CN102384923B - Method for testing trace elements in coating - Google Patents
Method for testing trace elements in coating Download PDFInfo
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- CN102384923B CN102384923B CN201110221346.0A CN201110221346A CN102384923B CN 102384923 B CN102384923 B CN 102384923B CN 201110221346 A CN201110221346 A CN 201110221346A CN 102384923 B CN102384923 B CN 102384923B
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Abstract
The invention provides a method for testing trace elements in a coating, which comprises the following steps that: A. original tabletting press molds are respectively reduced to be the tabletting press molds with the diameters being respectively of 20mm, 15mm, 10mm and 5mm according to a proportion; B. boric acid powder with approximate quantity is taken to carry out a tabletting test, a wafer conforming to a test requirement is selected from the molds, and the test of a next step is continued; C. a standard powder sample comprising multiple inorganic trace elements is selected to be pressed into wafers through the molds selected in the previous step, and then the wafers are placed onto an X-ray fluorescent spectrometer to carry out a primary test; D. a set of standard powder samples is selected to carry out multi-time back-test experiments to conform the test effect; and E. a long-term stability effect test is carried out to finally confirm the test effect. By improving a sample making method of the X-ray fluorescent spectrometer, the test precision and the test accuracy of the inorganic trace elements in the coating can be improved.
Description
Technical field
The present invention relates to a kind of method of testing of trace elements in coating, particularly a kind of x-ray fluorescence Method of Energy Spectrum Analysis that uses is to micro-method of testing in figure layer.
Background technology
At present, the inorganic constituents analysis of the coating material such as toy, alloy, plastics, pottery, glass mainly adopts test chemical method, x-ray fluorescence spectrometry method.Wherein chemical method pre-treatment more complicated, and length consuming time, but ratio of precision is higher; X-ray fluorescence spectrometry method is efficient and convenient, and along with progress and the development of technology, some field precision can compare favourably with chemical analysis, and the test of x-ray fluorescence energy spectrometer is a kind of method wherein.As a kind of analytical approach quickly and easily, x-ray fluorescence energy spectrometer is mainly used in the composition qualitative and quantitative analysis in the fields such as alloy, Di Kuang, plastics, cement, fire resistive material, the Thickness Analysis of coating, and the analysis of trace elements in coating.
For x-ray fluorescence energy spectrometer, the analysis of trace elements in coating mainly adopts fundamental parameters method (FP), for proofreading and correct due to the interference between coating thickness, matrix and element.But fundamental parameters method is a kind of semiquantitative analytical approach, its precision cannot be compared with classical empirical coefficient method (EC) with accuracy.Therefore,, for the test of trace elements in coating, empirical coefficient method still cannot replace.But the sample that existing empirical coefficient method needs is conventionally more, weight, more than 5g, can not meet the detection analysis of less weight sample conventionally.
Summary of the invention
In order to solve existing empirical coefficient method, cannot measure the micro-content problem in less weight sample, the present invention proposes following technical scheme:
A method of testing for trace elements in coating, comprises the following steps:
A, the size of original mould for tabletting press is dwindled in proportion, the die size after dwindling is respectively: φ 20mm, φ 15mm, φ 10mm, φ 5mm;
B, get conventional compressing tablet boric acid powder 30mg used, with the mould of different size, carry out compressing tablet experiment, the amount of boric acid used when record can be pressed into disk, the disk being pressed into should meet the requirement of conventional x-ray fluorescence energy spectrometer test aspect hardness and thickness, from mould, select one or severally boric acid can be pressed into the disk that meets test request, proceed next step experiment;
C, select a kind of standard powdered sample that contains more micro-inorganic elements, the mould that utilization is selected from previous step is pressed into the disk that test needs, then disk is placed on x-ray fluorescence energy spectrometer and is made a preliminary test, from the spectrogram of sample, carry out judgment experiment effect;
D, select a set of standard powdered sample that contains more micro-inorganic elements, then use the compression mold of selecting to carry out compressing tablet, field experience Y-factor method Y is demarcated x-ray fluorescence energy spectrometer, then repeatedly return and survey one or more standard model, the parameters such as the mean value of statistical test, standard deviation, relative standard deviation, extreme difference, contrast with standard value, thereby confirm test effect;
E, long-time stability measure of merit: carry out experimental implementation in previous step every day, continue one week, then add up one week data of testing of doing, contrast with the standard of trace element in standard model, final confirmation test effect;
F, get certain coating sample and test.
As a preferred embodiment of the present invention, in described step C judge index as: whether can be by the trace element detection in standard specimen out, the height of scattering strength and background intensity in spectrogram, thus the compression mold size of testing effect optimum selected, to carry out next step experiment.
The beneficial effect that the present invention brings is: the present invention is by improving the method for making sample of x-ray fluorescence spectroscopy, improve measuring accuracy and the accuracy of micro-inorganic elements in coating, thereby avoided the lower problem of precision of the miscellaneous or fundamental parameters method test of chemical method test; The inventive method can be tested ppm rank.
Embodiment
Below preferred embodiment of the present invention is described in detail, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that, protection scope of the present invention is made to more explicit defining.
