Spectrographic Determination of Boron in Clay Shales

1968 ◽  
Vol 22 (4) ◽  
pp. 272-274 ◽  
Author(s):  
R. D. Cody
Keyword(s):  
Internal Standard ◽  
Chemical Analyses ◽  
Spectrographic Determination ◽  
Clay Shales ◽  
Average Coefficient ◽  
Wet Chemical ◽  
Acceptable Agreement

Cobalt has been found to be an acceptable internal standard for the spectrographic determination of boron in shale. Its use leads to acceptable agreement between spectrochemical and wet-chemical analyses, and has given an average coefficient of varation of ±3.57% for 57 clay samples.

Spectrographic Determination of Calcium in Latex of Natural Rubber (Hevea Brasiliensis)

1970 ◽  
Vol 24 (6) ◽  
pp. 583-587 ◽  
Author(s):  
S. K. Ng ◽  
R. C. H. Hsia ◽  
P. T. Lai
Keyword(s):  
Natural Rubber ◽  
Atomic Absorption ◽  
Hevea Brasiliensis ◽  
Internal Standard ◽  
Lithium Carbonate ◽  
Cathode Layer ◽  
Spectrographic Determination ◽  
Dc Arc

A cathode layer dc arc method of determining microgram amounts of calcium in latex of Hevea brasiliensis is described. Using lithium carbonate and lanthanum sulphate as buffers, a working curve covering 0.032% to 10.0% Ca in ash of latex can be constructed with palladium as internal standard. Phosphate and silica suppress Ca emission but silica has a considerably greater effect. Of the four matrices examined, the composition with 44.7% K2O, 22.3% P2O5, and 13.4% MgO, which is most representative of the composition of latex ash, gives reproducible Ca values and these are in closest agreement with those obtained by atomic absorption. The spectrographic technique may be extended to simultaneously determine trace amounts of Mn, Fe, Cu, and Si.

scholarly journals Total-Burn Spectrographic Determination of Silicon in Plutonium

1967 ◽  
Vol 21 (2) ◽  
pp. 86-88 ◽  
Author(s):  
Roy Ko
Keyword(s):  
Internal Standard ◽  
Germanium Dioxide ◽  
Plutonium Dioxide ◽  
Graphite Electrodes ◽  
Spectrographic Determination ◽  
Spectrographic Method ◽  
Trace Concentrations ◽  
Dc Arc ◽  
Ppm Level

A total-burn spectrographic method has been applied to the determination of trace concentrations of silicon in plutonium. The sample is oxidized to plutonium dioxide, mixed with a germanium dioxide—graphite mixture containing tin internal standard, packed into cupped graphite electrodes, and burned to completion in a high-amperage dc arc. Plutonium spectral interference is avoided by using the less sensitive Si 2506.90-Å line. The lower limit of the determination is 25 ppm of silicon in plutonium. The precision of the method is estimated to be ±8% (coefficient of variation) at the 270-ppm level and ±14% at 40 ppm.

The Determination of Iron in Used Lubricating Oil

1971 ◽  
Vol 25 (6) ◽  
pp. 668-671 ◽  
Author(s):  
Gerald S. Golden
Keyword(s):  
Internal Standard ◽  
Rotating Disk ◽  
Lubricating Oil ◽  
X Ray ◽  
Chemical Technique ◽  
Used Lubricating Oil ◽  
Wet Chemical ◽  
Wet Chemical Technique ◽  
Instrumental Methods

Iron analyses performed on used gas turbine lubricating oil samples by several variations of rotating disk–spark emission spectrography, atomic absorptiometry, and x-ray fluorescence spectrometry are compared with a quantitative wet chemical technique. The results indicate that emission spectrography with a cobalt internal standard, atomic absorptiometry with a nitrous oxide–acetylene flame, and x-ray fluorescence, both dispersive and nondispersive, are the most reliable instrumental methods. The iron contained in the samples exists primarily as particulates 1 µ or less in diameter.

