Literatura académica sobre el tema "Single particle inductively coupled plasma mass spectrometry (SP-ICPMS)"

This work is a study of gold nanoparticle (NP) degradation upon laser ablation and provides guidelines for the optimal laser fluence for NP analysis by laser ablation single particle inductively coupled plasma mass spectrometry (LA-sp-ICPMS).

An analytical method based on single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) was developed to study the release of ZnO nanoparticles from fabric face mask samples upon washing.

Silver nanoparticles (AgNPs) are frequently found in everyday products and, as a consequence, their release into the environment cannot be avoided. Once in aquatic systems, AgNPs interact with natural constituents and undergo different transformation processes. Therefore, it is important to characterize and quantify AgNPs in environmental waters in order to understand their behavior, their transformation, and their associated toxicological risks. However, the coexistence of ionic silver (Ag+) with AgNPs in aquatic systems is one of the greatest challenges for the determination of nanosilver. Ion-exchange resins can be used to separate Ag+ from AgNPs, taking advantage of the different charges of the species. In this work, Dowex 50W-X8 was used to separate Ag+ and AgNPs in order to easily determine AgNP concentrations using inductively coupled plasma optical emission spectroscopy. The separation methodology was successfully applied to river water samples with different ratios of Ag+ and AgNPs. However, the methodology is not useful for wastewater samples. The described methodology also demonstrated an improvement in the determination of the particle size of AgNPs present in river waters by single particle inductively coupled plasma mass spectrometry when a significant amount of Ag+ is also present.

Single-particle inductively coupled plasma-mass spectrometry (SP-ICP-MS) has emerged as an important tool for the characterization of inorganic nanoparticles (NPs) in the environment. Although most SP-ICP-MS applications rely on the quadrupole ICP-MS (ICP-QMS), it is limited by the slow scanning speed of the quadrupole. Recent advancements in instrumentation have led to the development of inductively coupled plasma time-of-flight mass spectrometry (ICP-TOF-MS) which offers a viable solution. In this review, we discuss the recent advances in instrumentation and methodology of ICP-TOF-MS, followed by a detailed discussion of the applications of SP-ICP-TOFMS in analyzing NPs in the environment. SP-ICP-TOFMS has the potential to identify and quantify both anthropogenic and natural NPs in the environment, providing valuable insights into their occurrence, fate, behavior, and potential environmental risks.

Detection of microplastics in environmental samples requires fast, sensitive and selective analytical techniques, both in terms of the size of the microparticles and their concentration. Single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) allows the detection of plastic particles down to ca. 1 µm and down to concentrations of 100 particles per mL. In SP-ICP-MS, detection of carbon-containing particles is hampered by the presence of other forms of carbon (carbonates, organic matter, microorganisms…). An acidic pre-treatment of river water samples with 10% (v/v) nitric acid for 24 h allowed the reduction of the presence of dissolved carbon to ultrapure water levels and the digestion of potential microorganisms in the samples, recovering polystyrene microparticles up to 80%. Carbon-containing particles were detected in most of the samples analysed from Spanish and French Pyrenean rivers. The presence of microplastics in these samples was confirmed by Raman microscopy and their morphology was defined by electron microscopy combined with energy-dispersive X-ray spectroscopy. The developed SP-ICP-MS method is suitable for the rapid screening of river waters for the presence of microplastics, which can then be analysed by inherently slower but more selective techniques (e.g., Raman microscopy).

