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黑色圓珠筆的色譜法鑒定

發(fā)布時(shí)間:2018-11-11 18:13
【摘要】:隨著計(jì)算機(jī)和網(wǎng)絡(luò)的發(fā)展,電子通信,電子署名和整體電子經(jīng)濟(jì)業(yè)務(wù)變得越來越流行,但是以筆墨書寫的文件依然是人們?cè)谏虡I(yè)交往中廣泛使用和信任的法律文件。因此,可疑文件的檢測(cè)依然是法庭科學(xué)中的重要課題。本文主要針對(duì)國內(nèi)外不同生產(chǎn)廠家的33種黑色圓珠筆進(jìn)行色譜法分類的研究,主要包括薄層色譜法(TLC),,高效液相色譜法(HPLC)和氣相色譜法(GC)。 首先,本文概述了油墨的主要成分,包括染料,溶劑,樹脂以及抗氧化劑,耐熱劑以及防水劑和耐光劑等。并對(duì)TLC,HPLC以及GC在該領(lǐng)域的研究進(jìn)行了總結(jié)。 其次,通過薄層色譜法,高效液相色譜法以及氣相色譜法對(duì)樣品筆進(jìn)行了系統(tǒng)的分析。其中,薄層色譜法由于具備操作方便,廉價(jià)以及快速等優(yōu)點(diǎn)得到廣泛應(yīng)用。根據(jù)油墨中不同的化學(xué)組分在薄層色譜測(cè)定中產(chǎn)生的斑點(diǎn)的個(gè)數(shù)以及比移值的不同對(duì)圓珠筆進(jìn)行分類。根據(jù)本實(shí)驗(yàn)的薄層色譜條件,將黑色圓珠筆分為12類。薄層色譜法分辨能力有其局限性,對(duì)于組分的微小的差異不能區(qū)分,由于高效液相色譜具有更高的靈敏度和分辨率,因此,研究了高效液相色譜法對(duì)這些圓珠筆進(jìn)行測(cè)定的方法。該方法中,使用SunFire C-18色譜柱,以乙腈:水(NH_4HCO_3)=60:40(PH=8)做流動(dòng)相,二極管陣列多波長檢測(cè)器對(duì)200-700nm進(jìn)行掃描。該方法大大提高了靈敏度和分辨率,同時(shí)用流程圖根據(jù)不同波長下的色譜峰進(jìn)行了再次分類,HPLC進(jìn)一步區(qū)分了TLC不能區(qū)分的油墨。HPLC不能被廣泛應(yīng)用的原因主要是它要求取樣量大,操作者需具有一定儀器操作的熟練程度以及耗資昂貴等局限性。氣相色譜法主要用于分析油墨中的揮發(fā)性組分,本實(shí)驗(yàn)中,用氣相色譜法對(duì)樣品筆進(jìn)行了分析,將其分為四大類。但是氣相色譜法更多的用于鑒定油墨的書寫時(shí)間而不是圓珠筆的分類。 最后,用本文中建立的實(shí)驗(yàn)方法對(duì)北京市刑事技術(shù)研究所送檢的盲測(cè)樣品(6個(gè)黑色圓珠筆油墨字跡)進(jìn)行測(cè)定,經(jīng)送檢者確證,實(shí)驗(yàn)結(jié)果與真實(shí)結(jié)果完全吻合。
[Abstract]:With the development of computer and network, electronic communication, electronic signature and the whole electronic economic business become more and more popular, but the documents written in pen and ink are still the legal documents widely used and trusted by people in business exchanges. Therefore, the detection of suspicious documents is still an important subject in forensic science. This paper focuses on the classification of 33 kinds of black ballpoint pens from different manufacturers at home and abroad, including thin layer chromatography (TLC), (TLC), high performance liquid chromatography (HPLC) and gas chromatography (GC). First of all, this paper summarizes the main components of ink, including dyes, solvents, resins and antioxidants, heat resistant agents and water-repellent and light resistance. The research of TLC,HPLC and GC in this field is summarized. Secondly, the sample pen was systematically analyzed by thin layer chromatography, high performance liquid chromatography and gas chromatography. TLC has been widely used because of its advantages of convenient operation, low cost and fast operation. The ball-point pen was classified according to the number of spots produced by TLC and the specific shift value of different chemical components in ink. According to the conditions of TLC, black ballpoint pens are classified into 12 categories. The resolution ability of TLC has its limitations, and the small differences in components can not be distinguished. Because of the higher sensitivity and resolution of HPLC, therefore, A method for the determination of these ballpoint pens by high performance liquid chromatography (HPLC) was studied. In this method, SunFire C-18 column was used, acetonitrile: water (NH_4HCO_3) = 60:40 (PH=8) was used as mobile phase, diode array multi-wavelength detector was used to scan 200-700nm. The sensitivity and resolution of the method are greatly improved, and the flow chart is used to reclassify the chromatographic peaks at different wavelengths. HPLC further distinguishes the inks that TLC can't distinguish. The main reason why HPLC can not be widely used is that it requires a large amount of sampling, the operator must have a certain degree of proficiency in the operation of the instrument, and the cost is expensive and so on. Gas chromatography is mainly used for the analysis of volatile components in ink. In this experiment, sample pens were analyzed by gas chromatography and divided into four categories. But gas chromatography is more used to identify ink writing times than ballpoint pen classification. Finally, the blind test samples (6 black ballpoint pen ink handwriting) submitted by Beijing Institute of Criminal Technology are determined by the experimental method established in this paper. The experimental results are in good agreement with the real results.
【學(xué)位授予單位】:首都師范大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2006
【分類號(hào)】:D918.92

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