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At least 127 records · Page 7Linked to original sources
USGS2002

Nephelometric determination of fluorine

Fluorine in minerals may be determined with the nephelometer to about 1 per cent of the fluorine. The determination is made on an aliquot of the sodium chloride solution of the fluorine, obtained by the Berzelius method of extraction. The fluorine is precipitated as colloidal calcium fluoride in alcoholic solution, gelatin serving as a protective colloid. Arsenates, sulfates, and phosphates, which interfere with the determination, must be removed.

Industrial And Engineering Chemistry Analytical Ed↗
USGS2002

Characteristic constants of 2,2',4'-trihydroxyazobenzene-5-sulfonic acid, a reagent for spectrophotometric analysis

The dye 2,2',4'-trihydroxyazobenzene-5-sulfonic acid, has shown promise as a reagent for the determination of zirconium. As the literature contains very little information about this dye, basic data pertinent to its use as a reagent were determined. The sulfonic acid group and all three of the hydroxy groups show acidic characteristics. Apparent dissociation constants were determined for the three more labile protons and the approximate order of magnitude for the fourth constant was estimated. Absorption spectra for the different ionization species are given. A curve is also included which shows the fraction of dye in the different ionization forms at acidities from 10.35M hydrochloric acid to pH 11.9. A sixth dye species was found in 1.0 to 8.4M potassium hydroxide solutions, but its nature is unknown.

Analytical Chemistry↗
USGS2002

Determination of lithium in rocks by distillation

A method for the quantitative extraction and recovery of lithium from rocks is based on a high temperature volatilization procedure. The sample is sintered with a calcium carbonate-calcium chloride mixture at 1200° C. for 30 minutes in a platinum ignition tube, and the volatilization product is collected in a plug of Pyrex glass wool in a connecting Pyrex tube. The distillate, which consists of the alkali chlorides with a maximum of 5 to 20 mg. of calcium oxide and traces of a few other elements, is removed from the apparatus by dissolving in dilute hydrochloric acid and subjected to standard analytiaal procedures. The sinter residues contained less than 0.0005% lithium oxide. Lithium oxide was recovered from synthetic samples with an average error of 1.1%.

Analytical Chemistry↗
USGS2002

Determination of fluorine in organic compounds: Microcombustion method

A reliable and widely applicable means of determining fluorine in organic compounds has long been needed. Increased interest in this field of research in recent years has intensified the need. Fluorine in organic combinations may be determined by combustion at 900° C. in a quartz tube with a platinum catalyst, followed by an acid-base titration of the combustion products. Certain necessary precautions and known limitations are discussed in some detail. Milligram samples suffice, and the accuracy of the method is about that usually associated with the other halogen determinations. Use of this method has facilitated the work upon organic fluorine compounds in this laboratory and it should prove to be equally valuable to others.

Analytical Chemistry↗
USGS2002

Cooperative investigation of precision and accuracy in chemical analysis of silicate rocks

This is the preliminary report of the first extensive program ever organized to study the analysis of igneous rocks, a study sponsored by the United States Geological Survey, the Massachusetts Institute of Technology, and the Geophysical Laboratory of the Carnegie Institution of Washington. Large samples of two typical igneous rocks, a granite and a diabase, were carefully prepared and divided. Small samples (about 70 grams) of each were sent to 25 rock-analysis laboratories throughout the world; analyses of one or both samples were reported by 34 analysts in these laboratories. The results, which showed rather large discrepancies, are presented in histograms. The great discordance in results reflects the present unsatisfactory state of rock analysis. It is hoped that the ultimate establishment of standard samples and procedures will contribute to the improvement of quality of analyses. The two rock samples have also been thoroughly studied spectrographically and petrographically. Detailed reports of all the studies will be published.

Analytical Chemistry↗
USGS2002

Semiquantitative spectrographic method for analysis of minerals, rocks, and ores

The quantity and complex nature of materials received for analysis in the spectrographic laboratories of the U. S. Geological Survey have emphasized the need for a spectrographic method to determine a maximum number of elements in a limited time with a reasonable degree of accuracy. The semiquantitative method described determines 68 elements in one arcing of a 10-mg. sample. The method has been used to complete 245,000 determinations during a 3-year period. Each determination is reported as a concentration range or bracket (0.001 to 0.01, 0.01 to 0.1%, etc.). A chemical check of 500 such determinations showed 92% in agreement; the remaining 8% agreed to within one bracket. The method requires a minimum of sample handling, thus reducing the chances of contamination, detects low concentrations of elements, and is rapid. Analyses have been completed on a wide variety of materials.

