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CN108802084A - X ray fluorescence spectrometry analyzes method, aluminium hydroxide and its application of component content in aluminium hydroxide - Google Patents

X ray fluorescence spectrometry analyzes method, aluminium hydroxide and its application of component content in aluminium hydroxide Download PDF

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CN108802084A
CN108802084A CN201810604889.2A CN201810604889A CN108802084A CN 108802084 A CN108802084 A CN 108802084A CN 201810604889 A CN201810604889 A CN 201810604889A CN 108802084 A CN108802084 A CN 108802084A
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aluminum hydroxide
ray fluorescence
sample
content
fluorescence spectrometry
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李欣
庞振辉
丁天龙
贺立侠
吴宏
王长军
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CSG Holding Co Ltd
Hebei CSG Glass Co Ltd
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Hebei CSG Glass Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating 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
    • G01N23/22Investigating 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
    • G01N23/223Investigating 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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2866Grinding or homogeneising

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Abstract

本发明属于化工分析处理技术领域,涉及一种X射线荧光光谱法分析氢氧化铝中成分含量的方法、氢氧化铝及其应用。本发明的X射线荧光光谱法分析氢氧化铝中成分含量的方法,包括以下步骤:研磨;粉末压片;采用X射线荧光光谱法,测定样片中各成分的发射强度,利用已建立的各成分的工作曲线,进行待测氢氧化铝样片中Al2O3、Fe2O3、SiO2和Na2O含量的分析。本发明方法操作简单,分析速度快,可同时分析氢氧化铝中Al2O3、Fe2O3、SiO2、Na2O四项成分,通过确认该方法具有科学性、先进性、适用性、分析时间短、准确度高、重复性好、无污染等特点;重复性和再现性均优于国家标准的氢氧化铝中化学成分的测定方法。The invention belongs to the technical field of chemical analysis and treatment, and relates to a method for analyzing component content in aluminum hydroxide by X-ray fluorescence spectrometry, aluminum hydroxide and application thereof. The method for analyzing the content of components in aluminum hydroxide by X-ray fluorescence spectrometry of the present invention comprises the following steps: grinding; powder pressing; adopting X-ray fluorescence spectrometry to measure the emission intensity of each component in the sample, and using the established components The working curve is used to analyze the content of Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O in the aluminum hydroxide sample to be tested. The method of the invention is simple in operation and fast in analysis speed, and can simultaneously analyze four components of Al 2 O 3 , Fe 2 O 3 , SiO 2 , and Na 2 O in aluminum hydroxide. It has been confirmed that the method is scientific, advanced, and applicable , short analysis time, high accuracy, good repeatability, no pollution, etc.; the repeatability and reproducibility are better than the national standard method for the determination of chemical components in aluminum hydroxide.

Description

X射线荧光光谱法分析氢氧化铝中成分含量的方法、氢氧化铝 及其应用Method for analyzing component content in aluminum hydroxide by X-ray fluorescence spectrometry, aluminum hydroxide and its application

技术领域technical field

本发明属于化工分析处理技术领域,具体而言,涉及一种X射线荧光光谱法分析氢氧化铝中成分含量的方法、氢氧化铝及其应用。The invention belongs to the technical field of chemical analysis and processing, and in particular relates to a method for analyzing component content in aluminum hydroxide by X-ray fluorescence spectrometry, aluminum hydroxide and applications thereof.

背景技术Background technique

氢氧化铝是一种应用广泛的工业原料,可以用于制造药物、阻燃剂、防水织物、油墨、玻璃等领域。例如,氢氧化铝应用在浮法玻璃生产领域时,主要起着引入Al2O3成分的作用,而玻璃配料计算需采用氢氧化铝化学成分。氢氧化铝的质量直接影响玻璃的成分、成型粘度、物理化学等性能;在玻璃生产过程中,氢氧化铝的成分大部分转入玻璃之中,因而氢氧化铝中成分及成分的含量的变化会引起玻璃成分及含量变化,对玻璃的实际应用或使用性能造成影响。由于氢氧化铝中的主要成分不仅包含Al2O3,还包含Fe2O3、SiO2、Na2O等成分。因此准确测定出氢氧化铝中主要化学成分及其含量对于浮法玻璃的生产具有一定的指导意义。Aluminum hydroxide is a widely used industrial raw material, which can be used in the manufacture of medicines, flame retardants, waterproof fabrics, inks, glass and other fields. For example, when aluminum hydroxide is used in the field of float glass production, it mainly plays the role of introducing Al 2 O 3 components, and the chemical composition of aluminum hydroxide is required for the calculation of glass batching. The quality of aluminum hydroxide directly affects the composition, molding viscosity, physical and chemical properties of the glass; in the process of glass production, most of the composition of aluminum hydroxide is transferred into the glass, so the composition and content of aluminum hydroxide change It will cause changes in the composition and content of the glass, and affect the actual application or performance of the glass. Because the main components in aluminum hydroxide include not only Al 2 O 3 , but also Fe 2 O 3 , SiO 2 , Na 2 O and other components. Therefore, the accurate determination of the main chemical components and their contents in aluminum hydroxide has certain guiding significance for the production of float glass.

目前分析氢氧化铝原料中各成分含量的方法多采用如下氢氧化铝行业相关标准(YS/T534.2~534.5)(GB/T6610.2~6610.5)化学分析方法:At present, the method of analyzing the content of each component in the raw material of aluminum hydroxide mostly adopts the following chemical analysis method of the relevant standards of the aluminum hydroxide industry (YS/T534.2~534.5) (GB/T6610.2~6610.5):

烧失量(灼减)的测定采用重量法;The loss on ignition (loss on ignition) is measured by gravimetric method;

二氧化硅含量的测定采用钼蓝光度法;The determination of silicon dioxide content adopts the molybdenum blue photometric method;

三氧化二铁含量的测定采用邻二氮杂菲光度法;The determination of ferric oxide content adopts o-phenanthrene photometry;

氧化钠含量的测定采用火焰分光光度法/火焰原子吸收光谱法;The determination of sodium oxide content adopts flame spectrophotometry/flame atomic absorption spectrometry;

三氧化二铝含量为:100%减去二氧化硅、氧化钠、三氧化二铁和灼减量的总和,即w(Al2O3)=100%-w(SiO2)-w(Na2O)-w(Fe2O3)-灼减。The content of aluminum oxide is: 100% minus the sum of silicon dioxide, sodium oxide, iron oxide and ignition loss, that is, w(Al 2 O 3 )=100%-w(SiO 2 )-w(Na 2 O)-w(Fe 2 O 3 )-Ignition loss.

