Search results for "010401 analytical chemistry"
showing 10 items of 1284 documents
A multi-analytical approach for the characterization of black crusts on the facade of an historical cathedral
2020
Abstract This study focuses on the characterization of black crusts collected from the Monza cathedral located in the homonymous city (N Italy), a hot spot from the point of view of the atmospheric pollution. Black crusts and substrate marble specimens were analyzed by a multi-analytical approach including X-ray Diffraction (XRD), Fourier Transform-Infrared spectroscopy (FT-IR), Stereomicroscopy (SM), Polarized Light Microscopy (PLM), High Resolution Scanning Electron Microscopy coupled with Energy Dispersive X-ray spectroscopy (HRSEM-EDX) and Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP/MS). The characterization of the carbon fraction (organic carbon, OC, and element…
Reconsidering the accuracy of X-ray fluorescence and ion beam based methods when used to measure the thickness of ancient gildings
2017
Since at least 5000 years ago, gilding techniques have been used for decoration purposes or to make artefacts appear as made of solid gold. Investigation of ancient gildings inevitably requires measuring their thickness, which is usually done either through the observation of cross-sections or by methods such as Rutherford backscattering spectroscopy, particle-induced X-ray emission and X-ray fluorescence. Whereas the former method requires sampling, the latter ones are non-invasive and therefore preferable. These non-invasive methods, however, measure the number of atoms per unit area, which can be converted into thickness only if the density is known. So far this has not been considered a…
Detectability of cannabinoids in the serum samples of cannabis users: Indicators of recent cannabis use? A follow‐up study
2021
Forensic toxicologists are frequently required to predict the time of last cannabis consumption. Several studies suggested the utility of minor cannabinoids as indicators of recent cannabis use. Because several factors influence blood cannabinoid concentrations, the interpretation of serum cannabinoid concentrations remains challenging. To assess the informative value of serum cannabinoid levels in cannabis users (in total N = 117 patients, including 56 patients who stated an exact time of last cannabis use within 24 h before blood sampling), the detectability of cannabinoids, namely delta-9-tetrahydrocannabinol (delta-9-THC), 11-hydroxy-delta-9-THC, 11-nor-9-carboxy-delta-9-THC, cannabichr…
Benefits of solvent concentration pulses in retention time modelling of liquid chromatography
2019
The advantages and disadvantages of the use of isocratic experimental designs including transient increments of organic solvent (i.e., pulses) in the mobile phase(s) of lowest elution strength are explored with modelling purposes. For retained solutes, this type of mixed design offers similar or better predictive capability than gradient designs, shorter measurement time than pure isocratic designs, and retention model parameters that agree with those derived from pure isocratic experiments, with similar uncertainties. The predicted retention times are comparable to those offered by models adjusted from pure isocratic designs, and the solvent waste is appreciably lower. Under a practical st…
Global retention models and their application to the prediction of chromatographic fingerprints
2020
Abstract The resolution of samples containing unknown compounds of different nature, or without standards available, as is the case of chromatographic fingerprints, is still a challenge. Possibly, the most problematic aspect that prevents systematic method development is finding models that describe without bias the retention behaviour of the compounds in the samples. In this work, the use of global models (able to describe the whole sample) is proposed as an alternative to the use of individual models for each solute. Global models contain parameters that are specific for each solute, while other parameters ‒related to the column and solvent‒ are common for all solutes. A special regressio…
Protein dynamics observed by tunable mid-IR quantum cascade lasers across the time range from 10 ns to 1 s
2017
We have developed a spectrometer based on tunable quantum cascade lasers (QCLs) for recording time-resolved absorption spectra of proteins in the mid-infrared range. We illustrate its performance by recording time-resolved difference spectra of bacteriorhodopsin in the carboxylic range (1800–1700 cm− 1) and on the CO rebinding reaction of myoglobin (1960–1840 cm− 1), at a spectral resolution of 1 cm− 1. The spectrometric setup covers the time range from 4 ns to nearly a second with a response time of 10–15 ns. Absorption changes as low as 1 × 10− 4 are detected in single-shot experiments at t > 1 μs, and of 5 × 10− 6 in kinetics obtained after averaging 100 shots. While previous time-res…
Time-Gated Raman Spectroscopy for Quantitative Determination of Solid-State Forms of Fluorescent Pharmaceuticals
2018
Raman spectroscopy is widely used for quantitative pharmaceutical analysis, but a common obstacle to its use is sample fluorescence masking the Raman signal. Time-gating provides an instrument-based method for rejecting fluorescence through temporal resolution of the spectral signal and allows Raman spectra of fluorescent materials to be obtained. An additional practical advantage is that analysis is possible in ambient lighting. This study assesses the efficacy of time-gated Raman spectroscopy for the quantitative measurement of fluorescent pharmaceuticals. Time-gated Raman spectroscopy with a 128 X (2) X 4 CMOS SPAD detector was applied for quantitative analysis of ternary mixtures of sol…
In-situ high spatial resolution LA-MC-ICPMS 230Th/U dating enables detection of small-scale age inversions in speleothems
2017
Abstract We present an in-situ method for Th and U isotope measurements by laser ablation multi-collector inductively coupled plasma mass spectrometry (LA-MC-ICPMS) to determine possible age inversions of stalagmites, using a 213 nm Nd:YAG laser connected to an MC-ICPMS. Due to the low ion beam intensity of 230 Th (20–120 counts per second, cps), we carefully optimized the operating parameters to get highest possible ion beam intensities, i.e., laser fluence (25 J cm −2 ), spot size (110 μm), pulse repetition rate (20 Hz), scan speed (4 μm s −1 ), integration time (1000 s), and He and Ar gas flow (∼0.9 L min −1 and ∼0.6 L min −1 respectively). A precision (2 relative standard error, 2RSE) o…
Evaluation of Mycotoxins in Infant Breast Milk and Infant Food, Reviewing the Literature Data
2021
In this review, an analysis focusing on mycotoxin determination in infant breast milk and infant food has been summarised for the last fifteen years of research focused on the intended population group of 1–9 months. The objective was to know the level of exposure of the child population to an estimated daily intake (EDI) of mycotoxins from the consumption of habitual foods. The EDI was compared with the tolerable daily intake (TDI) established by EFSA to estimate risk. In breast milk, the high prevalence and levels were for samples from Africa (Egypt and Tanzania) with aflatoxin M1 (1.9 μg/L and 10%), and Asia (Iran) with ochratoxin-A (7.3 μg/L and 100%). In infant formulas, high incidence…
Occurrence of mycotoxins in refrigerated pizza dough and risk assessment of exposure for the Spanish population.
2016
Mycotoxins are toxic metabolites produced by filamentous fungi, as Aspergillus, Penicillium and Fusarium. The first objective of this research was to study the presence of mycotoxins in 60 samples of refrigerated pizza dough, by extraction with methanol and determination by liquid chromatography associated with tandem mass spectrometry (LC-MS/MS). Then, the estimated dietary intakes (EDIs) of these mycotoxins, among the Spanish population, was calculated and the health risk assessment was performed, comparing the EDIs data with the tolerable daily intake values (TDIs). The mycotoxins detected in the analyzed samples were aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1), zearale…