Atomic fluorescence method for measuring content of arsenic, antimony and bismuth contained in high-temperature alloy FGH96
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A technology of atomic fluorescence and superalloy, applied in the direction of fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of low analysis precision, high cost, interference, etc., and achieve the effect of good selectivity and high sensitivity
Inactive Publication Date: 2014-01-29
AVIC BEIJING INST OF AERONAUTICAL MATERIALS
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However, when ICP-MS analyzes the low melting point elements As, Sb, and Bi in FGH96, there are problems of high cost and serious interference; when AAS analyzes the low melting point elements As, Sb, and Bi in FGH96, there are problems of serious interference and low analysis accuracy.
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preparation example Construction
[0109] (3.3.1) Preparation of calibration curve solution
[0110] In several 100mL beakers, add 10mL nickel standard solution solution (1.21) to process the sample synchronously, and then add 0, 0.50, 1.00, 2.00, 5.00 arsenic C (1.18), antimony C (1.21), bismuth C ( 1.24) Standard solution.
[0111] (3.3.2) Preparation of carrier liquid
[0112] In a 500mL beaker, add 240mL of water, then add 160mL of hydrochloric acid, mix well, and cool to room temperature.
[0113] (3.4) Measurement
[0114] According to the working conditions of arsenic, antimony and bismuth, set the atomic fluorescence spectrometer, measure the calibration curve solution (3.3.1) and the sample solution in sequence, take the solution concentration as the abscissa, and take the fluorescence intensity as the ordinate, draw the working curve and print it .
[0115] (3.5) Calculation of analysis results
[0116] The analysis results are output directly from the instrument.
Embodiment 1
[0118]1. A method for measuring the content of arsenic, antimony and bismuth in superalloy FGH96, characterized in that: atomic fluorescence spectrometer is used, and the working conditions of the instrument for measuring elemental arsenic are as follows: photomultiplier tube negative high voltage: 260V; atomizer height: 8mm; Lamp current: 60mA; carrier gas flow: 400ml / mim; shielding gas flow: 900ml / mim. The measurement conditions for elemental arsenic are as follows: reading time: 10s; measurement method: standard curve method; delay time: 1s; reading method: peak area integration; repetition times: 1 time. The working conditions of the instrument for measuring element antimony are as follows: photomultiplier tube negative high voltage: 300V; atomizer height: 8mm; lamp current: 80mA; carrier gas flow rate: 400ml / mim; shielding gas flow rate: 900ml / mim. The measurement conditions for the measurement element antimony are as follows: reading time: 10s; measurement method: standa...
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Abstract
The invention belongs to the field of alloy trace element analysis technologies, and relates to an atomic fluorescence method for measuring the content of arsenic, antimony and bismuth which are contained in a high-temperature alloy FGH96. The atomic fluorescence method comprises the following analysis steps of: weighing a sample material; preparing a sample solution; preparing a calibration solution; preparing a low-standard solution; preparing a high-standard solution; measuring the concentration of the arsenic, the antimony and the bismuth which are contained in the sample solution; calculating a measurement result to obtain the content of the arsenic, the antimony and the bismuth. The invention provides a hydride generation atomic fluorescence method which has the advantages of high analysis sensitivity, easiness and convenience for operation, short analysis cycle and high efficiency and is used for measuring the content of the arsenic, antimony and bismuth which are contained in the high-temperature alloy FGH96. The hydride generation atomic fluorescence method provided by the invention is wide in application prospect, can meet the requirement that the content requirements of impurity elements are more and more strict with the engineering application of the FGH96 alloy and the requirement for control of low-melting point elements, namely the arsenic, the antimony and the bismuth, especially. The atomic fluorescence method provided by the invention meets the requirements of scientific research and production on the quality control of raw materials, reduces the rejection rate of products and saves the development and production cost.
Description
technical field [0001] The invention belongs to alloy trace element analysis technology, and relates to an atomic fluorescence method for measuring the content of arsenic, antimony and bismuth in superalloy FGH96. Background technique [0002] In response to the engine's demand for high thrust-to-weight ratio, the powder superalloy FGH96 is used in the key hot end parts of the engine. In order to improve the purity level of the disk alloy, it is necessary to strictly control the content of impurity elements in the alloy, especially the content of low melting point elements arsenic, antimony, and bismuth, so as to improve the safety and reliability of engine operation. . [0003] According to literature research, atomic fluorescence technology is an analysis technology with Chinese characteristics, and there is no relevant analysis content in ASTM and foreign literature. The analysis methods of trace elements in superalloys mainly include the methods provided by the nationa...
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