2012Physical Testing and Chemical AnalysisRequires access

RP-HPLC Determination of Bromonitrofluorenones in the Reaction Products of Synthesis

Zhao Zhang

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Abstract

RP-HPLC was applied to the determination of 2,7-dibromo-4-nitrofluorenone(DBNFN) in the reaction products of synthesis of bromonitrofluorenones.Sample was dissolved in methyl alcohol ultrasonically.Elite Hypersil ODS2 C18 chromatographic column and mixture of CH3OH+H2O(85+15) were used as mobile phase for separation.Under the optimized conditions,complete separation of DBNFN from the raw material of 2,7-dibromofluorenone and the derivatives of fluorenone(as by-products) was attained.UV detection at 254 nm and external standard calibration were adopted for determination of DBNFN.Linear relationship between values of peak area and mass concentration of DBNFN was obtained in the range of 0.1-2.5 g·L-1.Detection limit(2S/N) found was 3.8 μg·L-1.Values of recovery found by standard addition method were in the range of 99.2%-99.8%,with values of RSD′s(n=6) ranged from 0.35% to 0.48%.

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RP-HPLC was applied to the determination of 2,7-dibromo-4-nitrofluorenone(DBNFN) in the reaction products of synthesis of bromonitrofluorenones.Sample was dissolved in methyl alcohol ultrasonically.Elite Hypersil ODS2 C18 chromatographic column and mixture of CH3OH+H2O(85+15) were used as mobile phase for separation.Under the optimized conditions,complete separation of DBNFN from the raw material of 2,7-dibromofluorenone and the derivatives of fluorenone(as by-products) was attained.UV detection at 254 nm and external standard calibration were adopted for determination of DBNFN.Linear relationship between values of peak area and mass concentration of DBNFN was obtained in the range of 0.1-2.5 g·L-1.Detection limit(2S/N) found was 3.8 μg·L-1.Values of recovery found by standard addition method were in the range of 99.2%-99.8%,with values of RSD′s(n=6) ranged from 0.35% to 0.48%.

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Available abstract

RP-HPLC was applied to the determination of 2,7-dibromo-4-nitrofluorenone(DBNFN) in the reaction products of synthesis of bromonitrofluorenones.Sample was dissolved in methyl alcohol ultrasonically.Elite Hypersil ODS2 C18 chromatographic column and mixture of CH3OH+H2O(85+15) were used as mobile phase for separation.Under the optimized conditions,complete separation of DBNFN from the raw material of 2,7-dibromofluorenone and the derivatives of fluorenone(as by-products) was attained.UV detection at 254 nm and external standard calibration were adopted for determination of DBNFN.Linear relationship between values of peak area and mass concentration of DBNFN was obtained in the range of 0.1-2.5 g·L-1.Detection limit(2S/N) found was 3.8 μg·L-1.Values of recovery found by standard addition method were in the range of 99.2%-99.8%,with values of RSD′s(n=6) ranged from 0.35% to 0.48%.

Key concepts: Chromatography, Chemistry, Fluorenone, Detection limit, High-performance liquid chromatography, Standard addition, Analytical Chemistry (journal), Calibration curve

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