静电复印纸的FT－Raman光谱检验

对23种品牌的静电复印纸的拉曼图进行了分析,根据填料峰的不同可将其分为三大类根据纤维素峰和木素峰的相对峰强度比的不同,利用正态分布的t检验方法对静电复印纸作了进一步区分,为区分不同牌号的静电复印纸提供了一种参考方法.     

红外光谱在刑事案件中的应用

目的针对各类案件繁多的物证检材,结合实验室的工作范围、特点,积累适用的商品材料光谱图[1],切合实际、提高工作效率.方法选择生活中常见的多组分材料采用FTIR分析方法.结果将其制作成标准谱图,作为案件的参照物进行比对.结论该方法在刑事案件鉴定中取得了良好的效果.     

A detailed mechanistic fragmentation analysis of methamphetamine and select regioisomers by GC/MS

A novel ring-substituted methamphetamine regioisomer, N,alpha,4-trimethyl phenmethylamine, was synthesized in order to study the validity of proposed structures for various mass spectrometry (MS)-derived peaks in a methamphetamine fragmentation pattern. While other research efforts have studied aspects of methamphetamine in detail, a full fragmentation study has not been reported previously. In addition to showing molecular structures represented by fragment peaks, mechanisms for selected processes are detailed. An empirically derived procedure to easily determine by simple spectral peak pattern recognition the geometry of dimethyl- or ethyl-substituted immonium ions (RRC = N+ RR) where m/z = 58 is outlined. These results are platform independent for electron ionization (EI) instruments, but have also proven to be helpful in explaining spectral peaks observed in spectra from ion trap systems. The spectrum for the synthesized methamphetamine regioisomer was accurately predicted using this methodology. While this approach is useful in some casework, the converse may be more useful: when an unexpected or unusual peak pattern arises in a spectrum, being able to analyze it to determine the structure of the molecule. This paper gives an analyst the means to begin such retro-synthetic analyses.     

Analysis of Explosives by GC‐UV

A mixture of explosives was analyzed by gas chromatography (GC) linked to ultraviolet (UV) spectrophotometry that enabled detection in the range of 178–330 nm. The gas‐phase UV spectra of 2,4,6‐trinitrotoluene (TNT), 2,4‐dinitrotoluene (DNT), ethylene glycol dinitrate (EGDN), glycerine trinitrate (NG, nitroglycerine), triacetone triperoxide (TATP), and pentaerythritol tetranitrate (PETN) were successfully recorded. The most interesting aspect of the current application is that it enabled simultaneous detection of both the target analyte and its decomposition products. At suitable elevated temperatures of the transfer line between the GC instrument and the UV detector, a partial decomposition was accomplished. Detection was made in real time and resulted in overlaid spectra of the mother compound and its decomposition product. Hence, the presented approach added another level to the qualitative identification of the explosives in comparison with traditional methods that relies only on the detection of the target analyte. As expected, the decomposition product of EGDN, NG, and PETN was NO, while TATP degraded to acetone. DNT and TNT did not exhibit any decomposition at the temperatures used.     

Identifying reliable ions for the statistical differentiation of structurally similar fentanyl analogs

Definitive identification of fentanyl analogs based on mass spectral comparison is challenging given the high degree of structural and, hence, spectral similarity. To address this, a statistical method was previously developed in which two electron-ionization (EI) mass spectra are compared using the unequal variance t-test. Normalized intensities of corresponding ions are compared, testing the null hypothesis (H₀) that the difference in intensity is equal to zero. If H₀ is accepted at all m/z values, the two spectra are statistically equivalent at the specified confidence level. If H₀ is not accepted at any m/z value, then there is a significant difference in intensity at that m/z value between the two spectra. In this work, the statistical comparison method is applied to distinguish EI spectra of valeryl fentanyl, isovaleryl fentanyl, and pivaloyl fentanyl. Spectra of the three analogs were collected over a 9-month period and at different concentrations. At the 99.9% confidence level, the spectra of corresponding isomers were statistically associated. Spectra of different isomers were statistically distinct, and ions responsible for discrimination were identified in each comparison. To account for inherent instrument variations, discriminating ions for each pairwise comparison were ranked based on the magnitude of the calculated t-statistic (t_calc) value. For a given comparison, ions with higher t_calc values are those with the greatest difference in intensity between the two spectra and, therefore, are considered more reliable for discrimination. Using these methods, objective discrimination among the spectra was achieved and ions considered most reliable for discrimination of these isomers were identified.     

