Photolysis of Short-Lived Transient Species in Solutions: Product Analysis Studies

Author(s):  
Firmansyah A. ◽  
Winingsih W. ◽  
Soebara Y S

Analysis of natural product remain challenging issues for analytical chemist, since natural products are complicated system of mixture. The most popular methods of choice used for quality control of raw material and finished product are high performance liquid chromatography (HPLC), gas chromatography (GC) and mass spectrometry (MS). The utilization of FTIR-ATR (Fourier Transform Infrared-Attenuated Total Reflectance) method in natural product analysis is still limited. This study attempts to expand the use of FTIR spectroscopy in authenticating Indonesian coffee powder.The coffee samples studied were taken from nine regions in Indonesia, namely Aceh Gayo, Flores, Kintamani, Mandheling, Papua, Sidikalang, Toraja, Kerinci and Lampung.The samples in the form of coffee bean from various regions were powdered . The next step conducted was to determine the spectrum using the FTIR-ATR (Attenuated Total Reflectance) using ZnSe crystal of 8000 resolution. Spectrum samples, then, were analyzed using chemometrics. The utilized chemometric model was the principal component analysis (PCA) and cluster analysis (CA). Based on the chemometric analysis, there are similarities between Aceh Gayo coffee with Toraja coffee, Mandailing coffee, Kintamani coffee and Flores coffee. Sidikalang coffee has a similarity to Flores coffee; Papua coffee has a similarity to Sidikalang coffee; Lampung coffee has a similarity to Sidikalang coffee, while Kerinci coffee has a similarity to Papua coffee.


1983 ◽  
Vol 48 (12) ◽  
pp. 3660-3673 ◽  
Author(s):  
Pavel Kočovský

5(O)n and 6(O)π,n participations by some oxygen containing functional groups in the course of reaction with hypobromous acid have been studied on olefinic models of steroid type (I and II). The ability of these groups to participate has been compared on the basis of their relative reactivity with water (as externally attacking nucleophile) competing with participation. The results of the product analysis show that the ability to react with 5(O)n participation decreases in the order HO > CH3O ≃ CH3OCH2O > CH3CO2 > HCO2 > CH3SO3 ≥ (C2H5O)2PO2 > C6H5CO2 > O2NO ≫ CF3CO2, C2H5OCO2; in the last two functional groups is this ability completely suppressed. The 6(O)π,n participation comes in consideration only for compounds of the type II bearing the groups with the -X=O moiety which are ordered in the following sequence: C2H5OCO2 ≃ CH3CO2 ≥ (C2H5O)2PO2 > HCO2 > C6H5CO2. The remaining functional groups (CF3CO2, O2NO and CH3SO3do not undergo this process. Generally, it is valid that introduction of electron-withdrawing substituents into a participating group impedes or completely suppresses its ability to participate.


1981 ◽  
Vol 44 (5) ◽  
pp. 1059-1066 ◽  
Author(s):  
J.M. Dyke ◽  
N.B.H. Jonathan ◽  
A. Morris ◽  
M.J. Winter

Author(s):  
Jako S. Eensalu ◽  
Kaia Tõnsuaadu ◽  
Jasper Adamson ◽  
Ilona Oja Acik ◽  
Malle Krunks

AbstractThermal decomposition of tris(O-ethyldithiocarbonato)-antimony(III) (1), a precursor for Sb2S3 thin films synthesized from an acidified aqueous solution of SbCl3 and KS2COCH2CH3, was monitored by simultaneous thermogravimetry, differential thermal analysis and evolved gas analysis via mass spectroscopy (TG/DTA-EGA-MS) measurements in dynamic Ar, and synthetic air atmospheres. 1 was identified by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance (NMR) measurements, and quantified by NMR and elemental analysis. Solid intermediates and final decomposition products of 1 prepared in both atmospheres were determined by X-ray diffraction (XRD), Raman spectroscopy, and FTIR. 1 is a complex compound, where Sb is coordinated by three ethyldithiocarbonate ligands via the S atoms. The thermal degradation of 1 in Ar consists of three mass loss steps, and four mass loss steps in synthetic air. The total mass losses are 100% at 800 °C in Ar, and 66.8% at 600 °C in synthetic air, where the final product is Sb2O4. 1 melts at 85 °C, and decomposes at 90–170 °C into mainly Sb2S3, as confirmed by Raman, and an impurity phase consisting mostly of CSO 2 2− ligands. The solid-phase mineralizes fully at ≈240 °C, which permits Sb2S3 to crystallize at around 250 °C in both atmospheres. The gaseous species evolved include CS2, C2H5OH, CO, CO2, COS, H2O, SO2, and minor quantities of C2H5SH, (C2H5)2S, (C2H5)2O, and (S2COCH2CH3)2. The thermal decomposition mechanism of 1 is described with chemical reactions based on EGA-MS and solid intermediate decomposition product analysis.


Separations ◽  
2021 ◽  
Vol 8 (7) ◽  
pp. 104
Author(s):  
Leah M. Arrigo ◽  
Jun Jiang ◽  
Zachary S. Finch ◽  
James M. Bowen ◽  
Staci M. Herman ◽  
...  

