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Advances in Detection of Trace Elements by Analytical Spectroscopy
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Advances in Detection of Trace Elements by Analytical Spectroscopy

A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (30 September 2023) | Viewed by 12244

Special Issue Editor

Prof. Dr. Michael Bolshov

E-Mail Website
Guest Editor
Institute of Spectroscopy, Russian Academy of Sciences, 5 Fizicheskaya Street, Troitsk, 108840 Moscow, Russia
Interests: laser spectroscopy; spectroscopy with diode lasers; elemental analysis with inductively coupled plasma; reversible sorption preconcentration
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

The detection of ultralow (trace) concentrations of different elements was and still is a challenging problem in analytical spectroscopy. The detection of trace elements is now a key problem in a wide spectrum of scientific and technologic applications: the production of pure materials, fundamental geochemistry, evaluation of the commercial efficiencies of new mineral resources and industrial wastes for recycling, ecological and food control, medicine, the development of new drugs etc. The continuous development of spectroscopic instrumentation, analytical methods and specific techniques of sample pretreatment has provided a noticeable increase in the sensitivities of different spectroscopic techniques and appropriate reductions to the limits of detection (LODs).

The meaning of the term “trace” has gradually changed over time according to the demands of science, industry, medical care, health protection etc. In the mid 20th century concentrations 1–10 ppm were considered as very low (trace), while by the end of the 20th century concentrations of 1–100 ppt were considered trace level! Importantly, the sensitivity of a specific spectroscopic technique is defined not only by low detectable concentrations but also low absolute detectable mass of the analytes, while the analysis of micrograms of sample appears to be very critical.

The second half of the 20th century saw the fast development of laser analytical spectroscopic techniques, such as laser-induced fluorescence, multistep resonance ionization spectroscopy, and laser-enhanced ionization. Extremely low LODs were demonstrated down to low ppt levels, which were the lowest at that time. The critical disadvantage of all laser-based techniques was their intrinsic “single element” nature. Only one element could be detected in a single measurement cycle. This disadvantage was overcome by the new analytical techniques based on inductively coupled plasma (ICP), which were explosively developed beginning in the 1980s. Both versions of ICP with atomic emission (ICP-AES) or mass-spectrometric (ICP-MS) detectors took the leading position in elemental analysis. Combining high sensitivity and multi-element capability both techniques have the drawback that they enable the analysis of mostly liquid samples. On the other hand, this feature has caused active development of different techniques and methods for solid sample pretreatment.

At present techniques for the direct analysis of solid samples are extremely popular: laser ablation (LA) with detection of the emission of the hot ablated material, the combination of LA with the analysis of the ablated material by ICP-MS, the X-ray fluorescence spectroscopy (XRF) of a bulk sample or total reflection XRF.

This Special Issue is devoted to the survey of the modern state of the art of different spectroscopic techniques for the detection of low concentrations or total quantities of analytes in different types of samples. Papers on different sample preparation techniques for the final detection of the analytes by spectroscopic techniques are also welcomed. 

Prof. Dr. Michael Bolshov
Guest Editor

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Molecules is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2700 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • analytical spectroscopy
  • trace elements
  • ICP
  • ICP-AES
  • ICP-MS
  • LA-ICP-MS
  • XRF

Published Papers (9 papers)

