Multimodal spectroscopy with chemometrics for the forensic analysis of the inorganic content of Western Australian sandy soils

This study demonstrates a multi-modal analytical sequence suited to the characterisation of sandy soils, which remain an underutilised form of forensic trace evidence. Within the Swan Coastal Plain in Perth, Western Australia, most soils are heavily leached with only small deviations in their mineral compositions. Traditional soil analyses are hence rendered inappropriate for use due to the lack of clay and organic matter. This has led to inorganic methods of analysis predominating, in addition to experimentation with modified techniques. One example is utilisation of the quartz-recovered fine fraction, which is suitable for dry, quartz-dominated sandy soils. In this study, preliminary investigations used the spectroscopic techniques microspectrophotometry, infrared spectroscopy, and x-ray diffraction, to develop a multi-faceted approach for the forensic analysis of the quartz fine fraction of soils. These data were then combined with principal component analysis to demonstrate how chemometrics can assist with objective characterisation and differentiation of sandy soil samples for forensic purposes. Chemometric analysis has not previously been attempted with data obtained from the quartz fine fraction. This methodology is transferable to other jurisdictions where dry, sandy soils predominate.

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Structural Characterization of Gallbladder Stones Using Energy Dispersive X-ray Spectroscopy and X-ray Diffraction

Combinatorial Chemistry & High Throughput Screening ◽

10.2174/1386207321666180913113803 ◽

2018 ◽

Vol 21 (7) ◽

pp. 495-500 ◽

Cited By ~ 1

Author(s):

Hassan A. Almarshad ◽

Sayed M. Badawy ◽

Abdalkarem F. Alsharari

Keyword(s):

Electron Microscopy ◽

Scanning Electron Microscopy ◽

Energy Dispersive ◽

Spectroscopic Techniques ◽

X Ray Diffraction ◽

Major Health Problem ◽

X Ray ◽

Gallbladder Stones ◽

Pure Cholesterol ◽

Scanning Electron

Aim and Objective: Formation of the gallbladder stones is a common disease and a major health problem. The present study aimed to identify the structures of the most common types of gallbladder stones using X-ray spectroscopic techniques, which provide information about the process of stone formation. Material and Method: Phase and elemental compositions of pure cholesterol and mixed gallstones removed from gallbladders of patients were studied using energy-dispersive X-ray spectroscopy combined with scanning electron microscopy analysis and X-ray diffraction. Results: The crystal structures of gallstones which coincide with standard patterns were confirmed by X-ray diffraction. Plate-like cholesterol crystals with laminar shaped and thin layered structures were clearly observed for gallstone of pure cholesterol by scanning electron microscopy; it also revealed different morphologies from mixed cholesterol stones. Elemental analysis of pure cholesterol and mixed gallstones using energy-dispersive X-ray spectroscopy confirmed the different formation processes of the different types of gallstones. Conclusion: The method of fast and reliable X-ray spectroscopic techniques has numerous advantages over the traditional chemical analysis and other analytical techniques. The results also revealed that the X-ray spectroscopy technique is a promising technique that can aid in understanding the pathogenesis of gallstone disease.

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Synthesis and Characterisation of Nickel(II) Diphenylalkenylphosphine Complexes

Journal of Chemical Research ◽

10.1177/174751989902300707 ◽

1999 ◽

Vol 23 (7) ◽

pp. 418-419

Author(s):

Simon J. Coles ◽

Paul Faulds ◽

Michael B. Hursthouse ◽

David G. Kelly ◽

Georgia C. Ranger ◽

...

Keyword(s):

Single Crystal ◽

Spectroscopic Techniques ◽

X Ray Diffraction ◽

X Ray ◽

Phosphine Complexes

Nickel(II) phosphine complexes are prepared with a series of diphenylalkenylphosphine ligands and characterised by single crystal X-ray diffraction and spectroscopic techniques.