上述化学分析方法每个项目需要单独检测,只能单个元素分析,操作过程复杂,样品前处理繁杂,环节多,涉及知识点多,仪器操作难度大,耗时长(单个样品需一周时间),消耗试剂多、涉及危化品使用,化学药剂投入费用多,同时大量药品的使用也增加了污染物的排放,会对环境造成污染。此外,测量的重复性较差,结果的准确性较差,各项检测结果(SiO2、Fe2O3、Na2O、灼减的检测结果)误差容易叠加在Al2O3上。Each item of the above-mentioned chemical analysis method needs to be tested separately, and only a single element can be analyzed. The operation process is complicated, the sample pretreatment is complicated, there are many links, and many knowledge points are involved. There are many reagents, the use of hazardous chemicals is involved, and the cost of chemical agents is high. At the same time, the use of a large number of drugs also increases the discharge of pollutants, which will pollute the environment. In addition, the repeatability of the measurement is poor, and the accuracy of the results is poor, and the errors of various test results (SiO 2 , Fe 2 O 3 , Na 2 O, and burn-off test results) are easily superimposed on Al 2 O 3 .

鉴于此,特提出本发明。In view of this, the present invention is proposed.

发明内容Contents of the invention

本发明的第一目的在于提供一种操作简单,样品处理简单,分析周期短,没有化学污染,准确度高,重复性好的X射线荧光光谱法分析氢氧化铝中成分含量的方法,以缓解现有技术中测量氢氧化铝中成分含量存在的问题。The first object of the present invention is to provide a kind of simple operation, simple sample processing, short analysis cycle, no chemical pollution, high accuracy, good repeatability X-ray fluorescence spectrometry analysis of the composition content of aluminum hydroxide method, to alleviate There are problems in measuring the content of components in aluminum hydroxide in the prior art.

本发明的第二目的在于提供一种经过所述的X射线荧光光谱法分析氢氧化铝中成分含量的方法分析后得到的氢氧化铝。本发明的第三目的在于提供一种所述的氢氧化铝在作为生产浮法玻璃的原料中的应用。通过本发明的方法能够快速、准确的得到氢氧化铝中成分含量的检验数据,将该氢氧化铝应用到生产浮法玻璃中,能够确保玻璃的成分含量,使玻璃的质量得到保证。The second object of the present invention is to provide an aluminum hydroxide obtained after analysis by the method for analyzing the content of components in aluminum hydroxide by the X-ray fluorescence spectrometry. The third object of the present invention is to provide an application of the aluminum hydroxide as a raw material for producing float glass. The method of the invention can quickly and accurately obtain the inspection data of the component content in the aluminum hydroxide, and the application of the aluminum hydroxide to the production of float glass can ensure the component content of the glass and ensure the quality of the glass.

为实现上述目的,本发明采用的技术方案为:To achieve the above object, the technical solution adopted in the present invention is:

根据本发明的一个方面,本发明提供一种X射线荧光光谱法分析氢氧化铝中成分含量的方法,包括以下步骤:According to one aspect of the present invention, the present invention provides a kind of X-ray fluorescence spectrometry method analysis composition content method in aluminum hydroxide, comprises the following steps:

研磨;grinding;

粉末压片;powder compression;

采用X射线荧光光谱法,测定样片中各成分的发射强度,利用已建立的各成分的工作曲线,进行待测氢氧化铝样片中Al2O3、Fe2O3、SiO2和Na2O含量的分析。Use X-ray fluorescence spectrometry to measure the emission intensity of each component in the sample, and use the established working curve of each component to measure Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O in the aluminum hydroxide sample to be tested. content analysis.

作为进一步优选技术方案,研磨的时间为15~35min,研磨得到的试样的粒度≤200目,优选为80~150目。As a further preferred technical solution, the grinding time is 15-35 minutes, and the particle size of the sample obtained by grinding is ≤200 mesh, preferably 80-150 mesh.

作为进一步优选技术方案,粉末压片过程中,压力30~50MPa,静压20~40s。As a further preferred technical solution, during the powder compression process, the pressure is 30-50 MPa, and the static pressure is 20-40s.

作为进一步优选技术方案,建立各成分的工作曲线的方式包括:As a further preferred technical solution, the mode of establishing the working curve of each component includes:

提供多个氢氧化铝标准样品,各标准样品中Al2O3、Fe2O3、SiO2和Na2O所占的质量比各不相同;Provide multiple aluminum hydroxide standard samples, and the mass ratios of Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O in each standard sample are different;

将标准样品分别进行研磨和粉末压片,制得标准样品压片;Grinding and powder pressing the standard samples respectively to obtain standard sample pressing;

采用X射线荧光光谱仪分别测定标准样品压片中各成分的发射强度;Adopt X-ray fluorescence spectrometer to measure the emission intensity of each component in the standard sample compression tablet respectively;

将X射线荧光特征谱线强度和相对应的Al2O3、Fe2O3、SiO2和Na2O质量百分含量进行线性回归,分别得到Al2O3、Fe2O3、SiO2和Na2O对应X射线荧光特征谱线强度的标准工作曲线。Perform linear regression on the intensity of X-ray fluorescence characteristic lines and the corresponding mass percentages of Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O to obtain Al 2 O 3 , Fe 2 O 3 , and SiO 2 The standard working curve of X-ray fluorescence characteristic line intensity corresponding to Na 2 O.

作为进一步优选技术方案,标准样品的数量为≥4个。As a further preferred technical solution, the number of standard samples is ≥4.

作为进一步优选技术方案,研磨的时间为15~35min,研磨得到的试样的粒度≤200目,优选为80~150目;As a further preferred technical solution, the grinding time is 15-35 minutes, and the particle size of the sample obtained by grinding is ≤200 mesh, preferably 80-150 mesh;

和/或,粉末压片过程中,压力30~50MPa,静压20~40s。And/or, during the powder compression process, the pressure is 30-50MPa, and the static pressure is 20-40s.