L'objectif principal de cette recherche est le développement de méthodes analytiques utilisant une technique de séparation couplée à la spectrométrie de masse pour l'analyse de complexes de fer de faible poids moléculaire et une technique de single-particle ICP MS pour la détection de nanoparticules bimétalliques.Dans la première partie, une méthode utilisant la chromatographie liquide avec spectrométrie de masse à double détecteur, spectrométrie de masse (MS) à haute résolution par électrospray (HRAM) et spectrométrie de masse à couplage inductif (ICPMS), a été développée pour les complexes du fer (Fe) de faible poids moléculaire, appelés 'sideophore', dans un échantillon d'un sol. La complexité des échantillons étudiés, les faibles concentrations et la labilité des analytes ont posé un défi dans le développement de méthodes pour leur identification et leur quantification. Pour éliminer la matrice, une extraction en phase solide (SPE) a été développée dans des conditions acides pour purifier la majeure partie des complexes 56Fe-sidérophore et concentrée par évaporation. Les complexes 56Fe-sidérophore ont été identifiés par chromatographie d'exclusion stérique rapide (FastSEC) - Orbitrap MSn sur la base de la masse moléculaire exacte (+ 1 ppm) et de la fragmentation MS2 ou MS3. Leur capacité à échanger facilement le 56Fe naturel contre le 58Fe ajouté a été démontrée par SEC avec détection par l'ICP MS et l'ESI MS. La méthode a été appliquée à l'analyse de tourbe prélevée dans la partie orientale des montagnes pyrénéennes françaises. Dix-neuf sidérophores appartenant à quatre classes différentes ont été identifiés et quantifiés sans avoir besoin d'un standard authentique. Les résultats ont été validés à l'aide de la détection ICP MS du fer en comparant la somme des complexes de fer déterminés par échange isotopique - ESI MS dans chaque pic observé par FastSEC-ICP MS.Dans la deuxième partie du manuscrit, une méthode utilisant la spectrométrie de masse à plasma à couplage inductif -ICP-MS en mode particule unique (SP-ICP-MS) et en mode conventionnel couplée au fractionnement d'écoulement de champ (FlFFF) a été développée. Les conditions de synthèse de nanoparticules bimétalliques (BNP) Ag-Au ont été optimisées pour appliquer celles-ci à la détection colorimétrique basée sur le concept d'agrégation. Les BNP Ag-Au, synthétisés par la réduction par le citrate des ions Ag et Au, ont été utilisées comme capteurs pour la détection du Co2+. Pour mieux comprendre la détection colorimétrique du Co2+ à l'aide de BNP Ag-Au, divers mélanges de solutions ont été étudiés, notamment : (i) uniquement des BNP Ag-Au ; (ii) BNP Ag-Au avec thiosulfate; (iii) BNP Ag-Au avec thiosulfate et éthylènediamine; et (iv) Ag-Au BNPs avec thiosulfate, Co2+ et éthylènediamine. SP-ICP-MS a été utilisé pour déterminer la taille du noyau, la distribution de taille et la concentration en nombre de particules, ainsi que l'hétérogénéité des particules synthétisées en utilisant diverses concentrations de citrate et un rapport de métal. FlFFF-ICP-MS a également été utilisé pour observer la taille hydrodynamique et le rapport d'intensité du signal de Ag et Au dans les BNP et donc pour étayer les informations obtenues à partir de SP-ICP-MS. La combinaison des techniques proposées dans des conditions appropriées a permis de surveiller la réaction de détection colorimétrique. Les informations supplémentaires du fractogramme fournies par FlFFF-ICP-MS ont également été utiles pour comprendre l'agrégation des BNP due au complexe [Co(II)(en)3]2+ autour de la surface des BNP. En outre, par rapport à la détection colorimétrique classique, la limite de détection (LOD) pour la détection des ions Co2+ a été réduite de 20 fois, du niveau ppb au niveau ppt
The research focuses on an analytical method development using chromatography coupled to mass spectrometry for the analysis of low molecular weight iron complexes. In the second part, the study explores the utilization of bimetallic nanoparticles for Co2+ detection.In the first part, a method using liquid chromatography with two detector mass spectrometry, i.e., electrospray high-resolution accurate mass (HRAM) mass spectrometry (MS) and inductively coupled mass spectrometry (ICP-MS), was developed for the analysis of low molecular weight iron (Fe) complexes, called ‘siderophores'. The complexity of the samples, their low concentrations, and the lability of the iron complexe were challenges in the development of methods for their identification and quantification. For the sample clean-up, solid phase extraction (SPE) using acidic conditions was developed to purify the samples, followed by evaporation to dryness. The individual 56Fe-siderophore complexes were identified by fast size-exclusion chromatography (FastSEC) - Orbitrap MSn based on the exact molecular mass (+ 1 ppm) and MS2. Their capability of exchanging the natural 56Fe with the spiked 58Fe was demonstrated by SEC with ICP-MS and ESI-MS detection. The method was applied to the analysis of peat collected in the Eastern part of the French Pyrenean mountains. Nineteen siderophores belonging to four different classes were presumptively identified and quantified. The results were compared with ICP-MS detection of iron and matching of the sum of the moles of iron complexes determined by the isotopic- ESI-MS within each peak as eluted from the fastSEC column.In the second part, a method using inductively coupled plasma mass spectrometry in the single particle mode and the conventional mode coupled to a flow field flow fractionation was developed to select suitable conditions for the synthesis of Ag-Au bimetallic nanoparticles and to monitor the colorimetric changes due to aggregations. Ag-Au BNPs, synthesized by using citrate reduction of Ag and Au ions, were used as sensors for the detection of Co2+. To better understand the colorimetric sensing of Co2+ using the Ag-Au BNPs, various mixtures were studied, viz. (i) only Ag-Au BNPs; (ii) Ag-Au BNPs with thiosulfate; (iii) Ag-Au BNPs with thiosulfate and ethylenediamine; and (iv) Ag-Au BNPs with thiosulfate, Co2+ and ethylenediamine. SP-ICP-MS was used to determine the core size, size distribution, and number concentration, as well as the heterogeneity of the particles synthesized by using various citrate concentrations and metal ratios. Fl-FFF-ICP-MS was also used to observe the hydrodynamic size and the Ag: Au signal intensity ratio of the BNPs to support information obtained from the SP-ICP-MS. The combination of the proposed techniques has been applied to monitor the reaction during colorimetric sensing. Additional information from fractograms provided by Fl-FFF-ICP-MS was also useful for the understanding of the aggregation of BNPs arising from the [Co(II)(en)3]2+ complex surrounding the surface of the BNPs. Furthermore, when compared to colorimetric sensing, the limit of detection for Co2+ ion, using the BNPs and SP-ICP-MS, were 20-fold lower, decreasing from ppb to ppt levels