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Research

17 pages, 1987 KiB  
Article
Possibilities and Limitations of ICP-Spectrometric Determination of the Total Content of Tin and Its Inorganic and Organic Speciations in Waters with Different Salinity Levels—Part 2: Separate Determination of Inorganic and Organic Speciations of Tin
by Zaual Temerdashev, Pavel Abakumov, Mikhail Bolshov, Darya Abakumova and Alexander Pupyshev
Molecules 2023, 28(18), 6615; https://doi.org/10.3390/molecules28186615 - 14 Sep 2023
Viewed by 593
Abstract
In this study, determination of the inorganic and organic forms of tin in waters of different salinities is considered. The possibility of the separation of speciations of tin using liquid–liquid extraction (LLE); precipitation with fluorides, iodides, ammonia, and iron (III) chloride; and sorption [...] Read more.
In this study, determination of the inorganic and organic forms of tin in waters of different salinities is considered. The possibility of the separation of speciations of tin using liquid–liquid extraction (LLE); precipitation with fluorides, iodides, ammonia, and iron (III) chloride; and sorption of organotin compounds (OTCs) was studied. The LLE and analyte precipitation methods proved to be ineffective. Inorganic and organic forms of tin were separated by the sorption of OTCs using silica gel sorbent Diapak C18. Under optimized conditions, a technique for the separate determination of the forms of tin in natural waters was developed. The technique combines hydride generation and microwave mineralization of solutions followed by ICP spectrometry. The inorganic forms of tin were determined after their solid-phase separation from organotin compounds. The lower limits of analyte quantification were 0.03 μg/L (ICP-MS) and 0.05 μg/L (ICP-OES), which provide separate determinations of inorganic and organic forms of tin in waters with different salinities. The content of OTCs in water was determined by subtracting the inorganic concentration from the total concentration of tin. The technique will allow a comprehensive assessment of the toxicological impact of tin speciations on the aquatic ecosystem. Full article
(This article belongs to the Special Issue Advances in Detection of Trace Elements by Analytical Spectroscopy)
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20 pages, 3573 KiB  
Article
Possibilities and Limitations of ICP-Spectrometric Determination of the Total Content of Tin, Its Inorganic and Organic Speciations in Waters with Different Salinity Levels—Part 1: Determination of the Total Tin Content
by Zaual Temerdashev, Pavel Abakumov, Mikhail Bolshov, Darya Abakumova and Alexander Pupyshev
Molecules 2023, 28(16), 5967; https://doi.org/10.3390/molecules28165967 - 09 Aug 2023
Cited by 1 | Viewed by 1008
Abstract
This paper considers the features of determining the total tin content in waters with different salinity. Direct ICP-spectrometric analysis of sea waters with a salinity of more than 6‰ significantly reduced the analytical signal of tin by 70% (ICP-MS) and 30% (ICP-OES). The [...] Read more.
This paper considers the features of determining the total tin content in waters with different salinity. Direct ICP-spectrometric analysis of sea waters with a salinity of more than 6‰ significantly reduced the analytical signal of tin by 70% (ICP-MS) and 30% (ICP-OES). The matrix effect of macrocomponents was eliminated by generating hydrides using 0.50 M sodium borohydride and 0.10 M hydrochloric acid. The effect of transition metals on the formation of tin hydrides was eliminated by applying L-cysteine at a concentration of 0.75 g/L. The total analyte concentrations, considering the content of organotin compounds, were determined after microwave digestion of sample with oxidizing mixtures based on nitric acid. The generation of hydrides with the ICP-spectrometric determination of tin leveled the influence of the sea water matrix and reduced its detection limit from 0.50 up to 0.05 µg/L for all digestion schemes. The developed analysis scheme made it possible to determine the total content of inorganic and organic forms of tin in sea waters. The total content of tin was determined in the waters of the Azov and Black seas at the levels of 0.17 and 0.24 µg/L, respectively. Full article
(This article belongs to the Special Issue Advances in Detection of Trace Elements by Analytical Spectroscopy)
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13 pages, 2165 KiB  
Article
