微波消解-电感耦合等离子体质谱(ICP-MS)法同时测定土壤中8种重金属元素

采用微波消解-电感耦合等离子体质谱法同时测定土壤中砷、镉、铬、铜、汞、镍、铅、锌8种痕量元素,对质谱干扰和非质谱干扰进行了校正。8种重金属元素在一定的质量浓度范围内与其信号强度呈线性关系,方法的检出限(3s)在0.001 2~0.029μg/L。用加标回收测定其回收率,加标回收率范围在90.0%~96.3%,对土壤样品平行测定6次,测定值的相对标准偏差在2.1%~3.0%。对湛江南柳河附近土壤进行重金属监测,监测结果符合标准要求。     

电镜-能谱仪在柳树叶重金属污染研究中的应用

采用自然干燥、化学处理、冷冻处理3种方法制备待测样本,运用扫描电镜和透射电镜结合X射线能谱仪研究柳树叶肉组织对重金属的累积状况,并定位到栅栏组织的细胞壁,为定性定量以及定位分析组织细胞固定、转移重金属污染探索合适的制样方法.结果表明:(1)重金属Pb、Cu、Cd、Zn在柳树叶肉组织被检测到,并已进入到细胞壁内,同时定量结果显示污染越严重,重金属累积量越多,证明了柳树叶对重金属污染的吸收能力;(2)通过综合比较,认为冷冻处理的样本比较适合进行植物组织微区的元素定性定量以及定位分析,因此推测冷冻制样加冷冻电镜的方法将会最为理想.     

Heavy metals in lake water: a review on occurrence and analytical determination

Many lakes especially in Asia are source of livelihood for the surrounding communities. With increased urbanisation and industrialisation, however, these lakes are threatened with emerging environmental contaminants, including heavy metals. Some heavy metals are harmful to human health and the environment. This review aims to describe the different sampling, sample preparation and pretreatment, and instrumental methods of analysis for heavy metals in lake water. Filtration and acid digestion are common sample treatment methods used prior to analytical determination. Atomic absorption spectroscopy and inductively-coupled plasma – mass spectrometry (ICP-MS) are typical analytical techniques but nowadays ICP-MS is frequently used. This review also describes the sources and extent of heavy metals contamination in different lakes. Although some lakes still have natural levels of heavy metals in the water, many have elevated concentrations due to anthropogenic sources, such as vehicular, household, agricultural, industrial and mining activities.     

电感耦合等离子体质谱(ICP-MS)法测定葡萄酒中的铜、镉、铅

建立了电感耦合等离子体质谱(ICP-MS)法直接测定葡萄酒中铜、镉、铅含量的一种快速、灵敏、准确的定量方法。采用微波消解及直接进样技术比对,结果表明,以钪(Sc)、铟(In)、铽(Tb)为内标元素,消除基体干扰及仪器漂移。在选定的仪器条件下,直接进样,外标法定量,相对标准偏差小于3%,加标回收率在86.4%~100%,精密度和准确度都能满足测定要求,成功用于能力验证样品的测定,结果令人满意。     

烟草制品及烟气中重金属检测方法的研究进展

从烟草制品及其烟气的前处理方法和检测方法两方面对烟草中重金属含量测定的研究进展进行了综述。重点介绍了湿法消解、微波消解、萃取和悬浮进样技术等样品前处理方法,以及原子光谱法、质谱法和液相色谱法等测定方法。列举了不同方法的灵敏度、准确性和适用范围,对各方法的优缺点进行了比较,并对烟草中重金属检测方法的发展进行了展望。     

电感耦合等离子体原子发射光谱(ICP-AES)法和电感耦合等离子体质谱(ICP-MS)法测定大气降尘中的铅、镉、铬、锌、锰、镍、铜、铊

大气中Pb、Cd、Cr、Mn、Ni、Tl等重金属污染物是目前国内外城市大气污染的主要因子之一,研究大气降尘中重金属元素含量具有重大意义。本文采用盐酸-硝酸混合酸为消解体系,在105℃条件下用电热板消解回流大气降尘样品2小时后定容测定,通过电感耦合等离子发射光谱法仪(ICP-AES)和电感耦合等离子体质谱仪(ICP-MS)测定大气降尘中铅、镉、铬、锌、锰、镍、铜和铊等8种重金属元素。测定结果表明： ICP-AES(铅、镉、铬、锌、锰、镍、铜)和ICP-MS(铊)两种方法的曲线线性好,准确度高,测定范围宽,检出限在0.024mg/kg-0.548mg/kg之间,精密度在0.15%-2.38%之间,能准确测定大气降尘中的重金属元素含量。     

