Method for determining TOPO content in organic solvent by employing capillary gas chromatography
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A technology of gas chromatography and organic solvents, which is applied in the detection field of TRPO, can solve the problems affecting the extraction effect, and achieve the effect of simple and fast method and good repeatability
Inactive Publication Date: 2014-07-09
傅培
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During continuous use, the concentration of TRPO in the system will gradually decrease, thus affecting the extraction effect
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Embodiment 1
[0024] The method of capillary gas chromatography for the determination of TOPO content in organic solvents includes the following steps:
[0025] (1) Instrument connection: Connect the outlet of the Agilent 6890 gas chromatograph to the inlet of the FID hydrogen flame ion detector;
[0026] (2) Set the instrument parameters: the chromatographic column is a 30m×0.32mm fused silica capillary column, the carrier gas is high-purity nitrogen, the outlet velocity is 100ml / min, the column velocity is 4.3ml / min, and the split ratio: 23 / 1; Detector temperature is 340℃, sample inlet: 340℃, column temperature is 220℃ to 330℃, heating rate is 10℃ / min, sample injection volume: 0.2μl, 0.5μl, 1.0μl, peak area is measured by electronic integration ;
[0027] (3) Draw calibration curve:
[0028] ① Recrystallization and purification of TOPO: Weigh about 20g of industrial product TOPO, add 30-70ml of hot n-hexane to dissolve it, and let it stand for about 2 hours to recrystallize it once. Filter with...
Embodiment 2
[0044] The method of capillary gas chromatography for the determination of TOPO content in organic solvents includes the following steps:
[0045] (1) Instrument connection: Connect the outlet of the Agilent 6890 gas chromatograph to the inlet of the FID hydrogen flame ion detector;
[0046] (2) Set the instrument parameters: the chromatographic column is a 30m×0.32mm fused silica capillary column, the carrier gas is high-purity nitrogen, the outlet velocity is 100ml / min, the column velocity is 4.3ml / min, and the split ratio: 23 / 1; Detector temperature is 340℃, sample inlet: 340℃, column temperature is 220℃ to 330℃, heating rate is 10℃ / min, sample injection volume: 0.2μl, 0.5μl, 1.0μl, peak area is measured by electronic integration ;
[0047] (3) Draw calibration curve:
[0048] ① Recrystallization and purification of TOPO: Weigh about 20g of industrial product TOPO, add 30-70ml of hot n-hexane to dissolve it, and let it stand for about 2 hours to recrystallize it once. Filter with...
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Abstract
A method for determining TOPO content in an organic solvent by employing capillary gas chromatography comprises the following steps: (1) connecting apparatuses; (2) setting apparatus parameters; (3) drawing a calibration curve; and (4) detecting a to-be tested sample: (a) performing centrifugation separation on a to-be tested solution or employing PS paper to filter to remove water and suspend solids; (b) accurately weighing 2 g of didecyl phthalate, putting in a 50 mL of a volumetlric flask, transferring 25 mL of the clear solution to a same volumetlric flask by employing a pipet, and setting the volume with hexane; (c) according to gas chromatography conditions to inject the sample with sample injection amount of 1.0 mu L and 0.5 mu L for multiple times, and obtaining the peak area ratio and the peak height ratio of the sample to an internal standard substance from the chromatogram; and (d) according to an internal standard calibration curve to find the mass ratio of the sample to the internal standard substance, and calculating the content. Didecyl phthalate is selected as the internal standard substance, and the peak height internal standard method and the peak area internal standard method are employed. The relative standard deviation of the peak area internal standard method is 0.31%, the linearly dependent coefficient is 1.0000, the detection limit is 0.0014 g/mL, and the method is simple, rapid, good in repeatability and applicable to determination of trace ingredients.
Description
Technical field [0001] The invention relates to a method for detecting TRPO, in particular to a method for measuring TOPO content in organic solvents by using capillary gas chromatography. Background technique [0002] With the rapid economic development, my country will gradually increase the proportion of nuclear energy in the total energy supply. According to the "Vision Plan" of nuclear power, my country's installed nuclear power capacity will increase to 36 million kilowatts by 2020, accounting for 4% of the country's total installed capacity. However, as the nuclear power plant is put into operation, a large amount of spent fuel will be produced. Doing a good job in the post-processing of spent fuel can save 35% of natural uranium resources and achieve full use of energy. However, the reprocessing of spent fuel will produce a large amount of high-level liquid waste (HLLW), which is extremely radioactive and extremely toxic, and some radionuclides have a long half-life (up ...
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