作为进一步优选技术方案,对样片利用X射线荧光光谱仪测定氢氧化铝中各成分的测定条件分别为:As a further preferred technical solution, the measurement conditions for the samples to be determined by X-ray fluorescence spectrometer for each component in aluminum hydroxide are respectively:

Al2O3:2θ144.65,波长电压30kV,电流80mA,分光晶体PET,准直器0.25,PHD40~100,干扰元素无,扫描时间20s;Al 2 O 3 : 2θ144.65, wavelength Voltage 30kV, current 80mA, spectroscopic crystal PET, collimator 0.25, PHD40~100, no interference elements, scan time 20s;

Fe2O3:2θ57.53,波长电压30kV,电流80mA,分光晶体LiF200,准直器0.15,PHD40~100,干扰元素无,扫描时间20s;Fe 2 O 3 : 2θ57.53, wavelength Voltage 30kV, current 80mA, spectroscopic crystal LiF200, collimator 0.15, PHD40~100, no interference elements, scan time 20s;

SiO2:2θ109.001,波长电压30kV,电流80mA,分光晶体PET,准直器0.60,PHD50~95,干扰元素无,扫描时间12s;SiO 2 : 2θ109.001, wavelength Voltage 30kV, current 80mA, spectroscopic crystal PET, collimator 0.60, PHD50~95, no interference elements, scan time 12s;

Na2O:2θ23.951,波长电压30kV,电流80mA,分光晶体AX06,准直器0.60,PHD40~100,干扰元素无,扫描时间20s。Na2O: 2θ23.951 , wavelength Voltage 30kV, current 80mA, spectroscopic crystal AX06, collimator 0.60, PHD40~100, no interference elements, scan time 20s.

作为进一步优选技术方案,所述样片包括待测氢氧化铝样片和标准样品样片。As a further preferred technical solution, the samples include aluminum hydroxide samples to be tested and standard sample samples.

根据本发明的另一个方面,本发明提供一种经过上述的X射线荧光光谱法分析氢氧化铝中成分含量的方法分析后得到的氢氧化铝。According to another aspect of the present invention, the present invention provides an aluminum hydroxide obtained after being analyzed by the above-mentioned method for analyzing component content in aluminum hydroxide by X-ray fluorescence spectrometry.

根据本发明的另一个方面,本发明还提供一种所述的氢氧化铝在作为生产浮法玻璃的原料中的应用。According to another aspect of the present invention, the present invention also provides an application of the above-mentioned aluminum hydroxide as a raw material for producing float glass.

与现有技术相比,本发明的有益效果在于:Compared with prior art, the beneficial effect of the present invention is:

1、本发明用X射线荧光光谱分析法确定氢氧化铝中化学成分的含量,通过对氢氧化铝原料进行研磨处理,粉末直接压片制样,然后直接用X射线荧光光谱分析仪扫描,测定其中的化学成分的含量。该方法操作简单,分析速度快,可同时分析氢氧化铝中Al2O3、Fe2O3、SiO2、Na2O四项成分,准确度高,重复性好,填补了用X射线荧光粉末压片分析测试氢氧化铝中化学成分的空白。1. The present invention uses X-ray fluorescence spectroscopic analysis to determine the content of chemical components in aluminum hydroxide. By grinding the aluminum hydroxide raw material, the powder is directly pressed into tablets to prepare samples, and then directly scanned with an X-ray fluorescence spectrometer to measure The content of chemical components in it. The method is easy to operate and fast in analysis speed. It can simultaneously analyze the four components of Al 2 O 3 , Fe 2 O 3 , SiO 2 , and Na 2 O in aluminum hydroxide with high accuracy and good repeatability. Powder tablet analysis to test the blank for chemical composition in aluminum hydroxide.

2、本发明粉末压片法制样,操作方法简单,样品前处理操作简单,分析周期短、速度快,准确度高,重复性和再现性均优于国家标准中的氢氧化铝中化学成分的测定方法,具有科学性、先进性、适用性、可推广性、无污染、分析时间短、准确度高、重复性好、无损分析等特点。2. The powder tableting method of the present invention has the advantages of simple operation method, simple sample pretreatment operation, short analysis period, fast speed, high accuracy, repeatability and reproducibility are better than the chemical composition of aluminum hydroxide in the national standard The determination method has the characteristics of scientificity, advancement, applicability, scalability, no pollution, short analysis time, high accuracy, good repeatability, and non-destructive analysis.

具体实施方式Detailed ways

下面将结合实施方式和实施例对本发明的实施方案进行详细描述,但是本领域技术人员将会理解,下列实施方式和实施例仅用于说明本发明,而不应视为限制本发明的范围。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。未注明具体条件者,按照常规条件或制造商建议的条件进行。The embodiments of the present invention will be described in detail below in conjunction with the embodiments and examples, but those skilled in the art will understand that the following embodiments and examples are only for illustrating the present invention, and should not be regarded as limiting the scope of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention. If the specific conditions are not specified, follow the general conditions or the conditions suggested by the manufacturer.

第一方面,在至少一个实施例中提供一种X射线荧光光谱法分析氢氧化铝中成分含量的方法,包括以下步骤:In a first aspect, in at least one embodiment, there is provided a method for X-ray fluorescence spectrometry analysis of component content in aluminum hydroxide, comprising the following steps:

研磨;grinding;

粉末压片;powder compression;

采用X射线荧光光谱法,测定样片中各成分的发射强度,利用已建立的各成分的工作曲线,进行待测氢氧化铝样片中Al2O3、Fe2O3、SiO2和Na2O含量的分析。Use X-ray fluorescence spectrometry to measure the emission intensity of each component in the sample, and use the established working curve of each component to measure Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O in the aluminum hydroxide sample to be tested. content analysis.

X射线荧光光谱分析法(XRF)具有准确、快速、分析范围广的特点,广泛应用于地质、冶金、机械制造、环保、化工等领域,该方法相对于化学分析方法,样品前处理简单,化学试剂用量少,排放废弃物少,准确度和精密度高。但是目前还没有该法完整的检测方法应用于氢氧化铝材料中成分的含量的测定。基于此,本发明提供了一种X射线荧光光谱法分析氢氧化铝中成分含量的方法,填补了用X射线荧光粉末压片分析测试氢氧化铝中化学成分的空白。X-ray fluorescence spectrometry (XRF) has the characteristics of accuracy, rapidity and wide analysis range, and is widely used in geology, metallurgy, machinery manufacturing, environmental protection, chemical industry and other fields. Compared with chemical analysis methods, this method has simple sample pretreatment and chemical Less reagent consumption, less waste discharge, high accuracy and precision. However, there is no complete detection method of this method applied to the determination of the content of components in aluminum hydroxide materials. Based on this, the present invention provides a method for analyzing the content of components in aluminum hydroxide by X-ray fluorescence spectrometry, which fills the blank of using X-ray fluorescence powder tablet analysis to test the chemical components in aluminum hydroxide.

