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Volume 5, September
 
 

Separations, Volume 5, Issue 4 (December 2018) – 13 articles

Cover Story (view full-size image): Forensic fire debris analysis presents data interpretation challenges due to the partial evaporation of ignitable liquids (IL) and highly varied contributions by compounds originating from the thermal breakdown of building materials and furnishings (SUB). Current data interpretation methods rely on visual chromatographic pattern recognition. Unsupervised machine learning techniques can assist fire debris analysts in identifying groups of IL and SUB with similar chromatographic or mass spectral patterns. This report details the use of a Kohonen self-organizing map (SOM) coupled with extracted ion mass spectra to organize IL and SUB pyrolysis samples on a two-dimensional grid. Groupings corresponding to the ASTM E1618-defined IL classes and SUB pyrolysis are observed. The SOM component planes give important information regarding the ions that contribute to the different groups. View this paper.
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9 pages, 2093 KiB  
Article
Effect of Physical and Chemical Activation on Arsenic Sorption Separation by Grape Seeds-Derived Biochar
by Vladimír Frišták, Eduardo Moreno-Jimenéz, Teresa Fresno and Elena Diaz
Separations 2018, 5(4), 59; https://doi.org/10.3390/separations5040059 - 19 Dec 2018
Cited by 12 | Viewed by 3260
Abstract
The utilization of carbon-rich pyrolysis materials in the separation processes of metalloids plays a crucial role in analytes pre-concentration techniques and opens a burning issue in new sorbents development. This study characterized the effect of physical and chemical activation with subsequent iron impregnation [...] Read more.
The utilization of carbon-rich pyrolysis materials in the separation processes of metalloids plays a crucial role in analytes pre-concentration techniques and opens a burning issue in new sorbents development. This study characterized the effect of physical and chemical activation with subsequent iron impregnation of grape seed-derived biochar on sorption removal of As from model aqueous solutions. Sorbents that were produced in slow pyrolysis process at 600 °C were characterized by SEM, elemental, and specific surface area analysis. Sorption separation of As by the studied materials was characterized as on contact time and an initial concentration dependent process reaching sorption equilibrium in 1440 min. Air activated biochar (A1GSBC) showed about 7.7 times and HNO3 activated biochar (A2GSBC) about 6.8 times higher values of Qmax as compared to control (GSBC). A1GSBC and A2GSBC can be easily and effectively regenerated by alkali agent in several cycles. All of these results showed the practical use of the activation process to produce effective sorption materials with increased surface area and improved sorption potential for anionic forms separation from liquid wastes. Full article
(This article belongs to the Special Issue Sorption Separation)
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18 pages, 3520 KiB  
Article
Modern Instrumental Limits of Identification of Ignitable Liquids in Forensic Fire Debris Analysis
by Robin J. Abel, Grzegorz Zadora, P. Mark L. Sandercock and James J. Harynuk
Separations 2018, 5(4), 58; https://doi.org/10.3390/separations5040058 - 10 Dec 2018
Cited by 7 | Viewed by 6000
Abstract
Forensic fire debris analysis is an important part of fire investigation, and gas chromatography–mass spectrometry (GC-MS) is the accepted standard for detection of ignitable liquids in fire debris. While GC-MS is the dominant technique, comprehensive two-dimensional gas chromatography–mass spectrometry (GC×GC-MS) is gaining popularity. [...] Read more.
