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Determination method of plutonium age in trace plutonium sample

A measurement method and sample technology, applied in measuring devices, material analysis through electromagnetic means, instruments, etc., can solve the problems of cumbersome sample processing process and poor repeatability of weapon-grade plutonium age results, and achieve short sample analysis time , good background control and high method accuracy

Active Publication Date: 2009-10-21
CHINA INSTITUTE OF ATOMIC ENERGY
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  • Abstract
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  • Claims
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Problems solved by technology

In Journal of Radioanalytical and Nuclear Chemistry, Vol.272, No.1 (2007) 45-51, U.Nygren et al. used inductively coupled plasma mass spectrometry to measure the plutonium age of plutonium standard samples, and the sample processing process is relatively cumbersome , the age results for weapons-grade plutonium are not very reproducible

Method used

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  • Determination method of plutonium age in trace plutonium sample
  • Determination method of plutonium age in trace plutonium sample
  • Determination method of plutonium age in trace plutonium sample

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] This embodiment implements according to the following steps:

[0017] Step 1, weigh the plutonium concentration to be 107ng·g -1 The plutonium sample solution 0.0403g, adding concentration is 47.93pg·g -1 of 243 Am tracer 0.3287g, the concentration is 1.0409ng·g -1 of 242 Pu Diluent 0.0108g, and 600μL 4×10 -3 mol L -1 NaNO 2 , evaporated to dryness after reacting for 10 minutes.

[0018] Step 2, add the evaporated sample to 1mL 2mol L -1 HNO 3 Transfer to TEVA resin column, resin volume 1mL, first use 1.5mL 2mol L -1 HNO 3 The Am' component was collected by elution, and then 5mL of 2mol·L -1 HNO 3 Rinse the exchange column, and finally use 6mL of 0.15mol·L -1 Nitric acid-0.025mol·L -1 The oxalic acid solution was washed and collected as the Pu component, which was used for MC-ICP-MS analysis.

[0019] Step 3, transfer the Am' component to the used 5mol L -1 HCl equilibrated TRU resin column, resin volume 1mL, use 5mol L -1 Rinse with HCl, and collect th...

Embodiment 2

[0029] The measurement steps and samples are the same as in Example 1, except for steps 2 and 3. Steps 2 and 3 of the present embodiment are as follows:

[0030] Step 2, add the evaporated sample to 1mL 2mol L -1 HNO 3 Transfer to TEVA resin column, resin volume 1mL, first use 2.0mL 1mol L -1 HNO 3 The Am' component was collected by elution, and then 5mL of 2mol·L -1 HNO 3 Rinse the exchange column, and finally use 7mL 0.1mol·L -1 Nitric acid-0.01mol·L -1 The oxalic acid solution was washed and collected as the Pu component, which was used for MC-ICP-MS analysis.

[0031] Step 3, transfer the Am' component to the used 5mol L -1 HCl equilibrated TRU resin column, resin volume 1mL, use 4mol L -1 Rinse with HCl and collect the effluent from the 5th to 15mL as the Am fraction. After the Am component was evaporated to dryness, 3 mL of 2% HNO 3 Dissolved for MC-ICP-MS analysis.

[0032] The plutonium age was determined to be 21.42 years.

Embodiment 3

[0034] The measurement steps and samples are the same as in Example 1, except for steps 2 and 3. Steps 2 and 3 of the present embodiment are as follows:

[0035] Step 2, add the evaporated sample to 1mL 2mol L -1 HNO 3 Transfer to TEVA resin column, resin volume 1mL, first use 1mL 3mol L -1 HNO 3 The Am' component was collected by elution, and then 5mL of 2mol·L -1 HNO 3 Rinse the exchange column, and finally use 5mL 0.15mol·L -1 Nitric acid-0.10mol·L -1 The oxalic acid solution was washed and collected as the Pu component, which was used for MC-ICP-MS analysis.

[0036] Step 3, transfer the Am' component to the used 5mol L -1 HCl equilibrated TRU resin column, resin volume 1mL, use 6mol L -1 Rinse with HCl and collect the effluent from the 3rd to 15mL as the Am fraction. After the Am component was evaporated to dryness, 3 mL of 2% HNO 3 Dissolved for MC-ICP-MS analysis.

[0037] The plutonium age was determined to be 23.56 years.

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Abstract

The invention discloses a determination method of plutonium age in a trace plutonium sample. The method comprises the following steps of: adding plutonium and the isotopic diluents of daughter americium thereof, namely, Pu and Am, in the sample; adding sodium nitrite for price adjustment; and then loading a TEVA resin column, using a chemical separation method to respectively obtain a Pu component and an Am component, and using a multi-receiving inductive coupling plasma mass spectrometry to measure the Pu component and the Am component respectively to obtain the values of Pu / Pu and Am / Am . According to the amount of the added diluents, the value of Pu / Am is calculated and substituted in the age-calculating formula to obtain the age of plutonium. The deviation between the age measured by the method and the reference value is within 5%.

Description

technical field [0001] The invention belongs to the technical field of radioisotope measurement, in particular to the detection technology of trace plutonium age. Background technique [0002] In the field of nuclear forensics and verification, there is a need to detect the age properties of trace plutonium. Scholars at home and abroad mainly use gamma spectrometer to determine the age of plutonium. The measurement object of this method is plutonium material, and it is generally believed that the sample size needs to be at least 100mg, and there are certain requirements for the shape of the sample. For smaller samples, due to the limitation of the detection limit of the instrument, the deviation of the plutonium age measured by the gamma spectrometer is relatively large, and the required measurement time is also relatively long. In Radiochim.Acta 96, (2008) 327-331, Zhang Haitao et al. developed a method for measuring the age of plutonium material by α spectrum combined wi...

Claims

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Application Information

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IPC IPC(8): G01N27/64
Inventor 陈彦常志远赵永刚张继龙
Owner CHINA INSTITUTE OF ATOMIC ENERGY
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