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The adsorption behavior of gold (Au), silver (Ag) and palladium (Pd) on nanometer-size titanium dioxide (NSTD) at low concentrations was studied using inductively coupled plasma atomic emission spectrometry (ICP-AES). A preconcentration procedure of the analytes was carried out using NSTD as a solid-phase extractant before their determination by ICP-AES. The optimum conditions for adsorption were studied in detail, and under the condition that Au, Ag and Pd ions could be adsorbed and recovered quantitatively. The static adsorption capacities of Au, Ag and Pd on NSTD were 22.63, 14.06 and 11.82 mg/g, respectively. For the elution of gold, silver and palladium, a mixture of 5% thiourea solution and 3 mol L(-1) HNO3 was used. The parameters tested included: pH conditions, contact time of the analytes with NSTD, flow rate, adsorption capacity and sorption kinetics. According to the definition of IUPAC, the detection limits (3sigma) of this method for Au, Ag and Pd with an enrichment factor of 50 were (0.016), (0.006) and (0.012) microg mL(-1), respectively, the relative standard deviations (RSD) were 8.7%, 4.5% and 7.4%, respectively (n = 6). Some geological samples were determined with satisfactory results.
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PMID:Adsorption behavior of noble metal ions (Au, Ag, Pd) on nanometer-size titanium dioxide with ICP-AES. 1459 9

Ten tumor tissue and normal tissue around tumors were collected from the patients with lung cancer. After digested by mixed acids(HNO3:HClO4 = 10:1), 15 rare-earth elements (REEs) in the tissue were measured directly by ELAN 5000 ICP-MS. Tissue levels and distribution of 15 REEs were analyzed and compared with those in healthy human lung tissue measured in the same condition. Re (rhenium) was used as an internal standard element to compensate for matrit inhibition and sensitivity drift. Recoveries of standard addition for REEs was 92.9%-111.3% and the precision was 0.96%-3.07%. Results showed that levels of 15 REEs in normal tissues around the tumor was as 2.07-2.51 times high as those in the tumor tissue, while the REE distribution curves of them was similar. There were positive abnormalities of Ce and negative abnormalities of Eu in REE curves of both tissue after chondrite-normalized. Compared REE level and distribution pattern in normal tissue with those in tumor tissue from patients with lung cancer, it was found that contents of light REE in lung tissue of health human were much higher while the contents of media and heavy REE were much lower. LREE/HREE in the tumor tissue and normal tissue with lung cancer and health human lung tissue were 12.99, 13.72 and 44.11 respectively. This study suggested that there might be light REEs accumulation in human lung tissue compared with REE distribution in the air particulates and soil. Light REEs accumulation in the lung of healthy people was more obviously than that in patients with lung cancer.
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PMID:[Levels and distribution of 15 rare earth elements in tumor and normal lung tissue from the patients with lung cancer]. 1465 Jan 79

The concentrations and distributions of chemical elements (Ag, Al, As, Au, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, Hg, K, La, Mg, Mn, Mo, Na, Ni, P, Pb, S, Sb, Sc, Se, Sr, Te, Th, Ti, Tl, U, V, W and Zn) were studied in till, humus and urban soil in Jakobstad, a small town (20,000 inhabitants) in W. Finland. The analyses were performed with ICP-MS after aqua regia leaching of till (n = 37), urban topsoil (n = 32) and subsoil (n = 32), and HNO3 leaching of humus (n = 37). The till and humus samples, collected at the same sites, were divided into urban and rural samples. The urban till was not significantly enriched in metals. In contrast, a majority of the elements occurred in higher concentrations in the urban than the rural humus samples. Statistical and spatial interpretations of the humus data revealed that traffic (Pb, V and Ni), metal industry (Pb, Zn, Bi, Sb and Cr), an abandoned shooting range (Pb and Sb) and other sources contribute to higher metal levels in the urban humus. The urban soil samples were collected at parks, yards, abandoned industrial sites, roadsides, etc. The topsoil samples were enriched in most elements, also by elements not enriched in the urban humus (e.g. Cd). At several sites, the concentrations far exceeded the limit concentrations for contaminated soils in Finland. A large variety of sources were identified or indicated.
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PMID:Urban geochemistry: a multimedia and multielement survey of a small town in northern Europe. 1474 Sep 85

