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Liquid ammonia, trialkyl phosphites, and especially trialkylphosphines, are very powerful electron-pair donor solvents with soft bonding character. The solvent molecules act as strongly coordinating ligands towards mercury(ii), interacting strongly enough to displace halide ligands. In liquid ammonia mercury(ii) chloride solutions separate into two liquid phases; the upper contains tetraamminemercury(ii) complexes, [Hg(NH(3))(4)](2+), and chloride ions in low concentration, while the lower is a dense highly concentrated solution of [Hg(NH(3))(4)](2+) entities, ca. 1.4 mol dm(-3), probably ion-paired by hydrogen bonds to the chloride ions. Mercury(ii) bromide also dissociates to ionic complexes in liquid ammonia and forms a homogeneous solution for which (199)Hg NMR indicates weak bromide association with mercury(ii). When dissolving mercury(ii) iodide in liquid ammonia and triethyl phosphite solvated molecular complexes form in the solutions. The Raman nu(I-Hg-I) symmetric stretching frequency is 132 cm(-1) for the pseudo-tetrahedral [HgI(2)(NH(3))(2)] complex formed in liquid ammonia, corresponding to D(S) = 56 on the donor strength scale. For the Hg(ClO(4))(2)/NH(4)I system in liquid ammonia a (199)Hg NMR study showed [HgI(4)](2-) to be the dominating mercury(ii) complex for mole ratios n(I(-)) : n(Hg(2+)) > or = 6. A large angle X-ray scattering (LAXS) study of mercury(ii) iodide in triethyl phosphite solution showed a [HgI(2)(P(OC(4)H(9))(3))(2)] complex with the Hg-I and Hg-P bond distances 2.750(3) and 2.457(4) A, respectively, in near tetrahedral configuration. Trialkylphosphines generally form very strong bonds to mercury(ii), dissociating all mercury(ii) halides. Mercury(ii) chloride and bromide form solid solvated mercury(ii) halide salts when treated with tri-n-butylphosphine, because of the low permittivity of the solvent. A LAXS study of a melt of mercury(ii) iodide in tri-n-butylphosphine at 330 K resulted in the Hg-I and Hg-P distances 2.851(3) and 2.468(4) A, respectively. The absence of a distinct I-I distance indicates flexible coordination geometry with weak and non-directional mercury(ii) iodide association within the tri-n-butylphosphine solvated complex.
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PMID:Structure of solvated mercury(II) halides in liquid ammonia, triethyl phosphite and tri-n-butylphosphine solution. 1841 56

A sensing layer for a chemically sensitive field-effect transistor (CHEMFET) based on a composite of camphorsulfonic acid (CSA)-doped polyaniline (PANI) and the room-temperature ionic liquid (IL) 1-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)-imide, BMI(Tf2N), has been developed and characterized for the sensing of ammonia gas. The work function responses of the cast films with and without IL were analyzed by "stepwise" changes of ammonia gas concentration from 0.5 to 694 ppm in air as a function of the mole fraction of IL to PANI. The PANI x CSA/BMI(Tf2N) layers showed enhanced sensitivities, lower detection limits, and shorter response times. There is experimental evidence that PANI forms a charge-transfer complex with imidazolium cation.
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PMID:Chemically sensitive field-effect transistor with polyaniline-ionic liquid composite gate. 1845 15

Well-dispersed magnesium hydroxide nanoplatelets were synthesized by a simple water-in-oil (w/o) microemulsion process, blowing gaseous ammonia (NH(3)) into microemulsion zones solubilized by magnesium chloride solution (MgCl(2)). Typical quaternary microemulsions of Triton X-100/cyclohexane/n-hexanol/water were used as space-confining microreactors for the nucleation, growth, and crystallization of magnesium hydroxide nanoparticles. The obtained magnesium hydroxide was characterized by field-emission scanning electron microscopy (FESEM), high-resolution transmission election microscopy (HRTEM), X-ray powder diffraction (XRD), laser light scattering, Fourier transform infrared spectroscopy (FT-IR), and thermogravimetric analysis-differential scanning calorimetry (TGA-DSC). The mole ratio of water to surfactant (omega(0)) played an important role in the sizes of micelles and nanoparticles, increasing with the increase of omega(0). The compatibility and dispersibility of nanoparticles obtained from reverse micelles were improved in the organic phase.
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PMID:Magnesium hydroxide nanoparticles synthesized in water-in-oil microemulsions. 1851 Oct 61

Methanogenesis was studied in downflow stationary fixed-film bioreactors. The support materials in this study included ceramic Raschig rings, hardwood chips, and sized charcoal. The performances of these support materials have been compared using both synthetic acid mixture and acid products obtained from paper mill sludge. Woodchips appeared to be the most promising support material: The maximum methane productivity of 3.56 L/L day at a nominal retention time of 0.78 day was obtained using initial total acid concentrations of 9.125 g/L. Higher productivity was achieved at the cost of efficiency of the process in terms of conversion of acids. From nitrogen balances, it was deduced that ammonia supplemented methane generation by supplying hydrogen for there duction of carbon dioxide.An ionic balance was developed to ascertain the relationship between the composition and the pH of the liquid and the mole fraction of carbon dioxide in the gas phase. From these ionic balance equations, it was possible to predict the gas phase composition at various retention times. The maximum error between the computed and the experimental values was less than 13%.
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PMID:Methanogenesis from volatile fatty acids in downflow stationary fixed-film reactor. 1858 14