Forensic fire debris analysis is an important part of fire investigation, and gas chromatography–mass spectrometry (GC-MS) is the accepted standard for detection of ignitable liquids in fire debris. While GC-MS is the dominant technique, comprehensive two-dimensional gas chromatography–mass spectrometry (GC×GC-MS) is gaining popularity. Despite the broad use of these techniques, their sensitivities are poorly characterized for petroleum-based ignitable liquids. Accordingly, we explored the limit of identification (LOI) using the protocols currently applied in accredited forensic labs for two 75% evaporated gasolines and a 25% evaporated diesel as both neat samples and in the presence of interfering pyrolysate typical of fire debris. GC-MSD (mass selective detector (MS)), GC-TOF (time-of-flight (MS)), and GC×GC-TOF were evaluated under matched conditions to determine the volume of ignitable liquid required on-column for correct identification by three experienced forensic examiners performing chromatographic interpretation in accordance with ASTM E1618-14. GC-MSD provided LOIs of ~0.6 pL on-column for both neat gasolines, and ~12.5 pL on-column for neat diesel. In the presence of pyrolysate, the gasoline LOIs increased to ~6.2 pL on-column, while diesel could not be correctly identified at the concentrations tested. For the neat dilutions, GC-TOF generally provided 2× better sensitivity over GC-MSD, while GC×GC-TOF generally resulted in 10× better sensitivity over GC-MSD. In the presence of pyrolysate, GC-TOF was generally equivalent to GC-MSD, while GC×GC-TOF continued to show 10× greater sensitivity relative to GC-MSD. Our findings demonstrate the superior sensitivity of GC×GC-TOF and provide an important approach for interlaboratory benchmarking of modern instrumental performance in fire debris analysis. Full article
(This article belongs to the Special Issue Advances in Fire Debris Analysis)
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22 pages, 3628 KiB  
Article
Chemometric Characterization of Synthetic Dye Sorption onto Slovakian River Sediments: A Laboratory Batch Experiment
by Anna Koprdová, Miroslava Bachratá, Vanda Adamcová, Martin Valica, Martin Pipíška and Miroslav Horník
Separations 2018, 5(4), 57; https://doi.org/10.3390/separations5040057 - 4 Dec 2018
Cited by 2 | Viewed by 2606
Abstract
The aim of the work was to characterize the sorption of cationic dyes thioflavine T (ThT) and methylene blue (MB) onto selected Slovakian river sediments using chemometric approaches including principal component analysis (PCA) and cluster analysis (CA). Also, the potential of mentioned multivariate [...] Read more.
The aim of the work was to characterize the sorption of cationic dyes thioflavine T (ThT) and methylene blue (MB) onto selected Slovakian river sediments using chemometric approaches including principal component analysis (PCA) and cluster analysis (CA). Also, the potential of mentioned multivariate analyses for comparison of studied objects (river sediments or river and model waters) as well as in finding relationships between the variables describing the physico-chemical characteristics of studied matrices or waters and sorption/desorption characteristics of matrices for dyes binding under laboratory conditions was evaluated. Parameters describing the physico-chemical characteristics of sediments include: pH, pHzpc, or cation-exchange capacity; and in the case of waters: pH, conductivity, water hardness, content of dissolved solids or presence of organic compounds. From the comparison of dye sorption onto sediments, it was found that sorption of thiazine dye MB was minimally 1.5-times higher than sorption of benzothiazole dye ThT. Sorption capacities Qs reached the maximum values in the case of sediments originated from Dudvah River (MB-Qs = 8.70 ± 0.42 mg g−1; ThT-Qs = 5.03 ± 0.28 mg g−1; ±SD). Obtained results showed that applied methods of multivariate analyses represent a suitable tool for evaluation of sorption/desorption processes of organic xenobiotics binding in sediments. Full article
(This article belongs to the Special Issue Sorption Separation)
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25 pages, 3416 KiB  
Article
Challenges in Determining the Size Distribution of Nanoparticles in Consumer Products by Asymmetric Flow Field-Flow Fractionation Coupled to Inductively Coupled Plasma-Mass Spectrometry: The Example of Al2O3, TiO2, and SiO2 Nanoparticles in Toothpaste
by Manuel Correia, Toni Uusimäki, Allan Philippe and Katrin Loeschner
Separations 2018, 5(4), 56; https://doi.org/10.3390/separations5040056 - 27 Nov 2018
Cited by 16 | Viewed by 4573
Abstract
According to the current European regulation on cosmetics, any ingredient present as a nanomaterial should be indicated in the ingredient list. There is a need for analytical methods capable of determining the size of the relevant ingredients and thus assessing if these are [...] Read more.
