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Binding of metals in typical bath peat samples ("Grosses Gifhomer Moor", Sassenburg/North Germany) and their aqueous extracts was characterized by means of a multi-method approach. For that purpose a sequential extraction procedure based on peat-filled chromatography columns was developed. Water-soluble metal and DOM (dissolved organic matter) fractions were subdivided by use of a stepwise increased pH gradient (pH 3.8-5), finally by the chelator EDTA and 0.1 mol L(-1) hydrochloric acid. Metal fractions very strongly bound to peat were assessed by an aqua regia extraction. Metal determinations required were performed by atomic spectrometry methods (AAS, ICP-OES, and TXRF). The metal and DOM concentrations in the peat extracts varied significantly, depending on the natural variety of the peat matter under study (e.g., Al: 25-674, Cd: 0.05-0.2, Cu: 5-15.4, Fe: 77-1785, Mn: 21-505, Ni: 2-33, Pb: < 1, Zn: 9-715 (microg L(-1)); Na: 8-45, K: 1.3-14.9, Ca: 2-51, Mg: 1.1-7.9 (mg L(-1)); 26-73 mg L(-1) DOC). An increase of the pH increased the DOC (dissolved organic carbon) of the peat extracts, but hardly the concentration of heavy metals. The latter could only be re-mobilized by EDTA and dilute hydrochloric acid. Additional investigations of the peat extracts using tangential-flow ultrafiltration revealed that the heavy metals extracted at pH < 4 were predominantly dissociated. At higher pH (pH > 4.5) they were preferentially bound to macromolecular DOM. Moreover, using multistage ultrafiltration the size distribution of the DOM and their metal species was assessed.
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PMID:Metal distribution and binding in balneological peats and their aqueous extracts. 1149 67

Biogenic (e.g. phytochelatins, porphyrins, DOM) as well as anthropogenic (e.g. NTA, EDTA, phosphonates) chelators affect the mobility and cycling of heavy metals in environmental waters. Since such chelators can form strongly bound anionic heavy metal complexes that are stable and highly mobile, anion-exchange chromatography coupled to ICP-MS was investigated. A narrow bore HPLC system was connected to a micro concentric nebuliser for in-line sample introduction. A new chromatographic procedure based on a synthetic hydrophilic quaternary ammonium anion exchanger in combination with nitrate as a strong eluent anion, and gradient elution, provided high separation selectivity and a large analytical window. Low detection limits (nmol L(-1)) were achieved by on-column matrix removal and sample preconcentration. This allowed the method to be successfully applied to different environmental research areas. In ecotoxicological studies of heavy metal effects on algae low concentrations of metal EDTA complexes were determined in nutrient solutions without interference from high (buffer) salt concentrations. In groundwater, infiltrated by a polluted river, mobile metal EDTA species were observed. In river water of different pollution levels beside CuEDTA other anionic Cu-complexes were found in nmol L(-1) concentrations.
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PMID:Speciation of heavy metals in environmental water by ion chromatography coupled to ICP-MS. 1193 32

Transformations of metal species (particularly Al, Ca, Fe, Mg, Mn, Zn) in ageing humic hydrocolloids were studied, applying a competitive ligand and metal exchange approach. For this purpose, metal-containing hydrocolloids, freshly collected from humic-rich German bog lake waters (Hohlohsee (HO), Black Forest; Venner Moor (VM), Muensterland; Arnsberger Wald (AW), Northrhine-Westfalia) and conventionally pre-filtered through 0.45 microm membranes, were subjected on-site to an exchange with EDTA and Cu(II) ions, respectively, as a function of time. EDTA complexes gradually formed, metal fractions exchanged by Cu(II) (as well as free Cu(II) concentrations) were operationally discriminated by means of a small time-controlled tangential-flow ultrafiltration unit (nominal cutoff: 1 kDa). Metal and DOM (dissolved organic matter) fractions obtained this way were determined off-site using instrumental methods (AAS, ICP-OES, carbon analyzer). After weeks of storage, the collected hydrocolloids were studied again by this approach. The EDTA availability of colloid-bound metals (particularly Al and Fe) exhibited different ageing trends, dependent on the sample (VM: decrease of Fe availability (98-76%), HO: increase of Fe availability (76-82%)). In contrast, the Cu(II) exchange equilibria of colloid-bound metals revealed merely low availability of Al (16-38%) and Fe (5-11%) towards Cu(II) ions, also dependent on ageing effects. In particular, the conditional copper exchange constants Kex obtained from the exchange between Cu(II) ions and available metal species (such as Ca, Mg, Mn, Zn) exhibited a strong decrease (by a factor of 2-100) during sample storage, indicating considerable non-equilibria complexation of these metal ions in the original bogwaters studied on-site.
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PMID:Transformations of metal species in ageing humic hydrocolloids studied by competitive ligand and metal exchange. 1521 28

We evaluated trends (2005-2013) and patterns of dissolved organic nitrogen (DON) and its ratio with dissolved organic carbon (DOC), DOC:DON in atmospheric deposition and soil solution of five Level II plots of the International Co-operative Programme on Assessment and Monitoring of Air Pollution Effects on Forests (ICP Forests) in Flanders, Northern Belgium. The primary aim was to confirm positive postulated trends in DON levels and DOC:DON under on-going recovery from acidification. The DON concentrations (0.95-1.41 mg L(-1)) and fluxes (5.6-8.3 kg ha(-1)y(-1)) in throughfall were about twice as high compared to precipitation in the open field (0.40-0.48 mg L(-1), 3.0-3.9 kg ha(-1)y(-1)). Annual soil profile leaching losses of DON varied between 1.2 and 3.7 kg ha(-1)y(-1). The highest soil DON concentrations and fluxes were observed beneath the O horizon (1.84-2.36 mg L(-1), 10.1-12.3 kg ha(-1)y(-1)). Soil solution concentrations and fluxes of DON showed significant increasing trends. Temporarily soil solution DOC:DON rose following an exceptionally long spring drought in 2007, suggesting an effect of drying and rewetting on DOM composition. Further research is needed to test the dependence of DON and DOC:DON on factors such as latitude, forest cover, length of the growing season, hydrology and topography. Nonetheless, even with considerable variation in soil type, level of base saturation, and soil texture in the five included ICP Forests Level II plots, all data revealed a proportionally larger positive response of DON flux than DOC to recovery from acidification.
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PMID:Increasing trends of dissolved organic nitrogen (DON) in temperate forests under recovery from acidification in Flanders, Belgium. 2690 98