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Spectrophotometric investigation of the deep blue colored, water-soluble complex of
1. Stability constant and free energy of formation of Cu-NMS complex at 30 ± 1 °C
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11.
The oxidation of glycolaldehyde with hexaquomanganese(III) ions in a noncomplexing perchloric acid medium was studied. The optimum conditions have been found for analytical use of the reaction. The recommended procedure is based on the oxidation of the test substance with the oxidant in the absence of atmospheric oxygen and back-titration of the unconsumed reagent with ferrous sulfate.
2. Accuracy and Reproducibility of the Determination of Glycolaldehyde with Hexaquomanganese(III) Ions in a Noncomplexing Perchloric Acid Medium
MethodlogKsΔF (Kcal/mole)
Mukherji and Dey (4)4.11?5.70
Subhrana and Raghavrao (6)4.80?6.66
Taken (μg)Found (μg)aStandard deviation (μg)
75174812
1501148515
225221927
a
The values are the average of seven determinations, from which the standard deviation value was calculated.
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12.
A simple, rapid, and accurate method for determination of total sulfur and inorganic sulfate in biological materials by barium chloranilate colorimetry is presented. Criteria required
3. Precision of S Determination, Whole Blood, Blood Plasma, TCA Extracts, and Urine
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14.
A polarographic method for the determination of antimony in lead-antimony alloys has been developed. It was found that the interference due to the presence of varying concentrations of lead and hydrochloric acid would be eliminated by the addition of potassium chloride.
t001. The method gave satisfactory results within the range:
SampleDeterminationsMean (μg)SD (μg)
Whole blood10100421
Blood plasma105434
TCA extracts10242
Urine (totals)1059831
Urine (inorganic S)10374.419
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15.
Conditions were found under which manganese(III) acetate can be electrochemically generated at a platinum anode with 100% current efficiency. It was found that even traces of
5. Time Dependence of the Consumption of the Oxidizing Reagent in the Indirect Determination of Hydroquinone with Coulometric Generated Manganese(III) Acetate
Hydrochloric acid4 — 8M
Lead0 — 0.03M
Antimony0 — 0.002M
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16.
A kinetic method is described for the determination of trace amounts of magnesium in the presence of calcium. The procedure is based on the inhibition of the manganese(II) catalyzed aerial oxidation of 1,4-dihydroxyphthalimide dithiosemicarbazone reaction by
2. Effect of Transition Metalsa
Time (min)05103060
Consumption of Mn(III) (mol/mol)2.001.992.002.012.00
Transition metalConcentration (M)Percentage inhibitionMg(II) found (×l05M)
Fe(II)3.6.10?554.14.62
Fe(III)3.6.10?547.84.48
Co(II)3.4.10?550.04.53
Ni(II)3.4.10?550.04.53
Cu(II)3.1.10?552.04.56
Zn(II)3.0.10?554.14.62
Cd(II)1.7.10?552.04.56
Hg(II)9.9.10?645.84.44
Sn(II)2.1.10?650.04.52
Pb(II)1.2.10?654.14.62
a
Conditions: 4.53.10?5M Mg(II), 35 ng Mn ml?1, 0.429 M ammonia, 1.6.10?4M OH-PDT.
3. Determination of Magnesium in Natural Waters
Mg(II) found (M)b
Natural waterCa(II) presentaAtomic absorption
sampleMKinetic absorptionmethod
Commercial3.45 · 10?41.65 · 10?31.74 · 10?3
Commercial5.46 · 10?41.57 · 10?41.81 · 10?4
Untreated6.13 · 10?42.16 · 10?42.40 · 10?4
Treated4.95 · 10?41.93 · 10?42.17 · 10?4
a
EDTA titration less the magnesium.
b
Average of three separate determinations. traces of magnesium(II). The reaction is followed spectrophotometrically by measuring the rate of change in absorbance at 594 nm. The calibration graph (percentage inhibition vs magnesium concentration) is linear in the range 329–535 · 10?5M with an accuracy and precision of 1.2%. The method has been applied to the determination of magnesium in natural waters at low concentrations.
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17.
