Inductive coupling plasma atomic emission spectrometry for determining elements in nuclear-grade zirconium alloy

A technology of atomic emission spectroscopy and plasma, which is applied in the preparation of test samples, thermal excitation analysis, material excitation analysis, etc., can solve the problems of cumbersome operation steps, poor precision, long cycle, etc., and achieve the effect of simplifying the detection steps

Inactive Publication Date: 2015-04-29
QINGDAO TIANHENG MACHINERY
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Problems solved by technology

Because of its narrow measurement range, cumbersome operation steps, long period, and poor precision, at pre

Method used

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Embodiment

[0016] The inductively coupled plasma atomic emission spectrometry of the determination of elements in the nuclear grade zirconium alloy of the present embodiment comprises the following steps:

[0017] (1) Preparation of sample solution and matrix mother solution: Weigh 0.5g sample into a PFA beaker, add water 10mL, HF0.5mL, HNO 3 Dissolve 0.5mL without heating. After the sample is completely dissolved, cool it to room temperature, dilute to 100mL with water, shake well, and to be tested, weigh 10g of high-purity zirconium sponge, put it in a PFA cup, add 40mL of water, HF10mL, HNO 3 Dissolve 10mL, after cooling, dilute to 100mL PFA volumetric flask to obtain 100.000mg / L zirconium matrix mother liquor;

[0018] (2) Preparation of the calibration curve solution: According to the content of the measured elements in the sample, the standard stock solution of each element is properly diluted, and the zirconium matrix solution and the main alloy element standard solution equivale...

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Abstract

The invention discloses an inductive coupling plasma atomic emission spectrometry for determining elements in a nuclear-grade zirconium alloy. The inductive coupling plasma atomic emission spectrometry is used for determining 4 types of macroelements and 13 types of trace elements in the nuclear-grade zirconium alloy. The macroelements including tin, niobium, iron and chromium, and the trace elements including aluminum, cobalt, copper, molybdenum, magnesium, manganese, nickel, lead, silicon, tantalum, titanium, vanadium and tungsten in the nuclear-grade zirconium alloy are successfully determined by carrying out base body match on high-purity sponge zirconium and main alloy elements and selecting a suitable spectral line as an analysis line of detected elements. The determination of tin, iron, chromium and nickel in a 360b zirconium alloy in NIST is carried out and determination results are the same as standard values of a standard substance certificate. The nuclear-grade zirconium alloy is subjected to a marking recovery test; and a result shows that the recovery rates of niobium, cobalt, copper, molybdenum, magnesium, manganese, silicon, titanium, vanadium and tungsten are 92%-108% except that the recovery rate of tantalum is low and the recovery rates of aluminum and lead are high. According to the method, the determination result is stable; and the relative standard deviations (RSD) of the determination results of 3 days are lower than 6% and can meet the requirements of Westinghouse certification standards (RSD is less than 10%).

Description

[0001] technical field [0002] The invention belongs to the technical field of casting, and in particular relates to an inductively coupled plasma atomic emission spectrometry for determining elements in nuclear-grade zirconium alloys. [0003] Background technique [0004] Conventional detection and analysis methods for major elements in zirconium alloys mostly use spectrophotometry, flame atomic absorption method, etc. Because of the low content of trace elements and serious spectral interference, silver chloride is generally used as a single carrier distillation method (GB / T13747-92). Because of its narrow measurement range, cumbersome operation steps, long period, and poor precision, at present, inductively coupled plasma atomic emission spectrometry is mostly used for measurement; See report. [0005] Contents of the invention [0006] In order to overcome the above-mentioned technical problems existing in the prior art, the object of the present invention is...

Claims

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Application Information

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IPC IPC(8): G01N21/71G01N1/28G01N1/38
Inventor 刘升迁
Owner QINGDAO TIANHENG MACHINERY
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