Analytical methods used for the discrimination of substances suspected to be bar soap: a preliminary study

The submission to forensic laboratories of unknown specimens suspected of being biological or chemical warfare agents has increased tremendously with the threat of terrorism. Oftentimes, a threatening correspondence that contains hoax materials is intended to make the recipient(s) believe they have been exposed to a toxin. In some cases, the perpetrator can use standard household products, such as detergents and soaps. Once these materials are received, they become forensic evidence and may be analyzed for identification and/or comparison with known seized material from a suspect(s). Two separate studies were conducted using different analytical protocols for bar soaps. In the first set, the forensic laboratory at the United States Secret Service conducted tests on 68 bars of soap using solid-phase microextraction and gas chromatography coupled with mass spectrometry. The 68 different soaps displayed unique total ion chromatogram profiles. Energy-dispersive X-ray analysis in conjunction with scanning electron microscopy was also used to characterize 46 of the 68 soaps as a preliminary study. In a second set of studies, as part of a homicide investigation, the laboratory at the California Department of Justice, Riverside, conducted examinations on 13 bars of soap by utilizing Fourier transform-infrared spectroscopy. The case study demonstrated that it is possible to distinguish some bar soaps using infrared analysis. Furthermore, the bar soaps could be distinguished from typical laundry detergents using this technique.     

血手印显现的实验研究

目的 提出了采用荧光显现试剂显现血手印的新方法。方法 在比较使用联苯胺及其衍生物显现血手印的同时,实验了通过强氧化剂破坏血红素、沉淀珠蛋白,采用激活血痕、蛋白染色的方法,使血手印清晰显出。结果 显现效果不受客体表面颜色的影响,不受血手印遗留时间的影响。结论 适用客体范围广,灵敏度高。     

傅里叶红外图像——单点模式法无损鉴别中性笔墨水色痕

中性笔墨水色痕形成文件的检验是目前法庭科学实验室经常遇到的问题,文中对市场上收集到的15种不同品牌的中性笔进行了鉴别,采用单点模式无损鉴别的方法区分墨水的色痕。实验结果表明,根据红外特征谱图所形成红外吸收峰的位置、峰的数量、峰的强度及形状和二阶导数光谱可将不同生产厂家或牌号的黑色中性笔墨水区分开来。     

A preliminary investigation into the use of FTIR microscopy as a probe for the identification of bullet entrance holes and the distance of firing

FTIR spectroscopy has been found to be a valuable probe for the analysis of the distribution of organic components such as nitroglycerine in gunshot residues deposited on and around the bullet entrance hole of the clothing of the victim in short range firearm discharges. The method can be utilised for the detection and estimation of organic gunshot residues (OGSR) on the hands and clothing of the shooter. The method is specific and sensitive and is likely to be free from interference from, for example, environmental pollution. The method shows potential to be utilised as a suitable alternative to the widely used SEM-EDX analysis of the total contents of lead, barium and antimony present in the gunshot deposits around the bullet entrance hole. The method was tested in the laboratory and the results were validated by Gas Chromatography-Mass Spectrometry (GC-MS).     

Analysis of Hypodermic Needles and Syringes for the Presence of Blood and Polydimethylsiloxane (Silicone) Utilizing Microchemical Tests and Infrared Spectroscopy

Suspect hypodermic needles and syringes were seized from an unlicensed individual who was allegedly injecting patients with silicone (polydimethylsiloxane [PDMS]) for cosmetic enhancement. Since control syringe barrels and needles often contain an interfering PDMS lubricant, a risk for false positives of foreign PDMS exists. The focus of this report was to minimize this risk and determine a quick and reliable test for the presence of blood in PDMS matrices. Using ATR‐FT‐IR spectroscopy, the risk for false‐positive identification of foreign PDMS was reduced by (i) overfilling the sampling aperture to prevent spectral distortions and (ii) sampling a region of the suspect syringe/needle assembly where manufacturer‐applied PDMS is not typically located. Analysis for blood indicated that the Teichman microchemical test was effective for detecting blood in the presence of PDMS. Overall, detecting PDMS established intent and detecting blood established that the needle containing the PDMS had been used for injection.