本发明用X射线荧光光谱分析法测定氢氧化铝中化学成分,对氢氧化铝进行研磨处理,粉末直接压片制样,直接用X射线荧光光谱分析仪扫描,测定其中化学成分的含量,操作简单,分析速度快,可同时分析氢氧化铝中Al2O3、Fe2O3、SiO2、Na2O四项成分。本发明经过对氢氧化铝试样的特性分析的特点是:操作简单,重复性和再现性均优于国家标准的氢氧化铝中化学成分的测定方法(YS/T534.2~534.5)(GB/T6610.2~6610.5),具有科学性、先进性、适用性、可推广性,分析时间短、没有化学污染、准确度高、重复性好、无损分析等特点。进一步地讲,相对与现有的标准化学法测定氢氧化铝中的成分含量,本发明主要具有以下优势:The present invention uses the X-ray fluorescence spectroscopic analysis method to measure the chemical components in aluminum hydroxide, grinds the aluminum hydroxide, directly compresses the powder to prepare samples, and scans directly with an X-ray fluorescence spectrometer to measure the content of the chemical components. Simple, fast analysis speed, can simultaneously analyze four components of Al 2 O 3 , Fe 2 O 3 , SiO 2 , and Na 2 O in aluminum hydroxide. The characteristics of the present invention through the characteristic analysis of the aluminum hydroxide sample are: simple operation, repeatability and reproducibility all better than the determination method of chemical composition in the aluminum hydroxide of national standard (YS/T534.2~534.5) (GB /T6610.2~6610.5), with scientific, advanced, applicability, scalability, short analysis time, no chemical pollution, high accuracy, good repeatability, non-destructive analysis and other characteristics. Further speaking, relative to the existing standard chemical method for determining the composition content in aluminum hydroxide, the present invention mainly has the following advantages:

(1)经济效益:节约了大量化学药品的使用,降低了检测成本;操作简单,减少了操作人员的配置,降低了人员成本。(1) Economic benefits: the use of a large number of chemicals is saved, and the cost of detection is reduced; the operation is simple, the configuration of operators is reduced, and the cost of personnel is reduced.

(2)时间效益:样品前处理简单、快速,可以多元素同时测定,一个样品分析由原来的1-2天缩短至1-2小时,减少了检测时间和人力消耗,检测周期短,还解决了人员劳动强度大、人员不足的问题。(2) Time benefit: sample pretreatment is simple and fast, and multiple elements can be determined at the same time. The analysis of a sample is shortened from the original 1-2 days to 1-2 hours, which reduces the detection time and manpower consumption, and the detection cycle is short. Solved the problem of high labor intensity and insufficient personnel.

(3)环境效益:大大减少有毒有害化学药品的使用和废酸液等废弃物的排放,无环境污染,环保效益好。(3) Environmental benefits: greatly reduce the use of toxic and harmful chemicals and the discharge of wastes such as waste acid, no environmental pollution, and good environmental protection benefits.

(4)分析误差小,准确度高,重复性好,可以够快速、准确的发出检验数据结果,及时为生产提供有利的分析数据指导,确保最终得到的产品质量。(4) The analysis error is small, the accuracy is high, and the repeatability is good. It can quickly and accurately send out the test data results, and provide favorable analysis data guidance for production in time to ensure the final product quality.

本发明的工作原理可以理解为:Working principle of the present invention can be understood as:

X射线照射在物质上而产生的次级X射线叫X射线荧光,每一种元素会放射出对应的X射线荧光,测量这些放射出来的X射线荧光,转换成样品中各种元素的种类及含量。The secondary X-rays produced by X-rays irradiating on the material are called X-ray fluorescence. Each element will emit corresponding X-ray fluorescence. The emitted X-ray fluorescence is measured and converted into the types and types of various elements in the sample. content.

动作关系:Action relationship:

研磨→压片→X射线荧光光谱仪检测Grinding→pressing→X-ray fluorescence spectrometer detection

本发明用X射线荧光光谱分析法测定氢氧化铝中化学成分的方法,包含如下工艺步骤:对氢氧化铝进行研磨处理,粉末直接压片制样,直接用X射线荧光光谱分析仪扫描,测定其中化学成分的含量。The method for determining the chemical components in aluminum hydroxide by X-ray fluorescence spectroscopic analysis in the present invention comprises the following process steps: grinding the aluminum hydroxide, directly compressing the powder to prepare samples, scanning directly with an X-ray fluorescence spectrometer, and measuring The content of chemical components in it.

在一种优选的实施方式中,本发明的方法主要包括(a)建立标准工作曲线和(b)测定待测氢氧化铝试样中的Al2O3、Fe2O3、SiO2和Na2O的含量。In a preferred embodiment, the method of the present invention mainly includes (a) establishing a standard working curve and (b) determining Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na in the aluminum hydroxide sample to be tested. 2 O content.

优选地,(a)建立标准工作曲线,包括:Preferably, (a) establish a standard working curve, including:

1)提供多个氢氧化铝标准样品,各标准样品中Al2O3、Fe2O3、SiO2和Na2O所占的质量比各不相同;1) Provide multiple aluminum hydroxide standard samples, and the mass ratios of Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O in each standard sample are different;

即,在选取标准样品时,需按照氢氧化铝中各元素不同含量水平选用用以建立曲线的标准样品至少4个;That is, when selecting standard samples, it is necessary to select at least 4 standard samples for establishing curves according to the different content levels of each element in aluminum hydroxide;

需要说明的是,氢氧化铝标准样品的数量并不受特别限制,本领域技术人员可以根据实际需要进行选择,根据本发明的一个具体实施例,氢氧化铝标准样品的数量可以不少于4个。发明人发现,当氢氧化铝标准样品的数量不少于4个时,可以更好的满足后续标准工作曲线的精度要求,从而使得本发明提供的基于X射线荧光光谱法测定氢氧化铝待测样品中各成分含量所得的数值与化学法得到的定值误差更小。It should be noted that the number of aluminum hydroxide standard samples is not particularly limited, and those skilled in the art can select according to actual needs. According to a specific embodiment of the present invention, the number of aluminum hydroxide standard samples can be no less than 4 indivual. The inventors have found that when the number of aluminum hydroxide standard samples is not less than 4, the accuracy requirements of the follow-up standard working curve can be better met, so that the determination of aluminum hydroxide based on X-ray fluorescence spectrometry provided by the present invention The value obtained by the content of each component in the sample has smaller errors than the fixed value obtained by the chemical method.