Can Rare Earth Elements Be Considered as Markers of the Varietal and Geographical Origin of Wines?
by Zaual Temerdashev, Mikhail Bolshov, Aleksey Abakumov, Alexan Khalafyan, Anastasia Kaunova, Alexander Vasilyev, Olga Sheludko and Arsen Ramazanov
Molecules 2023, 28(11), 4319; https://doi.org/10.3390/molecules28114319 - 24 May 2023
Viewed by 1120
Abstract
The possibility of establishing the varietal and territorial affiliation of wines by the content of rare earth elements (REE) in them was studied. ICP–OES and ICP–MS with subsequent chemometric processing of the results were applied to determine the elemental image of soils containing [...] Read more.
The possibility of establishing the varietal and territorial affiliation of wines by the content of rare earth elements (REE) in them was studied. ICP–OES and ICP–MS with subsequent chemometric processing of the results were applied to determine the elemental image of soils containing negligible REE amounts, grapes grown on these soils, and wine materials of Cabernet Sauvignon, Merlot, and Moldova varieties produced from these grapes. To stabilize and clarify wine materials, the traditional processing of wine materials with various types of bentonite clays (BT) was used, which turned out to be a source of REE in the wine material. Discriminant analysis revealed that the processed wine materials were homogeneous within one denomination and that those of different denominations were heterogeneous with respect to the content of REE. It was found that REE in wine materials were transferred from BT during the processing, and thus they can poorly characterize the geographical origin and varietal affiliation of wines. Analysis of these wine materials according to the intrinsic concentrations of macro- and microelements showed that they formed clusters according to their varietal affiliation. In terms of their influence on the varietal image of wine materials, REE are significantly inferior to macro- and microelements, but they enhance their influence to a certain extent when used together. Full article
(This article belongs to the Special Issue Advances in Detection of Trace Elements by Analytical Spectroscopy)
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10 pages, 3867 KiB  
Communication
Hybrid Wetting Surface with Plasmonic Alloy Nanocomposites for Sensitive SERS Detection
by Shanjiang Wang, Dan Su, Huanli Zhou, Xiaohan Jiang, Xiaoyang Zhang and Tong Zhang
Molecules 2023, 28(5), 2190; https://doi.org/10.3390/molecules28052190 - 27 Feb 2023
Viewed by 1200
Abstract
In this paper, a hybrid wetting surface (HWS) with Au/Ag alloy nanocomposites was proposed for rapid, cost-effective, stable and sensitive SERS application. This surface was fabricated in a large area by facile electrospinning, plasma etching and photomask-assisted sputtering processes. The high-density ‘hot spots’ [...] Read more.
In this paper, a hybrid wetting surface (HWS) with Au/Ag alloy nanocomposites was proposed for rapid, cost-effective, stable and sensitive SERS application. This surface was fabricated in a large area by facile electrospinning, plasma etching and photomask-assisted sputtering processes. The high-density ‘hot spots’ and rough surface from plasmonic alloy nanocomposites promoted the significant enhancement of the electromagnetic field. Meanwhile, the condensation effects induced by HWS further improved the density of target analytes at the SERS active area. Thus, the SERS signals increased ~4 orders of magnitude compared to the normal SERS substrate. In addition, the reproducibility, uniformity, as well as thermal performance of HWS were also examined by comparative experiments, indicating their high reliability, portability and practicability for on-site tests. The efficient results suggested that this smart surface had great potential to evolve as a platform for advanced sensor-based applications. Full article
(This article belongs to the Special Issue Advances in Detection of Trace Elements by Analytical Spectroscopy)
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15 pages, 1538 KiB  
Article
A Novel Method for the Background Signal Correction in SP-ICP-MS Analysis of the Sizes of Titanium Dioxide Nanoparticles in Cosmetic Samples
by Zaual A. Temerdashev, Olga A. Galitskaya and Mikhail A. Bolshov
Molecules 2022, 27(22), 7748; https://doi.org/10.3390/molecules27227748 - 10 Nov 2022
Cited by 4 | Viewed by 1347
Abstract