A simple extractive spectrophotometric method has been described for the determination of metribuzin herbicide. Metribuzin was reacted with copper and a stable complex in the presence of ammonia (0.2M) at pH 10.5 was formed. The resulting yellow coloured complex was extracted in chloroform and showed absorption maxima at 340 nm. Beer's law was obeyed in the range of 0.8-25 microg mL(-1) with molar absorptivity of 5.67 x 10(3)L mol(-1)cm(-1). The composition of the complex was studied by Job's method of continuous variation and the results indicated that the mole ratio of metribuzin:Cu(2+) is 2:1. The optimum reaction conditions for complexation and other analytical parameters were evaluated. A two-level factorial design was also used to determine the effect of different parameters and their interaction on metribuzin:Cu(2+) complex formed. The method was successfully applied for the determination of metribuzin in commercial formulations and real samples.
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PMID:Extractive spectrophotometric method for determination of metribuzin herbicide and application of factorial design in optimization of various factors. 1893 May 95

A procedure for the determination of the sum of metals, which are extractable with dithizone, in gallium arsenide is given. After the dissolution of the sample the impurities are extracted with several portions of 10(-4)M dithizone in carbon tetrachloride, gallium being screened by tartrate ion. The excess of the reagent is extracted into 0.1M aqueous ammonia and after stripping into carbon tetrachloride the dithizone is determined by spectrophotometric extractive titration. The effect of pH is considered. The limit of detection, based on the evaluation of twenty blanks, is 2.30 x 10(-8) mole, the equivalent of 1.50 mug of zinc.
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PMID:Spectrophotometric extractive titrations-II Determination in gallium arsenide of the sum of metals extractable with dithizone. 1895 19

The thermal decomposition of copper tetra-ammine sulphate monohydrate has been investigated by a combined derivatographic and thermo-gas-titrimetric method. It has been found that decomposition starts with splitting off of the water of crystallization and only after part of this water has departed does stepwise release of ammonia begin. First two moles, then one and finally again one mole of ammania (per mole of compound) are released. It has been established that a small amount of sulphur trioxide splits off during the last decomposition step, and that about 20 % of the last ammonia to be released is thermally decomposed.
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PMID:Combined derivatographic and thermo-gas-titrimetric examination of the thermal decomposition of copper tetra-ammine sulphate monohydrate. 1896 Aug 57

Xylenol Orange and mercury(II) react in the presence of various bases, such as hexamine, pyridine and ammonia, to form ternary complexes, which conform to Beer's law. The 1:1:1 Hg(II)/XO/ base complex at pH 6.1 has an absorption maximum at 590 nm and a molar absorptivity of 2.2 x 10(5) l.mole(-1).cm(-1). In the absence of the base the Hg(II)(XO)(2) complex at pH 7.5 and 580 nm has a molar absorptivity of 1.7 x 10(5) l.mole(-1).cm(-1). Interferences are discussed.
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PMID:Reaction of mercury(II) and xylenol orange-III: determination of microamounts of mercury. 1896 73

Conditions for the extraction of the thiocyanate complex of palladium by polyether-type polyurethane foam are reported. Distribution ratios of more than 10(6) with a capacity of about 0.8 mole per kg of foam were obtained. The palladium could be rapidly recovered from the foam with high efficiency by use of ammonia solution. The efficiency of palladium extraction depends on how well the cation associated with the complex fits into the polyether segment of the polyurethane foam.
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PMID:Extraction of palladium thiocyanate with polyurethane foam. 1896 74

Cobalt reacts with N-(dithiocarboxy)sarcosine (DTCS) to form a 1:3 Co:DTCS complex which is so stable that after its formation no decomposition occurs even in 4M hydrochloric acid. The complex is sorbed on a column of Amberlite XAD-4 copolymer from an acidic solution and eluted with 10 ml of a 1:1:3 v v mixture of 1.0M ammonia solution (pH = 9), 0.1M EDTA and methanol. The absorbance of the eluted chelate is measured at 320 nm against water ( = 2.15 x 10(4) l.mole(-1).cm(-1)). The recovery of cobalt from 1 litre of tap-water or sea-water is quantitative. The effect of diverse ions can be eliminated by the addition of EDTA after chelation of the cobalt. The copper complex with DTCS is partly sorbed on the column because of its slow rate of decomposition by EDTA, but most of the copper chelate sorbed can be eluted with hydrochloric acid and any co-eluted with the cobalt chelate can be completely decomposed by heating the eluate. Cobalt enrichment factors of at least 100 are obtained, so the method is applicable to the determination of cobalt at the ng ml level.
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PMID:Preconcentration of cobalt with N-(dithiocarboxy)sarcosine and amberlite xad-4 resin. 1896 53


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