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Coumarin-Based Triapine Derivatives and Their Copper(II) Complexes: Synthesis, Cytotoxicity and mR2 RNR Inhibition Activity

Biomolecules ◽

10.3390/biom11060862 ◽

2021 ◽

Vol 11 (6) ◽

pp. 862

Author(s):

Iryna Stepanenko ◽

Maria V Babak ◽

Gabriella Spengler ◽

Marta Hammerstad ◽

Ana Popovic-Bijelic ◽

...

Keyword(s):

Cell Lines ◽

2D Nmr ◽

Multidrug Resistant ◽

Lung Fibroblasts ◽

Spectroscopic Techniques ◽

Tyrosyl Radical ◽

X Ray Diffraction ◽

Healthy Human ◽

12 Steps ◽

Esi Mass Spectrometry

A series of thiosemicarbazone-coumarin hybrids (HL1-HL3 and H2L4) has been synthesised in 12 steps and used for the preparation of mono- and dinuclear copper(II) complexes, namely Cu(HL1)Cl2 (1), Cu(HL2)Cl2 (2), Cu(HL3)Cl2 (3) and Cu2(H2L4)Cl4 (4), isolated in hydrated or solvated forms. Both the organic hybrids and their copper(II) and dicopper(II) complexes were comprehensively characterised by analytical and spectroscopic techniques, i.e., elemental analysis, ESI mass spectrometry, 1D and 2D NMR, IR and UV–vis spectroscopies, cyclic voltammetry (CV) and spectroelectrochemistry (SEC). Re-crystallisation of 1 from methanol afforded single crystals of copper(II) complex with monoanionic ligand Cu(L1)Cl, which could be studied by single crystal X-ray diffraction (SC-XRD). The prepared copper(II) complexes and their metal-free ligands revealed antiproliferative activity against highly resistant cancer cell lines, including triple negative breast cancer cells MDA-MB-231, sensitive COLO-205 and multidrug resistant COLO-320 colorectal adenocarcinoma cell lines, as well as in healthy human lung fibroblasts MRC-5 and compared to those for triapine and doxorubicin. In addition, their ability to reduce the tyrosyl radical in mouse R2 protein of ribonucleotide reductase has been ascertained by EPR spectroscopy and the results were compared with those for triapine.

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Synthesis, Characterization, and Non-Covalent Interactions of Palladium(II)-Amino Acid Complexes

Molecules ◽

10.3390/molecules26144331 ◽

2021 ◽

Vol 26 (14) ◽

pp. 4331

Author(s):

David B. Hobart ◽

Michael A. G. Berg ◽

Hannah M. Rogers ◽

Joseph S. Merola

Keyword(s):

Amino Acid ◽

High Resolution Mass Spectrometry ◽

Resonance Spectroscopy ◽

Spectroscopic Techniques ◽

X Ray Diffraction ◽

Amino Acid Complexes ◽

Acetone Water ◽

Square Planar ◽

Non Covalent Interactions ◽

Covalent Interactions

The reaction of palladium(II) acetate with acyclic amino acids in acetone/water yields square planar bis-chelated palladium amino acid complexes that exhibit interesting non-covalent interactions. In all cases, complexes were examined by multiple spectroscopic techniques, especially HRMS (high resolution mass spectrometry), IR (infrared spectroscopy), and 1H NMR (nuclear magnetic resonance) spectroscopy. In some cases, suitable crystals for single crystal X-ray diffraction were able to be grown and the molecular structure was obtained. The molecular geometries of the products are discussed. Except for the alanine complex, all complexes incorporate water molecules into the extended lattice and exhibit N-H···O and/or O···(HOH)···O hydrogen bonding interactions. The non-covalent interactions are discussed in terms of the extended lattice structures exhibited by the structures.

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UV-Accelerated Photocatalytic Degradation of Pesticide over Magnetite and Cobalt Ferrite Decorated Graphene Oxide Composite

Plants ◽

10.3390/plants10010006 ◽

2020 ◽

Vol 10 (1) ◽

pp. 6

Author(s):

Asma Tabasum ◽

Mousa Alghuthaymi ◽

Umair Yaqub Qazi ◽

Imran Shahid ◽

Qamar Abbas ◽

...

