KR100206491B1 - Metal quantity analyzing method of plated steel plate - Google Patents
Metal quantity analyzing method of plated steel plate Download PDFInfo
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- KR100206491B1 KR100206491B1 KR1019950068484A KR19950068484A KR100206491B1 KR 100206491 B1 KR100206491 B1 KR 100206491B1 KR 1019950068484 A KR1019950068484 A KR 1019950068484A KR 19950068484 A KR19950068484 A KR 19950068484A KR 100206491 B1 KR100206491 B1 KR 100206491B1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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Abstract
합금호 용융아연 도금강판내의 철함량을 분석함에 있어서, 형광 X-선 분석기에 의해 얻은 철의 X-선 강도와 원자흡광 분석기를 이용하여 얻은 철함량과의 관계식을 도출한 후 측정하고자 하는 시료에 대한 형광 X-선 분석법으로 얻은 철의 X-선 강도값을 상기 관계식에 대입함으로써 간단하게 철함량을 정량분석할 수 있다.In analyzing the iron content in the hot-dip galvanized steel sheet, the relation between the X-ray intensity of iron obtained by the fluorescence X-ray analyzer and the iron content obtained by the atomic absorption analyzer was derived, The iron content can be easily quantitatively analyzed by substituting the X-ray intensity value of iron obtained by the fluorescence X-ray analysis method into the above relation.
Description
제1도는 본 발명의 방법에 따라 철의 X선 강도값과 합금화 용융아연 도금강판의 도금층내 철함량과의 관계의 일예를 나타내는 그래프.1 is a graph showing an example of the relationship between the X-ray intensity value of iron and the iron content in the plating layer of an alloyed hot dip galvanized steel sheet according to the method of the present invention.
본 발명은 합금화 용융아연 도금강판의 철함량 분석방법에 관한 것이며, 보다 상세하게는 합금화 용융아연 도금강판 내의 철함량을 형광 X-선 분석법을 이용하여 분석하는 방법에 관한 것이다.The present invention relates to a method for analyzing the iron content of an alloyed hot-dip galvanized steel sheet, and more particularly to a method for analyzing the iron content in an alloyed hot-dip galvanized steel sheet using a fluorescent X-ray analysis method.
용융아연 도금강판은 제조비용이 저렴하고 비교적 용이하게 도금할 수 있어서 건축자재 및 가전 등 실제로 산업에서 널리 이용되고 있다. 적정 조성의 도금욕을 460℃로 유지하고 침적되는 강판온도도 460℃로 하여 침적 도금을 행하는 일반 용융아연 도금강판의 제조와는 달리, 합금화 용융아연 도금강판은 연속적으로 약 450-600℃ 범위에서 가열하여 소지철과 아연의 상호 확산에 의해 도금층내에 철성분을 일정한 비율로 포함시킨 것이다. 따라서 합금화 용융아연 도금강판은 합금화 반응에 기인하는 표면 조직에 의해서 도장성, 용접성 및 도장내식성 등에서 우수한 성질을 나타낸다.Hot-dip galvanized steel sheet is inexpensive to manufacture and relatively easy to plate, so it is widely used in industries such as building materials and home appliances. Unlike the manufacture of hot-dip galvanized steel sheet which maintains the plating bath of proper composition at 460 ° C and deposits the steel plate temperature at 460 ° C, the alloyed hot-dip galvanized steel sheet is continuously in the range of about 450-600 ° C. The iron is contained in the coating layer at a constant ratio by the mutual diffusion of the base iron and zinc by heating. Therefore, the alloyed hot-dip galvanized steel sheet exhibits excellent properties in paintability, weldability and coating corrosion resistance due to the surface structure resulting from the alloying reaction.
그러나, 합금화 용융아연 도금강판은 합금화의 정도에 따라 가공성, 도장내식성 등제특성이 다르게 나타나고 용도에 적합한 합금화도를 설정하여 관리하고 있을 정도로 합금화도에 다라 제특성이 민감하게 영향을 받는다. 따라서 우선적으로 도금층 내의 철함량을 분석하는 것이 중요하다.However, alloying hot-dip galvanized steel sheet is affected by the degree of alloying degree sensitively depending on the degree of alloying, such as workability, coating corrosion resistance and other properties, and the degree of alloying suitable for the application is managed. Therefore, it is important to first analyze the iron content in the plating layer.