According to the current European regulation on cosmetics, any ingredient present as a nanomaterial should be indicated in the ingredient list. There is a need for analytical methods capable of determining the size of the relevant ingredients and thus assessing if these are nanomaterials or not. An analytical method based on asymmetric flow field-flow fractionation (AF4) and inductively coupled plasma-mass spectrometry (ICP-MS) was developed to determine the size of particles present in a commercial toothpaste. Multi-angle light scattering (MALS) was used for on-line size determination. The number-based particle size distributions (PSDs) of the particles were retrieved upon mathematical conversion of the mass-based PSDs recovered from the AF4-ICP-MS fractograms. AF4-ICP-MS allowed to separate and detect Al2O3 and TiO2 particles in the toothpaste and to retrieve a correct TiO2 number-based PSD. The potential presence of particles in the lower size range of the Al2O3 mass-based PSD had a strong impact on sizing and nanomaterial classification upon conversion. AF4 coupled with ICP-MS and MALS was found to be a powerful approach for characterization of different particles in a multiple-particle system such as toothpaste. Confirmation of particle size by a secondary method such as single particle ICP-MS or hydrodynamic chromatography was crucial. Full article
(This article belongs to the Special Issue Analytic Techniques for Nano- and Microparticles Analysis)
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9 pages, 3230 KiB  
Article
A Low-Cost Approach Using Diatomaceous Earth Biosorbent as Alternative SPME Coating for the Determination of PAHs in Water Samples by GC-MS
by Naysla Paulo Reinert, Camila M. S. Vieira, Cristian Berto Da Silveira, Dilma Budziak and Eduardo Carasek
Separations 2018, 5(4), 55; https://doi.org/10.3390/separations5040055 - 20 Nov 2018
Cited by 10 | Viewed by 3555
Abstract
In this study, the use of recycled diatomaceous earth as the extraction phase in solid phase microextraction (SPME) technique for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples, with separation/detection performed by gas chromatography-mass spectrometry (GC-MS), is proposed. The optimized [...] Read more.
In this study, the use of recycled diatomaceous earth as the extraction phase in solid phase microextraction (SPME) technique for the determination of polycyclic aromatic hydrocarbons (PAHs) in river water samples, with separation/detection performed by gas chromatography-mass spectrometry (GC-MS), is proposed. The optimized extraction conditions are extraction time 70 min at 80 °C with no addition of salt. The limits of quantification were close to 0.5 μg L−1 with RSD values lower than 25% (n = 3). The linear working range was 0.5 μg L−1 to 25 μg L−1 for all analytes. The method was applied to samples collected from the Itajaí River (Santa Catarina, Brazil) and the RSD values for repeatability and reproducibility were lower than 15% and 17%, respectively. The efficiency of the recycled diatomaceous earth fiber was compared with that of commercial fibers and good results were obtained, confirming that this is a promising option to use as the extraction phase in SPME. Full article
(This article belongs to the Special Issue Five Years of Separations: Feature Paper 2018)
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14 pages, 482 KiB  
Review
Biosorption and Bioaccumulation Abilities of Actinomycetes/Streptomycetes Isolated from Metal Contaminated Sites
by Ivana Timková, Jana Sedláková-Kaduková and Peter Pristaš
Separations 2018, 5(4), 54; https://doi.org/10.3390/separations5040054 - 12 Nov 2018
Cited by 98 | Viewed by 8521
Abstract
Heavy metal pollution is of great concern. Due to expansion of industrial activities, a large amount of metal is released into the environment, disturbing its fragile balance. Conventional methods of remediation of heavy metal-polluted soil and water are expensive and inefficient. Therefore, new [...] Read more.