电感耦合等离子体质谱(ICP-MS)法同时测定荞麦秸秆中的8种重金属元素

基于硝酸-盐酸-氢氟酸消解体系,建立了马弗炉-微波消解-电感耦合离子体质谱(ICP-MS)法同时测定荞麦秸秆中的Cr、Cu、Ag、Mn、Fe、As、Ni、Pb等重金属含量测定方法。在微波消解的过程中,分别考察5种不同组合的混合酸体系及两种消解方法对荞麦秸秆中8种重金属测试结果的影响。实验结果表明,浓硝酸-浓盐酸-氢氟酸(6∶2∶2)混酸体系和马弗炉-微波消解样品前处理优于其他方法。在优化条件下,8种重金属加标回收率为91.2%~102%,相对标准偏差(RSD,n=5)为0.22%~4.7%,检出限为0.18~9.41μg/L。方法操作简便、快速、准确,结果可靠,能同时测定荞麦秸秆中8种重金属元素。     

Different Lubricating Oil Treatments for the Determination of Cu,Cr, Fe,Ni, Sb,Pb, and Zn by HR-CS FAAS

Abstract

Microwave-assisted acid decomposition, direct dilution in kerosene, and oil-in-water emulsion were evaluated as lubricating oil pretreatment procedures for Cu, Cr, Fe, Ni, Pb, Sb, and Zn determination by High-Resolution Continuum Source Flame Atomic Absorption Spectrometry (HR-CS FAAS). For wet digestion, results were compared with those obtained by Flame Atomic Absorption Spectrometry (FAAS). The ultrasound probe used in emulsions sonication contaminated samples with Cr, although better results have been observed for the other six elements in this condition. In general, recovery percentages ranging from 81–106% (Cu), 80–107% (Cr), 85–114% (Fe), 82–116% (Ni), 86–117% (Pb), 85–115% (Sb), and 81–114% (Zn) were obtained. The HR-CS FAAS showed to be faster and more sensitive than FAAS.     

川西食用菌重金属含量测定和食用风险评估

目的 测定川西地区食用菌重金属含量水平并评估其食用风险,为川西食用菌生产提供基础资料与参考依据。 方法 于川西8个地区随机采集市售食用菌干制品12种共41批次,采用微波消解-电感耦合等离子体-质谱法测定As、Cd、Hg、Pb含量,采用高效液相色谱法-电感耦合等离子体-质谱法检测松茸中As元素各形态化合物含量;分别使用污染指数法和靶标危害系数法评估样品中重金属污染状况和潜在食用风险。结果 川西地区综合污染指数为1.824,As为川西地区主要污染,单因子污染指数为2.471。八个地区中雅江县综合污染指数为5.048,理塘县综合污染指数为1.775。干松茸成人与儿童总靶标危害系数（TTHQ）大于1。结论 川西食用菌干制品中重金属存在超标问题,川西食用菌存在一定食用风险,建议对食用菌中重金属的污染状况和健康风险进行持续检测和评估。     

Comparison of Microwave-Assisted Digestion Methods and Selection of Internal Standards for the Determination of Rh, Pd and Pt in Dust Samples by ICP-MS

Different temperature-pressure controlled microwave-assisted digestion methods were compared for the digestion of dust samples prior to the determination of rhodium and platinum by inductively coupled plasma mass spectrometry (ICP-MS). The results obtained for platinum and rhodium in the digested reference material (BCR-723, road dust) were generally in good agreement with the certified values. However, the determination of matrix elements (Zn, Rb, Sr, Y, Hf and Pb) showed clear differences between the digestion methods. In addition, different internal standards were compared in the determination rhodium, palladium and platinum by ICP-MS. According to the results, even serious non-spectral interferences can be corrected by choosing a suitable internal standard or combination of internal standards.     

