生物样品中的金属毒物电感耦合等离子发射光谱检验

目的建立有毒金属元素在肝、脾和肾脏组织中的快速检测方法。方法通过模拟样品,采用微波消解炉对样品进行预处理,用电感耦合等离子发射光谱仪同时对多种可疑有毒金属元素进行检测。结果在中毒剂量,对肝脏和肾脏组织中的可疑毒金属元素,可以采用电感耦合等离子发射光谱仪进行检测。     

玻璃中痕量金属元素检测方法研究

目的建立玻璃中金属元素的快速检测方法。方法采用高温消解法对样品进行预处理,用电感耦合等离子体发射光谱仪同时对多种金属元素进行检测,同时对方法的精密度和准确度进行了测定。结果采用氢氟酸对样品进行预处理,各元素同时测定的发射光谱图相互无干扰。在所设定的条件下,各种元素的回收率均〉75％,相对标准偏差均〈10％。结论玻璃中金属元素可以通过高温消解进行预处理,应用电感耦合等离子体发射光谱仪同时进行检测。     

应用等离子发射光谱分析技术测定人体组织中的汞含量

汞中毒案件的传统分析是将洁净的铜片或铜丝放入酸性检材试料中煮沸,如表面被一层银灰色沉积物所覆盖,则可以证实检材中含有汞。也可做汞的升华实验来确定汞的存在。用原子吸收光谱仪、原子发射光谱仪、扫描电子显微镜、离子色谱法等分析技术来确定汞的存在与定量,检材需要一定的前处理,有些只能进行半定量分析。本文在改进湿法消化人体生物组织样品(肝、肾)方法的同时,应用等离子体发射光谱分析技术测定人体组织中的汞含量,此法具有可靠、准确、简便、快速、抗干扰性强等特点,同时还可对多种有毒金属元素进行定性、定量。     

微波消解ICP-MS法检测生物检材中汞元素

目的 建立生物检材中汞的电感耦合等离子体质谱分析方法.方法 采用微波消解法处理样品,以铟(115In)作内标,用电感耦合等离子体质谱仪对血液、尿液和头发中的汞含量进行分析.选择金与汞形成金汞齐,对金消除汞记忆效应的能力进行考察.结果 方法检出限为0.01μg/L,准确度为97.0%～107.1%.检测中添加金质量浓度在...     

激光剥蚀电感耦合等离子体质谱技术检测车辆油漆金属元素

目的建立车辆油漆的激光剥蚀电感耦合等离子体质谱（laser ablation inductively coupled plasma mass spectrometry,LA—ICP—MS）分析方法。方法对38种车辆油漆样品采用激光剥蚀,电感耦合等离子体质谱进行测定,通过各油漆样品本含有金属元素种类和金属元素响应相对比值的差异对油漆样品进行区分。结果38种样品中有30种可直接依据所含金属元素种类的差异进行对其进行区分,其余8种依据元素间响应值比值的差异进行区分,方法重现性良好,精密度（RSD）小于10％。结论所建立的LA—ICP—MS方法简便快速、精密度良好、对样品微损,适用于法庭科学对车辆油漆的检测。     

微波消解ICP-MS法测定人发中的汞

目的建立人发中汞的电感耦合等离子体质谱分析方法。方法采用微波消解法处理样品,以铟（115In）作内标,用电感耦合等离子体质谱分析人发中的汞含量。结果方法检出限为0.0032μg/g,准确度通过测定人发标准物质GBW07601、GBW09101b进行验证,检测结果与标准参考值相符。结论该方法快捷、高效,灵敏度、准确度高,适用于人发中汞含量的检测。     

