Forensic Characterization of Papers. II: Determination of Batch Differences by Scanning Electron Microscopic Elemental Analysis of the Inorganic Components

Polk, D.E.; Attard, Alfred E.; Giessen, B.C.

doi:10.1520/jfs10623j

Cited by 22 publications

(21 citation statements)

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“…Typically, the forensic characterization of paper relies upon the analysis of physical properties such as thickness, strength and morphology of the fibers, which offers very limited informative value [17]. These methods are often insufficient to detect statistically significant variations within and between sources of paper, therefore they lack the scientific foundation to differentiate one paper source from another or to associate sheets of paper that share a common origin [18].…”

Section: Introductionmentioning

confidence: 99%

Micro-spectrochemical analysis of document paper and gel inks by laser ablation inductively coupled plasma mass spectrometry and laser induced breakdown spectroscopy

Trejos

Flores²,

Almirall

2010

Spectrochimica Acta Part B: Atomic Spectroscopy

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Section: Introductionmentioning

confidence: 99%

Micro-spectrochemical analysis of document paper and gel inks by laser ablation inductively coupled plasma mass spectrometry and laser induced breakdown spectroscopy

Trejos

Flores²,

Almirall

2010

Spectrochimica Acta Part B: Atomic Spectroscopy

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“…Other analysis techniques have been successfully applied to inks, including highperformance liquid chromatography (HPLC) [13][14][15], capillary zone electrophoresis [15,16], Xray fluorescence [15,[17][18][19], surface-enhanced Raman spectroscopy (SERS) [20][21][22], and FT-IR spectroscopy [7,15,18,23,24]. These generally provide more compositional information than TLC does, and some of them lend themselves to computer-searchable libraries, so a reference collection of inks need not be maintained.…”

Section: Introductionmentioning

confidence: 99%

Analysis of writing inks on paper using direct analysis in real time mass spectrometry

Jones¹,

McClelland²

2013

Forensic Science International

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Ink analysis is central to questioned document examination. We applied direct analysis in real time mass spectrometry (DART MS) to ballpoint, gel, and fluid writing ink analysis. DART MS acquires the mass spectrum of an ink while it is still on a document without altering the appearance of the document. Spectra were acquired from ink on a variety of papers, and the spectrum of the blank paper could be subtracted out to produce a cleanly isolated ink spectrum in most cases. Only certain heavy or heavily processed papers interfered. The time since an ink is written on paper has a large effect on its spectrum. DART spectra change radically during the first few months after an ink is written as the more volatile components evaporate, but the spectra stabilize after that. A library-search study involving 166 well-aged inks assessed the ability to identify inks from their DART spectra. The aggregate success rate was 92%. ABSTRACTInk analysis is central to questioned document examination. We applied direct analysis in real time mass spectrometry (DART MS) to ballpoint, gel, and fluid writing ink analysis. DART MS acquires the mass spectrum of an ink while it is still on a document without altering the appearance of the document. Spectra were acquired from ink on a variety of papers, and the spectrum of the blank paper could be subtracted out to produce a cleanly isolated ink spectrum in most cases. Only certain heavy or heavily processed papers interfered. The time since an ink is written on paper has a large effect on its spectrum. DART spectra change radically during the first few months after an ink is written as the more volatile components evaporate, but the spectra stabilize after that. A library-search study involving 166 well-aged inks assessed the ability to identify inks from their DART spectra. The aggregate success rate was 92%.

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“…The inorganic analysis of ink has been also reported in the literature and has shown its potential to improve the discrimination value of the evidence [Polk 1977;Ferrero 1999;Rozic et al, 2005;Malzer et al2004;Ouija et al 2005 Moreover, some limitations remain on the existing methods; such as: a) the sensitivity does not allow the detection of elements present at trace elements, [Polk 1977, Zieba-Palus et al, 2008 b) the depth of the x-ray penetration its not easily controlled by the operator and may affect the results, [Zieba-Palus et al, 2006, Zieba-Palus et al, 2008 c) the contribution of the paper and the ink can not be easily isolated, [Malzer et al, 2004, Zieba-Palus et al, 2006, d) the technique is not readily available in forensic laboratories [Grassi 2007, Oujja 2005, Melessanaki et al, 2001], f) the technique consumes large amount of sample which may not be available or acceptable in a particular case [Spence et al, 2000;Rozic et al, 2005;Maind et al, 2006;Maind et al, 2008] or g) the technique is mainly qualitative [Polk 1977, Ferrero 1999, Ouija 2005, Zieba-Palus et al, 2008.…”

