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The method of the atomic emission spectrometry with an excitation in the inductively coupled plasma ICP-AES has been applied to the simultaneous analysis of the elements: Al, Cd, Cr, Cu, Fe, Li, Mg, Mn, Ni, P, Pb, S, Sr and V in the tobacco leaves samples CTA-OTL-1. The spectrometric analyses have been carried out on the emission spectrometer Spectroflame ICP M. About 300 mg of the sample and 1 cm3 of the concentrated HNO3 acid have been sealed in the quartz tube and mineralized by the pressure method. Since the ICP-AES technique is the most suitable to the direct analysis of the solutions, the main problem to solve was a mineralization of the sample. An application of the HNO3 acid alone did not give satisfactory results--unsolved residue remained. As a consequence the results for Mg, Ni, Pb were too low, whereas for the Al-nearly twice lower than the respective values given in the sample reference data. It has been observed that an addition of the conc. HF acid helps to dissolve the residue and, consequently, the optimalization of the mineralization process in the presence of the HNO3-HF mixture has been carried out. The results show that the appropriate amount of the HF acid to be added is 0.25 cm3. The other methods of mineralization using various mixtures of acids did not give good results. Only HNO3-HF mixture used in appropriate proportions give results in agreement with provided sample characteristics.(ABSTRACT TRUNCATED AT 250 WORDS)
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PMID:[Use of the ICP-AES method for multi-element analysis of tobacco leaves]. 748 4

The lowest possible sample weight for performing multielemental trace element analysis on environmental and biological samples by ICP-MS has been investigated. The certified reference materials Bovine Liver NIST SRM 1577b, Human Hair NCS DC 73347 and Oriental Tobacco Leaves CTA-OTL-1 were applied at sample weights (1, 5, 20 and 50 mg aliquots, n = 10) which were significantly lower than those recommended with most recoveries in the range of 95-110%. Samples were digested in a mixture of nitric acid, hydrogen peroxide and hydrogen fluoride by closed-vessel microwave digestion. Multielemental analysis was performed with an optimized ICP-QMS method. Aqueous standard solutions were applied for external calibration with rhodium as the internal standard element. The detection limits varied between 0.02-0.38 microg/g for Li, Na, Cr, Mn, Ni, Cu, Zn, Sr, Cd, Ba and Pb, and up to 1.92 microg/g for Mg, Al, Ca, Fe and Ni. Digested human plasma samples were spiked with multielemental solution (0.5-10 microg/L) to test the analytical method and the recoveries were 95-105% for most analytes. Our results show that in the case of homogeneous SRMs it is possible to use them in very low amounts (1-5 mg) for method development and quality control.
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PMID:Multielemental analysis in small amounts of environmental reference materials with inductively coupled plasma mass spectrometry. 1122 66

Application of microwave assisted extraction for the decomposition and dissolution of plant samples for trace metal determination by ICP-AES was examined. Dried onion, leaves of spinach beet and three reference materials CTA-OTL-1, CTA-VTL-2 and CL-1 were analyzed. Water, EDTA and hydrochloric acid (0.01, 0.10 and 1.0 M, respectively) were used as leaching solutions. The extraction efficiency was investigated by comparison of the results with those obtained after microwave wet digestion. HCl was found to be very suitable for quantitative extraction of B, Ba, Cd, Cu, Mn, Ni, Pb, Sr and Zn from the samples. For reference materials, the measured concentrations are well consistent with the certified values. The use of EDTA led to a complete extraction of B, Cd, Ni, Pb, Sr and Zn. Water was found to be a good leaching solution for boron. For extraction with HCl and EDTA, the RSD values for the concentrations measured were below 8% for most of the elements.
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PMID:Microwave assisted extraction for trace element analysis of plant materials by ICP-AES. 1122 16

The possibilities for universal calibration based on multi-element aqueous standard solutions and graphite laboratory reference materials (graphite standards) for the electrothermal vaporization inductively coupled plasma optical emission spectrometric (ETV ICP OES) determination of Al, B, Ba, Cd, Co, Cr, Cu, Fe, Mn, Ni, P, Pb, S, Sr, Ti, V, and Zn in plant materials were investigated. A commercially available state-of-the-art ETV device was coupled with an Echelle ICP spectrometer equipped with a charge-injection-device (CID) camera for spectral detection. The transition area between transport tube and ETV graphite tube and the gas streams for inner gas, bypass gas, and modifier gas were optimized to achieve best transport efficiencies. The influence of four gaseous modifiers (CCl4, CHCl3, CCl2F2, and C3H8) added to the inner gas was studied. Five reference materials (RM P-Alfalfa, Lucerne; NIES CRM No.9 "Sargasso"; CTA-VTL-2 Virginia Tobacco Leaves; NIST SRM 1515 Apple Leaves; IAEA-V-10 Hay Powder) were used for method validation. If certified reference materials are not available, calibration against graphite standards or dried aqueous standard solutions is possible. Three carbonization procedures as sample pretreatment for the plant materials were investigated.
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PMID:Calibration possibilities and modifier use in ETV ICP OES determination of trace and minor elements in plant materials. 1946 19

Lanthanides represent an interesting group of elements which are steadily gaining importance in science and in industry. Literature data suggest that they may have a role in regulating cellular processes and also in agriculture enhancing plant growth. Only few instrumental methods like NAA, ICP-OES and ICP-MS have potential for the determination of low levels of all lanthanides, but in practice they often have to be combined with suitable separation/preconcentration methods to achieve maximum number of elements being determined and to assure good accuracy and precision. In this work an attempt has been made to compare the performance of both variants of NAA: purely instrumental activation analysis (INAA) and radiochemical mode (RNAA) with pre- and post-irradiation group separation for the determination of individual lanthanides with the special emphasis on rarely determined elements (Gd, Ho, Er, Tm, Lu). This has been done by the analysis of two reference materials with different matrices viz. biological (CTA-OTL-1) and mineral (CTA-FFA-1). The results are compared with those obtained by ion chromatography (IC) employing the same lanthanide group preseparation scheme as in the case of RNAA.
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PMID:Comparison of performance of INAA, RNAA and ion chromatography for the determination of individual lanthanides. 1980 83

Al3+ heteroions have been incorporated into the silicate layers of Na-RUB-18 in three different molar ratios Si/AlICP (22, 40 and 42) through a post-synthesis procedure under hydrothermal conditions. Systematic characterization (XRD, 29Si NMR, 27Al NMR and SEM) showed that these Na-[Al]-RUB-18 layered aluminosilicates are free from impurities, and the aluminum did not affect the crystallinity of the material, and also did not change its morphology. 27Al NMR showed that aluminum was incorporated in the tetrahedral position and the layered sample with molar ratio Si/AlICP = 22 has also displayed octahedral coordination. These layered aluminosilicates which consist of lamella stacking in the c direction had their interlayer space expanded by ion exchange with CTA+. The swollen samples were pillared with TEOS, as the SiO2 pillar precursor, and octylamine, as the hydrolyzing agent and co-surfactant. Pillared materials presented type IV isotherms with a BET surface area in the range of 223-323 m2 g-1 and mesoporous with 2-4 nm, while their layered precursors Na-[Al]-RUB-18 showed type II isotherms with a BET surface area in the range of 7-12 m2 g-1. Additionally, the acidity present in the layers of these pillared solids was proved by in situ ethanol dehydration monitored by FTIR.
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PMID:2D-to-disguised 3D materials with built-in acid sites: H+-[Al]-RUB-18. 2882 29