Identification and differentiation of commercial and military explosives via high performance liquid chromatography – high resolution mass spectrometry (HPLC-HRMS), X-ray diffractometry (XRD) and X-ray fluorescence spectroscopy (XRF): Towards a forensic substance database on explosives

Schachel, Tilo D.; Stork, Alexandra; Schulte-Ladbeck, Rasmus; Vielhaber, Torsten; Kärst, Uwe

doi:10.1016/j.forsciint.2020.110180

Cited by 22 publications

(11 citation statements)

References 27 publications

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“…2 shows the effect of the increase of tG on the peak separation whereas Table II, Table III and Table IV display the effect of tG on the capacity factors (k), the number of theoretical plates (N), the resolutions (R) and selectivity (α) of each detected peak. For a further improvement of the separation, relative retention (peak spacing, selectivity, or separation factor α) is then adjusted by varying the organic solvent, temperature or type of column [17]. In order to improve the resolution of coeluting isomers, the column temperature was carried over the range of 25 -38°C.The separation runs were performed under the following conditions: a MeOH-H2O mixture with a flow rate of 1.2 mL/min is used as a mobile phase and the linear gradient as elution mode is varied from 5% to 100% of MeOH in H2O.…”

Section: Iii2 Effect Of Capacity Factor (K)mentioning

confidence: 99%

“…However, this research area remains an ongoing subject that needs more investigations to find new efficient approaches. Other advanced techniques such as nuclear magnetic resonance (NMR) have made it possible to identify the structural composition of explosives from post-blast debris [16] while combined techniques including HPLC-HRMS, XRD and XRF were used to gain fingerprints of various brands of explosives when including the analysis of additives and by-products [17]. These authors claim that these combined methods of analysis can be useful for the creation of a database on explosives that enables to assign specific formulations to certain manufacturers and countries of origin.…”

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confidence: 99%

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HPLC Method Development for the Fast Separation of a Complex Explosive Mixture

Boulesnam

Hami

Zaid

2021

ENPESJ

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The growing threat of terrorism in many parts of the world has called for the urgent need to find rapid and reliable means of analyzing explosives. This is in view to help forensic scientists to identify different swabs from post-blast debris. The present study aims to achieve an efficient separation and identification of a mixture of sixteen explosive compounds (including nitroaromatics, nitramines, and nitrate esters) by high performance liquid chromatography using a diode array detection (HPLC/DAD) and an Agilent Poroshell 120 EC-120 C18 column at two wavelengths (235 and 214 nm). Relevant chromatographic parameters such as capacity factors, resolution, selectivity and number of theoretical plates have been optimized in order to achieve the best separation of the different components. In this respect, the effects of various parameters such as gradient time, column temperature, flow rate of mobile phase and initial percentage organic mobile phase on the separation of these compounds were investigated. It was revealed that the method allowed a fairly acceptable separation of all the compounds in less than 15 minutes except for two isomers, namely 4-A-2,6-DNT, 2-A-4,6-DNT and 2,6- DNT which could not be resolved by the used C18 column. This shortcoming notwithstanding, the developed method produced satisfactory results and demonstrated sensitive and robust separation, furthermore indicating that the HPLC developed method can be both fast and efficient for the analysis of complex mixtures of explosive compounds.

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Section: Iii2 Effect Of Capacity Factor (K)mentioning

confidence: 99%

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confidence: 99%

HPLC Method Development for the Fast Separation of a Complex Explosive Mixture

Boulesnam

Hami

Zaid

2021

ENPESJ

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“…We have developed a method with a different analyte scope in our study, where a 10 min elution time was achieved. An High Pressure Liquid Chromatography-High Resolution Mass Spectrometry (HPLC-HRMS) method was developed in 2020, using 27 analytes, synthesis by-products and additives [32]. HPLC-HRMS, X-ray Diffraction (XRD) and X-ray Fluorescence (XRF) analyses were carried out to find out the composition.…”