Keyword(s):

Spectroscopic Techniques ◽

Combined Effects ◽

X Ray Diffraction ◽

Contributing Factors ◽

Reaction Conditions ◽

X Ray ◽

Oxidant Concentration ◽

Optimized Conditions ◽

High Degradation Rate ◽

Considerable Loss

Pesticides are one of the main organic pollutants as they are highly toxic and extensively used worldwide. The reclamation of wastewater containing pesticides is of utmost importance. For this purpose, GO-doped metal ferrites (GO-Fe3O4 and GO-CoFe2O4) were prepared and characterized using scanning electron microscopy, X-ray diffraction and Fourier transform infrared spectroscopic techniques. Photocatalytic potentials of catalysts were investigated against acetamiprid’s degradation. A detailed review of the parametric study revealed that efficiency of overall Fenton’s process relies on the combined effects of contributing factors, i.e., pH, initial oxidant concentration, catalyst dose, contact time, and acetamiprid load. ~97 and ~90% degradation of the acetamiprid was achieved by GO-CoFe2O4 and GO-Fe3O4, respectively during the first hour under UV radiations at optimized reaction conditions. At optimized conditions (i.e., pH:3, [H2O2]: 14.5 mM (for Fe3O4, GO-Fe3O4, and GO-CoFe2O4) and 21.75 mM (for CoFe2O4), catalysts: 100 mgL−1, time: 60min) the catalysts exhibited excellent performance, with high degradation rate, magnetic power, easy recovery at the end, and efficient reusability (up to 5 cycles without any considerable loss in catalytic activity). A high magnetic character offers its easy separation from aqueous systems using an external magnet. Moreover, the combined effects of experimental variables were assessed simultaneously and justified using response surface methodology (RSM).

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Diorganotin(iv) benzyldithiocarbamate complexes: synthesis, characterization, and thermal and cytotoxicity study

Open Chemistry ◽

10.1515/chem-2020-0037 ◽

2020 ◽

Vol 18 (1) ◽

pp. 453-462

Author(s):

Jerry O. Adeyemi ◽

Damian C. Onwudiwe ◽

Nirasha Nundkumar ◽

Moganavelli Singh

Keyword(s):

Cell Lines ◽

Human Tumor ◽

Complexation Reaction ◽

Spectroscopic Techniques ◽

X Ray Diffraction ◽

Human Tumor Cell Lines ◽

H Nmr ◽

Cytotoxicity Studies ◽

Final Residue ◽

Mcf 7

AbstractAmmonium benzyldithiocarbamate, represented as NH4L, was prepared and used in the complexation reaction involving three organotin(iv) salts, represented as R2SnCl2 (R = CH3, C4H9, and C6H5). The structures of the synthesized complexes [(CH3)2SnL2] (1), [(C4H9)2SnL2] (2), and [(C6H5)2SnL2] (3) were established using various spectroscopic techniques (Fourier transform infrared spectroscopy, 1H NMR, 13C NMR, and 119Sn NMR) and elemental analysis. Thermal decomposition of the complexes using thermogravimetric analysis under nitrogen showed no definite pathway in the pattern of the complexes even though they are structurally related. X-ray diffraction studies of the final residue showed a common diffraction pattern for the complexes and confirmed SnS as the product of the thermal treatment. Cytotoxicity studies of these complexes against the human tumor cell lines (HeLa and MCF-7) compared favorably with the used standard 5-fluorouracil drug, with complexes 2 and 3 showing very good activity toward the used cell lines.

