OBJECTIVE: The main objective of this study was to optimize the production of NPG diesters and to characterize the optimized esters with typical chemical, physical and electrical properties to study its potential as insulating oil.
METHODS: The transesterification reaction between HOPME and NPG was conducted in a 1L three-neck flask reactor at specified temperature, pressure, molar ratio and catalyst concentration. For the optimization, four factors have been studied and the diester product was characterized by using gas chromatography (GC) analysis. The synthesized esters were then characterized with typical properties of transformer oil such as flash point, pour point, viscosity and breakdown voltage and were compared with mineral insulating oil and commercial NPG dioleate. For formulation, different samples of NPG diesters with different concentration of pour point depressant were prepared and each sample was tested for its pour point measurement.
RESULTS: The optimum conditions inferred from the analyses were: molar ratio of HOPME to NPG of 2:1.3, temperature = 182°C, pressure = 0.6 mbar and catalyst concentration of 1.2%. The synthesized NPG diesters showed very important improvement in fire safety compared to mineral oil with flash point of 300°C and 155°C, respectively. NPG diesters also exhibit a relatively good viscosity of 21 cSt. The most striking observation to emerge from the data comparison with NPG diester was the breakdown voltage, which was higher than mineral oil and definitely in conformance to the IEC 61099 limit at 67.5 kV. The formulation of synthesized NPD diesters with VISCOPLEX® pour point depressant has successfully increased the pour point of NPG diester from -14°C to -48°C.
CONCLUSION: The reaction time for the transesterification of HOPME with NPG to produce NPG diester was successfully reduced to 1 hour from the 14 hours required in the earlier synthesis method. The main highlight of this study was the excess reactant which is no longer methyl ester but the alcohol (NPG). The optimum reaction conditions for the synthesis were molar ratio of 2:1.13 for NPG:HOPME, 182°C, 0.6 mbar and catalyst concentration of 1.2 wt%. The maximum NPG diester yield of 87 wt% was consistent with the predicted yield of 87.7 wt% obtained from RSM. The synthesized diester exhibited better insulating properties than the commercial products especially with regards to the breakdown voltage, flash point and moisture content.
OBJECTIVE: In this presented work, an analytical method by gas chromatography coupled with flame ionization detection (GC-FID) has been developed to determine organic solvents in radiopharmaceutical samples. The effect of injection holding time, temperature variation in the injection port, and the column temperature on the analysis time and resolution (R ≥ 1.5) of ethanol and acetonitrile was studied extensively.
METHODS: The experimental conditions were optimized with the aid of further statistical analysis; thence, the proposed method was validated following the International Council for Harmonisation (ICH) Q2 (R1) guideline.
RESULTS: The proposed analytical method surpassed the acceptance criteria including the linearity > 0.990 (correlation coefficient of R2), precision < 2%, LOD, and LOQ, accuracy > 90% for all solvents. The separation between ethanol and acetonitrile was acceptable with a resolution R > 1.5. Further statistical analysis of Oneway ANOVA revealed that the increment in injection holding time and variation of temperature at the injection port did not significantly affect the analysis time. Nevertheless, the variation in injection port temperature substantially influenced the resolution of ethanol and acetonitrile peaks (p < 0.05).
CONCLUSION: The proposed analytical method has been successfully implemented to determine the organic solvent in the [18F]fluoro-ethyl-tyrosine ([18F]FET), [18F]fluoromisonidazole ([18F]FMISO), and [18F]fluorothymidine ([18F]FLT).