Volatilization of metallic compounds from solutions in perchloric or sulfuric acid

Hoffman, J.I.; Lundell, G. E. F.

doi:10.6028/jres.022.030

Cited by 104 publications

(25 citation statements)

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“…The ranges of silver, tin, vanadium, lead, molybdenum, and cadmium concentrations were not obviously dissimilar for the Africans and the Americans, despite differences in their mean concentrations. In (4). The cause for the unsatisfactory titanium assay is not obvious.…”

Section: Part I Ofmentioning

confidence: 99%

Normal Concentrations of Some Trace Metals in Human Urine: Changes Produced by Ethylenediaminetetraacetate *

Hm¹,

Ef²

1959

J. Clin. Invest.

118

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Interest in the biologic role of trace elements prompted an investigation of their renal excretion. Preliminary qualitative analysis revealed that except for cobalt the entire first transition series of metals, namely, titanium, vanadium, chromium, manganese, iron, nickel and copper, were detectable in most human urines. In addition the heavier transition metals, molybdenum and silver, as well as the related metals, zinc, cadmium, tin and lead, were ordinarily present. A method was evolved by which the urinary concentrations of such metals could be quantitatively estimated. The procedure included initial chemical concentration followed by spectrographic analysis. Contamination was minimized by careful preparation of equipment and reagents. Since extraneous iron and copper were particularly difficult to avoid and since these two metals had frequently been studied by other techniques, no attempt was made to measure them spectrographically. The exclusion of significant positive contamination, the demonstration that the low renal excretion of cobalt permitted its use as an internal standard, and the determination of standard working curves and recovery data for each metal constituted the control data for the assay procedure. Estimations were less satisfactory for chromium and titanium than for the remaining nine metals.Collection and assay of 24 hour urines were performed in a standard manner. Such urines from normal persons served to indicate both the mean level and the variability of excretion for the nine trace metals which could be satisfactorily estimated. Daily differences in the renal excretion of metal as well as the effects produced by * Supported by grants-in-aid from the National Heart Institute of the United States Public Health Service, the American Heart Association, the Life Insurance Medical Research Fund and Abbott Laboratories.t Established Investigator, American Heart Association. extremes of urinary volume and pH were determined for 24 hour urines from one normal individual. A brief preliminary study was made of the metallic spectrum in single specimens of urine from hospitalized African natives. Finally, metal concentration was measured in consecutive 24 hour urines from hypercholesterolemic patients before, during and after the parenteral administration of the chelating agent, disodium calcium ethylenediaminetetraacetate, which had been observed to lower the level of cholesterol in human plasma (1). METHODSPrelimintary qutalitative uirinalysis. In order to select the metals to be assayed, 40 single urine specimens from different subjects were analyzed qualitatively. Half of. the samples were obtained from normal individuals and half from hospitalized patients with atherosclerosis and hypertension. The urines were evaporated to approximately one-twentieth of their original volume, after which most of the organic material was oxidized with hydrogen peroxide. The residues were then dried, mixed with an approximately equal amount of graphite, and burned to completion in a direct current arc. The ph...

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Section: Part I Ofmentioning

confidence: 99%

Normal Concentrations of Some Trace Metals in Human Urine: Changes Produced by Ethylenediaminetetraacetate *

Hm¹,

Ef²

1959

J. Clin. Invest.

118

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“…Germanium, boron, and molybdenum may accompany tin on digestion with nitric acid, and may distill [10] in part, but of these only molybdenum, which is uncommon in nonferrous alloys, would be precipitated by cupferron. Scherrer [11] found that with 100 mg of molybdenum originally present, 0.3 mg was found with the tin after one distillation, and only 0.01 mg after a second distillation.…”

Section: Discussion Of Procedures and Resultsmentioning

confidence: 99%

Determination of tin in nonferrous metals by distillation as bromide and precipitation with cupferron

Mogerman¹

1944

J. RES. NATL. BUR. STAN.

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A gravimetric method is described for the' determination of tin in copper-base and lead-base alloys. The procedure involves separation of the tin by distillation, precipitation with cupferron, and ignition to stannic oxide. Results obtained by applying the method to known amounts of tin and to a number of nonferrous alloys show that an accuracy to ± 0.2 mg can be expected for amounts of t in ranging from 0.05 to 0.24 g.

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“…The energy of the /3-radiation of "Mo is high enough to render ^-counting easy, and the intense y-radiation from the daughter 99m Tc in transient equilibrium makes y-counting straightforward. Based on methods and data reported by different authors [16][17][18][19][20][21][22] a radiochemical procedure was developed for the isolation of molybdenum from a fission mixture which allows the use of submilligram amounts of carrier. Molybdenum is adsorbed from 0.1 Μ nitric acid on an anion exchange column, and uranium and most of the fission products are removed by washing with the same solvent.…”

Section: B) Radiochemical Isolation Of the Fission Monitormentioning

confidence: 99%

“…The addition of phosphoric acid prevents loss of molybdenum by evaporation [20]. Several efficient methods for preparing oxalic-14 Cj acid are available, starting from 14 C-labeled sodium formate [1,2,3] or carbon dioxide [4,5].…”

Section: Appendixmentioning

confidence: 99%

Radiochemical Determination of Z35U Abundances by Activation Analysis

1966

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Volatilization of metallic compounds from solutions in perchloric or sulfuric acid

Cited by 104 publications

References 0 publications

Normal Concentrations of Some Trace Metals in Human Urine: Changes Produced by Ethylenediaminetetraacetate *

Normal Concentrations of Some Trace Metals in Human Urine: Changes Produced by Ethylenediaminetetraacetate *

Determination of tin in nonferrous metals by distillation as bromide and precipitation with cupferron

Radiochemical Determination of Z35U Abundances by Activation Analysis

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