Method for measuring beryllium and potassium content in zirconium and zirconium alloy at the same time

Method for measuring beryllium and potassium content in zirconium and zirconium alloy at the same time

CN
  • CN 104,697,985 A
  • Filed: 03/30/2015
  • Published: 06/10/2015
  • Est. Priority Date: 03/30/2015
  • Status: Active Application
First Claim
Patent Images

1. the method for beryllium potassium content in Simultaneously test zirconium and it'"'"'s alloy, it is characterized in that, the method comprises the following steps:

  • Step one, turning is carried out to pure zirconium or zircaloy, obtain bits shape sample, then bits shape sample is cleaned up post-drying for subsequent use;

    Step 2, employing coning and quartering carry out division sampling to the bits shape sample after oven dry in step one, obtain treating test sample;

    Step 3, to treating described in step 2 that dripping hydrofluorite-nitric acid compound acid solution in test sample dissolves, and then proceeds in volumetric flask by solution, shakes up with after pure water constant volume, obtain liquid to be measured;

    The volume V of described hydrofluorite-nitric acid compound acid solution meets;

    8m≤

    V≤

    10m, and wherein m is the quality treating test sample, and the unit of m is the unit of g, V is mL;

    Step 4, the 360B zircaloy standard substance several parts of quality being m are placed in multiple beaker, each dropping volume is that the hydrofluorite-nitric acid compound acid solution of V is dissolved, obtain many parts of matrix mother liquors, then multiple volumetric flask is got, each part matrix mother liquor and the beryllium standard solution of metering and the potassium standard solution of metering are moved in each volumetric flask respectively, use pure water constant volume respectively afterwards, after shaking up, obtain the beryllium-potassium calibration solution of a series of variable concentrations;

    The characteristic spectrum intensity of step 5, employing inductive coupling plasma emission spectrograph beryllium element in the 313.042nm place beryllium of variable concentrations described in determination step four one by one-potassium calibration solution, measure the characteristic spectrum intensity of potassium element in variable concentrations beryllium-potassium calibration solution one by one in 766.491nm place simultaneously, set up the concentration of beryllium and the calibration curve of beryllium element characteristic spectrum intensity corresponding relation in beryllium-potassium calibration solution thus, and beryllium-potassium calibrates the concentration of potassium and the calibration curve of potassium element characteristic spectrum intensity corresponding relation in solution;

    Step 6, adopt inductive coupling plasma emission spectrograph in the beryllium element characteristic spectrum intensity of liquid to be measured described in 313.042nm place determination step three, measure the potassium element characteristic spectrum intensity of liquid to be measured in 766.491nm place simultaneously, then the concentration of beryllium in liquid to be measured is calculated according to the concentration of beryllium and the calibration curve of beryllium element characteristic spectrum intensity corresponding relation in the beryllium set up in step 5-potassium calibration solution, the concentration of potassium in liquid to be measured is calculated according to the concentration of potassium and the calibration curve of potassium element characteristic spectrum intensity corresponding relation in beryllium-potassium calibration solution, finally calculate the mass content of beryllium and the mass content of potassium in pure zirconium or zircaloy sample.

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