例如可以为,根据日常检测样品的含量,选择适合的一系列标样,所选用的系列标准样品如表1所示。For example, a series of standard samples can be selected according to the content of daily detection samples, and the selected series of standard samples are shown in Table 1.

表1标准样品Table 1 standard sample

2)试样研磨:在每个样品中称取5-10克氢氧化铝标准样品于研钵中,连续研磨15~35min,例如可以为研磨15min、20min、25min、30min或35min,试样粒度达到≤200目,例如可以为粒度200目、180目、160目、150目、120目、100目、90目、80目、60目、50目或40目等,优选为80~150目,保证试样均匀,满足荧光粉末压片要求即可。2) Sample grinding: Weigh 5-10 grams of aluminum hydroxide standard sample in a mortar and grind it continuously for 15-35 minutes. For example, it can be ground for 15 minutes, 20 minutes, 25 minutes, 30 minutes or 35 minutes. Reach ≤200 mesh, for example, the particle size can be 200 mesh, 180 mesh, 160 mesh, 150 mesh, 120 mesh, 100 mesh, 90 mesh, 80 mesh, 60 mesh, 50 mesh or 40 mesh, etc., preferably 80-150 mesh, Ensure that the sample is uniform and meet the requirements for fluorescent powder compression.

需要说明的是,本发明在研磨过程中不加入任何的助剂。这样不仅可以减少粘结剂或其他助剂等带来的环境污染,还可以进一步降低检测成本,提升检测速度。It should be noted that the present invention does not add any auxiliary agent during the grinding process. This can not only reduce the environmental pollution caused by binders or other additives, but also further reduce the detection cost and increase the detection speed.

3)粉末压片:采用压样机将标准样品进行粉末压片,制得标准样品压片;具体包括:擦洗压样用托盘,塑料环内壁、外壁、两个断面,置于1/100天平上,清零,一次性称量5克研磨后样品,压平,压样机压样,压力30~50MPa,静压20~40s,保持样片表面光滑,粒度均匀,清扫塑料环边缘残余粉末,样品标识待用。清洗研钵备用。典型但非限制的,压力可以为30MPa、35MPa、40MPa、45MPa或50MPa,静压20s、25s、30s、35s或40s。3) Powder compression: Use a press to perform powder compression on the standard sample to obtain a standard sample compression; specifically include: scrubbing the tray for sample compression, the inner wall, outer wall, and two sections of the plastic ring, and placing them on a 1/100 balance , clear, weigh 5 grams of the ground sample at one time, press it flat, press the sample with a press, press 30-50MPa, and press statically for 20-40s to keep the surface of the sample smooth and uniform in particle size, clean the residual powder on the edge of the plastic ring, and identify the sample stand-by. Clean the mortar and set aside. Typically but not limited, the pressure can be 30MPa, 35MPa, 40MPa, 45MPa or 50MPa, and the static pressure is 20s, 25s, 30s, 35s or 40s.

需要说明的是,本发明对于粉末压片过程中的具体操作参数不做特殊限制,本领域技术人员可以根据实际情况进行调整,只要得到的压片满足后续的X射线荧光光谱仪的分析测定即可。该粉末压片可以在配备的专用压样机上常温操作,步骤简单,速度快,易于操作。It should be noted that the present invention has no special restrictions on the specific operating parameters in the process of powder compression, and those skilled in the art can adjust them according to the actual situation, as long as the obtained compression meets the analysis and determination of the subsequent X-ray fluorescence spectrometer. . The powder compression tablet can be operated at room temperature on the equipped special press, with simple steps, fast speed and easy operation.

4)荧光分析:采用X射线荧光光谱仪分别测定标准样品压片中各成分的发射强度;4) Fluorescence analysis: adopt X-ray fluorescence spectrometer to measure the emission intensity of each component in the standard sample compression tablet respectively;

本发明确定最佳分析条件的思路包括:选择化学成分与待测样接近的样品进行扫描,一般选择Kα1,2线作为分析谱线,最大峰位为实际检测峰位;分光晶体的一般选择原则是LiF适合Ni~Te范围内的大部分元素,PET适合于Al~Cl范围内的元素;光管电压、电流、准直器等因素要综合考虑,尽量保持荧光强度处于仪器最佳分辨率范围;PHD(脉冲高度分布)窗口分析尽可能加大窗口;背景一般选择两点作为背景,当特征信号强度高于背景信号10倍以上时,可以忽略背景强度,以缩短扫描时间;分析时间在扫描信号偏差小于0.3%时作为最佳分析时间。The idea of determining the optimal analysis conditions in the present invention includes: selecting a sample whose chemical composition is close to the sample to be tested for scanning, generally selecting the Kα1, 2 line as the analysis line, and the maximum peak position is the actual detection peak position; the general selection principle of the spectroscopic crystal LiF is suitable for most elements in the range of Ni~Te, and PET is suitable for elements in the range of Al~Cl; factors such as light tube voltage, current, and collimator should be considered comprehensively, and the fluorescence intensity should be kept within the optimal resolution range of the instrument as much as possible. ; PHD (Pulse Height Distribution) window analysis should enlarge the window as much as possible; the background generally chooses two points as the background, when the characteristic signal intensity is more than 10 times higher than the background signal, the background intensity can be ignored to shorten the scanning time; When the signal deviation is less than 0.3%, it is regarded as the best analysis time.

本发明最终确定的最佳分析条件如表2所示。The optimal analytical conditions finally determined by the present invention are shown in Table 2.

