Part A. Chemical neutron activation analysis of aluminum in biological samples. Part B. Stereochemical consequences of chlorine substitution reactions with (2S,3S)dl-2-chloro-3-fluoropentane and (2S,3S)dl-3-chloro-2-fluoropentane in the gas, liquid and solid phase

Thesis/Dissertation · Sun Jan 01 04:00:00 EST 1989

OSTI ID:7292103

Roman, F R

A method was developed for determination of aluminum in biological samples by anion exchange chromatography and neutron activation analysis (NAA). The samples were digested with nitric acid at 65{degree}C, converting the aluminum to Al{sup +3}. The remaining solids were dissolved with dilute tiron solution, and the pH adjusted to six with ammonium hydroxide. The tiron forms a negative complex with aluminum, which is retained on the anion exchange resin. To remove the interfering ions ({sup 31}P, {sup 24}Na, {sup 37}Cl) present in biological material, ammonium citrate was eluted through the resin. The aluminum was stripped from the resin with nitric acid. Fractions eluting from the column were assayed for aluminum content using NAA. The aluminum recoveries were determined to be quantitative by the method of additive spikes. Urine, bone and tissue samples were analyzed for aluminum content. Previously reported recoil halogen-for-halogen substitution reactions of diastereomeric compounds in the gas, liquid and solid phases occurred predominantly with retention of configuration. The stereo-chemical consequences of translationally excited chlorine-for-halogen substitution reactions in 2,3-dihalopentanes were studied in the gas, liquid and solid phases, (2S,3S)-dl-3-chloro-2-fluoropentane and (2S,3S)dl-2-chloro-3-fluoropentane were prepared stereospecifically from cis-2-pentane. The purified diastereomers were individually activated by thermal neutrons, and the {sup 38}Cl-labeled substitution products separated by capillary-radio-gas chromatography. Two substitution reactions pathways were found. Retention of configuration was determined to be the dominant pathway for {sup 38}Cl-for-X (X = Cl,F) substitution reactions. The percent retention of configuration in the {sup 38}Cl-for-Cl substitution was found to be phase-dependent, while the {sup 38}Cl-for-F substitution was found to be relatively phase-independent.

• Research Organization: Nebraska Univ., Lincoln, NE (United States)
• OSTI ID: 7292103
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400101* -- Activation
Nuclear Reaction
Radiometric & Radiochemical Procedures
400102 -- Chemical & Spectral Procedures
ACTIVATION ANALYSIS
ALKALI META
ALKALI METAL COMPOUNDS
ALUMINIUM
ANIONS
AROMATICS
BETA DECAY RADIOISOTOPES
BETA-MINUS DECAY RADIOISOTOPES
BIOLOGICAL MATERIALS
CATIONS
CHARGED PARTICLES
CHEMICAL ANALYSIS
CHEMICAL REACTIONS
CHLORINE 37
CHLORINE ISOTOPES
CHROMATOGRAPHY
DATA
ELEMENTS
EXPERIMENTAL DATA
GAS CHROMATOGRAPHY
HOURS LIVING RADIOISOTOPES
HYDROXY COMPOUNDS
INFORMATION
INTERFERING ELEMENTS
ION EXCHANGE CHROMATOGRAPHY
IONS
ISOMERIC TRANSITION ISOTOPES
ISOTOPES
LIGHT NUCLEI
MATERIALS
METALS
MILLISEC LIVING RADIOISOTOPES
NEUTRON ACTIVATION ANALYSIS
NUCLEI
NUMERICAL DATA
ODD-EVEN NUCLEI
ODD-ODD NUCLEI
ORGANIC ACIDS
ORGANIC COMPOUNDS
ORGANIC HALOGEN COMPOUNDS
ORGANIC SULFUR COMPOUNDS
PHENOLS
PHOSPHORUS 31
PHOSPHORUS ISOTOPES
POLYPHENOLS
RADIOISOTOPES
REAGENTS
SAMPLE PREPARATION
SECONDS LIVING RADIOISOTOPES
SEPARATION PROCESSES
SODIUM 24
SODIUM COMPOUNDS
SODIUM ISOTOPES
STABLE ISOTOPES
STEREOCHEMISTRY
SULFONIC ACIDS
TIRON