In order to elucidate the distributions of the elements among the particulate and dissolved fractions in pond water, major-to-ultratrace elements in different sizes of particles as well as in the filtrate passed through the 0.05 microm filter were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The different sizes of particle samples (ca. 100-300 microg each) were collected on the membrane filters with pore sizes of 10, 3.0, 1.2, 0.4, 0.2 and 0.05 microm, respectively, by sequential fractionation. As a result, about 40 elements in different sizes of particles could be determined by ICP-AES and ICP-MS, after acid digestion using HNO3/HF/HClO4. Then, the fractional distribution factors of major-to-ultratrace elements among the particulate and dissolved fractions were estimated from the analytical results. The total contents of Al, Fe, Ti, REEs (rare earth elements), Bi, Pb and Ag in the particulate fractions (larger than 0.05 microm) were more than 80-90%, while those of Ca, Sr, Cs, W, Ba, Mn and Co in the dissolved fraction, which corresponded to the filtrate passed through the 0.05 microm membrane filter, were more than 80%. It was further found that the fractional distributions of Cu and Zn in the dissolved fraction were ca. 50%. In addition, the enrichment factors (EFs) of the elements in the particulate fractions with particle sizes of 3.0-10 microm and 0.05-0.2 microm were estimated to elucidate their geochemical characteristics in natural water.
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PMID:Distributions of major-to-ultratrace elements among the particulate and dissolved fractions in natural water as studied by ICP-AES and ICP-MS after sequential fractionation. 1475 54

Adopting strict cleanroom procedures, ice samples from the Canadian High Arctic have been analyzed for Pb concentrations and Pb isotopes (206Pb, 207Pb, 208Pb) using ICP-SMS. The detection limit for Pb (0.06 pg g(-1)) was approximately 2 orders of magnitude lower than the lowest concentration of Pb in the ice samples (range, 4.3-1660 pg g(-1); median, 45 pg g(-1)). Acidification of ice samples with high-purity HNO3 for stabilization purposes contributed only 0.004 pg of Pb g(-1), which is an insignificant source of Pb. Using a new sample introduction system consisting of a heated (140 degrees C) minicyclonic spray chamber and a Peltier cooled condenser (2 degrees C) and by replacing the conventional sample cone with a high-performance cone, signal intensities for Pb were increased by approximately 1 order of magnitude. Thus, it was possible not only to measure Pb isotope ratios directly using ICP-SMS but also to achieve reasonable precision (approximately 0.2%) at low picogram per gram concentrations of total Pb. This precision is comparable to that achievable by thermal ionization mass spectrometry at such low Pb concentrations, but the ICP-SMS requires much less sample volume (approximately 2 mL), needs no sample pretreatment, and therefore is considerably faster and less expensive than the conventional approach. Even though absolute Pb concentrations in two ice samples dating from 1974 and 1852 were very similar (9 and 6 pg g(-1)) their fundamentally different isotopic signature (206Pb/207Pb: 1.169 +/- 0.002 vs 1.147 +/- 0.003) clearly indicates different sources of Pb. The analytical procedures described here, therefore, offer great promise for fingerprinting the predominant sources of atmospheric Pb in polar snow and ice.
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PMID:Direct determination of lead isotopes (206Pb, 207Pb, 208Pb) in arctic ice samples at picogram per gram levels using inductively coupled plasma-sector field MS coupled with a high-efficiency sample introduction system. 1536 14

A technique using a flow injection microcolumn separation coupled with ICP-MS detection has been developed for the speciation of Al in drink samples. The retention behaviors of different Al species were studied with 8-hydroxyquinoline (8-HQ) loaded silylanization silica gel as the packing material and inorganic acid (HNO3) as the elution. The results indicated that in a pH range of 5.0 to 8.0, all labile monomeric Al species were retained on the microcolumn while nonlabile monomeric Al species were directly passed through the column. Various Al species after separation were detected by ICP-MS. The detection limit of 0.2 ng mL(-1) and a relative standard deviation (RSD) of 4.2% at 10 ng mL(-1) (n = 11) were achieved, and the recoveries for the spiked samples were 95-108%. The proposed method has been applied to the analysis of Al species in tea infusions, coffee, and tap waters with satisfactory results. The results obtained by this method were compared with that obtained by the cation exchange microcolumn separation and ICP-MS detection system, and some valuable conclusions were drawn.
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PMID:Speciation of aluminum in drink samples by 8-hydroxyquinoline loaded silylanization silica gel microcolumn separation with off-line ICP-MS detection. 1553 84