Heavy metal pollution is of great concern. Due to expansion of industrial activities, a large amount of metal is released into the environment, disturbing its fragile balance. Conventional methods of remediation of heavy metal-polluted soil and water are expensive and inefficient. Therefore, new techniques are needed to provide environmentally friendly and highly selective remediation. Streptomycetes, with their unique growth characteristics, ability to form spores and mycelia, and relatively rapid colonization of substrates, act as suitable agents for bioremediation of metals and organic compounds in polluted soil and water. A variety of mechanisms could be involved in reduction of metals in the environment, e.g., sorption to exopolymers, precipitation, biosorption and bioaccumulation. Studies performed on biosorption and bioaccumulation potential of streptomycetes could be used as a basis for further development in this field. Streptomycetes are of interest because of their ability to survive in environments contaminated by metals through the production of a wide range of metal ion chelators, such as siderophores, which provide protection from the negative effects of heavy metals or specific uptake for specialized metabolic processes. Many strains also have the equally important characteristic of resistance to high concentrations of heavy metals. Full article
(This article belongs to the Special Issue Sorption Separation)
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13 pages, 1825 KiB  
Article
Evaluation of Lipases from Wild Microbial Strains as Biocatalysts in Biodiesel Production
by Carlos Luna, Diego Luna, Felipa M. Bautista, Juan Calero, Antonio A. Romero, Alejandro Posadillo, Enrique D. Sancho and Rafael Estevez
Separations 2018, 5(4), 53; https://doi.org/10.3390/separations5040053 - 5 Nov 2018
Cited by 3 | Viewed by 2971
Abstract
In this study, the evaluation of the catalytic behavior of several wild bacterial strains in the 1,3-selective ethanolysis of triglycerides with ethanol to produce a new type of biodiesel (Ecodiesel) that integrates glycerol as monoacylglycerols was carried out. The Ecodiesel production not only [...] Read more.
In this study, the evaluation of the catalytic behavior of several wild bacterial strains in the 1,3-selective ethanolysis of triglycerides with ethanol to produce a new type of biodiesel (Ecodiesel) that integrates glycerol as monoacylglycerols was carried out. The Ecodiesel production not only avoids the elimination of glycerol, which is largely generated as a by-product in the biodiesel industry, but also results in an increase in the biofuel yield. The wild microbial strain samples were obtained from several lipophilic organisms. In addition to evaluate the enzymatic extracts, the minimum grade of purification of the strains, necessary to obtain similar results to those attained with commercial lipases was studied. This purification treatment included a dialysis followed by a lyophilization process. Such extracts were directly used as biocatalysts in the transesterification reaction of sunflower oil with ethanol, attaining much better results (yield close to 100%) than those obtained with strains which were not submitted to the purification process (yields lower than 10%). Furthermore, the results here obtained are similar to those obtained with commercial lipases but were achieved under mild conditions and lower reaction time (2 h). In addition, the stability of the enzymatic extracts was corroborated by subsequent reactions, showing no loss of activity. Thus, this study brings to light that enzymatic extracts obtained by a very simple purification process can be economically competitive with the conventional biodiesel production methods. Full article
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9 pages, 2809 KiB  
Article
Application of Self-Organizing Maps to the Analysis of Ignitable Liquid and Substrate Pyrolysis Samples
by Nicholas Thurn, Mary R. Williams and Michael E. Sigman
Separations 2018, 5(4), 52; https://doi.org/10.3390/separations5040052 - 31 Oct 2018
Cited by 7 | Viewed by 3692
Abstract
Classification of un-weathered ignitable liquids is a problem that is currently addressed by visual pattern recognition under the guidelines of Standard Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography-Mass Spectrometry, ASTM E1618-14. This standard method does [...] Read more.
Classification of un-weathered ignitable liquids is a problem that is currently addressed by visual pattern recognition under the guidelines of Standard Test Method for Ignitable Liquid Residues in Extracts from Fire Debris Samples by Gas Chromatography-Mass Spectrometry, ASTM E1618-14. This standard method does not separately address the identification of substrate pyrolysis patterns. This report details the use of a Kohonen self-organizing map coupled with extracted ion spectra to organize ignitable liquids and substrate pyrolysis samples on a two-dimensional map with groupings that correspond to the ASTM-classifications and separate the substrate pyrolysis samples from the ignitable liquids. The component planes give important information regarding the ions from the extracted ion spectra that contribute to the different classes. Some additional insight is gained into grouping of substrate pyrolysis samples based on the nature of the unburned material as a wood or non-wood material. Further subclassification was not apparent from the self-organizing maps (SOM) results. Full article
(This article belongs to the Special Issue Advances in Fire Debris Analysis)
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6 pages, 408 KiB  
Article
Investigation of Hg Content by a Rapid Analytical Technique in Mediterranean Pelagic Fishes
by Giuseppa Di Bella, Roberta Tardugno and Nicola Cicero
Separations 2018, 5(4), 51; https://doi.org/10.3390/separations5040051 - 24 Oct 2018
Cited by 10 | Viewed by 4367
Abstract
Mercury (Hg) fish and seafood contamination is a global concern and needs worldwide sea investigations in order to protect consumers. The aim of this study was to investigate the Hg concentration by means of a rapid and simple analytical technique with a direct [...] Read more.