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Ultrasonic Shaking of Glauconite Pellets with Diverse Reagents for a Comparison of Their K–Ar with Already Published Rb–Sr Results

Geosciences ◽

10.3390/geosciences11110439 ◽

2021 ◽

Vol 11 (11) ◽

pp. 439

Author(s):

Norbert Clauer ◽

Edward Keppens ◽

I. Tonguç Uysal ◽

Amélie Aubert

Keyword(s):

Clay Material ◽

Similar Data ◽

X Ray Diffraction ◽

Metallic Trace Elements ◽

Three Samples ◽

Isotopic Studies ◽

Mineral Assemblages ◽

Preparation Step ◽

Mineral Compositions ◽

Sr Method

A combined ultrasonic treatment, with de-ionized H2O, dilute HAc or dilute HCl, of three Mid-Miocene glauconite samples was applied to K–Ar date the different separates in order to compare the results with those obtained by the Rb–Sr method using the same three samples and that were analyzed strictly in the same way. Two aliquots yield opposite elemental and K–Ar trends, which suggests different initial mineral compositions for the various pellets. The K–Ar data of two untreated and leached L7 and L8 aliquots are almost within analytical uncertainty from 17.3 ± 0.6 Ma to 19.6 ± 0.7 Ma (2σ), while those of the third L10 sample are slightly higher at 22.1 ± 1.2 Ma (2σ). Comparatively, the earlier published Rb–Sr ages of the three untreated samples and of the leached aliquots gave similar data for the L7 aliquots by an isochron at 18.1 ± 3.1 (2σ) Ma and for the sample L8 by an isochron with an age of 19.6 ± 1.8 (2σ) Ma, while the untreated L10 aliquot yields a very high Rb–Sr date of 42.1 ± 1.6 (2σ) Ma. This untreated L10 glauconite fraction contains blödite, a Sr-rich carbonate that impacted the two isotopic systems differently. Generally, dilute HCl or HAc acids dissolve carbonates, sulfates, sulfites and oxides, while they do not affect the clay-type crystals such as glauconites. These soluble minerals can be identified indirectly, as here, by X-ray diffraction and the amounts of leached Na2O, CaO and Fe2O3 contents. Together with the leaching of some metallic trace elements, those of NaO confirm the leaching of metals and of blödite that are both hosted by the glauconite pellets. The occurrence of this Sr-enriched mineral explains the age differences of the non-treated aliquots and suggests a systematic leaching of any glauconite separate before isotope determination and, possibly, a comparison of the Rb–Sr and K–Ar results. Ultrasonic shaking appears appropriate for physical disaggregation of any contaminating grains that may remain hosted within the pellets, even after a preliminary H2O wash, which may dissolve and remove the soluble minerals but not the H2O-insoluble silicates. The K–Ar study completed here as a complement to a previous Rb–Sr study highlights, again, the importance of the preparation step in isotopic studies of glauconite-type and, by extension, of any clay material, as all occurring minerals can interfere in the final age determinations and, therefore, differently in the mineral assemblages. All those not in isotopic equilibrium need to be removed before analysis, including the soluble Sr or alkali-enriched ones.

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Forensic analysis on printer inks via chemometrics

IOP Conference Series Materials Science and Engineering ◽

10.1088/1757-899x/1192/1/012029 ◽

2021 ◽

Vol 1192 (1) ◽

pp. 012029

Author(s):

L H Mohd Zawawi ◽

N F Mohamed Azmin ◽

M F Abd. Wahab ◽

S I Ibrahim ◽

M Y Mohd Yunus

Keyword(s):

Principal Component Analysis ◽

Digital Media ◽

Graphical Representation ◽

Rapid Development ◽

Principal Component ◽

Component Analysis ◽

Forensic Analysis ◽

Criminal Cases ◽

Trial Court ◽

Wide Range

Abstract Printer inks are becoming necessary for utilization for wide range of purposes by society in current times with rapid development in technology and digital media area. Thus, forgery and counterfeiting becoming easier for the criminals. It is dangerous as some criminals will misused the technology by mean of addition and adulteration of parts of text or numbers on document as the inks and document can be made as an evidence in the trial court. Thus, the characterization and differentiation of the printed inks in the suspected documents (civil or criminal cases) may provide important information about the authenticity of the printer inks. The focus of this study to differentiate the chemical component of three different types of sample inks by incorporation of FTIR spectrophotometer with principal component analysis. The unique features of the ink samples were unmasked from the score plots of the principal component analysis. Thus, the graphical representation provided by the FTIR spectra with principal component analysis enabled the discrimination certain chemical in the printer inks.