Wprowadzenie do powszechnego użytku katalizatorów samochodowych spowodowało wzrost emisji metali z grupy platynowców (PGE) do środowiska. Podwyższony poziom zawartości platyny, palladu i rodu jest obserwowany szczególnie w okolicach dużych szlaków komunikacyjnych, rzadko jednak przekracza 1 μg g-1. Celem pracy doktorskiej było określenie wpływu, jaki pierwiastki z tej grupy wywierają na środowisko. Aby to było możliwe konieczne jest dysponowanie metodami gwarantującymi zarówno oznaczanie całkowitych zawartości analitów na odpowiednich poziomach stężeń, jak i śledzenie przemian jakim ulegają i identyfikację ich form chemicznych. Aby uzyskane wyniki oznaczeń były wiarygodne należy szczególną uwagę zwrócić na sposób przygotowania badanych materiałów do analizy. Pod względem analitycznym, oznaczanie śladowych ilości platyny, rodu czy palladu w próbkach środowiskowych nie jest zadaniem prostym. Złożoność matrycy próbek oraz niski poziom stężeń sprawiają, że metody oznaczeń muszą charakteryzować się odpowiednio niskimi granicami oznaczalności. Często w procedurze analitycznej wprowadza się dodatkowy etap zatężania analitów i uproszczenia matrycy próbki. W ramach prowadzonych badań zoptymalizowano procedury roztwarzania próbek gleb i piasków kwarcowych z wykorzystaniem mieszaniny kwasów HNO3 i HCl. W oparciu o wyniki uzyskane dla certyfikowanego materiału odniesienia – pyłu drogowego BCR-723 wykazano efektywne przeprowadzenie PGE do roztworu. Do wydzielania analitów z matrycy wykorzystano metodę ekstrakcji do fazy stałej. W trakcie badań zastosowano sorbenty kationo- i anionowymienne oraz eluenty o różnej sile elucyjnej: 0,1 mol L-1 tiomocznik w 0,1 mol L-1 HCl, 2 mol L-1 HCl, 0,025-0,053 mol L-1 bufor amonowy. Opracowane procedury przygotowania próbek zastosowano do monitorowania PGE w próbkach gleb i piasków kwarcowych, pobieranych z poletek monitoringowych rozmieszczonych wzdłuż ciągów komunikacyjnych i eksponowanych na zanieczyszczenia związane z ruchem drogowym. Szczególną uwagę zwrócono na możliwość zastosowania w oznaczeniach metody woltamperometrii inwersyjnej z adsorpcyjnym zatężaniem (AdSV), która, ze względu na niskie granice oznaczalności może być alternatywą do metody spektrometrii mas z plazmą indukcyjnie sprzężoną (ICP MS). Na podstawie uzyskanych wyników wykazano wpływ ruchu drogowego na wzrastające skażenie środowiska oraz wskazano katalizatory samochodowe, jako główne emitery pierwiastków z grupy platynowców. Odkładanie się PGE w glebach sprawia, że mogą być one pobierane i akumulowane przez rośliny, co może powodować zaburzenia ich prawidłowego funkcjonowania. W oparciu o materiał roślinny pozyskany w ramach upraw hydroponicznych określono wpływ platyny, palladu i rodu na rozwój gorczycy białej (Sinapis alba L.). Rośliny narażone na stres związany z obecnością różnych soli i nanocząstek PGE zostały scharakteryzowane pod kątem całkowitej zawartości metali pobranych z pożywki i przetransportowanych do części nadziemnych (ICP MS), obecności nanocząstek w wybranych tkankach (SP ICP MS, TEM), jak i tworzenia kompleksów z ligandami obecnymi lub syntezowanymi de novo w roślinie. Powstałe w tkankach fitochelatyny (PC2, PC3 i PC4) zidentyfikowano metodą wysokosprawnej chromatografii cieczowej z detekcją fluorescencyjną (HPLC FLD) oraz spektrometrią mas z jonizacją przez elektrorozpraszanie (ESI MS). Dodatkowo dzięki wykorzystaniu metody SEC ICP MS, wykryto i rozdzielono grupy związków palladu powstających w komórkach Sinapis alba L. Z kolei zastosowanie metody HILIC ESI MS umożliwiło zidentyfikowanie wybranych połączeń Pd z ligandami organicznymi, jak histydyna i nikotianamina, odpowiedzialnymi za procesy detoksykacji metali.
