CN104568916A - Inductive coupling plasma atomic emission spectrometry for determining elements in nuclear-grade zirconium alloy - Google Patents
Inductive coupling plasma atomic emission spectrometry for determining elements in nuclear-grade zirconium alloy Download PDFInfo
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- CN104568916A CN104568916A CN201310517665.5A CN201310517665A CN104568916A CN 104568916 A CN104568916 A CN 104568916A CN 201310517665 A CN201310517665 A CN 201310517665A CN 104568916 A CN104568916 A CN 104568916A
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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
Technical field
The invention belongs to casting technology field, be specifically related to a kind of ICP-AES measuring element in nuclear grade zirconium alloy.
Background technology
Conventional sense analytical approach many employings spectrophotometric method, flame atomic absorption method etc. of macroelement in zircaloy.Trace element is because its content is lower, spectra1 interfer-serious, and general employing silver chloride is the single carrier distillation method (GB/T13747-92) of carrier.Because its measurement range is narrower, and complex operation step, the cycle is long, and accuracy is poor, and current more options ICP-AES measures; But 17 kinds need the method for control element to have no report in Simultaneously test zircaloy.
Summary of the invention
In order to overcome the above-mentioned technical matters that prior art field exists, the object of the invention is to, provide a kind of ICP-AES measuring element in nuclear grade zirconium alloy, disposable detection 17 kinds of elements, detecting step is simplified.
The ICP-AES of element in mensuration nuclear grade zirconium alloy provided by the invention, comprises the following steps:
(1) sample solution and matrix mother liquor: take 0.5g sample in PFA beaker, add water 10mL, HF0.5mL, HNO
30.5mL dissolves, and does not need heating; Sample dissolves completely, is cooled to room temperature, is settled to 100mL with water, shake up, to be measured; Take the high-purity sponge zirconium of 10g, be placed in PFA cup, add water 40mL, HF10mL, HNO
310mL dissolves; After cooling, be settled in 100mL PFA volumetric flask, obtain 100.000mg/L zirconium matrix mother liquor;
(2) preparation of calibration curve solution: tested constituent content per sample, suitably dilutes each elemental standards stock solution, and adds the zirconium Matrix Solution suitable with sample size and main alloying element standard solution, is mixed with hybrid standard serial solution;
(3) INSTRUMENT MODEL: direct-reading plasma emission spectrometer (German SPECTRO) composed entirely by ARCOS-SOP type, HF acid resistant device, chiasma type atomizer; Instrument condition of work: wavelength coverage: 160 ~ 770nm, power: 1400W, carrier gas flux: 1.0 ~ 2.0L/min, cooling gas flow: 10 ~ 15L/min; Assisted gas flow: 0.5 ~ 1.0L/min, sample rate: 2 ~ 5mL/min;
(4) first bioassay standard serial solution, then measure sample at identical conditions.
The ICP-AES of element in mensuration nuclear grade zirconium alloy provided by the invention, its beneficial effect is, disposable detection 17 kinds of elements, simplify detecting step, in nuclear grade zirconium alloy analysis measures, macroelement relative standard deviation is below 2.5%, and trace element relative standard deviation, below 6%, all can meet and analyze requirement and western room Valuation Standard (< 10%).
Embodiment
Below in conjunction with an embodiment, the ICP-AES of mensuration nuclear grade zirconium alloying element provided by the invention is described in detail.
Embodiment
The ICP-AES of element in the mensuration nuclear grade zirconium alloy of the present embodiment, comprises the following steps:
(1) sample solution and matrix mother liquor: take 0.5g sample in PFA beaker, add water 10mL, HF0.5mL, HNO
30.5mL dissolves, and does not need heating, and sample dissolves completely, is cooled to room temperature, is settled to 100mL with water, shake up, to be measured, takes the high-purity sponge zirconium of 10g, is placed in PFA cup, add water 40mL, HF10mL, HNO
310mL dissolves, and after cooling, is settled in 100mL PFA volumetric flask, obtains 100.000mg/L zirconium matrix mother liquor;
(2) preparation of calibration curve solution: tested constituent content per sample, suitably dilutes each elemental standards stock solution, and adds the zirconium Matrix Solution suitable with sample size and main alloying element standard solution, is mixed with hybrid standard serial solution;
(3) INSTRUMENT MODEL: direct-reading plasma emission spectrometer (German SPECTRO) composed entirely by ARCOS-SOP type, HF acid resistant device, chiasma type atomizer; Instrument condition of work: optimal wavelength is: 600nm, best power: 1400W, carrier gas flux: 1.0L/min, cooling gas flow: 12L/min; Assisted gas flow: 0.8L/min, sample rate: 3mL/min;
(4) first bioassay standard serial solution, then measure sample at identical conditions.