Mercury (Hg) fish and seafood contamination is a global concern and needs worldwide sea investigations in order to protect consumers. The aim of this study was to investigate the Hg concentration by means of a rapid and simple analytical technique with a direct Mercury Analyzer (DMA-80) in pelagic fish species, Tetrapturus belone (spearfish), Thunnus thynnus (tuna) and Xiphias gladius (swordfish) caught in the Mediterranean Sea. Hg contents were evaluated also in Salmo salar (salmon) as pelagic fish not belonging to the Mediterranean area. The results obtained were variable, ranging between 0.015–2.562 mg kg−1 for T. thynnus species, 0.477–3.182 mg kg−1 for X. gladius, 0.434–1.730 mg kg−1 for T. belone and 0.004–0.019 mg kg−1 for S. salar, respectively. The total Hg tolerable weekly intake (TWI) and tolerable weekly intake % (TWI%) values according to the European Food Safety Authority (EFSA) were calculated. The results highlighted that the pelagic species caught in the Mediterranean Sea should be constantly monitored due to their high Hg contents as well as their TWI and TWI% with respect to S. salar samples. Full article
(This article belongs to the Special Issue Analytical Tools for Food Analysis)
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16 pages, 3913 KiB  
Article
Characterization of the Natural Colloidal TiO2 Background in Soil
by Allan Philippe, Daniel Armando Campos, Jean-Michel Guigner, Christian Buchmann, Dörte Diehl and Gabriele E. Schaumann
Separations 2018, 5(4), 50; https://doi.org/10.3390/separations5040050 - 20 Oct 2018
Cited by 20 | Viewed by 4964
Abstract
An increasing amount of TiO2 engineered nanoparticles (TNP) is released into soils and sediments, increasing the need for dedicated detection methods. Titanium is naturally present in soils at concentrations typically much higher than the estimated concentrations for TNP. Therefore, a precise knowledge [...] Read more.
An increasing amount of TiO2 engineered nanoparticles (TNP) is released into soils and sediments, increasing the need for dedicated detection methods. Titanium is naturally present in soils at concentrations typically much higher than the estimated concentrations for TNP. Therefore, a precise knowledge of this natural background, including the colloidal fraction, is required for developing adapted strategies for detecting TNP. In this study, we characterized the natural colloidal Ti-background by analyzing eight soils with different properties and origins. A combination of X-ray fluorescence analysis and ICP-OES was used for determining the silicate bound fraction, which was a minor fraction for all soils (0–32%). The colloidal fraction obtained by extracting colloids from soil prior to ICP-OES measurements ranged between 0.3% and 7%. Electron microscopy and hydrodynamic chromatography confirmed that Ti in the form of colloids or larger particles was mostly present as TiO2 minerals with a fraction smaller than 100 nm. The size distribution mode of the extracted colloids determined using hydrodynamic chromatography ranged between 80 and 120 nm. The chromatograms suggested a broad size distribution with a significant portion below 100 nm. In addition to these data, we also discuss possible implications of our findings for the method development for detecting TNP in soils. Full article
(This article belongs to the Special Issue Analytic Techniques for Nano- and Microparticles Analysis)
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13 pages, 646 KiB  
Article
Estimating Detection Limits in Chromatography from Calibration Data: Ordinary Least Squares Regression vs. Weighted Least Squares
by Juan M. Sanchez
Separations 2018, 5(4), 49; https://doi.org/10.3390/separations5040049 - 8 Oct 2018
Cited by 16 | Viewed by 6867
Abstract
It is necessary to determine the limit of detection when validating any analytical method. For methods with a linear response, a simple and low labor-consuming procedure is to use the linear regression parameters obtained in the calibration to estimate the blank standard deviation [...] Read more.
