scholarly journals Synthesis and characterization of Zr- and Hf-doped nano-TiO 2 as internal standards for analytical quantification of nanomaterials in complex matrices

2018 ◽  
Vol 5 (6) ◽  
pp. 171884 ◽  
Author(s):  
Laura-Jayne A. Ellis ◽  
Anastasios G. Papadiamantis ◽  
Stefan Weigel ◽  
Eugenia Valsami-Jones

The reliable quantification of nanomaterials (NMs) in complex matrices such as food, cosmetics and biological and environmental compartments can be challenging due to interactions with matrix components and analytical equipment (vials and tubing). The resulting losses along the analytical process (sampling, extraction, clean-up, separation and detection) hamper the quantification of the target NMs in these matrices as well as the compatibility of results and meaningful interpretations in safety assessments. These issues can be overcome by the addition of known amounts of internal/recovery standards to the sample prior to analysis. These standards need to replicate the behaviour of target analytes in the analytical process, which is mainly defined by the surface properties. Moreover, they need to carry a tag that can be quantified independently of the target analyte. As inductively coupled plasma mass spectrometry is used for the identification and quantification of NMs, doping with isotopes, target analytes or with chemically related rare elements is a promising approach. We present the synthesis of a library of TiO 2 NMs doped with hafnium (Hf) and zirconium (Zr) (both low in environmental abundance). Zirconia NMs doped with Hf were also synthesized to complement the library. NMs were synthesized with morphological and size properties similar to commercially available TiO 2 . Characterization included: transmission electron microscopy coupled with energy-dispersive X-ray spectroscopy, X-ray diffraction spectroscopy, Brunauer–Emmett–Teller total specific surface area analysis, cryofixation scanning electron microscopy, inductively coupled plasma optical emission spectroscopy and UV–visible spectrometry. The Ti : Hf and Ti : Zr ratios were verified and calculated using Rietveld refinement. The labelled NMs can serve as internal standards to track the extraction efficiency from complex matrices, and increase method robustness and traceability of characterization/quantification.

Chemija ◽  
2020 ◽  
Vol 31 (1) ◽  
Author(s):  
Jolita Jablonskienė ◽  
Dijana Šimkūnaitė ◽  
Jūratė Vaičiūnienė ◽  
Algirdas Selskis ◽  
Audrius Drabavičius ◽  
...  

MnO2/C nanocomposites have been prepared using a simple onestep microwave heating method by applying different concentrations of cationic surfactant – cetyl trimethylammonium bromide (CTAB). The morphology and composition of the prepared MnO2/C nanocomposites have been investigated using X-ray photoelectron spectroscopy (XPS), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), and inductively coupled plasma optical emission spectroscopy (ICP-OES). The electrochemical performance of the prepared nanocomposites has been analysed using cyclic voltammetry. It was found that a high specific capacitance (Cs) of 742 F g−1 at a scan rate of 10 mV s−1 in a 1 M Na2SO4 solution has been obtained for the MnO2/C nanocomposite that has the mass loading of 0.140 mg cm−2 and has been synthesized in the absence of CTAB. Meanwhile, the application of CTAB allowed the increase in the mass loading of MnO2 in the nanocomposites. In the presence of CTAB, the highest value of 654 F g−1 at a scan rate of 10 mV s−1 has been obtained for MnO2/C that has the mass loading of 0.570 mg cm−2. This result confirmed a good performance of the prepared MnO2/C nanocomposites as the electrode material for supercapacitors.


1981 ◽  
Vol 35 (2) ◽  
pp. 226-235 ◽  
Author(s):  
Robert L. Eklund

Remembering where we came from, points out author Alex Haley in Roots, helps us know who we are today. The roots of spectroscopy are closely intertwined with those of Bausch & Lomb-ARL, known to the industry for more than 45 years as Applied Research Laboratories. A member of Bausch & Lomb's Instrument Group, ARL today is a major multinational supplier of spectrochemical instruments in the optical emission, inductively coupled plasma (ICP), X-ray fluorescence and diffraction, microanalysis, and scanning electron microscopy fields. Its story begins with a graduate student's dream—which, unlike most dreams, came true.


Catalysts ◽  
2021 ◽  
Vol 11 (4) ◽  
pp. 490
Author(s):  
Rudaviro Garidzirai ◽  
Phillimon Modisha ◽  
Innocent Shuro ◽  
Jacobus Visagie ◽  
Pieter van Helden ◽  
...  

The effects of Mg and Zn dopants on the catalytic performance of Pt/Al2O3 catalyst were investigated for dehydrogenation of perhydrodibenzyltoluene (H18-DBT) as a liquid organic hydrogen carrier. Al2O3 supports were modified with Mg and Zn to produce Mg-Al2O3 and Zn-Al2O3 with a target loading of 3.8 wt.% for dopants. The modified supports were impregnated with chloroplatinic acid solution to produce the catalysts Pt/Al2O3, Pt/Mg-Al2O3 and Pt/Zn-Al2O3 of 0.5 wt.% Pt loading. Thereafter, the catalysts were characterised using inductively coupled plasma- optical emission spectrometry, scanning electron microscopy-energy dispersive X-ray spectroscopy, hydrogen temperature-programmed reduction, carbon-monoxide pulse chemisorption, ammonia temperature-programmed desorption, X-ray diffraction and transmission electron microscopy. The dehydrogenation experiments were performed using a horizontal plug flow reactor system and the catalyst time-on-stream was 22 h. Pt/Mg-Al2O3 showed the highest average hydrogen flowrate of 29 nL/h, while an average of 27 nL/h was obtained for both Pt/Al2O3 and Pt/Zn-Al2O3. This has resulted in a hydrogen yield of 80% for Pt/Mg-Al2O3, 71% for Pt/Zn-Al2O3 and 73% for Pt/Al2O3. In addition, the conversion of H18-DBT ranges from 99% to 92%, Pt 97–90% and 96–90% for Pt/Mg-Al2O3, Pt/Zn-Al2O3 and Pt/Al2O3, respectively. Following the latter catalyst order, the selectivity to dibenzyltoluene (H0-DBT) ranges from 78% to 57%, 75–51% and 71–45%. Therefore, Pt/Mg-Al2O3 showed improved catalytic performance towards dehydrogenation of H18-DBT.