합금층내의 철함량을 분석하는 종래의 방법은 원자흡광분석법(AAS)로서 통상적으로 습식분석에 사용되고 있는데, 일정 면적의 합금화 용융아연 도금강판을 보통 염산 : 증류수 = 1 : 3 인 용액으로 용해시켜 그 용액을 원자흡광 분석기로 정량하는 방법이다.The conventional method of analyzing the iron content in the alloy layer is atomic absorption spectroscopy (AAS), which is commonly used for wet analysis. An alloyed hot-dip galvanized steel sheet of a certain area is usually dissolved in a solution of hydrochloric acid: distilled water = 1: 3. This method is used to quantify the solution by atomic absorption analyzer.
그러나, 상기 방법은 시편을 용해시키므로 한번 측정한 후에는 다시 그 시편을 이용할 수 없으며, 시편이 용해될 때까지 기다려야 하므로 시간이 많이 드는 등의 문제점이 있었다.However, since the method dissolves the specimen, it is not possible to use the specimen again after the measurement once, and there is a problem that it takes a lot of time because the specimen must wait until the specimen is dissolved.
이에 본 발명의 목적은 시편에 손상이 없는 형광 X-선 분석법을 이용하여 신속하고 비파괴적으로 합금화 용융아연 도금강판의 도금층내 철함량을 분석하는 방법을 제공하는데 있다.Accordingly, an object of the present invention to provide a method for analyzing the iron content in the plating layer of the alloyed hot-dip galvanized steel sheet quickly and non-destructively by using a fluorescence X-ray analysis without damage to the specimen.
본 발명에 의하면, 상기 형광 X-선 분석기에 의한 철의 X-선 강도와 상기 원자흡광 분석기를 이용하여 얻은 철함량과의 관계를 직선회귀식을 이용하여 X-선 강도와 도금층내의 철함량에 대한 1차 검량식을 구하고 측정하고자 하는 합금화 용융아연 도금강판을 절단하여 형광 X-선 분석기에 장입하여 X-선 강도를 측정한 다음 그 X-선 강도값을 상기 검량식에 대입함, 을 포함하는 합금화 용융아연 도금강판의 도금층내 철함량 정량분석방법이 제공한다.According to the present invention, the relationship between the X-ray intensity of iron by the fluorescence X-ray analyzer and the iron content obtained by using the atomic absorption analyzer is determined by the linear regression equation to the X-ray intensity and the iron content in the plating layer. Obtain the first calibration equation for the alloy, cut the alloyed hot-dip galvanized steel sheet to be measured and insert it into the fluorescence X-ray analyzer to measure the X-ray intensity, and then substitute the X-ray intensity value in the calibration equation. Provided is a method for quantitative analysis of iron content in a plating layer of an alloyed hot dip galvanized steel sheet.
이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.
본 발명에 따라 합금화 용융아연 도금강판의 도금층내 철함량을 정량 분석하기 위해서는 먼저 도금층내 철함량이 서로 다른 합금화 용융아연 도금강판을 준비하여 형광 X-선 분석기의 시편 홀더에 맞게 시편을 절단하여 형광 X-선 분석기에 장입하여 철의 X-선 강도를 측정한다.In order to quantitatively analyze the iron content in the plating layer of the alloyed hot-dip galvanized steel sheet according to the present invention, by first preparing an alloyed hot-dip galvanized steel sheet having different iron contents in the coated layer, cut the specimen to fit the specimen holder of the fluorescent X-ray analyzer It is loaded into an X-ray analyzer and the iron's X-ray intensity is measured.
또한 원자흡광 분석법을 통하여 다음과 같이 철함량을 측정한다. 형광 X-선 분석을 행한 시료를 염산 : 증류수 = 1 : 3인 용액으로 용해시킨 후 이를 여과지에서 여과하고 여액을 중탕하여 100ml로 채운 다음, 원자 흡광분석에 의하여 정량화한다.In addition, the iron content is measured by atomic absorption spectrometry as follows. The sample subjected to fluorescence X-ray analysis was dissolved in a solution of hydrochloric acid: distilled water = 1: 3, filtered on a filter paper, filled with 100 ml of a filtrate, and quantified by atomic absorption analysis.
