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      Atomic spectrometry update – a review of advances in environmental analysis

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          This review covers advances in the analysis of air, water, plants, soils and geological materials by a range of atomic spectrometric techniques including atomic emission, absorption, fluorescence and mass spectrometry.


          This is the 32 nd annual review of the application of atomic spectrometry to the chemical analysis of environmental samples. This update refers to papers published approximately between August 2015 and June 2016 and continues the series of Atomic Spectrometry Updates (ASUs) in environmental analysis1 that should be read in conjunction with other related ASUs in the series, namely: clinical and biological materials, foods and beverages;2 advances in atomic spectrometry and related techniques;3 elemental speciation;4 X-ray spectrometry;5 and metals, chemicals and functional materials.6 In the field of air analysis, highlights within this review period included the development of a new prototype fluorescence instrument for the ultratrace determination of oxidised mercury species, and coupling of elemental analysers to CRDS alongside the development of FTIR and Raman techniques for the improved characterisation of carbonaceous aerosols. In the arena of water analysis, methods continued to be reported for the speciation of As, Cr and Hg species and, following on from last year, Gd species derived from MRI agents discharged at low level from medical facilities into water courses. Improved methods for the determination of legacy compounds such as organoleads and tins made use of plasma techniques that nowadays are more tolerant of organic solvents. Instrumental developments reported included the use of MC-ICP-MS for isotopic tracer studies and a review of TXRF techniques and associated preconcentration procedures for trace element analysis. In the field of plant and soil analysis, there is a welcome trend in that more workers appear to be optimising their analytical methods (or at least checking their performance, e.g. by analysis of CRMs) even if the main purpose of their study is environmental application rather than fundamental spectroscopy. On-going challenges include: the fact that most speciation methods reported are still too complicated, costly or time consuming, for routine use; the need for more and a wider range of CRMs, especially for speciation analysis and for use with laser-based techniques; and the lack of harmonised analytical methodology, which hinders international environmental regulatory monitoring efforts. In geological applications, a variety of techniques have been employed in the drive towards high resolution multi-elemental imaging of complex solid samples. Recent developments in cell design, aerosol transport and data acquisition for LA-ICP-MS, combined with improvements in ICP mass spectrometer design, provided evidence of its potential for very rapid quantitative 3D imaging. Elemental and isotope imaging by NanoSIMS enabled accurate U–Pb dating of mineral domains too small for reliable measurements by LA-ICP-MS. Although megapixel synchrotron XRFS is still in its infancy, it too should open up new horizons in the study of trace and major element distributions and speciation in geological materials and offer a complementary method to other imaging techniques. The deployment of ICP-MS/MS technology has resulted in successful method development to overcome several intractable isobaric interferences in the analysis of geological materials by single quadrupole ICP-MS with LA and solution sample introduction. Many more environmental applications using this approach are likely to be reported in future ASUs.

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          Detection, characterization and quantification of inorganic engineered nanomaterials: A review of techniques and methodological approaches for the analysis of complex samples.

          The increasing demand of analytical information related to inorganic engineered nanomaterials requires the adaptation of existing techniques and methods, or the development of new ones. The challenge for the analytical sciences has been to consider the nanoparticles as a new sort of analytes, involving both chemical (composition, mass and number concentration) and physical information (e.g. size, shape, aggregation). Moreover, information about the species derived from the nanoparticles themselves and their transformations must also be supplied. Whereas techniques commonly used for nanoparticle characterization, such as light scattering techniques, show serious limitations when applied to complex samples, other well-established techniques, like electron microscopy and atomic spectrometry, can provide useful information in most cases. Furthermore, separation techniques, including flow field flow fractionation, capillary electrophoresis and hydrodynamic chromatography, are moving to the nano domain, mostly hyphenated to inductively coupled plasma mass spectrometry as element specific detector. Emerging techniques based on the detection of single nanoparticles by using ICP-MS, but also coulometry, are in their way to gain a position. Chemical sensors selective to nanoparticles are in their early stages, but they are very promising considering their portability and simplicity. Although the field is in continuous evolution, at this moment it is moving from proofs-of-concept in simple matrices to methods dealing with matrices of higher complexity and relevant analyte concentrations. To achieve this goal, sample preparation methods are essential to manage such complex situations. Apart from size fractionation methods, matrix digestion, extraction and concentration methods capable of preserving the nature of the nanoparticles are being developed. This review presents and discusses the state-of-the-art analytical techniques and sample preparation methods suitable for dealing with complex samples. Single- and multi-method approaches applied to solve the nanometrological challenges posed by a variety of stakeholders are also presented.
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            Is Open Access

            ACTRIS ACSM intercomparison – Part 1: Reproducibility of concentration and fragment results from 13 individual Quadrupole Aerosol Chemical Speciation Monitors (Q-ACSM) and consistency with co-located instruments

            Abstract. As part of the European ACTRIS project, the first large Quadrupole Aerosol Chemical Speciation Monitor (Q-ACSM) intercomparison study was conducted in the region of Paris for 3 weeks during the late-fall – early-winter period (November–December 2013). The first week was dedicated to the tuning and calibration of each instrument, whereas the second and third were dedicated to side-by-side comparison in ambient conditions with co-located instruments providing independent information on submicron aerosol optical, physical, and chemical properties. Near real-time measurements of the major chemical species (organic matter, sulfate, nitrate, ammonium, and chloride) in the non-refractory submicron aerosols (NR-PM 1 ) were obtained here from 13 Q-ACSM. The results show that these instruments can produce highly comparable and robust measurements of the NR-PM 1 total mass and its major components. Taking the median of the 13 Q-ACSM as a reference for this study, strong correlations ( r 2 > 0.9) were observed systematically for each individual Q-ACSM across all chemical families except for chloride for which three Q-ACSMs showing weak correlations partly due to the very low concentrations during the study. Reproducibility expanded uncertainties of Q-ACSM concentration measurements were determined using appropriate methodologies defined by the International Standard Organization (ISO 17025, 1999) and were found to be 9, 15, 19, 28, and 36 % for NR-PM 1 , nitrate, organic matter, sulfate, and ammonium, respectively. However, discrepancies were observed in the relative concentrations of the constituent mass fragments for each chemical component. In particular, significant differences were observed for the organic fragment at mass-to-charge ratio 44, which is a key parameter describing the oxidation state of organic aerosol. Following this first major intercomparison exercise of a large number of Q-ACSMs, detailed intercomparison results are presented, along with a discussion of some recommendations about best calibration practices, standardized data processing, and data treatment.
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              Detection of gold nanoparticles with different sizes using absorption and fluorescence based method


                Author and article information

                [1 ]Health and Safety Laboratory
                [2 ]Buxton
                [3 ]UK SK17 9JN
                [4 ]CNR-IDPA
                [5 ]Universita Ca' Foscari
                [6 ]30123 Venezia
                [7 ]Italy
                [8 ]British Geological Survey
                [9 ]Nottingham
                [10 ]UK NG12 5GG
                [11 ]University of Strathclyde
                [12 ]Glasgow
                [13 ]UK G1 1XL
                Journal of Analytical Atomic Spectrometry
                J. Anal. At. Spectrom.
                Royal Society of Chemistry (RSC)
                : 32
                : 1
                : 11-57
                © 2017
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