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Coupled to Nanospray Mass Spectrometry for Localized Chemical Analysis of Document Inks

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Coupled to Nanospray Mass Spectrometry for Localized Chemical Analysis of Document Inks The author(s) shown below used Federal funds provided by the U.S. Department of Justice and prepared the following final report: Document Title: Microscopy with Direct Analyte Probe Nanoextraction (DAPNe)-Coupled to Nanospray Mass Spectrometry for Localized Chemical Analysis of Document Inks Author(s): Guido Verbeck, Teresa Golden, Vivian Huynh, Kristina Williams Document No.: 250335 Date Received: October 2016 Award Number: 2013-R2-CX-K007 This report has not been published by the U.S. Department of Justice. To provide better customer service, NCJRS has made this federally funded grant report available electronically. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. Microscopy with Direct Analyte Probe Nanoextraction (DAPNe)-Coupled to Nanospray Mass Spectrometry for Localized Chemical Analysis of Document Inks Award Number: 2013-R2-CX-K007 Authors: Guido Verbeck, Teresa Golden, Vivian Huynh, Kristina Williams 1 This document is a research report submitted to the U.S. Department of Justice. This report has not been published by the Department. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. Abstract A method for the extraction and analysis of ink samples was developed using microscopy with direct analyte probe nanoextraction coupled to nanospray mass spectrometry (DAPNe-NSI-MS) for localized chemical analysis of document inks. Nanomanipulation can be effectively coupled to nanospray ionization mass spectrometry providing picomolar sensitivity, the capability to analyze femtograms to attograms of material and reduce the required sample volume to as low as 300 nL. This new and innovative technique does not leave destructive footprints on the surface of a document. As proof of concept, analysis of inks from various eras were tested, iron gall ink and modern inks, as well as the capability to detect the oxidative products of polyethylene glycol (PEG), a common binding agent in India inks. The experimental results showed that DAPNe-NSI- MS was able to chelate iron (II) and manganese (II) ions of iron gall ink and organic components of modern and carbon-based inks. Regardless of whether the ink composition is modern or ancient, organic or inorganic, this new approach is able to identify and characterize the ingredients by modifying the extraction solvent, illustrating the potential diversity of the extraction chemistries. DAPNe also has been coupled to Raman spectroscopy, fluorescence microscopy, and NSI-MS to determine if an ink entry from a document was falsified. A handwritten number was altered using a different ink pen to test if the aforementioned techniques could discriminate the original number from the altered number, qualitatively and/or quantitatively. Chemical species from part of the original number, altered number, and a point at which both inks intersect were successfully differentiated by all techniques when using different pens. DAPNe coupled to fluorescence microscopy and Raman spectroscopy was not able to discriminate the forged ink entry when the exact same pen was used to modify the text (due to similar ink formula). However, DAPNe-NSI-MS successfully discerned that the pen was dispensed on different days by quantitating the oxidation process. The research for this proposal will take the sensitive nanomanipulation technique and combine it with spectroscopic techniques for ultra-trace analysis of chemical inks in document analysis. To establish the proof of concept, reproducibility, sensitivity, and qualitative and quantitative nature, the developed techniques will be used for forensic science trace analysis on paint, ink, and trace document residue from transfer. This will demonstrate the versatility of the techniques, and broad spectrum uses for basic and advanced document forensic analysis. 2 This document is a research report submitted to the U.S. Department of Justice. This report has not been published by the Department. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. Table of Contents Abstract ........................................................................................................................................... 2 Executive Summary ........................................................................................................................ 4 Main Body ...................................................................................................................................... 9 1. Introduction ............................................................................................................................. 9 2. Methods................................................................................................................................. 11 2.1. Materials ......................................................................................................................... 11 2.2. Instrumentation............................................................................................................... 12 2.3. Direct Extraction Analytical Scheme ............................................................................. 12 2.4. Analyzing Modern and Ancient inks ............................................................................. 13 2.5. Analyzing forged documents ......................................................................................... 14 3. Results ................................................................................................................................... 15 3.1. Analyzing modern and ancient inks ............................................................................... 15 3.2. Analyzing forged documents ......................................................................................... 21 4. Conclusions ........................................................................................................................... 27 4.1. Implications for Policy and Practice .............................................................................. 28 4.2. Implications for Further Research .................................................................................. 29 5. References ............................................................................................................................. 29 6. Dissemination of Research Findings .................................................................................... 33 6.1. Presentations................................................................................................................... 33 6.2. Publications .................................................................................................................... 34 3 This document is a research report submitted to the U.S. Department of Justice. This report has not been published by the Department. Opinions or points of view expressed are those of the author(s) and do not necessarily reflect the official position or policies of the U.S. Department of Justice. Executive Summary Problem Investigation of forged documents is crucial when determining authenticity. There have been many cases where checks, notes, contracts, or other important written certificates have been falsified. Forensic document examiners (FDEs) conduct physical and chemical analyses on these documents in order to decipher if a signature was altered or a number was changed and when the alteration occurred. Numerous procedures have been used for the extraction and analysis of ink from documents. Traditional, non-destructive methods involve a visual examination of the document by microscopy and/or Video Spectral Comparison (VSC). VSC relies on a visual comparison of grey levels, but fails to discern between inks in suspected alterations. Common procedures in analyzing these documents, such as separation techniques, are destructive. Although chromatographic methods give significant information about the ink, the extraction of ink from the document is harmful. Ink analysis plays a significant role in questioned and authentic documents. The courts prefer nondestructive methods so most forensic approaches focus on nondestructive means of analysis. Material evidence found at crime scenes must be kept in its pristine state in order to preserve its evidentiary value. However, a non-destructive method is difficult to achieve when analyzing ink markings. Purpose The proposed method was to develop a forensic science technique and instrumentation for the trace and ultra-trace analysis of inks, dyes, paints, and transferred chemistries on documents. This method focused on direct sampling and microphase extraction of chemical residues to isolate and analyze key components present in inks and transfer on documents. This was combined on a single package adapted to multiple platforms with broad range capabilities for the field of forensic science. The multistage workstation developed in our group has wide-ranging applications in the biological and chemical sciences. The workstation consists of a platform with 2-nano-positioners that hold end-effectors and capillaries used to manipulate, probe, and characterize objects of interest. The multistage workstation has been coupled to nanospray mass spectrometry allowing for precise and accurate analysis
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