The harmful elements such as the lead in certain Toys paint coat sample, cadmium, chromium, mercury are detected, the coating on toy surface is scraped off, then carry out compressing tablet test, testing procedure is as follows:
A, the size of original mould for tabletting press is dwindled in proportion, the die size after dwindling is respectively: φ 20mm, φ 15mm, φ 10mm, φ 5mm;
B, get conventional compressing tablet boric acid powder 30mg used, with the mould of different size, carry out compressing tablet experiment, the amount of boric acid used when record can be pressed into disk, the disk being pressed into should meet the requirement of conventional x-ray fluorescence energy spectrometer test aspect hardness and thickness, from mould, select one or severally boric acid can be pressed into the disk that meets test request, proceed next step experiment;
C, select a kind of standard powdered sample that contains more micro-inorganic elements, the mould that utilization is selected from previous step is pressed into the disk that test needs, then disk is placed on x-ray fluorescence energy spectrometer and is made a preliminary test, from the spectrogram of sample, carry out judgment experiment effect, judge index as: whether can be by the trace element detection in standard specimen out, the height of scattering strength and background intensity in spectrogram, thus the compression mold size of testing effect optimum selected, to carry out next step experiment;
D, select a set of standard powdered sample that contains more micro-inorganic elements, then use the compression mold of selecting to carry out compressing tablet, field experience Y-factor method Y is demarcated x-ray fluorescence energy spectrometer, then repeatedly return and survey one or more standard model, the parameters such as the mean value of statistical test, standard deviation, relative standard deviation, extreme difference, contrast with standard value, thereby confirm test effect;
| Test elements | Ba/ppm | As/ppm | Cr/ppm | Pb/ppm | Zn/ppm |
| Mean value | 518 | 845 | 101 | 1155 | 991 |
| Relative standard deviation/% | 0.039 | 0.05 | 0.048 | 0.053 | 0.045 |
| Standard value | 522 | 841 | 99 | 1141 | 982 |
Table one
E, long-time stability measure of merit: carry out experimental implementation in previous step every day, continue one week, obtain one week data of testing of doing as shown in Table 1, contrast with the standard of trace element in standard model, final confirmation test effect;
F, the sample scraping from toy is tested, the relative standard deviation that obtains test result is controlled in 1%.
The above; it is only the specific embodiment of the present invention; but protection scope of the present invention is not limited to this; any those of ordinary skill in the art are in the disclosed technical scope of the present invention; the variation that can expect without creative work or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claims were limited.
Claims (1)
1. a method of testing for trace elements in coating, is characterized in that: this method of testing comprises the following steps:
A, the size of original mould for tabletting press is dwindled in proportion, the die size after dwindling is respectively: φ 20mm, φ 15mm, φ 10mm, φ 5mm;
B, get boric acid powder 30mg, with the mould of above-mentioned size, carry out compressing tablet experiment respectively, the amount of boric acid used when record can be pressed into disk, the disk being pressed into should meet the requirement of conventional x-ray fluorescence energy spectrometer test aspect hardness and thickness, from the mould of different size, select boric acid to be pressed into and meet one of disk of test request or several, proceed next step experiment;
C, select a kind of standard powdered sample that contains more micro-inorganic elements, the mould that utilization is selected from previous step is pressed into the disk that test needs, then disk is placed on x-ray fluorescence energy spectrometer and is made a preliminary test, from the spectrogram of sample, carry out judgment experiment effect, whether judge index is: can be by the trace element detection in standard specimen out, the height of scattering strength and background intensity in spectrogram, thus the compression mold size of testing effect optimum selected, to carry out next step experiment;
D, select a set of standard powdered sample that contains more micro-inorganic elements, then use the compression mold of selecting to carry out compressing tablet, field experience Y-factor method Y is demarcated x-ray fluorescence energy spectrometer, then repeatedly return and survey one or more standard model, four parameters such as the mean value of statistical test, standard deviation, relative standard deviation, extreme difference, contrast with standard value, thereby confirm test effect;
E, long-time stability measure of merit: carry out experimental implementation in previous step every day, continue one week, then add up one week data of testing of doing, contrast with the standard value of trace element in standard model, final confirmation test effect;
F, get certain coating sample and test.
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| CN201110221346.0A CN102384923B (en) | 2011-08-03 | 2011-08-03 | Method for testing trace elements in coating |
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| CN201110221346.0A CN102384923B (en) | 2011-08-03 | 2011-08-03 | Method for testing trace elements in coating |
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| CN102384923B true CN102384923B (en) | 2014-02-05 |
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| CN105628725A (en) * | 2015-12-23 | 2016-06-01 | 芜湖东旭光电装备技术有限公司 | Pull roll coating material component determination method |
| JP7190751B2 (en) * | 2020-10-30 | 2022-12-16 | 株式会社リガク | X-ray fluorescence analyzer |
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Effective date of registration: 20131216 Address after: Gangtian Road Industrial Park in Suzhou city of Jiangsu Province, No. 99 215024 Applicant after: Suzhou Falab Failure Analysis Laboratory Co., Ltd. Address before: 200433, room 3, building 300, No. 105 East National Road, Shanghai, Yangpu District Applicant before: Shanghai Failure Analysis Laboratory Co., Ltd. |
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