2014 ◽  
Vol 2014 ◽  
pp. 1-8 ◽  
Author(s):  
Izabela Michalak ◽  
Krzysztof Marycz ◽  
Katarzyna Basińska ◽  
Katarzyna Chojnacka

The biomass ofVaucheria sessilisforms algal mats in many freshwaters. There is a need to find the method of algal biomass utilization.Vaucheria sessilisis a rich source of micro- and macronutrients and can be used as a soil amendment. In the paper, the elemental composition of enriched, via bioaccumulation process, macroalga was investigated. For this purpose, two independent techniques were used: scanning electron microscopy with an energy dispersive X-ray analytical system (SEMEDX) and inductively coupled plasma optical emission spectroscopy (ICP-OES). The biomass was exposed to two microelemental solutions, with Cu(II) and Zn(II) ions. After two weeks of the experiment, macroalga accumulated 98.5 mg of Zn(II) ions in 1 g of dry biomass and 68.9 mg g−1of Cu(II) ions. Micrographs performed by SEM proved that bioaccumulation occurred. Metal ions were bound on the surface and in the interior of cells. Mappings of all cations showed that in the case of the surface of biomass (biosorption), the elements constituted aggregations and in the case of the cross section (bioaccumulation) they were evenly distributed. The algal biomass with permanently bound microelements can find an application in many branches of the industry (feed, natural fertilizers, etc.).


Minerals ◽  
2019 ◽  
Vol 10 (1) ◽  
pp. 12
Author(s):  
Dimitrina Dimitrova ◽  
Vassilka Mladenova ◽  
Lutz Hecht

The colloform pyrite variety incorporates many trace elements that are released in the environment during rapid oxidation. Colloform pyrite from the Chiprovtsi silver–lead deposit in Bulgaria and its oxidation efflorescent products were studied using X-ray diffractometry, scanning electron microscopy, electron microprobe analysis, and laser ablation inductively coupled plasma mass spectrometry. Pyrite is enriched with (in ppm): Co (0.1–964), Ni (1.8–3858), Cu (2.9–3188), Zn (3.1–77), Ag (1.2–1771), As (8179–52,787), Se (2.7–21.7), Sb (48–17792), Hg (4–2854), Tl (1.7–2336), Pb (13–7072), and Au (0.07–2.77). Gypsum, anhydrite, szomolnokite, halotrichite, römerite, copiapite, aluminocopiapite, magnesiocopiapite, coquimbite, aluminocoquimbite, voltaite, and ammoniomagnesiovoltaite were identified in the efflorescent sulfate assemblage. Sulfate minerals contain not only inherited elements from pyrite (Cr, Fe, Co, Ni, Cu, Zn, Ag, In, As, Sb, Hg, Tl, and Pb), but also newly introduced elements (Na, Mg, Al, Si, P, K, Ca, Sc, Ti, V, Mn, Ga, Rb, Sr, Y, Zr, Sn, Cs, Ba, REE, U, and Th). Voltaite group minerals, copiapite, magnesiocopiapite, and römerite incorporate most of the trace elements, especially the most hazardous As, Sb, Hg, and Tl. Colloform pyrite occurrence in the Chiprovtsi deposit is limited. Its association with marbles would further restrict the oxidation and release of hazardous elements into the environment.


2008 ◽  
Vol 22 (15) ◽  
pp. 1487-1495 ◽  
Author(s):  
YEXIA FAN ◽  
HONGTAO LI ◽  
LIANCHENG ZHAO

Congruent Ce (0.1 wt %): Cu (0.05 wt %): LiNbO 3 single crystals doped with 0, 1, 3, 4, 5, 6 mol% MgO respectively were grown by the Czochrolski method in air along the C direction. The inductively coupled plasma optical emission/mass spectrometry (ICP-OE/MS), the X-ray powder diffraction (XRD), the differential thermal analysis (DTA), the ultraviolet-visible (UV-Vis) absorption spectra and the infrared (IR) absorption spectrum were measured and discussed in terms of the spectroscopic characterization and the defect structure of the Mg:Ce:Cu:LiNbO 3 crystals. The results indicated that the Mg:Ce:Cu:LiNbO 3 crystal grown from the congruent composition melt showed large [ Li ]/[ Nb ] ratios, which was closer to stoichiometry, an increase in the Curie temperature and a non-linear shift in the absorption edge with MgO concentration increasing. The threshold concentration of MgO in Mg:Ce:Cu:LiNbO 3 of nearly 5.52 mol% was estimated.


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