摘要
随着社会经济的快速发展,法庭科学和刑侦领域涉及文档真伪鉴定的案件呈逐年增加的趋势,对圆珠笔字迹种类和书写时间的鉴定一直是法庭科学中的难题。由于油墨组成成分的多样性和测定的干扰性,更对油墨的分类和老化的研究增加了挑战。我们结合5种仪器方法对市售的54支红色圆珠笔进行了综合考察。
首先,介绍了油墨分析、鉴定的研究进展,综述了近年来国内外对可疑文件的种类鉴定和书写时间鉴定的发展和应用,介绍了常用的仪器分析方法,包括:薄层色谱法、气相色谱法、液相色谱法、毛细管电泳法和液质联用技术,并对圆珠笔的发展史、原理及结构、分类和油墨的成分进行了阐述。
其次,通过紫外可见分光光度法、电化学方法、薄层色谱法、高效液相色谱法和液质联用法对样品笔进行测定,并选择了最佳的实验条件。由于高效液相色谱法具有很高的灵敏度和分辨率,我们根据液相中350nm和528nm波长下出峰的个数、峰的保留时间和最大吸收波长的不同将红色圆珠笔分为六大类,每一类都结合其他的四种方法进行综合分析。五种仪器分析方法的检出信号之间存在着一一对应关系。为以后结合多种方法对红色圆珠笔的分析鉴定奠定了基础。
最后,还对其他的分类方法进行了研究。在液相色谱更低的波段,出峰更多,样品笔之间的区别更明显。我们选择254nm波长下检测,用分级流程图可以将属于一大类的笔进一步细分。我们还根据不同厂家不同品牌的笔所添加的油墨染料的配比的不同,对红色圆珠笔进一步分类。
With the fast development of social economy, the case involved detecting and discriminating of distrustful document grows very year in forensic science and criminal reconnaissance. It is a big problem to examine the type and the dating of writing inks because of having too many ingredients and inaccurateness in measuring process. We tested 54 red ballpoint pens using 5 instrumental measures.
Initially ,it was summarized the resent advance of questioned documents and dating writing inks and introduced some instrumental methods in common use including thin layer chromatography, gas chromatography, high performance liquid chromatography, capillary electrophoresis and high performance liquid chromatography-mass spectrometry. It was expounded the phylogeny, elements, configuration, class and component of red ballpoint Pen.
54 red ballpoint pens were analyzed by ultraviolet-visible photography, electrochemical method, thin layer chromatography, high performance liquid chromatography and high performance liquid chromatography-mass spectrometry under the optimal experimental condition. Owing to HPLC greater sensitivity and resolving power, red ballpoint pens were separated into 6 kinds depending on numbers, reservation time and the most absorbing wavelength of chromatographic peaks in 350nm, 528nm.We had compared the signals and found the correlation of the 5 instrumental measures.
The pens were categorized using other methods. Because of more peaks appearance in lower wavelength, we could classify red ballpoint pens better. A classifier flowchart was designed for more categorization depending on chromatographic peaks in 254nm. Every red ballpoint pen was distinguished with others on account of difference in quantity of ink components.
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