We discuss the features involved in determining the titanium dioxide nanoparticle (TiO2NP) sizes in cosmetic samples via single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) in the millisecond-time resolution mode, and methods for considering the background signal. In the SP-ICP-MS determination [...] Read more.
We discuss the features involved in determining the titanium dioxide nanoparticle (TiO2NP) sizes in cosmetic samples via single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) in the millisecond-time resolution mode, and methods for considering the background signal. In the SP-ICP-MS determination of TiO2NPs in cosmetics, the background signal was recorded in each dwell time interval due to the signal of the Ti dissolved form in deionized water, and the background signal of the cosmetic matrix was compensated by dilution. A correction procedure for the frequency and intensity of the background signal is proposed, which differs from the known procedures due to its correction by the standard deviation above the background signal. Background signals were removed from the sample signal distribution using the deionized water signal distribution. Data processing was carried out using Microsoft Office Excel and SPCal software. The distributions of NP signals in cosmetic product samples were studied in the dwell time range of 4–20 ms. The limit of detection of the NP size (LODsize) with the proposed background signal correction procedure was 71 nm. For the studied samples, the LODsize did not depend on the threshold of the background signal and was determined by the sensitivity of the mass spectrometer. Full article
(This article belongs to the Special Issue Advances in Detection of Trace Elements by Analytical Spectroscopy)
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16 pages, 22657 KiB  
Article
Reversible Sorptive Preconcentration of Noble Metals Followed by FI-ICP-MS Determination
by Yulia A. Maksimova, Alexander S. Dubenskiy, Lyudmila A. Pavlova, Ilya V. Shigapov, Dmitry M. Korshunov, Irina F. Seregina, Vadim A. Davankov and Mikhail A. Bolshov
Molecules 2022, 27(19), 6746; https://doi.org/10.3390/molecules27196746 - 10 Oct 2022
Viewed by 1429
Abstract
In this paper, we propose the combined procedure of noble metal (NM) determination, including fire assay, acid digestion, and reversible dynamic sorptive preconcentration, followed by flow-injection ICP-MS. Reversible preconcentration of all NMs was carried out using micro-column packed new PVBC-VP sorbent and elution [...] Read more.
In this paper, we propose the combined procedure of noble metal (NM) determination, including fire assay, acid digestion, and reversible dynamic sorptive preconcentration, followed by flow-injection ICP-MS. Reversible preconcentration of all NMs was carried out using micro-column packed new PVBC-VP sorbent and elution with a mixture of thiourea, potassium thiocyanate, and HCl, which recovers Pd, Ir, Pt, and Au by 95% and Ru, and Rh by 90%. The proposed procedure was approved using certified reference materials. Full article
(This article belongs to the Special Issue Advances in Detection of Trace Elements by Analytical Spectroscopy)
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12 pages, 1518 KiB  
Article
Distribution of Platinum and Palladium between Dissolved, Nanoparticulate, and Microparticulate Fractions of Road Dust
by Mikhail S. Ermolin, Alexandr I. Ivaneev, Anton S. Brzhezinskiy, Natalia N. Fedyunina, Vasily K. Karandashev and Petr S. Fedotov
Molecules 2022, 27(18), 6107; https://doi.org/10.3390/molecules27186107 - 19 Sep 2022
Cited by 3 | Viewed by 1589
Abstract
Ageing processes of vehicle catalytic converters inevitably lead to the release of Pt and Pd into the environment, road dust being the main sink. Though Pt and Pd are contained in catalytic converters in nanoparticulate metallic form, under environmental conditions, they can be [...] Read more.
Ageing processes of vehicle catalytic converters inevitably lead to the release of Pt and Pd into the environment, road dust being the main sink. Though Pt and Pd are contained in catalytic converters in nanoparticulate metallic form, under environmental conditions, they can be transformed into toxic dissolved species. In the present work, the distribution of Pt and Pd between dissolved, nanoparticulate, and microparticulate fractions of Moscow road dust is assessed. The total concentrations of Pt and Pd in dust vary in the ranges 9–142 ng (mean 35) and 155–456 (mean 235) ng g−1, respectively. The nanoparticulate and dissolved species of Pt and Pd in dust were studied using single particle inductively coupled plasma mass spectrometry. The median sizes of nanoparticulate Pt and Pd were 7 and 13 nm, respectively. The nanoparticulate fraction of Pt and Pd in Moscow dust is only about 1.6–1.8%. The average contents of dissolved fraction of Pt and Pd are 10.4% and 4.1%, respectively. The major fractions of Pt and Pd (88–94%) in road dust are associated with microparticles. Although the microparticulate fractions of Pt and Pd are relatively stable, they may become dissolved under changing environmental conditions and, hence, transformed into toxic species. Full article