微波消解ICP/AES标准加入法测定尿液中金属毒物

目的建立微波消解ICP/AES标准加入法测定尿液中As、Ba、Pb、Cd、Cr、Zn、Sb金属毒物。方法取1.0mL尿样,加入3mL浓硝酸和0.5mL双氧水,进行微波消解。冷却后,用2%的硝酸定容至10.0mL。采用标准加入ICP/AES法进行定量分析,并优选实验条件及考察方法可靠性。结果尿液中As、Ba、Pb、Cd、Cr、Zn、Sb回收率在98.6%～104%之间;检出限在2.0～5.1ng/mL之间;线性范围Zn为5.0～200.0μg/mL,其余元素为0.5～20.0μg/mL。采用本文方法测定与国家标准物质人发和牛肝数据测定值基本一致。结论该方法回收率高、检测限低、能多元素同时测定,可以用于尿液中金属元素的检测。     

电感耦合等离子体质谱法检测电流损伤皮肤中金属元素

目的探讨应用电感耦合等离子体质谱(inductively coupled plasma mass spectrometry,ICP-MS)技术检测电流损伤皮肤中金属元素的可行性,建立检测电流损伤皮肤中金属元素的方法。方法用黄铜、紫铜、铝、铁电极材料以220V交流电电击家兔后肢,ICP-MS对电流损伤皮肤中金属元素进行检测。结果与对照组比较:黄铜电击组皮肤中的Cr、Ni、Cu、Zn、Pb含量升高(P0.05),紫铜电击组皮肤中的Cr、Cu、Pb含量升高(P0.05),铝电击组皮肤中的Al、Cr、Mn、Co、Ni、Cu、Pb含量升高(P0.05),铁电击组皮肤中的Cr、Mn、Fe、Ni含量升高(P0.05)。不同电极材料电击后皮肤中元素种类及含量也存在明显差异。结论ICP-MS可作为检测电流损伤皮肤中金属元素的有效方法,且可应用于触电材料的推断。     

电感耦合等离子体质谱在白酒检验中的应用研究

目的 为了准确检验和区分不同的白酒,利用电感耦合等离子质谱法同时定量检测白酒中多种微量元素,根据多个元素含量参数对白酒样品进行分类,以实现对不同白酒的有效区分。方法 在优化的ICP-MS检测条件下,用标准溶液建立7Li、39K、51V、63Cu、75As、88Sr、208Pb 7种元素在确定范围内的标准工作曲线。用移液枪取待测白酒样品20mL于烧杯中,加热挥发至一定量后,用光谱纯硝酸消解,超纯水定容,然后用ICP-MS进行检测。利用所建立的标准工作曲线,计算出白酒中这7种元素的含量。结合21种常见白酒中不同元素的含量和ICP-MS方法参数,将不同元素含量划分为不同的区间范围,并根据不同白酒中元素含量对其进行归类编码。结果 将每种元素的含量范围划分为4个区间范围,分别记为A、B、C、D,并根据白酒中7Li、39K、51V、63Cu、75As、88Sr、208Pb 7种元素的含量所在的区间范围确定该种白酒的7位编码,通过比对21种常见白酒的编码,可以清晰准确地将这些白酒进行区分。结论 本文所采用的ICP-MS方法精密度好、可同时对多种元素进行定量检测,结合白酒中多元素含量分类方法,能够准确区分不同种类的白酒,因此可以广泛地应用于假冒伪劣白酒的检验鉴定。     

微波消解ICP-MS法测定人头发中24种元素的含量

目的建立人头发中24种无机元素的电感耦合等离子体质谱（inductively coupled plasma-mass spec-trometry,ICP-MS）分析方法。方法采用微波消解法处理样品,以铟（115In）作内标,用ICP-MS分析人头发中的24种元素含量。同时检测56例健康志愿者和10例海洛因滥用者头发中24种元素含量。结果 24种元素的方法检出限范围为0.0003~10.14μg/g,标准物质的测得值与标准值基本相符。海洛因滥用者经戒毒治疗后头发中镁、镓、钡含量下降。结论该方法灵敏度、准确度高,适用于头发中24种元素的测定。     

