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Analysis method of N,N-dimethylhydroxylamine

A dimethylhydroxylamine and analysis method technology, applied in the field of nuclear fuel reprocessing, can solve the problems of contamination, uneconomical and practical, high price of gas chromatography or ion chromatography instruments, and achieve the effect of avoiding precipitation and hydrolysis

Inactive Publication Date: 2011-11-23
CHINA INSTITUTE OF ATOMIC ENERGY
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Problems solved by technology

The existing analytical methods have the following disadvantages. On the one hand, gas chromatography or ion chromatography instruments are expensive and uneconomical and practical.
On the other hand, when the solution contains Pu 3+ When waiting for radioactive ions, the radioactive ions will contaminate the gas chromatography or ion chromatography instrument, and produce permanent radiation to the stationary phase used to separate various substances in the gas chromatography or ion chromatography instrument, which may cause damage to the instrument and Interference effects, as well as interference effects when measuring other substances, are unpredictable

Method used

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  • Analysis method of N,N-dimethylhydroxylamine
  • Analysis method of N,N-dimethylhydroxylamine
  • Analysis method of N,N-dimethylhydroxylamine

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Embodiment 1

[0033] This embodiment is Pu 3+ , Methanol, formaldehyde, formic acid, methylamine, dimethylamine, ethanol, methylhydrazine and N, N-dimethylhydroxylamine, the analysis method of N,N-dimethylhydroxylamine coexists.

[0034] (1) The configuration concentration is 3.89×10 -4mol / L N,N-dimethylhydroxylamine aqueous solution, as a standard solution.

[0035] (2) Weigh 0.5112g of phenanthroline + 0.45mL of 11.10mol / L hydrochloric acid + 0.4995g of ferric ammonium sulfate into a 250.00ml volumetric flask, dilute with water to the mark, shake well, and use it as a developer.

[0036] (3) Prepare a 0.05 mol / L potassium hydrogen phthalate solution, add a small amount of NaOH solution to adjust the pH to 5.0, and use it as a buffer solution.

[0037] (4) Add 2.00 mL of buffer solution and 1.2 mL of chromogen to eight 10.00 mL volumetric flasks respectively; 400.00 μL with a concentration of 3.89×10 -4 mol / L standard solution of N,N-dimethylhydroxylamine. Dilute it with water to the ...

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Abstract

The invention discloses an analysis method of N,N-dimethylhydroxylamine. The method comprises the following steps: (1) preparing standard solution of N,N-dimethylhydroxylamine; (2) preparing acidic aqueous solution of Fe3+ / phenanthroline as a color-developing agent; (3) making a standard curve showing variation of the absorbance value along with the concentration of N,N-dimethylhydroxylamine; (4) extracting the acidic solution containing Pu3<+>, methanol, formaldehyde, formic acid, methylamine, dimethylamine, ethanol, methylhydrazine and N,N-dimethylhydroxylamine multiple times with TODGA (N,N,N,N-tetraoctyl-3-oxy-glutaramide) solution; and (5) measuring the absorbance value of each sample at 510nm with an ultraviolet-visible spectrophotometer and computing the concentrations of N,N-dimethylhydroxylamine in the samples according to the standard curve. The analysis method has the advantages of simple and convenient operation, effective avoidance of interference, small sampling amount and low measuring lower limit.

Description

technical field [0001] The invention relates to the technical field of nuclear fuel reprocessing, in particular to an analysis method for N,N-dimethylhydroxylamine. Background technique [0002] N,N-Dimethylhydroxylamine is an organic weak base with reducing properties. Its aqueous solution and acid solution are colorless liquids. N,N-Dimethylhydroxylamine can quickly reduce Pu(IV) to Pu(III), and it does not react with U(VI); so it can be used in spent fuel reprocessing to separate uranium from plutonium , and stripping and purification of plutonium. Usually it is added to the post-treatment process together with methylhydrazine. Applicants developed an advanced two-cycle Purex process based on N,N-dimethylhydroxylamine (DMHAN) and methylhydrazine (MMH) as reducing systems. When N,N-dimethylhydroxylamine undergoes a redox reaction with an oxidizing agent or an oxidizing metal ion such as Pu(IV), it is oxidized to formaldehyde, methanol and formic acid. When N,N-dimethy...

Claims

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Application Information

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IPC IPC(8): G01N21/31G01N21/33
Inventor 李传博刘金平郑卫芳宴太红张宇左臣卞晓艳鲜亮袁中伟张柏青张琪臻娄海林
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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