(This article belongs to the Special Issue Advances in Detection of Trace Elements by Analytical Spectroscopy)
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9 pages, 1081 KiB  
Article
Estimation of the Number of Scans Required per Hard-to-Clean Location and Establishing the Limit of Quantification of a Partial Least Squares Calibration Model When the FTIR Is Used for Pharmaceutical Cleaning Verification
by Apu Sarwar, Conor McSweeney, Mark Smith and Eric Moore
Molecules 2022, 27(14), 4569; https://doi.org/10.3390/molecules27144569 - 18 Jul 2022
Cited by 1 | Viewed by 1253
Abstract
This study aims to identify two critical components required for pharmaceutical cleaning verification when an FTIR is used: (a) the number of scans required per hard-to-clean location, and (b) the limit of quantification (LOQ) of the FTIR instrument when measuring the surface contamination. [...] Read more.
This study aims to identify two critical components required for pharmaceutical cleaning verification when an FTIR is used: (a) the number of scans required per hard-to-clean location, and (b) the limit of quantification (LOQ) of the FTIR instrument when measuring the surface contamination. The current practice in pharmaceutical manufacturing does not require multiple samples as it is standard practice to collect a single swab sample from a 25 × 25 cm area from a difficult-to-reach area of the manufacturing equipment. However, since the FTIR will only scan a tiny portion of the surface compared to the swab, a sufficient number of samples (data points) are required to provide enough confidence to ensure that the measurement results are close to the true value with a maximum degree of certainty. Similarly, calculating the LOQ for a linear regression could be straightforward. However, complexity arises when the experimental data are complex; in this case, the complexity arises due to the nature of the measurement and the lack of the defined peak in the pre-processed spectra. Therefore, this study uses the practical approach of calculating the sample size and the LOQ. Full article
(This article belongs to the Special Issue Advances in Detection of Trace Elements by Analytical Spectroscopy)
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13 pages, 3120 KiB  
Article
Carbon Quantum Dots Based Chemosensor Array for Monitoring Multiple Metal Ions
by Tianlei Qin, Jiayi Wang, Yuanli Liu and Song Guo
Molecules 2022, 27(12), 3843; https://doi.org/10.3390/molecules27123843 - 15 Jun 2022
Cited by 4 | Viewed by 1877
Abstract
The simultaneous identification of multiple metal ions in water has attracted enormous research interest in the past few decades. We herein describe a novel method for multiple metal ion detection using a carbon quantum dots (CQDs)-based chemosensor array and the CQDs are functionalized [...] Read more.
The simultaneous identification of multiple metal ions in water has attracted enormous research interest in the past few decades. We herein describe a novel method for multiple metal ion detection using a carbon quantum dots (CQDs)-based chemosensor array and the CQDs are functionalized with different amino acids (glutamine, histidine, arginine, lysine and proline), which act as sensing elements in the sensor array. Eleven metal ions are successfully identified by the designed chemosensor array, with 100% classification accuracy. Importantly, the proposed method allowed the quantitative prediction of the concentration of individual metal ions in the mixture with the aid of a support vector machine (SVM). The sensor array also enables the qualitative detection of unknown metal ions under the interference of tap water and local river water. Thus, the strategy provides a novel high-throughput approach for the identification of various analytes in complex systems. Full article
(This article belongs to the Special Issue Advances in Detection of Trace Elements by Analytical Spectroscopy)
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