Section: The Astm Standard Guide For Test Methods For Forensic Writinmentioning

confidence: 99%

“…[Manso et al, 2009]. In spite of the application to historical documents, forensic paper characterization has focused mainly on the measurement of physical properties, such as thickness, color, fluorescence, strength, fiber content and fiber morphology [Polk et al, 1977]. These methods are often deficient to detect differences between different brands of papers produced by the different manufacturers or to associate two sheets of paper with a high degree of certainty [Spence et al, 2000].…”

Section: Paper Manufacturingmentioning

confidence: 99%

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Evaluation of the Evidential Value of the Elemental Composition of Glass, Ink and Paper by Laser-Based Micro-Spectrochemical Methods

Trejos¹

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DEDICATIONThis dissertation is dedicated to my family, especially to my husband and my mom who are my day-to-day inspiration. I have learned from you both how to be perseverant and keep believing in our dreams. I also dedicate this work to my lovely kids: Montserrat and Anthony, being your mom has been God's greatest gift and privilege. In the first part of this study, the analytical performance of LIBS and LA-ICP-MS methods was evaluated for paper, writing inks and printing inks. A total of 350 ink specimens were examined including black and blue gel inks, ballpoint inks, inkjets and toners originating from several manufacturing sources and/or batches. The paper collection set consisted of over 200 paper specimens originating from 20 different paper sources produced by 10 different plants.Micro-homogeneity studies show smaller variation of elemental compositions within a single source (i.e., sheet, pen or cartridge) than the observed variation between different sources (i.e., brands, types, batches). Significant and detectable differences in the elemental profile of the inks and paper were observed between samples originating from different sources (discrimination of 87 -100% of samples, depending on the sample set under investigation and the method applied). These results support the use of vii elemental analysis, using LA-ICP-MS and LIBS, for the examination of documents and provide additional discrimination to the currently used techniques in document examination.In the second part of this study, a direct comparison between four analytical methods (µ-XRF, solution-ICP-MS, LA-ICP-MS and LIBS) was conducted for glass analyses using interlaboratory studies. The data provided by 21 participants were used to assess the performance of the analytical methods in associating glass samples from the same source and differentiating different sources, as well as the use of different match criteria (confidence interval (±6s, ±5s, ±4s, ±3s, ±2s), modified confidence interval, t-test (sequential univariate, p=0.05 and p=0.01), t-test with Bonferroni correction (for multivariate comparisons), range overlap, and Hotelling's T 2 tests. Error rates (Type 1 and Type 2) are reported for the use of each of these match criteria and depend on the heterogeneity of the glass sources, the repeatability between analytical measurements, and the number of elements that were measured. The study provided recommendations for analytical performance-based parameters for µ-XRF and LA-ICP-MS as well as the best performing match criteria for both analytical techniques, which can be applied now by forensic glass examiners.

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Forensic Characterization of Papers. II: Determination of Batch Differences by Scanning Electron Microscopic Elemental Analysis of the Inorganic Components

Abstract: Paper is often used in the course of criminal activities, including kidnapping, bombings, forgery, conspiracy, threatening letters, and gambling. Thus the examination of paper is a common task for the document examiner [1].

Cited by 22 publications

References 3 publications

Micro-spectrochemical analysis of document paper and gel inks by laser ablation inductively coupled plasma mass spectrometry and laser induced breakdown spectroscopy

Micro-spectrochemical analysis of document paper and gel inks by laser ablation inductively coupled plasma mass spectrometry and laser induced breakdown spectroscopy

Analysis of writing inks on paper using direct analysis in real time mass spectrometry

Evaluation of the Evidential Value of the Elemental Composition of Glass, Ink and Paper by Laser-Based Micro-Spectrochemical Methods

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