CuIn(1-x)Ga(x)Se2 [CIGS; x=Ga/(In+Ga)] thin films are among of the best candidates as absorber materials for solar cell applications. The material quality and main properties of the polycrystalline absorber layer are critically influenced by deviations in the stoichiometry, particularly in the Cu/(In+Ga) atomic ratio. In this work a simple, sensitive and accurate method has been developed for the quantitative determination of these thin films by inductively coupled plasma optical emission spectrometry (ICP-OES). The proposed method involves an acid digestion of the samples to achieve the complete solubilization of CIGS, followed by the analytical determination by ICP-OES. A digestion procedure with 50% HNO3 alone or in the presence of 10% HCl was performed to dissolve those thin films deposited on glass or Mo-coated glass substrates, respectively. Two analytical lines were selected for each element (Cu 324.754 and 327.396 nm, Ga 294.364 and 417.206 nm, In 303.936 and 325.609 nm, Se 196.090 and 203.985 nm, and Mo 202.030 and 379.825 nm) and a study of spectral interferences was performed which showed them to be suitable, since they offered a high sensitivity and no significant inter-element interferences were detected. Detection limits for all elements at the selected lines were found to be appropriate for this kind of application, and the relative standard deviations were lower than 1.5% for all elements with the exception of Se (about 5%). The Cu/(In+Ga) atomic ratios obtained from the application of this method to CIGS thin films were consistent with the study of the structural and morphological properties by X-ray diffraction (XRD) and scanning electron microscopy (SEM).
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PMID:Application of ICP-OES to the determination of CuIn(1-x)Ga(x)Se2 thin films used as absorber materials in solar cell devices. 1570 9

The geochemical fingerprint of sediment retrieved from the banks of the River Manzanares as it passes through the City of Madrid is presented here. The river collects the effluent water from several Waste Water Treatment (WWT) plants in and around the city, such that, at low flows, up to 60% of the flow has been treated. A total of 18 bank-sediment cores were collected along the course of the river, down to its confluence with the Jarama river, to the south-east of Madrid. Trace and major elements in each sample were extracted following a double protocol: (a) "Total" digestion with HNO3, HClO4 and HF; (b) "Weak" digestion with sodium acetate buffered to pH=5 with acetic acid, under constant stirring. The digests thus obtained were subsequently analysed by ICP-AES, except for Hg which was extracted with aqua regia and sodium chloride-hydroxylamine sulfate, and analysed by Cold Vapour-AAS. X-ray diffraction was additionally employed to determine the mineralogical composition of the samples. Uni- and multivariate analyses of the chemical data reveal the influence of Madrid on the geochemistry of Manzanares' sediments, clearly manifested by a marked increase in the concentration of typically "urban" elements Ag, Cr, Cu, Pb and Zn, downstream of the intersection of the river with the city's perimeter. The highest concentrations of these elements appear to be associated with illegal or accidental dumping of waste materials, and with the uncontrolled incorporation of untreated urban runoff to the river. The natural matrix of the sediment is characterised by fairly constant concentrations of Ce, La and Y, whereas changes in the lithology intersected by the river cause corresponding variations in Ca-Mg and Al-Na contents. In the final stretch of the river, the presence of carbonate materials seems to exert a strong geochemical control on the amount of Zn and, to a lesser extent, Cu immobilised in the sediments. This fact suggests that a variable but significant proportion of both elements may be susceptible to reincorporation in the aqueous phase under realistic environmental conditions.
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PMID:Geochemical fingerprints and controls in the sediments of an urban river: River Manzanares, Madrid (Spain). 1575 98

A method for determining trace Se in coal by microwave digestion and hydride generation ICP-AES is reported. The digestion system of HNO3-HCl-HF was evaluated. The hydride generation occurred in 3 mol x L(-1) hydrochloric acid media with 1% sodium tetrahydroborate as a reduction reagent. The experimental conditions of microwave digestion, prereduction, and interferences were investigated. This method is simple and rapid. The treatment method was applicable to Se and gave results that were in good agreement with the certified values of the standard reference material. Testing results showed that the detection limit was 0.3 microg x L(-1) and RSD was below 5%.
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PMID:[Determination of trace selenium in coal by microwave digestion and hydride generation ICP-AES]. 1575 97

Calcium is the necessity element in human body and its content has effect on exciting muscle or nerve. Calcium is important in the physiologic process of muscle or nervous reaction, nervous impulse transmission, heartbeat rhythm maintenance, blood solidification, cell coherence and so on. Determination of calcium element in Chinese medicine wild jujube seed decoction and radix puerariae was studied by ICP-AES after they were digested with HNO3-HClO4. The precision (RSD) is 1.7%. The average recovery of calcium in wild jujube seed decoction is 97.7% and in radix puerariae is 104.4%. Calcium was abundant in Chinese medicine and could play certain pharmacologic role in Chinese medicine. It is of important significance to assess the value of Chinese medicine by determination of calcium element in Chinese medicine with ICP-AES.
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PMID:[Study on the determination of calcium in Chinese medicine by ICP-AES]. 1576 36


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