影响,并对萃取机理进行了探讨。实验结果表明：以10.0%（φ）Alamine336为萃取剂,在有机相与水相的体积比为1∶2、萃取温度为298 K的条件下,对初始硝酸质量浓度为2.00 g/L的含硝酸废水进行两级逆流萃取操作后,理论上水相硝酸质量浓度低于15 mg/L,达到GB 8987—1996中的一级标准;以0.05 mol/L氢氧化钠溶液为反萃剂,在有机相与水相的体积比为1∶2、反萃温度为298 K的条件下,对硝酸负载量为1.50 g/L的有机相进行两级反萃后,理论上有机相硝酸残余量小于0.005 g/L。机理研究表明Alamine336通过与硝酸形成离子对络合物来萃取硝酸。     

加速溶剂萃取-高效液相色谱法测定固体废物中多环芳烃

建立了固体废物中多环芳烃的快速溶剂萃取(ASE)-高效液相色谱(HPLC)检测方法。加速溶剂萃取仪在温度100℃、压强1.05 MPa条件下,以体积比1:1的丙酮和二氯甲烷为萃取剂,萃取5 min,萃取液采用固相萃取柱或凝胶色谱净化。灰渣和污泥中的PAHs的方法检出限分别为1.03~1.96 μg/kg和4.71~7.04 μg/kg,相对标准偏差分别为4.0%~13.8%和3.3%~13%,加标回收率分别为73.2%~89.8%和67.7%~90.5%。     

FeCl3蚀刻液膜电解阴极液中Ni2+的萃取回收

采用自制的SSX萃取剂对FeCl₃蚀刻液膜电解阴极液（简称废液）中的Ni²⁺进行萃取回收。考察了萃取pH、SSX萃取剂含量、萃取相比（SSX萃取剂与废液的体积比）、萃取时间、萃取次数对Ni²⁺萃取率的影响，以及反萃剂HCl溶液浓度、反萃相比（反萃剂与萃取液的体积比）、反萃时间对Ni²⁺反萃率的影响。实验结果表明： 当SSX萃取剂质量分数20%、萃取pH 2.0、萃取相比1.0、萃取时间10 min、1次萃取时，Ni²⁺萃取率可达74.56%；当反萃剂HCl溶液浓度6.0 mol/L、反萃相比1.5、反萃时间10 min时，Ni²⁺反萃率达93.10%；再生后的SSX萃取剂重复使用4次后，Ni²⁺的累积萃取率达91.00%，萃取剂中Ni²⁺的质量浓度可达14.94 g/L；反萃液经浓缩、结晶处理可制备电镀用NiCl₂产品。     

液液萃取-气相色谱／质谱联用法测定地表水中四乙基铅

采用液液微萃取与气相色缈质谱法联用技术建立了测定水样中四乙基铅的方法。同时还对萃取溶剂进行选择，结果表明：选择了二氯甲烷作为萃取溶剂，氯化钠加入量10g，该方法检出限为0．03μg／L，线性范围为0．20-10．Oμg／L，线性相关系数为0．9999，测定饮用水源水和地表水中的四乙基铅，加标回收率为89．5％～101．7％，相对标准偏差为3．7％-5．9％。