Analysis method for coexistence of ammonium ion and N, N-Diethylhydroxyla
A technology of diethylhydroxylamine and analytical method, applied in the field of analytical chemistry, can solve problems such as long time
Inactive Publication Date: 2009-10-28
SHANGHAI UNIV
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Problems solved by technology
Separate analysis of ammonium ions and N, N-diethylhydroxylamine not only takes a long time, but also requires the use of highly toxic chemicals mercuric chloride or mercuric iodide
Method used
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Embodiment Construction
[0019] Embodiments of the present invention are now described below:
[0020] The analysis process and steps of the present embodiment are as follows:
[0021] a. Prepare a simulated sample, prepare a simulated sample containing a mixed solution of ammonium ions and N,N-diethylhydroxylamine.
[0022] b. Using ion chromatography, correctly load the cationic column: METROSEP C 2-250 into the ion chromatograph (column length: 250mm, column diameter: 4mm, packing particle size: 7um), and install 2mmol / L nitric acid to rinse liquid.
[0023] c. Turn on the power of the instrument, the indicator light is on, turn on the computer, start the IC NET 2.3 software, open the System in the main window, and open the system method cation.smt. Click Open to start the pump and start running. The flow rate of the eluent is 1ml / min; The column temperature was constant at 35°C, the injection volume was 20uL, and the pressure was 7Mpa. Take the baseline.
[0024] d. Put the sample solution to ...
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Abstract
The invention relates to a qualitative and quantitative analysis method for coexistence of ammonium ion and N, N-Diethylhydroxyla, belonging to the field of analytical chemistry technology. The method comprises the following steps of: preparing a simulative sample; adopting an ion chromatography, loading 2mmol / L of nitric acid eluent with the flux of 1ml / min; keeping the column temperature at a constant temperature of 35 DEG C, keeping the sampling quantity at 20 Mu L and the pressure at 7MPa; arranging the sample to be measured and high-purity water on a sample disc intermittently; starting to record data after the baseline is stable; adopting a retention time comparison method for the qualitative analysis and adopting an external marking method for the quantitative analysis after completing peak; injecting a certain component with certain concentration quantitatively by an automatic sampler and taking the component as the reference standard; detecting the results to obtain the peak area of the component; drawing the peak area-component concentration working curve; subsequently measuring the peak area of the certain component in the sample to be analyzed and querying the corresponding concentration from the quantitative sampling-working curve. The method can qualitatively and quantitatively analyze the ammonium ion and N, N-Diethylhydroxyla simultaneously in short time.
Description
technical field [0001] The invention relates to a qualitative and quantitative analysis method when ammonium ions and N,N-diethylhydroxylamine coexist, and belongs to the technical field of analytical chemistry. Background technique [0002] In the 21st century, my country will vigorously develop nuclear energy, so it is very important to develop advanced spent fuel reprocessing technology, which is an important link to ensure the sustainable development of nuclear energy. N,N-Diethylhydroxylamine (DEHA) is a new salt-free reductant that is expected to be used in spent fuel reprocessing. The reprocessing of spent fuel is carried out in a certain radiation environment. Under this condition, N, N-diethylhydroxylamine will undergo radiolysis, and the radiolysis may produce ammonium ions. The existence of this ion may affect the spent fuel. For the normal operation of the post-treatment process, it is necessary to qualitatively and quantitatively analyze the ammonium ions in th...
Claims
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Login to View More IPC IPC(8): G01N30/02G01N30/86
Inventor 王锦花吴明红张东平徐刚郑卫芳何辉张生栋李春王生秀曹东明万颖张杰
Owner SHANGHAI UNIV