Identify the injury implements by SEM/EDX and ICP-AES

The forensic investigator is frequently confronted with the discrimination and deduction of injury implements, which is one of the most important physical testimonies in courts. The usual method used in actual cases is from points of morphology. In the forensic discrimination of injury implements, such as metal implements, the analysis and comparison of elements are expected to provide excellent results, and simultaneous multi-elemental analysis is required to analyze various kinds of elements. This study was designed to establish discrimination and deduction of metal injury implements by scanning electron microscope/energy disperse X-ray microanalyzer (SEM/EDX) and inductively coupled plasma atomic emission spectrometry (ICP-AES). Examined metal particles in five wounds made on the skin of domestic pigs, respectively, using Cu-Zn or Cr-Ni coated and carbon steel kitchen implements by EDX. For carbon steel kitchen implements, analyzed five samples from the back and blade separately in the contents and varieties of elements by ICP-AES. In the wounds by the coated implements, the special particles only containing Cu, Zn or Cr, Ni were found. In the wounds by carbon steel kitchen implements, the particles containing Fe, Cr, Si or Fe, Mn, Si were found. The differences of contents of elements between the back and blade was no significant except No. 5 for carbon steel kitchen implements, and the significant differences of elements exited in Cr, Mn, Si, Cu, Mo among the stainless kitchen knives, Mn, Si among the other kitchen implements and for the blade of No. 5 knife, relative standard deviations (R.S.D.s) were significantly different in Mn, Si, Mo, Ti, S, P, Ni. Using EDX to examine the particles in wounds can deduce the categories of metal injury implements, and we can still deduce the different implements in the same category by ICP-AES.     

Trace Elemental Analysis of Titanium Dioxide Pigments and Automotive White Paint Fragments for Forensic Examination Using High‐Energy Synchrotron Radiation X‐Ray Fluorescence Spectrometry*

Abstract: High‐energy synchrotron radiation x‐ray fluorescence spectrometry (SR‐XRF) utilizing 116 keV x‐rays was used to characterize titanium dioxide pigments (rutile) and automotive white paint fragments for forensic examination. The technique allowed analysis of K lines of 9 trace elements in 18 titanium dioxide pigments (rutile), and 10 trace elements in finish coat layers of seven automotive white paint fragments. High‐field strength elements (HFSE) were found to strongly reflect the origin of the titanium dioxide (TiO₂) pigments, and could be used as effective parameters for discrimination and classification of the pigments and paint fragments. A pairwise comparison of the finish coat layers of seven automotive white paint fragments was performed. The trace elements in the finish coat layers detected by the high‐energy SR‐XRF were especially effective for identification. By introducing the trace element information of primer and electrocoat layers, all the automotive white paint fragments could be discriminated by this technique.     

SEM/EDS法和XRF法在电工胶带检验中的应用

目的探索电工胶带带基的元素检验方法。方法利用扫描电镜/能谱法（SEM/EDS）对电工胶带带基中的主体元素进行定量分析,通过SPSS软件对SEM/EDS定量分析法检测出的主体元素（Cl和Ca）相对含量进行统计分析;利用X射线荧光光谱法（XRF）对电工胶带带基中的微量元素进行定性分析。结果34个品牌红色电工胶带组成的561组样品对通过SEM/EDS定量分析法可以区分539组,区分率达到96.1%;根据XRF法定性分析测出的Mg、Al、Si、S、Ti、Sb、Ba、Pb微量元素的不同组合可将34种电工胶带分成11组,两种方法结合可使不同品牌红色电工胶带的区分率达到98.4%。结论SEM/EDS法和XRF法结合可以实现同种颜色、不同品牌电工胶带的高效区分。     

Discrimination between sediment and soil samples for forensic purposes using elemental data: an investigation of particle size effects

This paper reports the results of an investigation to quantify variations in elemental concentrations amongst different particle size fractions obtained from a suite of sediment samples collected from the River Avon, UK. Concentrations of 49 elements determined by inductively coupled plasma spectrometry (ICP-AES and ICP-MS) were compared using conventional and multivariate statistical methods in order to assess compositional differences between different size fractions and between different samples. The results showed significant differences between different size fractions and the bulk sediments, but indicated that all of the size fractions considered (<150, 63-150, 20-63 and <20microm) provided an adequate basis on which to identify associations and differences between samples. It was concluded that, while in certain specific circumstances it may be most appropriate to make forensic comparisons based on a very narrowly defined particle size range, for the majority of purposes the <150microm fraction provides the best compromise between sample size requirements and data resolution.     