X-Ray Spectrographic Determination of Uranium and Plutonium in Aluminum and Other Reactor Fuel Materials

1958 ◽  
Vol 2 ◽  
pp. 193-213
Author(s):  
Maurice C. Lambert
Keyword(s):  
Uranium Dioxide ◽  
Internal Standard ◽  
Reactor Fuel ◽  
Spectrographic Determination ◽  
X Ray ◽  
Counting Time ◽  
Powder Samples ◽  
Enriched Uranium ◽  
X Ray Absorption

AbstractSeveral instrument modifications are described including a shop-built turret mount which provides four water-cooled sample compartments, each accommodating samples up to 1.75 inches in diameter by 1.75 inches long.Sensitivity for detection of the elements throughout the Periodic Chart is discussed for several counters.Uranium and plutonium have been determined up to 20 w/o in metallic samples of aluminum alloys with a precision of ± one per cent in less than three minutes counting time. The determination of uranium dioxide in cryolite involved powder samples and the use of an internal standard. Uranium dioxide dispersions in bismuth metal were very heterogeneous; they were dissolved and precipitated to provide homogeneous, powders which were analyzed by measuring the intensity ratio of uranium and bismuth fluorescence.X-ray fluorescence has been used to measure aluminum cladding thickness over plutonium alloy cores. Precision is discussed in terms of cladding thickness, aperture size, and counting time. Thickness of 11 w/o and 14 w/o plutonium-aluminum and enriched uranium-aluminum cores in reactor fuel plates has been measured by X-ray absorption in the range 0.010 to 0.030 inch with a sensitivity of ± 0.00025 inch.

The Emission Spectrographic Determination of Boron in Silicate Materials

1979 ◽  
Vol 33 (4) ◽  
pp. 404-406 ◽  
Author(s):  
L. S. Dale
Keyword(s):  
Lithium Fluoride ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Coal Ash ◽  
Spectrographic Determination ◽  
Silicate Materials ◽  
Better Than

A procedure is described for the spectrographic determination of boron in silicate materials such as soils and coal ash. The method is based on the use of a lithium fluoride-graphite buffer with germanium as internal standard. A correction for SiO band interference is made. Standardization is facilitated using boron-in-graphite standards. The precision of the method is ±10% and the accuracy is better than 15%. The limit of detection is 10 μg g−1.

Concentration-Spectrographic Determination of Parts per Billion of Some Impurities in Metallurgical Products

1970 ◽  
Vol 24 (5) ◽  
pp. 514-518 ◽  
Author(s):  
G. S. Golden ◽  
M. G. Atwell
Keyword(s):  
Internal Standard ◽  
Chemical Recovery ◽  
Spectrographic Determination ◽  
Dc Arc ◽  
Sulfide Solution ◽  
Single Set

A method is described for the determination of Ag, As, Bi, Cd, Cu, Ge, In, Pb, Sb, Sn, Te, and l at the sub-part per million level in a variety of materials. The elements are concentrated as sulfides using molybdenum as a carrier. After conversion to MoO3, the residue is excited with a dc arc. Gold is used as both a chemical recovery and spectrographic internal standard. The method is applicable to any material whose matrix does not precipitate in acid sulfide solution. A single set of MoO3-base synthetic standards is used.

Rapid Gas-Liquid Chromatographic Method for Determination of Sulfamethazine in Swine Feed

1982 ◽  
Vol 65 (5) ◽  
pp. 1048-1053
Author(s):  
Robert K Munns ◽  
Jose E Roybal
Keyword(s):  
Quantitative Determination ◽  
Coefficient Of Variation ◽  
Chromatographic Method ◽  
Internal Standard ◽  
Liquid Chromatographic Method ◽  
Average Coefficient ◽  
Swine Feed ◽  
Liquid Chromatographic