Analytical Chemistry↗
USGS2002

Ultraviolet spectrophotometric determination of tantalum with pyrogallol

In a search for a more rapid method for the determination of tantalum in rocks and minerals, an intensive study was made of the tantalum-pyrogallol reaction recommended by Platanov and Krivoshlikov, and a better modified spectrophotometric procedure is given. The improved method consists in measuring the absorbancy of the tantalum-pyrogallol complex at 325 m μ in 4 N hydrochloric acid and a fixed concentration (0.0175 M ) of ammonium oxalate. Beer's law is followed for the concentration range up to 40 γ per ml. Sensitivity in terms of molar absorbancy index is 4775. Most interferences are additive in character and readily correctable. Separations or major corrections are required in the presence of significant amounts of molybdenum, tungsten, antimony, and uranium. The method has been successfully applied to three ores previously analyzed by gravimetric techniques. The method affords greater speed, sensitivity, and reproducibility in the determination of tantalum in rocks and minerals. A more reliable technique for preparing standard solutions of tantalum has been developed.

Analytical Chemistry↗
USGS2002

Quercetin as colorimetric reagent for determination of zirconium

Methods described in the literature for the determination of zirconium are generally designed for relatively large amounts of this element. A good procedure using colorimetric reagent for the determination of trace amounts is desirable. Quercetin has been found to yield a sensitive color reaction with zirconium suitable for the determination of from 0.1 to 50 of zirconium dioxide. The procedure developed involves the separation of zirconium from interfering elements by precipitation with p-dimethylaminoazophenylarsonic acid prior to its estimation with quercetin. The quercetin reaction is carried out in 0.5N hydrochloric acid solution. Under the operating conditions it is indicated that quercetin forms a 2 to 1 complex with zirconium; however, a 2 to 1 and a 1 to 1 complex can coexist under special conditions. Approximate values for the equilibrium constants of the complexes are K 1 = 0.33 x 10 -5 and K 2 = 1.3 x 10 -9 . Seven Bureau of Standards samples of glass sands and refractories were analyzed with excellent results. The method described should find considerable application in the analysis of minerals and other materials for macro as well as micro amounts of zirconium.

Analytical Chemistry↗
USGS2002

Spectrophotometric determination of uric acid and some redeterminations of its solubility

The present study was initiated in order to develop a rapid and accurate method for the determination of uric acid in fresh, brackish, and sea water. It was found that the spectrophotometric determination of uric acid based upon its reaction with arsenophosphotungstic acid reagent in the presence of cyanide ion meets this objective. The absorbancy of the blue complex was measured at 890 m μ . Slight variations from Beer's law were generally found. The results show the effects of pH, reaction time, concentration of reagents, and temperature upon color development and precipitate formation. Disodium dihydrogen ethylenediamine tetraacetate (Versene) was used as a buffering and complexirig agent. The results are significant in that they give the absorption spectrum of the blue complex and the effects of variables upon its absorbancy. Studies were made with the method to determine the stability of reagents and standard solutions and to determine the rate of bacterial decomposition of uric acid. Measurements of the solubility of uric acid are reported.

Analytical Chemistry↗
USGS2002

Quantitative radiochemical method for determination of major sources of natural radioactivity in ores and minerals

When an ore sample contains radioactivity other than that attributable to the uranium series in equilibrium, a quantitative analysis of the other emitters must be made in order to determine the source of this activity. Thorium-232, radon-222, and lead-210 have been determined by isolation and subsequent activity analysis of some of their short-lived daughter products. The sulfides of bismuth and polonium are precipitated out of solutions of thorium or uranium ores, and the α -particle activity of polonium-214, polonium-212, and polonium-210 is determined by scintillation-counting techniques. Polonium-214 activity is used to determine radon-222, polonium-212 activity for thorium-232, and polonium-210 for lead-210. The development of these methods of radiochemical analysis will facilitate the rapid determination of some of the major sources of natural radioactivity.

Analytical Chemistry↗