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Synthesis, Structural and Optical Investigations of (Pb, Bi)TiO3 Borosilicate Glasses

Physics Research International ◽

10.1155/2014/606709 ◽

2014 ◽

Vol 2014 ◽

pp. 1-7 ◽

Cited By ~ 6

Author(s):

Chandkiram Gautam

Keyword(s):

Spectroscopic Techniques ◽

Borosilicate Glasses ◽

X Ray Diffraction ◽

Raman Spectroscopic ◽

Spectral Bands ◽

Prepared Glass ◽

Infrared And Raman Spectroscopy ◽

Uv Visible ◽

Diffraction Patterns ◽

Spectral Patterns

A new series of lead bismuth titanate borosilicate glasses with addition of one percent lanthanum oxide have been synthesized using melt-quench technique. X-ray diffraction patterns have been recorded to confirm the amorphous nature of the prepared glass samples. The synthesized glasses have been characterized by using various spectroscopic techniques such as UV-visible, infrared, and Raman spectroscopy. UV-visible measurements were recorded in the wavelength range from 200 to 1100 nm whereas IR and Raman spectroscopic measurements were recorded over a continuous wavenumber range from 400 to 5000 cm−1 and 1000 to 2000 cm−1 respectively. The different absorption peaks/bands were formed in IR spectral patterns. The spectral bands appear towards the lower wavenumber sides due to the Bi and Pb, content while the bands appear towards the higher wavenumber sides due to the formation of diborate and triborate network units.

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Hydrolysis of Methionine- and Histidine-Containing Peptides Promoted by Dinuclear Platinum(II) Complexes with Benzodiazines as Bridging Ligands: Influence of Ligand Structure on the Catalytic Ability of Platinum(II) Complexes

Bioinorganic Chemistry and Applications ◽

10.1155/2018/3294948 ◽

2018 ◽

Vol 2018 ◽

pp. 1-12 ◽

Cited By ~ 2

Author(s):

Snežana Rajković ◽

Beata Warżajtis ◽

Marija D. Živković ◽

Biljana Đ. Glišić ◽

Urszula Rychlewska ◽

...

Keyword(s):

Catalytic Activity ◽

Amide Bond ◽

Spectroscopic Techniques ◽

X Ray Diffraction ◽

Bridging Ligands ◽

Metal Centers ◽

H Nmr ◽

Dinuclear Platinum ◽

Ph Range ◽

Hydrolysis Of

Dinuclear platinum(II) complexes, [{Pt(en)Cl}2(μ-qx)]Cl2·2H2O (1), [{Pt(en)Cl}2(μ-qz)](ClO4)2(2), and [{Pt(en)Cl}2(μ-phtz)]Cl2·4H2O (3), were synthesized and characterized by different spectroscopic techniques. The crystal structure of1was determined by single-crystal X-ray diffraction analysis, while the DFT M06-2X method was applied in order to optimize the structures of1–3. The chlorido Pt(II) complexes1–3were converted into the corresponding aqua species1a–3a, and their reactions with an equimolar amount of Ac–L–Met–Gly and Ac–L–His–Gly dipeptides were studied by1H NMR spectroscopy in the pH range 2.0 < pH < 2.5 at 37°C. It was found that, in all investigated reactions with the Ac–L–Met–Gly dipeptide, the cleavage of the Met–Gly amide bond had occurred, but complexes2aand3ashowed lower catalytic activity than1a. However, in the reactions with Ac–L–His–Gly dipeptide, the hydrolysis of the amide bond involving the carboxylic group of histidine was observed only with complex1a. The observed disparity in the catalytic activity of these complexes is thought to be due to different relative positioning of nitrogen atoms in the bridging qx, qz, and phtz ligands and consequent variation in the intramolecular separation of the two platinum(II) metal centers.

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