Metal alloy XRF spectrometry utilizing new sample preparation technology

A metal alloy, fluorescence spectroscopy technology, used in the preparation of test samples, material analysis using wave/particle radiation, measurement devices, etc., can solve the problem of high melting point, reduce the matrix effect, and achieve the effect of high accuracy

CN102207475BInactive Publication Date: 2012-10-03INSPECTION & QUARANTINE TECH CENT OF XIAMEN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2012-10-03
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention provides a metal alloy XRF spectrometry utilizing a new sample preparation technology. The technology comprises the following steps: 1) acid dissolution: dissolving a metal alloy with inorganic acid; 2) precipitation: adjusting the above dissolved sample solution to be alkaline to precipitate elements to be measured, and filtering the precipitation with ashless filter paper; 3) calcination: placing the filtered filter residues together with the filter paper in a porcelain crucible calcined to a constant weight, conversing the filter residues into metal oxides through steps of drying, carbonization, ashing, calcination, etc, and calculating a weight of calcined filter residues; 4) sheet melting: preparing the above calcined filter residues into a sample sheet by a fusion sample preparation method for detection by an XRF spectrometer, and obtaining contents of elements to be measured in the metal alloy through conversion of obtained data. The invention enables the XRF spectrometry to be applied to detections of some special metal alloys which have a high melting point, a high hardness and is easily oxidized.
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Description

technical field

[0001] The invention relates to a metal alloy X-ray fluorescence spectrum detection method using a new sample preparation technology. Background technique

[0002] X-ray fluorescence spectrometry (XRF) is an ideal and commonly used method for detecting metal alloys. However, XRF method has special sample preparation requirements for the sample to be tested, and the surface of the sample preparation is required to be smooth, flat and pollution-free. In the detection of XRF, the sample preparation techniques of metal alloys include cutting, polishing, grinding, casting and other methods, but these methods are powerless for rare earth alloys with high melting point, high hardness and easy oxidation, so there is no use of XRF report on the determination of rare earth alloys. Therefore, there must be a new metal alloy sample preparation technology to solve the above problems. Contents of the invention

[0003] The purpose of the present invention is to pro...

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Embodiment Construction

[0018] The metal alloy X-ray fluorescence spectrum detection method using the new sample preparation technology described in the present invention, hereinafter by selecting the neodymium-iron series rare earth permanent magnet alloy (the main components are six elements of La, Ce, Pr, Nd, Fe, Co) As the best embodiment of the present invention, the detailed description is as follows:

[0019] 1. Accurately weigh about 1.0 g (accurate to 0.1 mg) sample into a 50 mL glass beaker, add (1+1) HNO 3 20 mL, cover with a watch glass, heat and boil on an electric stove until the sample is completely dissolved, remove it, cool to room temperature, wash the watch glass with a small amount of distilled water, and combine the cleaning solution with the sample solution.

[0020] 2. Add (1+1) ammonia water dropwise to the above sample solution, and stir while adding, until the pH value of the sample solution is 8. At this time, each metal element was precipitated in the form of hydroxi...