Claims (1)
1. measure an ICP-AES for element in nuclear grade zirconium alloy, it is characterized in that: (1) sample solution and matrix mother liquor: take 0.5g sample in PFA beaker, add water 10mL, HF0.5mL, HNO
30.5mL dissolves, and does not need heating, and sample dissolves completely, is cooled to room temperature, is settled to 100mL with water, shake up, to be measured, takes the high-purity sponge zirconium of 10g, is placed in PFA cup, add water 40mL, HF10mL, HNO
310mL dissolves, and after cooling, is settled in 100mL PFA volumetric flask, obtains 100.000mg/L zirconium matrix mother liquor; (2) preparation of calibration curve solution: tested constituent content per sample, suitably dilutes each elemental standards stock solution, and adds the zirconium Matrix Solution suitable with sample size and main alloying element standard solution, is mixed with hybrid standard serial solution; (3) INSTRUMENT MODEL: direct-reading plasma emission spectrometer (German SPECTRO) composed entirely by ARCOS-SOP type, HF acid resistant device, chiasma type atomizer; Instrument condition of work: wavelength coverage: 160 ~ 770nm, power: 1400W, carrier gas flux: 1.0 ~ 2.0L/min, cooling gas flow: 10 ~ 15L/min; Assisted gas flow: 0.5 ~ 1.0L/min, sample rate: 2 ~ 5mL/min; (4) first bioassay standard serial solution, then measure sample at identical conditions.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106885799A (en) * | 2015-03-30 | 2017-06-23 | 国核宝钛锆业股份公司 | A kind of method for determining content of magnesium in core level sponge zirconium particle |
| CN107589107A (en) * | 2015-03-30 | 2018-01-16 | 国核宝钛锆业股份公司 | Method that is a kind of while determining beryllium potassium content in zirconium and zircaloy |
| CN109402432A (en) * | 2018-12-21 | 2019-03-01 | 西部新锆核材料科技有限公司 | A kind of preparation method of nuclear grade zirconium revert ingot casting |
| CN111982890A (en) * | 2020-08-12 | 2020-11-24 | 宁波江丰电子材料股份有限公司 | Mixed acid for dissolving molybdenum-titanium-nickel alloy and preparation method and application thereof |
| CN112229833A (en) * | 2020-10-12 | 2021-01-15 | 宁波江丰电子材料股份有限公司 | Mixed acid for dissolving molybdenum-niobium alloy sample and preparation method and application thereof |
| CN112268893A (en) * | 2020-10-14 | 2021-01-26 | 宁波江丰电子材料股份有限公司 | Method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using inductively coupled plasma emission spectrometer |
| CN113029731A (en) * | 2021-02-26 | 2021-06-25 | 宁波江丰电子材料股份有限公司 | Sample preparation method for ICP-OES analysis of CuMn alloy |
| CN114113044A (en) * | 2021-12-13 | 2022-03-01 | 宁波江丰电子材料股份有限公司 | Method for measuring nickel and iron content in NiFe alloy by using inductively coupled plasma emission spectrometer |
| CN114113043A (en) * | 2021-12-13 | 2022-03-01 | 宁波江丰电子材料股份有限公司 | Method for measuring nickel and vanadium content in NiV alloy by using inductively coupled plasma emission spectrometer |
-
2013
- 2013-10-29 CN CN201310517665.5A patent/CN104568916A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106885799A (en) * | 2015-03-30 | 2017-06-23 | 国核宝钛锆业股份公司 | A kind of method for determining content of magnesium in core level sponge zirconium particle |
| CN107589107A (en) * | 2015-03-30 | 2018-01-16 | 国核宝钛锆业股份公司 | Method that is a kind of while determining beryllium potassium content in zirconium and zircaloy |
| CN106885799B (en) * | 2015-03-30 | 2020-04-24 | 国核宝钛锆业股份公司 | Method for measuring magnesium content in nuclear-grade sponge zirconium particles |
| CN107589107B (en) * | 2015-03-30 | 2020-04-28 | 国核宝钛锆业股份公司 | Method for simultaneously determining beryllium and potassium content in zirconium and zirconium alloy |
| CN109402432A (en) * | 2018-12-21 | 2019-03-01 | 西部新锆核材料科技有限公司 | A kind of preparation method of nuclear grade zirconium revert ingot casting |
| CN111982890A (en) * | 2020-08-12 | 2020-11-24 | 宁波江丰电子材料股份有限公司 | Mixed acid for dissolving molybdenum-titanium-nickel alloy and preparation method and application thereof |
| CN112229833A (en) * | 2020-10-12 | 2021-01-15 | 宁波江丰电子材料股份有限公司 | Mixed acid for dissolving molybdenum-niobium alloy sample and preparation method and application thereof |
| CN112229833B (en) * | 2020-10-12 | 2023-12-29 | 宁波江丰电子材料股份有限公司 | Method for dissolving molybdenum-niobium alloy sample |
| CN112268893A (en) * | 2020-10-14 | 2021-01-26 | 宁波江丰电子材料股份有限公司 | Method for measuring molybdenum content and titanium content in molybdenum-titanium alloy by using inductively coupled plasma emission spectrometer |
| CN113029731A (en) * | 2021-02-26 | 2021-06-25 | 宁波江丰电子材料股份有限公司 | Sample preparation method for ICP-OES analysis of CuMn alloy |
| CN114113044A (en) * | 2021-12-13 | 2022-03-01 | 宁波江丰电子材料股份有限公司 | Method for measuring nickel and iron content in NiFe alloy by using inductively coupled plasma emission spectrometer |
| CN114113043A (en) * | 2021-12-13 | 2022-03-01 | 宁波江丰电子材料股份有限公司 | Method for measuring nickel and vanadium content in NiV alloy by using inductively coupled plasma emission spectrometer |
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Application publication date: 20150429 |