The measurement of radioactive fission products from nuclear events has important implications for nuclear data production, environmental monitoring, and nuclear forensics. In a previous paper, the authors reported the optimization of an intra-group lanthanide separation using LN extraction resin from Eichrom Technologies®, Inc. and a nitric acid gradient. In this work, the method was demonstrated for the separation and quantification of multiple short-lived fission product lanthanide isotopes from a fission product sample produced from the thermal irradiation of highly enriched uranium. The separations were performed in parallel in quadruplicate with reproducible results and high decontamination factors for 153Sm, 156Eu, and 161Tb. Based on the results obtained here, the fission yields for 144Ce, 153Sm, 156Eu, and 161Tb are consistent with published fission yields. This work demonstrates the effectiveness of the separations for the intended application of short-lived lanthanide fission product analysis requiring high decontamination factors.


Materials ◽  
2021 ◽  
Vol 14 (5) ◽  
pp. 1267
Author(s):  
David Längauer ◽  
Vladimír Čablík ◽  
Slavomír Hredzák ◽  
Anton Zubrik ◽  
Marek Matik ◽  
...  

Large amounts of coal combustion products (as solid products of thermal power plants) with different chemical and physical properties cause serious environmental problems. Even though coal fly ash is a coal combustion product, it has a wide range of applications (e.g., in construction, metallurgy, chemical production, reclamation etc.). One of its potential uses is in zeolitization to obtain a higher added value of the product. The aim of this paper is to produce a material with sufficient textural properties used, for example, for environmental purposes (an adsorbent) and/or storage material. In practice, the coal fly ash (No. 1 and No. 2) from Czech power plants was firstly characterized in detail (X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy with energy dispersive X-ray analysis (SEM-EDX), particle size measurement, and textural analysis), and then it was hydrothermally treated to synthetize zeolites. Different concentrations of NaOH, LiCl, Al2O3, and aqueous glass; different temperature effects (90–120 °C); and different process lengths (6–48 h) were studied. Furthermore, most of the experiments were supplemented with a crystallization phase that was run for 16 h at 50 °C. After qualitative product analysis (SEM-EDX, XRD, and textural analytics), quantitative XRD evaluation with an internal standard was used for zeolitization process evaluation. Sodalite (SOD), phillipsite (PHI), chabazite (CHA), faujasite-Na (FAU-Na), and faujasite-Ca (FAU-Ca) were obtained as the zeolite phases. The content of these zeolite phases ranged from 2.09 to 43.79%. The best conditions for the zeolite phase formation were as follows: 4 M NaOH, 4 mL 10% LiCl, liquid/solid ratio of 30:1, silica/alumina ratio change from 2:1 to 1:1, temperature of 120 °C, process time of 24 h, and a crystallization phase for 16 h at 50 °C.


1973 ◽  
Vol 248 (23) ◽  
pp. 8130-8136 ◽  
Author(s):  
David O. Lambeth ◽  
Kenneth L. Campbell ◽  
Robert Zand ◽  
Graham Palmer

Molecules ◽  
2021 ◽  
Vol 26 (15) ◽  
pp. 4525
Author(s):  
Franziska Schachinger ◽  
Hucheng Chang ◽  
Stefan Scheiblbrandner ◽  
Roland Ludwig

The accurate determination of analyte concentrations with selective, fast, and robust methods is the key for process control, product analysis, environmental compliance, and medical applications. Enzyme-based biosensors meet these requirements to a high degree and can be operated with simple, cost efficient, and easy to use devices. This review focuses on enzymes capable of direct electron transfer (DET) to electrodes and also the electrode materials which can enable or enhance the DET type bioelectrocatalysis. It presents amperometric biosensors for the quantification of important medical, technical, and environmental analytes and it carves out the requirements for enzymes and electrode materials in DET-based third generation biosensors. This review critically surveys enzymes and biosensors for which DET has been reported. Single- or multi-cofactor enzymes featuring copper centers, hemes, FAD, FMN, or PQQ as prosthetic groups as well as fusion enzymes are presented. Nanomaterials, nanostructured electrodes, chemical surface modifications, and protein immobilization strategies are reviewed for their ability to support direct electrochemistry of enzymes. The combination of both biosensor elements—enzymes and electrodes—is evaluated by comparison of substrate specificity, current density, sensitivity, and the range of detection.


2021 ◽  
Vol 55 (6) ◽  
pp. 3976-3987
Author(s):  
Cong Luo ◽  
Manasa Sadhasivan ◽  
Juhee Kim ◽  
Virender K. Sharma ◽  
Ching-Hua Huang

2021 ◽  
Vol 7 (3) ◽  
pp. eabd9954 ◽  
Author(s):  
Chenxi Li ◽  
Jan Krohn ◽  
Martina Lippe ◽  
Ruth Signorell

Gas phase nucleation is a ubiquitous phenomenon in planetary atmospheres and technical processes, yet our understanding of it is far from complete. In particular, the enhancement of nucleation by the addition of a more volatile, weakly interacting gaseous species to a nucleating vapor has escaped molecular-level experimental investigation. Here, we use a specially designed experiment to directly measure the chemical composition and the concentration of nucleating clusters in various binary CO2-containing vapors. Our analysis suggests that CO2 essentially catalyzes nucleation of the low vapor pressure component through the formation of transient, hetero-molecular clusters and thus provides alternative pathways for nucleation to proceed more efficiently. This work opens up new avenues for the quantitative assessment of nucleation mechanisms involving transient species in multicomponent vapors.


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