It is necessary to determine the limit of detection when validating any analytical method. For methods with a linear response, a simple and low labor-consuming procedure is to use the linear regression parameters obtained in the calibration to estimate the blank standard deviation from the residual standard deviation (sres), or the intercept standard deviation (sb0). In this study, multiple experimental calibrations are evaluated, applying both ordinary and weighted least squares. Moreover, the analyses of replicated blank matrices, spiked at 2–5 times the lowest calculated limit values with the two regression methods, are performed to obtain the standard deviation of the blank. The limits of detection obtained with ordinary least squares, weighted least squares, the signal-to-noise ratio, and replicate blank measurements are then compared. Ordinary least squares, which is the simplest and most commonly applied calibration regression methodology, always overestimate the values of the standard deviations at the lower levels of calibration ranges. As a result, the detection limits are up to one order of magnitude greater than those obtained with the other approaches studied, which all gave similar limits. Full article
(This article belongs to the Special Issue Chromatography and Chemometrics)
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8 pages, 1571 KiB  
Article
Monolithic Silica Capillary Columns with Improved Retention and Selectivity for Amino Acids
by Dana Moravcová and Josef Planeta
Separations 2018, 5(4), 48; https://doi.org/10.3390/separations5040048 - 2 Oct 2018
Cited by 4 | Viewed by 3097
Abstract
A strategy for the preparation of silica-based monolithic capillary columns (150 × 0.1 mm) with high selectivity to amino acids is presented. The zwitterionic columns were prepared by coating the silica monolith with [2-(methacryloyloxy)ethyl]-dimethyl-(3-sulfopropyl)-ammonium hydroxide via 3-(trimethoxysilyl)propyl methacrylate. The columns were evaluated under [...] Read more.
A strategy for the preparation of silica-based monolithic capillary columns (150 × 0.1 mm) with high selectivity to amino acids is presented. The zwitterionic columns were prepared by coating the silica monolith with [2-(methacryloyloxy)ethyl]-dimethyl-(3-sulfopropyl)-ammonium hydroxide via 3-(trimethoxysilyl)propyl methacrylate. The columns were evaluated under isocratic conditions in hydrophilic interaction liquid chromatography. The best separation of amino acids was obtained on the monolithic column prepared by a stepwise modification procedure where the modification step was repeated four times. The mixture of fifteen amino acids was separated within 13 min using the mobile phase consisting of 75% acetonitrile and 25% 5 mmol/L ammonium acetate at pH 4.5. Full article
(This article belongs to the Special Issue Advances in Capillary Liquid Chromatography)
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19 pages, 3949 KiB  
Article
Fixed- and Variable-Temperature Kinetic Models to Predict Evaporation of Petroleum Distillates for Fire Debris Applications
by John W. McIlroy, Ruth Waddell Smith and Victoria L. McGuffin
Separations 2018, 5(4), 47; https://doi.org/10.3390/separations5040047 - 25 Sep 2018
Cited by 11 | Viewed by 3744
Abstract
Forensic fire debris analysis focuses on the identification of a foreign ignitable liquid in debris collected from the scene of a suspected intentional fire. Chromatograms of the extracted debris are compared to a suitable reference collection containing chromatograms of unevaporated and evaporated ignitable [...] Read more.
Forensic fire debris analysis focuses on the identification of a foreign ignitable liquid in debris collected from the scene of a suspected intentional fire. Chromatograms of the extracted debris are compared to a suitable reference collection containing chromatograms of unevaporated and evaporated ignitable liquids. However, there is no standardized method for the evaporation of ignitable liquids and the process itself can be time consuming, which limits the number of chromatograms of evaporated liquids included in the reference collection. This work describes the development and application of a variable-temperature kinetic model to predict evaporation rate constants and mathematically predict chromatograms corresponding to evaporated ignitable liquids. First-order evaporation rate constants were calculated for 78 selected compounds in diesel, which were used to develop predictive models of evaporation rates. Fixed-temperature models were developed to predict the rate constants at five temperatures (5, 10, 20, 30, 35 °C), yielding a mean absolute percent error (MAPE) of 10.0%. The variable-temperature model was then created from these data by multiple linear regression, yielding a MAPE of 16.4%. The model was applied to generate a reference collection of predicted chromatograms of diesel and kerosene corresponding to a range of evaporation levels. Using the modeled reference collection, successful identification of the liquid and level of evaporation in a test set of chromatograms was demonstrated. Full article
(This article belongs to the Special Issue Advances in Fire Debris Analysis)
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