表2分析条件Table 2 Analysis conditions

5)利用对一系列内控标准样品测量得到的各成分的反射强度,结合各成分在试样中的质量百分含量,将X射线荧光特征谱线强度和相对应的Al2O3、Fe2O3、SiO2和Na2O质量百分含量进行线性回归,分别得到Al2O3、Fe2O3、SiO2和Na2O对应X射线荧光特征谱线强度的标准工作曲线。以质量百分含量为横坐标,XRF测定强度为纵坐标绘制各成分的工作曲线。5) Using the reflection intensity of each component measured for a series of internal control standard samples, combined with the mass percentage of each component in the sample, the X-ray fluorescence characteristic line intensity and the corresponding Al 2 O 3 , Fe 2 The standard working curves of Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O corresponding to X-ray fluorescence characteristic spectral line intensities were obtained through linear regression for the mass percentages of O 3 , SiO 2 and Na 2 O . The working curve of each component is drawn with the mass percent content as the abscissa and the XRF measured intensity as the ordinate.

所测标样中,各成分百分含量与强度相关联的标准工作曲线的相关参数如表3所示。In the measured standard sample, the relevant parameters of the standard working curve associated with the percentage content of each component and the strength are shown in Table 3.

表3工作曲线Table 3 Working Curve

项目project 截距intercept 斜率slope SEESEE Al2O3 Al 2 O 3 34.7332234.73322 0.045020.04502 0.0178200.017820 Fe2O3 Fe2O3 _ 0.001300.00130 0.013480.01348 0.0007760.000776 SiO2 SiO 2 -0.00352-0.00352 0.109410.10941 0.0037930.003793 Na2ONa 2 O -0.05169-0.05169 0.108910.10891 0.1037560.103756

可将表3得到的各成分的回归方程式的相关参数,通过计算机软件编入X射线荧光光谱仪的控制程序中。The relevant parameters of the regression equation of each component obtained in Table 3 can be programmed into the control program of the X-ray fluorescence spectrometer through computer software.

优选地,(b)测定待测氢氧化铝试样中的Al2O3、Fe2O3、SiO2和Na2O的含量,包括:Preferably, (b) determining the content of Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O in the aluminum hydroxide sample to be tested includes:

1)试样研磨;1) Sample grinding;

2)粉末压片;2) Powder compression;

该过程中的试样研磨和粉末压片的具体操作方式和操作参数与上述标准工作曲线的建立过程中的试样研磨和粉末压片的具体操作方式和操作参数相同,在此不再赘述;The specific operation mode and operating parameters of the sample grinding and powder pressing in this process are the same as the specific operating mode and operating parameters of the sample grinding and powder pressing in the establishment process of the above-mentioned standard working curve, and will not be repeated here;

3)采用X射线荧光光谱仪测定待测氢氧化铝样片中各成分的发射强度;荧光光谱仪中的控制程序会自动根据表3中的相关参数计算得出待测氢氧化铝样片中各成分的质量百分含量;3) Adopt X-ray fluorescence spectrometer to measure the emission intensity of each component in the aluminum hydroxide sample to be measured; the control program in the fluorescence spectrometer can automatically calculate the quality of each component in the aluminum hydroxide sample to be measured according to the relevant parameters in Table 3 percentage content;

该过程中的X射线荧光光谱仪的分析条件与上述标准工作曲线的建立过程中的分析条件相同,在此不再赘述。The analysis conditions of the X-ray fluorescence spectrometer in this process are the same as the analysis conditions in the process of establishing the above-mentioned standard working curve, and will not be repeated here.

在一个具体的实施方式中,利用本发明的方法测定氢氧化铝中成分含量的方法所采用的设备例如可以为:In a specific embodiment, the equipment adopted in the method for determining the component content in aluminum hydroxide by the method of the present invention can be, for example:

波长色散型X射线荧光光谱分析仪;探测器为流气正比计数器和闪烁计数器;最大功率3.6kW;Wavelength dispersive X-ray fluorescence spectrometer; the detector is a gas flow proportional counter and a scintillation counter; the maximum power is 3.6kW;

ZHY-401A压样机;以及Ф12cm的玛瑙研钵。ZHY-401A sample press; and Ф12cm agate mortar.

为分析通过本发明的方法测定样片中各成分的含量的准确度,本发明根据以上样品制备方法和分析条件对现有样品进行分析,并与市售产品提供的标准值、标准化学法的检测结果做对比,分析数据结果见表4。In order to analyze the accuracy of determining the content of each component in the sample sheet by the method of the present invention, the present invention analyzes the existing samples according to the above sample preparation method and analysis conditions, and compares with the standard value provided by commercially available products, the detection of standard chemical methods For comparison, the results of the analysis data are shown in Table 4.

表4准确度分析结果Table 4 Accuracy analysis results

对本发明所用方法测得结果的精密度进行试验,取一氢氧化铝试样,按照上述试样研磨和粉末压片方法分别制备10个样片,采用X射线荧光光谱仪按照上述分析条件分别对各样片进行测定,测定结果见表5。Test the precision of the results obtained by the method used in the present invention, get an aluminum hydroxide sample, prepare 10 sample sheets respectively according to the above-mentioned sample grinding and powder tabletting methods, adopt an X-ray fluorescence spectrometer to analyze each sample sheet according to the above-mentioned analysis conditions Determination was carried out, and the measurement results are shown in Table 5.

表5精密度测试结果Table 5 precision test results

检测项目Test items Al2O3 Al 2 O 3 Fe2O3 Fe2O3 _ SiO2 SiO 2 Na2ONa 2 O 样片1Sample 1 64.6364.63 0.00960.0096 0.0100.010 0.150.15 样片2Sample 2 64.4764.47 0.00900.0090 0.0110.011 0.130.13 样片3Sample 3 64.7564.75 0.00870.0087 0.0110.011 0.120.12 样片4Sample 4 64.7664.76 0.00880.0088 0.0100.010 0.140.14 样片5Sample 5 64.5964.59 0.00950.0095 0.0120.012 0.160.16 样片6Sample 6 64.8164.81 0.00890.0089 0.0100.010 0.130.13 样片7Sample 7 64.5764.57 0.00910.0091 0.0100.010 0.120.12 样片8Sample 8 64.5164.51 0.00940.0094 0.0110.011 0.130.13 样片9Sample 9 64.4364.43 0.00910.0091 0.0120.012 0.140.14 样片10Sample 10 64.4964.49 0.00930.0093 0.0090.009 0.110.11 平均值average value 64.6064.60 0.009140.00914 0.01060.0106 0.1330.133 SDSD 0.1330.133 0.0000.000 0.0010.001 0.0150.015 RSDRSD 0.0020.002 0.0330.033 0.0910.091 0.1120.112

其中,SD表示标准偏差,RSD表示相对标准偏差,二者的数值均在合理的范围内,本发明的方法的检测精确度高。Wherein, SD represents the standard deviation, and RSD represents the relative standard deviation, both values are within a reasonable range, and the detection accuracy of the method of the present invention is high.