Abstract A gas-liquid chromatographic method is described for the quantitative determination of trace amounts of sulfamethazine in swine feed. Sulfamethazine is extracted in ammoniated acetone and isolated from other extractants on a Sephadex LH-20 column. The eluate is methylated with diazomethane and evaporated to dryness. The residue is dissolved in a solvent containing an internal standard of methyl sulfasymazine before being injected onto an OV-25 GLC column. An estimation of precision was established by assaying 10 sets of swine feed fortified with 0.5, 1,2, and 5 ppm SMZ. Mean recoveries were 96.0,94.3, 93.5, and 94.0%, respectively, with an average coefficient of variation of 3.07%. The critical steps and ruggedness of the method were also determined.

scholarly journals Proposal for a semi-quantitative method for the determination of volatile compounds in cocoa liquors

Respuestas ◽  
2020 ◽  
Vol 25 (1) ◽  
Author(s):  
Cristian Palencia-Blanco ◽  
Alejandra Gualdrón-Zambrano ◽  
Isabel Guarín - Henao ◽  
Yuly Ojeda-Galeano ◽  
Arley Villamizar-Jaimes ◽  
...  
Keyword(s):  
Volatile Compounds ◽  
Mass Spectra ◽  
Quantitative Method ◽  
Solid Phase ◽  
Internal Standard ◽  
Good Precision ◽  
Response Factors ◽  
Average Coefficient ◽  
Degree Of Recovery

Seventy-four volatile compounds were identified and quantified from cocoa liquors of the ICS 95 and TCS 01 varieties produced in the department of Santander, Colombia. The compounds were extracted using the solid phase microextraction with head space (SPME-HS) technique, and identified by gas chromatography coupled to mass spectrometer (GC-MS) by comparing the mass spectra of each compound in the Wiley 275L library of mass spectra and the Kovats retention index (IK) ratio. A semi-quantitative method was proposed that included toluene as an internal standard to normalize the degree of recovery between samples and a response factor for each family, calculated using a compound characteristic of that functional group. The results associated with response factors for each family or group of compounds such as alcohols, acids, aldehydes, ketones, esters and pyrazines (2.19, 1.02, 2.84, 0.38, 6.38, 0.88 respectively) were different between families, however, there was no difference between compounds within the same family. The implemented method obtained a DOD and DML of 0.024 µg/kg and 0.037 µg/kg respectively and an accuracy expressed as percentage recovery (of characteristic compounds per family) of 96% on average. According to the precision of the method, the results show that the concentrations have an average coefficient of variation (%CV) of 7.38% assuring repeatability and good precision. Finally, for the analyzed and quantified samples, it was found that the compounds with higher concentration were acetic acid (42.633 mg/kg), 2-phenylethyl acetate (29.44 mg/kg), 2.3-butanediol (345.39 mg/kg), 2-phenylethanol (12.595mg/kg) and 2.3.5.6-tetramethylpyrazine (8.601 mg/kg).

Fire Assay-Emission Spectrographic Determination of Iridium, Ruthenium, and Osmium

1972 ◽  
Vol 26 (4) ◽  
pp. 461-467 ◽  
Author(s):  
K. G. Broadhead ◽  
B. C. Piper ◽  
H. H. Heady
Keyword(s):  
Analytical Method ◽  
Emission Spectroscopy ◽  
Graphite Electrode ◽  
Internal Standard ◽  
High Accuracy ◽  
Correction Factors ◽  
Spectrographic Determination ◽  
Fire Assay ◽  
Empirical Correction

A method is presented for the determination of microgram levels of Ir, Ru, and Os in ores, concentrates, and heavy sands. Radiotracers are used to monitor the recovery of these three metals in a 10-mg Pt bead during the normal fire assaying procedure. The Pt bead is arced at 20 A dc in a graphite electrode, and Pt serves as an internal standard. The precision of the method for Ir, Ru, and Os is about 5, 10, and 22% coefficient of variation, respectively. If high accuracy is not required, empirical correction factors may be applied for the assay losses of Ir and Ru, thereby eliminating the need for radiotracers. Index Headings: Analytical method; Fire assaying; Emission spectroscopy; Pt group metals.

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