상기와 같이 측정된 철의 X-선 강도와 철함량의 관계를 직선회귀식을 이용하여 1차선식의 검량선을 구한다.The first-line calibration curve is obtained from the linear regression relationship between the X-ray intensity and the iron content of iron measured as described above.
상기검량선의 일례는 하기 식(1)으로 나타낼 수 있으며 이를 그래프로 나타내면 제1도와 같이 된다.An example of the calibration curve may be represented by the following equation (1), which is shown in FIG.
Fe(도금층내 철함량 : wt％) = 12.5637 × I(철의 X-선 강도 kcps) - 98.9407．．(1)Fe (iron content in the plating layer: wt%) = 12.5637 × I (x-ray intensity kcps of iron)-98.9407. (1)
따라서, 도금층내 철함량을 측정하고자 하는 경우, 합금화 용융아연 도금강판의 시편을 채취하여 형광 X-선 분석법에 의해 철의 X-선 강도(I)를 측정하고, 이 측정된 값을 상기 식(1)에 대입하면 간편하게 합금화 용융아연 도금강판의 도금층내 철함량이 측정된다.Therefore, when the iron content in the plating layer is to be measured, a specimen of an alloyed hot-dip galvanized steel sheet is taken, and the X-ray intensity (I) of iron is measured by fluorescence X-ray analysis, and the measured value is expressed by the formula ( Substituting in 1), the iron content in the plating layer of the alloyed hot-dip galvanized steel sheet is easily measured.
이하, 본 실시예를 통해 본 발명을 보다 구체적으로 설명한다.Hereinafter, the present invention will be described in more detail with reference to the present embodiment.
[실시예]EXAMPLE
도금두께가 5.7㎛이고 아연도금층내 철함량이 서로 다른 합금화 용융아연 도금강판들을 준비하여 형관분석기 홀더에 적합한 크기로 절단하고, 형광 X-선 분석기에서 20㎸ × 2㎃의 조건으로 철의 X-선 강도를 kcps 단위로 측정한 다음, 상기 식(1)의 직선회귀식에 대입하여 철함량을 정량하고 그 결과를 하기표 1에 나타내었다.Alloyed hot-dip galvanized steel sheets having a plating thickness of 5.7 μm and having different iron contents in the galvanized layer were prepared and cut to a size suitable for a die tube analyzer holder. After measuring the line strength in kcps unit, the iron content was quantified by substituting the linear regression equation of Equation (1) and the results are shown in Table 1 below.
한편, 분석이 끝난 시편을 통상의 원자흡광분석법을 통하여 철함량을 측정하고, 그 결과를 하기표 1에 함께 나타내었다.On the other hand, the iron content of the analyzed specimens through a conventional atomic absorption spectrometry method was measured, and the results are shown in Table 1 together.
* 오차=본 발명법-원자흡광분석법* Error = Invention Method-Atomic Absorption Analysis Method
상기 표 1에 나타난 바와같이, 본 발명은 원자흡광법으로 측정된 값과의 오차가 ±0.8wt％ 이내 대체로 정밀도가 우수한 것을 알 수 있다.As shown in Table 1, the present invention can be seen that the error with the value measured by atomic absorption method is generally excellent within ± 0.8wt%.
상기한 바와같이 본 발명의 방법에 의하면, 시편을 형광 X-선 분석기에 장입하여 철의 X-선 강도값을 측정하여 철함량을 구함으로써 총 소요시간이 10분 이내이고 측정이 끝난 시편을 다시 사용할 수 있기 때문에 매우 신속하고 비파괴적으로 측정이 가능하게 된다.As described above, according to the method of the present invention, the specimen is charged into a fluorescence X-ray analyzer, and the iron content is obtained by measuring the X-ray intensity value of iron. This makes it possible to make measurements very quickly and nondestructively.
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