Forced-flow chromatographic determination of calcium and magnesium with continuous spectrophotometric detection
Modifications to the forced-flow chromatograph include a flow-through pH monitor to continuously monitor the pH of the final effluent and an active low-pass filter to eliminate noise in the spectrophotometric detector. All separations are performed using partially sulfonated XAD-2 as the ion exchanger. Elution of calcium and magnesium is accomplished using ammonium chloride and ethylenediammonium chloride solutions. Calcium and magnesium are detected by means of Arsenazo I and PAR-ZnEDTA color-forming reagents. Other metal ions are detected by means of PAR and Chromazurol S color-forming reagents. Calcium and magnesium distribution coefficients on partially sulfonated XAD-2 as functions of ammonium chloride and ethylenediammonium chloride concentration are given together with distribution coefficients of other metal ions. Methods for the selective elution of interfering metal ions prior to the elution of calcium and magnesium are described. Beryllium and aluminum are selectively eluted with sulfosalicylic acid. Those elements forming anionic chloride complexes are selectively eluted with HCl-acetone. Nickel is selectively eluted with HCl-acetone-dimethylglyoxime. Synthetic samples containing calcium and magnesium, both alone and in combination with alkali metals, strontium, barium, beryllium, aluminum, transition metals, and rare earths, are analyzed. Hard water samples are analyzed for calcium and magnesium and the results compared to those obtained by EDTA titration, atomic absorption spectroscopy, and plasma emission spectroscopy. Several clinical serum samples are analyzed for calcium and magnesium and the results compared to those obtained by atomic absorption spectroscopy.
- Research Organization:
- Ames Lab., Ames, IA (United States)
- DOE Contract Number:
- W-7405-ENG-82
- OSTI ID:
- 5001357
- Report Number(s):
- IS-T-806
- Resource Relation:
- Other Information: Thesis
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
CALCIUM
ION EXCHANGE CHROMATOGRAPHY
SPECTROPHOTOMETRY
MAGNESIUM
ARSENAZO
INTERFERING ELEMENTS
ION EXCHANGE MATERIALS
QUANTITATIVE CHEMICAL ANALYSIS
REMOVAL
SULFONATION
TRACE AMOUNTS
ALKALINE EARTH METALS
AROMATICS
ARSENIC COMPOUNDS
ARSONIC ACIDS
AZO COMPOUNDS
CHEMICAL ANALYSIS
CHEMICAL REACTIONS
CHROMATOGRAPHY
ELEMENTS
HYDROXY COMPOUNDS
METALS
ORGANIC ACIDS
ORGANIC ARSENIC COMPOUNDS
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC SULFUR COMPOUNDS
PHENOLS
POLYPHENOLS
REAGENTS
SEPARATION PROCESSES
SULFONIC ACIDS
400104* - Spectral Procedures- (-1987)