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M. H. Fletcher

Publications and source records attributed to M. H. Fletcher.

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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

Study of multicomponent mixtures in solution with a vertical-axis transmission-type filter-fluorometer

Fluorescence intensity, sensitivity, and the effect of diverse ions are discussed in relation to chemical equilibrium and the general equation for fluorescence. High sensitivity is the common denominator in eliminating or reducing all types of interference and the general equation is the key for quickly selecting conditions that give maximum sensitivity. With a transmission-type fluorometer, experimental fluorescence intensities adhere to the general equation over a very wide range of light absorption. If the instrument has a vertical axis, solution depth can be adjusted so that the data fall on that portion of the theoretical curve which is essentially a straight line. When the fluorescence wavelength selected for measurement is not absorbed by the solution, the general equation reduces to a much simpler expression, and then, under proper circumstances, fluorescence values can be used for calculations as confidently and as easily as absorbance values.

Analytical Chemistry

Fluorometric study of the beryllium-morin system

Three principal beryllium-morin complexes, a (1 + 1) monomer, a (1 + 1) dimer, and a (1 + 2) complex are found and conditional equilibrium constants for their formation are evaluated. Approximate ionization constants, absorption spectra, and the relative fluorescence intensities for five ionic species of morin are also determined in a spectrophotometric and fluorometric study of morin. The following interrelationships are discussed: pH, ionization of morin, absorption spectra of the various ionic species of morin and of the berylliummorin complexes, equilibria for the reactions between beryllium and morin, the period of time between preparation of the solution and measurement of the fluorescence, and fluorescence intensity.

Analytical Chemistry

A fluorimetric study of the thorium-morin system

Thorium reacts with morin to yield a yellow complex that fluoresces when irradiated with ultraviolet light. The effect on the fluorescence of such variables as concentration of acid, alcohol, thorium, morin, and complex; time, temperature and wave length of exciting light are studied to determine experimental conditions yielding maximum fluorescence. The effects of Zr+4, Al+3, Fe+3, Ca+2 and La+3 are discussed. The fundamental relationships between light absorption and fluorescence are expressed in a general equation that applies to a three-component system when the fluorescence is measured in a transmission-type fluorimeter. This general equation is used to obtain an expression for the fluorescence of the thoriummorin system. Equations, derived from experimental data, relate both the fraction of thorium reacted to form complex and the fraction of unquenched fluorescence to the concentration of uncombined morin. These functions, when combined with the general equation, give an expression whichrelates the total net fluorescence to the amount of uncombined morin in the solution. This last equation can be used to determine the one region for the concentration of uncombined morin that gives maximum sensitivity for the system. Calculated standard curves are in good agreement with experimental curves.

Journal of the American Chemical Society

Determination of lithium in rocks: Fluorometric method

The gravimetric method in general use for the determination of lithium is tedious, and the final weighed product often contains other alkali metals. A fluorometric method was developed to shorten the time required for the analysis and to assure that the final determination is for lithium alone. This procedure is based on the complex formed between lithium and 8-hydroxyquinoline. The fluorescence is developed in a slightly alkaline solution of 95% alcohol and measurement is made on a photoelectric fluorometer. Separation from the ore is carried out by the wet method or by the distillation procedure. Sodium and potassium are removed by alcohol and ether, but complete separation is not necessary. Comparison of analyzed samples shows excellent agreement with spectrographic and gravimetric methods. The fluorometric method is more rapid than the gravimetric and produces more conclusive results. Another useful application is in the preparation of standard lithium solutions from reagent quality salts when a known standard is available. In this case no separations are necessary.

Analytical Chemistry