通过表4和表5的对比数据可知,本发明的X射线荧光光谱法分析氢氧化铝中成分含量的方法的准确度及精密度极高,重复性和再现性优于标准化学法,完全可以替代现有技术中的标准化学法测定氢氧化铝。同时本发明的方法操作简单,分析时间短,无化学污染,成本低。By the comparative data of table 4 and table 5, it can be seen that the accuracy and precision of the method for analyzing the content of components in aluminum hydroxide by X-ray fluorescence spectrometry of the present invention are extremely high, and the repeatability and reproducibility are better than standard chemical methods, which can fully It replaces the standard chemical method in the prior art to determine aluminum hydroxide. Simultaneously, the method of the invention has simple operation, short analysis time, no chemical pollution and low cost.

第二方面,在至少一个实施例中提供一种经过上述的X射线荧光光谱法分析氢氧化铝中成分含量的方法分析后得到的氢氧化铝。In the second aspect, in at least one embodiment, an aluminum hydroxide obtained after being analyzed by the above-mentioned method for analyzing component content in aluminum hydroxide by X-ray fluorescence spectrometry is provided.

第三方面,在至少一个实施例中提供一种所述的氢氧化铝在作为生产浮法玻璃的原料中的应用。In a third aspect, at least one embodiment provides an application of the aluminum hydroxide as a raw material for producing float glass.

本发明的第二方面和第三方面与前述的X射线荧光光谱法分析氢氧化铝中成分含量的方法是基于同一发明构思的,因而至少具有与前述X射线荧光光谱法分析氢氧化铝中成分含量的方法相同的优势,本发明在此不再赘述。The second aspect and the third aspect of the present invention are based on the same inventive concept as the aforementioned X-ray fluorescence spectrometry method for analyzing the content of components in aluminum hydroxide, and thus at least have the same characteristics as the aforementioned X-ray fluorescence spectrometry method for analyzing the components in aluminum hydroxide. The same advantages as the method of content, the present invention will not repeat them here.

下面结合具体实施例对本发明作进一步说明。The present invention will be further described below in conjunction with specific examples.

实施例1-3Example 1-3

一种X射线荧光光谱法分析氢氧化铝中成分含量的方法,按照上述试样研磨和粉末压片方法,分别对3个氢氧化铝(上海氢氧化铝)试样进行研磨处理,粉末压片制备样品,利用X射线荧光光谱采用上述分析条件和工作曲线进行分析,测得数据结果如表6所示。A method for analyzing the content of components in aluminum hydroxide by X-ray fluorescence spectrometry. According to the above sample grinding and powder pressing methods, three aluminum hydroxide (Shanghai aluminum hydroxide) samples are ground and processed respectively, and the powder is pressed into tablets. The samples were prepared and analyzed by X-ray fluorescence spectroscopy using the above analysis conditions and working curves, and the measured data results are shown in Table 6.

表6实施例1-3测试结果Table 6 Example 1-3 test results

项目project Al2O3 Al 2 O 3 Fe2O3 Fe2O3 _ SiO2 SiO 2 Na2ONa 2 O 实施例1Example 1 65.5765.57 0.00850.0085 0.0110.011 0.120.12 实施例2Example 2 65.1265.12 0.00480.0048 0.0100.010 0.310.31 实施例3Example 3 64.8264.82 0.00920.0092 0.0120.012 0.140.14

最后应说明的是:以上各实施例仅用以说明本发明的技术方案,而非对其限制;尽管参照前述各实施例对本发明进行了详细的说明,本领域的普通技术人员应当理解:其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分或者全部技术特征进行等同替换;而这些修改或者替换,并不使相应技术方案的本质脱离本发明各实施例技术方案的范围。Finally, it should be noted that: the above embodiments are only used to illustrate the technical solutions of the present invention, rather than limiting them; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: It is still possible to modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the technical solutions of the various embodiments of the present invention. scope.

Claims (10)