Section: Introductionmentioning

confidence: 99%

LC-MS/MS monitoring for explosives residues and OGSR with diverse ionization temperatures in soil & hands: 30 minutes for extraction + elution

Şener¹,

Anılanmert

Maviş³

et al. 2022

AChrom

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A fast LC-APCI-MS/MS screening/confirmation method was developed and validated for trace analyses of 18 analytes which are explosives and organic gun shot residues including the challenging ones with diverse ionization conditions, in soil and on hands. (+) and (−) ionization modes were used after a single-step, low-volume solvent extraction procedure developed using methanol. Tape-lifting, stub, alcohol wipes, cotton bud were compared for collecting the residues from hands of a shooter. Tape-lifting and stub gave the highest recoveries and tape-lifting was chosen. Gradient elution system using ammonium chloride:methanol was developed. Whole procedure lasted approximately 30 min, was validated in both matrices, applied to real samples as post-blast residues, smokeless powder and the hands of a shooter, after shooting. Most of the recoveries were >80% and since all the precisions were <15%, quantitation was possible for all. Limit of Detection (LOD) and Limit of Quantification (LOQ) values were: 0.2–54.1 and 0.3–190.0 ngg−1 in soil, and 0.2–132.3 and 1.1–355.0 ngg−1 in tape-lift.

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“…For the elemental analysis of small samples, scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDS) [13], X-ray fluorescence (XRF) [14,15], laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) [16,17], and laserinduced breakdown spectroscopy (LIBS) [18,19] have been used in forensic science. SEM-EDS simultaneously allows the observation of micro-samples and elemental analysis of the primary components.…”

Section: Introductionmentioning

confidence: 99%

Nondestructive discrimination of red silk single fibers using total reflection X‐ray fluorescence spectrometry and synchrotron radiation X‐ray fluorescence spectrometry

Komatsu

Takahara

Matsuda

et al. 2021

Journal of Forensic Sciences

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In a strangulation case, when a necktie is used as a murder weapon, the dyed silk single fiber becomes an important evidence sample to solve the crime. Dyed silk single fibers contain elements, such as Cr and Co, which are obtained from dyeing using metal mordants. Currently, there are no nondestructive and sufficiently sensitive elementary analytical methods for the forensic analysis of single fibers. Therefore, in this study, eight commercially available red silk samples were collected and used for total reflection X-ray fluorescence (TXRF) and synchrotron radiation X-ray fluorescence (SR-XRF) spectrometry. Benchtop TXRF detected both S in the silk protein and Cl and Ca, which are elements absorbed from the environment by silkworms, but also Cr, which is a dyeing derivative for metal mordants. The presence of Cr and Zn, in addition to the Zn/Cr signal intensity ratios, was reported to be particularly useful identifiers. In SR-XRF, the presence of Cr, Co, Zn, and Br and the Zn/Cr signal intensity ratios were reported to be useful discriminating indicators. In this study, the nondestructive discrimination capabilities of TXRF and SR-XRF measurements for the samples were found to be 85.7% and 100%, respectively. Therefore, we propose a combination of TXRF and SR-XRF as a new nondestructive single fiber identification method for forensic science. Moreover, if partial destruction of a single fiber is allowed, the observation of the cross section and micro-Fourier-transform infrared spectroscopy measurements is useful for identifying red silk fibers.

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Identification and differentiation of commercial and military explosives via high performance liquid chromatography – high resolution mass spectrometry (HPLC-HRMS), X-ray diffractometry (XRD) and X-ray fluorescence spectroscopy (XRF): Towards a forensic substance database on explosives

Cited by 22 publications

References 27 publications

HPLC Method Development for the Fast Separation of a Complex Explosive Mixture

HPLC Method Development for the Fast Separation of a Complex Explosive Mixture

LC-MS/MS monitoring for explosives residues and OGSR with diverse ionization temperatures in soil & hands: 30 minutes for extraction + elution

Nondestructive discrimination of red silk single fibers using total reflection X‐ray fluorescence spectrometry and synchrotron radiation X‐ray fluorescence spectrometry

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