New chelating reagents for preconcentration, separation, determination of metal complexes by high performance liquid chromatography and solid phase extraction

Technical Report · Tue Dec 03 04:00:00 EST 1991

OSTI ID:6020959

Qian, Yan wen

A general scheme is outlined for rapid determination of metal cations by complexation and subsequent HPLC separation. The synthesis and general properties are described for several new thiohydrazone chelating reagents. Solubility considerations suggest that the metal complexes have a positive charge. Excellent chromatographic separations are obtained for mixtures of up to seven metal complexes. Addition of a positively charged additive to the eluent is shown to have a significant effect on both the retention times and sharpness of the chromatographic peaks. Separation of the metal complexes on resins with a permanent charge is also shown to be feasible. Two new hydrazone reagents have been synthesized and characterized. Trace metal ions in aqueous solution are complexed by one of the hydrazones and the resulting metal complexes are solid phase extracted onto a mini cation-exchange or polymeric column. The uptake of metal complexes is complete and the elution step is fast and complete. The quantitative recoveries of metal ions determined by both spectrophotometric method and ICP-MS are very satisfactory and agree with each other.

• Research Organization: Ames Lab., IA (United States)
• Sponsoring Organization: DOE; USDOE, Washington, DC (United States)
• DOE Contract Number: W-7405-ENG-82
• OSTI ID: 6020959
• Report Number(s): IS-T-1605; ON: DE92005153
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400105* -- Separation Procedures
CHARGED PARTICLES
CHELATING AGENTS
CHEMICAL ANALYSIS
CHEMICAL PREPARATION
CHROMATOGRAPHY
COMPLEXOMETRY
HYDRAZONES
IONS
LIQUID COLUMN CHROMATOGRAPHY
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC POLYMERS
PETROCHEMICALS
PETROLEUM PRODUCTS
PH VALUE
POLYMERS
QUANTITATIVE CHEMICAL ANALYSIS
RESINS
SEPARATION PROCESSES
SYNTHESIS