1.一种X射线荧光光谱法分析氢氧化铝中成分含量的方法,其特征在于,包括以下步骤:1. a method for X-ray fluorescence spectrometry analysis of component content in aluminum hydroxide, is characterized in that, comprises the following steps: 研磨;grinding; 粉末压片;powder compression; 采用X射线荧光光谱法,测定样片中各成分的发射强度,利用已建立的各成分的工作曲线,进行待测氢氧化铝样片中Al2O3、Fe2O3、SiO2和Na2O含量的分析。Use X-ray fluorescence spectrometry to measure the emission intensity of each component in the sample, and use the established working curve of each component to measure Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O in the aluminum hydroxide sample to be tested. content analysis. 2.根据权利要求1所述的X射线荧光光谱法分析氢氧化铝中成分含量的方法,其特征在于,研磨的时间为15~35min,研磨得到的试样的粒度≤200目,优选为80~150目。2. X-ray fluorescence spectrometry according to claim 1 analyzes the method for component content in aluminum hydroxide, it is characterized in that, the time of grinding is 15~35min, the particle size of the sample that grinds to obtain≤200 orders, is preferably 80 ~150 mesh. 3.根据权利要求1所述的X射线荧光光谱法分析氢氧化铝中成分含量的方法,其特征在于,粉末压片过程中,压力30~50MPa,静压20~40s。3. The method for analyzing the content of components in aluminum hydroxide by X-ray fluorescence spectrometry according to claim 1, characterized in that, during the powder compression process, the pressure is 30-50 MPa, and the static pressure is 20-40s. 4.根据权利要求1所述的X射线荧光光谱法分析氢氧化铝中成分含量的方法,其特征在于,建立各成分的工作曲线的方式包括:4. X-ray fluorescence spectrometry according to claim 1 analyzes the method for component content in aluminum hydroxide, it is characterized in that, the mode of setting up the working curve of each component comprises: 提供多个氢氧化铝标准样品,各标准样品中Al2O3、Fe2O3、SiO2和Na2O所占的质量比各不相同;Provide multiple aluminum hydroxide standard samples, and the mass ratios of Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O in each standard sample are different; 将标准样品分别进行研磨和粉末压片,制得标准样品压片;Grinding and powder pressing the standard samples respectively to obtain standard sample pressing; 采用X射线荧光光谱仪分别测定标准样品压片中各成分的发射强度;Adopt X-ray fluorescence spectrometer to measure the emission intensity of each component in the standard sample compression tablet respectively; 将X射线荧光特征谱线强度和相对应的Al2O3、Fe2O3、SiO2和Na2O质量百分含量进行线性回归,分别得到Al2O3、Fe2O3、SiO2和Na2O对应X射线荧光特征谱线强度的标准工作曲线。Perform linear regression on the intensity of X-ray fluorescence characteristic lines and the corresponding mass percentages of Al 2 O 3 , Fe 2 O 3 , SiO 2 and Na 2 O to obtain Al 2 O 3 , Fe 2 O 3 , and SiO 2 The standard working curve of X-ray fluorescence characteristic line intensity corresponding to Na 2 O. 5.根据权利要求4所述的X射线荧光光谱法分析氢氧化铝中成分含量的方法,其特征在于,标准样品的数量为≥4个。5. the method for X-ray fluorescence spectrometry analysis composition content in aluminum hydroxide according to claim 4, is characterized in that, the quantity of standard sample is ≥ 4. 6.根据权利要求4所述的X射线荧光光谱法分析氢氧化铝中成分含量的方法,其特征在于,研磨的时间为15~35min,研磨得到的试样的粒度≤200目,优选为80~150目;6. X-ray fluorescence spectrometry according to claim 4 analyzes the method for component content in aluminum hydroxide, it is characterized in that, the time of grinding is 15~35min, the particle size of the sample that grinds to obtain≤200 order, is preferably 80 ~150 mesh; 和/或,粉末压片过程中,压力30~50MPa,静压20~40s。And/or, during the powder compression process, the pressure is 30-50MPa, and the static pressure is 20-40s. 7.根据权利要求1~6任一项所述的X射线荧光光谱法分析氢氧化铝中成分含量的方法,其特征在于,对样片利用X射线荧光光谱仪测定氢氧化铝中各成分的测定条件分别为:7. according to the method for X-ray fluorescence spectrometry analysis composition content in aluminum hydroxide described in any one of claim 1~6, it is characterized in that, utilize X-ray fluorescence spectrometer to measure the measuring condition of each composition in aluminum hydroxide to sample They are: Al2O3:2θ144.65,波长电压30kV,电流80mA,分光晶体PET,准直器0.25,PHD40~100,干扰元素无,扫描时间20s;Al 2 O 3 : 2θ144.65, wavelength Voltage 30kV, current 80mA, spectroscopic crystal PET, collimator 0.25, PHD40~100, no interference elements, scan time 20s; Fe2O3:2θ57.53,波长电压30kV,电流80mA,分光晶体LiF200,准直器0.15,PHD40~100,干扰元素无,扫描时间20s;Fe 2 O 3 : 2θ57.53, wavelength Voltage 30kV, current 80mA, spectroscopic crystal LiF200, collimator 0.15, PHD40~100, no interference elements, scan time 20s; SiO2:2θ109.001,波长电压30kV,电流80mA,分光晶体PET,准直器0.60,PHD50~95,干扰元素无,扫描时间12s;SiO 2 : 2θ109.001, wavelength Voltage 30kV, current 80mA, spectroscopic crystal PET, collimator 0.60, PHD50~95, no interference elements, scan time 12s; Na2O:2θ23.951,波长电压30kV,电流80mA,分光晶体AX06,准直器0.60,PHD40~100,干扰元素无,扫描时间20s。Na2O: 2θ23.951 , wavelength Voltage 30kV, current 80mA, spectroscopic crystal AX06, collimator 0.60, PHD40~100, no interference elements, scan time 20s. 8.根据权利要求7所述的X射线荧光光谱法分析氢氧化铝中成分含量的方法,其特征在于,所述样片包括待测氢氧化铝样片和标准样品样片。8. The method for analyzing component content in aluminum hydroxide by X-ray fluorescence spectrometry according to claim 7, characterized in that, the samples include aluminum hydroxide samples to be measured and standard sample samples. 9.经过权利要求1~8任一项所述的X射线荧光光谱法分析氢氧化铝中成分含量的方法分析后得到的氢氧化铝。9. The aluminum hydroxide obtained after analyzing the method for analyzing the composition content in aluminum hydroxide by X-ray fluorescence spectrometry according to any one of claims 1 to 8. 10.权利要求9所述的氢氧化铝在作为生产浮法玻璃的原料中的应用。10. the application of the aluminum hydroxide described in claim 9 as the raw material for producing float glass.
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CN114994111A (en) * 2022-06-16 2022-09-02 宁波新材料测试评价中心有限公司 Method for rapidly measuring content of aluminum oxide in aluminum oxide ceramic substrate for integrated circuit

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CN111855719A (en) * 2020-07-29 2020-10-30 河北南玻玻璃有限公司 A kind of sample preparation method for analyzing the chemical composition of quartz sandstone by X-ray fluorescence spectrometry
CN112129798A (en) * 2020-10-21 2020-12-25 中国食品药品检定研究院 A kind of content determination method of natural copper in Chinese patent medicine
CN113075148A (en) * 2021-03-22 2021-07-06 久泰能源(准格尔)有限公司 Method for measuring carbon content on surface of catalyst in MTO (methanol to olefin) process
CN113075148B (en) * 2021-03-22 2023-06-16 久泰能源(准格尔)有限公司 Method for measuring carbon content of catalyst surface in MTO process
CN113237907A (en) * 2021-04-08 2021-08-10 中国铝业股份有限公司 Method for measuring fluorine content in fluorine-carrying alumina by X-ray fluorescence spectrometry
CN114460117A (en) * 2022-03-16 2022-05-10 清远南玻节能新材料有限公司 Method for detecting component content of aluminum hydroxide product
CN114460117B (en) * 2022-03-16 2023-06-06 清远南玻节能新材料有限公司 Method for detection of composition content of aluminum hydroxide products
CN114994111A (en) * 2022-06-16 2022-09-02 宁波新材料测试评价中心有限公司 Method for rapidly measuring content of aluminum oxide in aluminum oxide ceramic substrate for integrated circuit

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