Introduction of car catalysts for general use caused an increase in emissions of platinum group elements (PGEs) to the environment. The increased level of platinum, palladium and rhodium is observed, especially in the vicinity of main communication routes, but still, rarely exceeds 1 μg g-1. The aim of the doctoral thesis was to determine an impact which PGEs may have on the environment. To make that possible, it's necessary to develop procedures, guaranteeing both, determination of the total content of analytes at appropriate concentration levels, as well as monitoring the changes they undergo and identification of their chemical forms. In order to get the reliable results, particular attention should be paid to the proper way of sample preparation before analysis. The determination of trace amounts of platinum, rhodium or palladium in environmental samples is not a simple task. The complexity of the sample matrix and the low concentration level of analytes cause that the determination methods must have sufficiently low limits of quantification. Often an additional step of analytes pre-concentration and separation from the matrix is introduced in the analytical procedure. As a part of the conducted research, the digestion procedures of soil and quartz sands samples, using the mixture of HNO3 and HCl acids, were optimized. Based on the results obtained for certified reference material (BCR-723; road dust) the possibility of efficient analytes transfers into the solution was proven. To isolate analytes from the matrix the solid phase extraction method was suggested. During the experiments, cation and anion exchange sorbents, as well as the eluents of various elution strength were used: 0.10 mol L-1 thiourea in 0.10 mol L-1 HCl, 2.0 mol L-1 HCl, 0.025-0.053 mol L-1 ammonium buffer. Developed sample preparation procedures were used to monitor PGEs in soil and quartz sands samples received from the monitoring plots distributed along high-ways and exposed to traffic-related contamination. Particular attention was paid to the possibility of using adsorptive stripping voltammetry (AdSV), which, due to low limits of quantification, can be an alternative method to inductively coupled plasma mass spectrometry (ICP MS). Based on the results obtained, the influence of road traffic on the increasing environmental pollution was proven, along with the indication of car catalysts as main emitters of the platinum group elements. The deposition of PGEs in soils makes that they can be taken up and accumulated by plants, which may cause disturbances in their proper functioning. The influence of platinum, palladium and rhodium on the growth of white mustard (Sinapis alba L.) was defined based on the plant material obtained from hydroponic cultivation. The plants, exposed to stress from the presence of various salts and nanoparticles of PGEs, have been characterized for the total content of metals taken from the nutrient solution and transported to aboveground organs (ICP MS), the presence of nanoparticles in selected tissues (SP ICP MS, TEM) and the formation of complexes with ligands present or de novo synthesized in the plant. The phytochelatins (PC2, PC3 and PC4), formed in plant cells, were identified by high-performance liquid chromatography with fluorescence detection (HPLC FLD) and electrospray ionization mass spectrometry (ESI MS). Additionally, thanks to the use of the SEC ICP MS method, some palladium compounds formed in Sinapis alba L. cells were detected and separated. The application of HILIC ESI MS method enabled identification of several Pd complexes with organic ligands, like histidine and nicotianamine, responsible for metal detoxification processes.