Quantitative evaluation of europium in blue ballpoint pen inks/offset printing inks tagged with europium thenoyltrifluoroacetonate by spectrofluorometry and ICP-AES

Tagging of writing/printing inks with suitable inorganic taggants such as rare-earth chelates has the potential to help document examiners identify fraud in sensitive written/printed documents. Selection of rare-earth chelates as taggants primarily depends on the satisfactory sensitivity of analytical determination and the absence of the taggants in normal varieties of inks used for document writing/printing. Spectrofluorometric determination of trace amounts of europium in blue ballpoint pen inks and offset printing inks tagged with europium thenoyltrifluoroacetonate was carried out with sodium tungstate solution. Sodium tungstate acts as a specific reagent that enhances the fluorescence intensity of the Eu3+ ion. The excitation and emission wavelengths are 270 nm and 605 nm respectively. The results were compared with the data obtained with ICP-AES. Satisfactory recoveries were observed with precision better than 5% RSD and comparable accuracy. Under the optimized experimental conditions, detection limits and quantitation limits were determined. The detection limits obtained by spectrofluorometry and ICP-AES were 0.01 microg/mL and 0.006 microg/mL respectively whereas the limits of quantitation were about 0.03 microg/mL and 0.018 microg/mL respectively. The spectrofluorometric method is rapid, selective, sensitive and accurate for the determination of europium in blue ballpoint pen ink and offset printing inks and may be suitable for application in the examination of sensitive documents to aid in document related crime investigation. The advantages and limitations of the tagging approach and proposed analytical techniques are discussed.     

Comparison of glass fragments using particle-induced X-ray emission (PIXE) spectrometry

A procedure has been developed to analyze the trace element concentrations in glass fragments using particle-induced X-ray emission (PIXE) spectrometry. This method involves using accelerated protons to excite inner-shell electronic transitions of target atoms and recording the resultant X-rays to characterize the trace element concentrations. The protocol was able to identify those glass fragments that originated from different sources based on their elemental analyses. The protocol includes specific approaches to calculating uncertainties and handling measurements below the level of detection. The results indicate that this approach has increased sensitivity for several elements with higher atomic number compared with X-ray fluorescence methods. While not as sensitive as laser-ablation or inductively coupled plasma mass spectrometry methods of dissolved samples, it is entirely nondestructive and entails a much simpler sample preparation process that may be used to presort glass fragments for more comprehensive elemental analysis. As such, the technique described may have a niche role in forensic glass analysis.     

The use of a method of mathematical analysis in establishing the species affiliation of animal hair

Quantitative content of 10 trace elements in hair of 9 species of animals was determined by atomic-absorbtion spectroscopy. Analysis of the resulting digital data using discriminant algorithm makes it possible to determine species and sex of an animal by trace element content of hair.     

Lead Theft—A Study of the “Uniqueness” of Lead from Church Roofs

In the United Kingdom, theft of lead is common, particularly from churches and other public buildings with lead roofs. To assess the potential to distinguish lead from different sources, 41 samples of lead from 24 church roofs in Northamptonshire, U.K, have been analyzed for relative abundance of trace elements and isotopes of lead using X‐ray fluorescence (XRF) and inductively coupled plasma mass spectrometry, respectively. XRF revealed the overall presence of 12 trace elements with the four most abundant, calcium, phosphorus, silicon, and sulfur, showing a large weight percentage standard error of the mean of all samples suggesting variation in the weight percentage of these elements between different church roofs. Multiple samples from the same roofs, but different lead sheets, showed much lower weight percentage standard errors of the mean suggesting similar trace element concentrations. Lead isotope ratios were similar for all samples. Factors likely to affect the occurrence of these trace elements are discussed.