A sensitive spectrofluorimetric procedure with rhodamine B in the presence of aluminum chloride is given for determining submicrogram and microgram quantities of thallium in silicate rocks. Samples are decomposed with a mixture of hydrofluoric and nitric acids and then treated with hydrochloric acid. Thallium is extracted as its dithizonate with chloroform from an alkaline medium containing ascorbate, citrate, and cyanide and then back-extracted with dilute nitric acid. After destruction of the organic matter and treatment with bromine, hydrochloric acid, aluminum chloride, and rhodamine B, the
T001. Determination of thallium in U.S. Geological Survey standard rocks by different laboratories
Thallium (p.p.m.)MethodRef.
G-1W-1
1.060.102Neutron activation analysis1
1.080.121, 0.116Neutron activation analysis2
1.30.17Neutron activation analysis3
1.30.11Spectrographic4
0.105–0.110Flameless atomic absorption spectroscopy5
1.3a0.13a19
1.24b0.110b20
1.09 ± 0.010.110 ± 0.005SpectrofluorimetricPresent method
a
Values given by Fleischer.
b
Average value given by Flanagan. fluorescence intensity of the benzene-extracted rhodamine B chlorothallate is measured. The limit of determination is approximately 0.01 p.p.m. for a 1.0-g sample. The thallium contents of U.S. Geological Survey standard rocks G-1 and W-1 were found to be 1.09 ± 0.01 and 0.110 ± 0.005 p.p.m., respectively.
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18.
Sulfite ion reacts with mercury(II) ion in acid solution to form the mercury(I) ion. The reaction is rapid and quantitative. The mercury(I) ion absorbs at 237 nm with a molar
5. Beer's law Data for Sulfite Complexes of Covalent Mercury(II) Compounds
SO2 (ppm)?HgCl2a?HgBr2?Hg(Ac)2b?Hg(SCN)2
2.012,50010,00010,0009,200
4.012,50011,50010,0009,000
6.012,50011,50010,0009,200
8.012,00011,00010,5009,800
a
Molar absorptivity based on sulfite ion at 230 nm. Solution was 6.86 buffer.
b
Mercuric acetate solutions seemed to be somewhat unstable. absorptivity of about 25,000. The absorbance is linear over a range of approximately 0.5–5.0 ppm as SO2. Covalent mercury(II) compounds form a complex with sulfite, Hg(SO3)22?, which absorbs at 230 nm and shows a linear response over a range of 1–8 ppm as SO2.
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19.
A potentiometric method is described for the determination of thiosemicarbazones involving the formation of a complex with Ag(I). This method is proposed for thiosemicarbazones of the following carbonyl compounds: salicylaldehyde, p-hydroxybenzaldehyde, benzaldehyde, picolinaldehyde, 6-methylpicolinaldehyde and p-dimethylaminebenzaldehyde. Stability constants of the complexes are determined by Ringbom and Harju's method.
FIG. 2. Variation of pAg + logαPAT (H) + log ([Ag?PAT)]/[PAT])
2. Formation Constants of the Silver-Thiosemicarbazonates
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20.
In summary, this report describes the conditions under which luminol has been utilized to measure phagocytosis-associated metabolic events in activated human PMNs and rabbit and dog alveolar macrophages. We feel that this system may have wide applicability to both clinical and experimental situations. Some possible applications are shown in the following table.
Potential Applications of Luminol-Amplified Chemiluminescence
ThiosemicarbazoneLog Kf
-Benzaldehyde15.5 ± 0.1
-Picolinaldehyde14.0 ± 0.
-6-Methylpicolinaldehyde14.5 ± 0.
-Salicylaldehyde15.7 ± 0.1
-p-Hydroxybenzaldehyde15.6 ± 0.
-p-Dimethylaminebenzaldehyde17.2 ± 0.1
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Cell typeApplications
Human polymorphonuclear leukocytes(1) Detection of bactericidal defects, particularly chronic granulomatous disease
(2) Detection of host opsonic defects (both immunoglobulin and complement ?C3b opsonic defects).
(3) Analysis of drug effects on host cellular and opsonic defenses (9,11).
(4) Characterization of bacteria or other particulate matter in terms of ability to generate opsonic activity and/or be ingested by phagocytic cells (3,7).
Alveolar macrophages(1) Detection of environmental pollutant effects on respiratory defense mechanisms (against both particulate and soluble matter).
(2) Analysis of drug effects on respiratory defense mechanisms, particularly drugs administered in the treatment of respiratory diseases.
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