测定土壤中重金属元素的样品消解方法

摘要：探讨适用于重金属分析的土壤样品处理方法。利用原子吸收光谱法测定土壤中Cu,Mn,Ni,Pb和Zn 5种元素的含量,对电热板、微波和水浴3种消解方法进行比较,结果表明：3种样品预处理方法的检出限、准确度和精密度均满足分析检测要求。其中,电热板法样品消解较彻底,Cu和Pb的测定结果准确,但试剂、时间和人力消耗多,且为敞开式消解,高温及产生的大量酸雾危害环境与健康;微波法为密闭式消解,样品和试剂用量少,耗时短,自动化程度高,消解彻底,安全环保,Mn的测定结果准确,但成本高,不适于大批量样品分析;水浴法为半封闭式消解,简单易行,Ni和Zn的测定结果准确,但消解剂中不含氢氟酸,不适于含有大量硅酸盐样品的处理。     

Determination of parabens in wastewater samples via robot-assisted dynamic single-drop microextraction and liquid chromatography–tandem mass spectrometry

Dynamic single-drop microextraction (SDME) was automatized employing an Arduino-based lab-made Cartesian robot and implemented to determine parabens in wastewater samples in combination with liquid chromatography–tandem mass spectrometry. A dedicated Arduino sketch controls the auto-performance of all the stages of the SDME process, including syringe filling, drop exposition, solvent recycling, and extract collection. Univariate and multivariate experiments investigated the main variables affecting the SDME performance, including robot-dependent and additional operational parameters. Under selected conditions, limit of detections were established at 0.3 µg/L for all the analytes, and the method provided linear responses in the range between 0.6 and 10 µg/L, with adequate reproducibility, measured as intraday relative standard deviations (RSDs) between 5.54% and 17.94%, (n = 6), and inter-days RSDs between 8.97% and 16.49% (n = 9). The robot-assisted technique eased the control of dynamic SDME, making the process more feasible, robust, and reliable so that the developed setup demonstrated to be a competitive strategy for the automated extraction of organic pollutants from water samples.     

The Use of the PREPTM System for Handling of Body Fluids

Abstract

The Du Pont PREP^TM automated sample processor is a centrifugally based, microprocessor controlled instrument that was designed for extraction of samples from biological fluids. Extraction takes place in cartridges containing either organic resins or bonded silica packings as extraction sorbants. This paper will discuss the application of several lipophilic and ion exchange sorbants to the extraction of biological samples from body fluids. The advantages of these different types of sorbants will be compared and their performance with automated sample preparation will be shown. A variety of applications including the extraction of benzodiazepine, barbiturate, aminoglycoside and anticonvulsant drugs and their metabolites from serum, urine, and tissue homogenates will be discussed.     

微波消解-ICP-MS测定电镀污泥中的重金属

采用微波消解系统对某电镀污泥进行消解,利用ICP-MS对污泥中的重金属进行测定。称取制备后样品,置于消解罐中充分反应后,赶酸、定容后利用电感耦合等离子体质谱法进行测定。电镀污泥中的铬为18845.2mg/kg、镉为10.3mg/kg、镍为5200.0mg/kg、铅为189.7mg/kg、铜为3271.7mg/kg、锌为49632.6mg/kg。测定结果表明所检测项目工作曲线线性关系好,相关系数r均大于0.999。铬加标回收率在91.6～97.7%之间、镉加标回收率在92.0～97.0%之间、镍加标回收率在95.1～98.0%之间、铅加标回收率在94.3～95.2%之间、铜加标回收率在97.1～102%之间、锌加标回收率在96.3～98.7%之间,均满足相关测定要求。计算的潜在生态危害系数、潜在生态危害指数结果表明,电镀污泥中的铬、镉、铅、铜、锌为轻微生态危害,镍为强生态危害;潜在生态危害指数RI计算值为216.69,属于中等生态危害。