JPH11326246A - Method for measuring abundance of constitutive component element in inorganic ion exchanger - Google Patents
Method for measuring abundance of constitutive component element in inorganic ion exchangerInfo
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- JPH11326246A JPH11326246A JP13307798A JP13307798A JPH11326246A JP H11326246 A JPH11326246 A JP H11326246A JP 13307798 A JP13307798 A JP 13307798A JP 13307798 A JP13307798 A JP 13307798A JP H11326246 A JPH11326246 A JP H11326246A
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- inorganic ion
- ion exchanger
- measured
- internal standard
- constituent elements
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は無機イオン交換体中
の構成成分元素存在比をの測定方法に関するものであ
る。さらに詳しくは、無機触媒分野や吸着剤分野等に使
用される無機イオン交換体の構成成分元素の存在比の好
適な分析方法を提供するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for measuring the abundance ratio of constituent elements in an inorganic ion exchanger. More specifically, the present invention provides a suitable method for analyzing the abundance ratio of the constituent elements of the inorganic ion exchanger used in the field of inorganic catalysts, adsorbents, and the like.
【０００２】[0002]
【従来の技術】従来、無機イオン元素の分析方法として
はＪＩＳ−Ｈ−１３０６（昭和４９年５月１日制定、平
成４年１２月１日改正）、ＪＩＳ−Ｈ−１３０７（平成
５年２月１日制定）記載の原子吸光分析、誘導結合プラ
ズマ発光分析法が知られており、これは酸性溶液で試料
を溶解しその吸光度、発光強度を測定するものである。2. Description of the Related Art Conventionally, methods for analyzing inorganic ion elements include JIS-H-1306 (established on May 1, 1974, revised on December 1, 1992) and JIS-H-1307 (February 1993). Atomic absorption spectrometry and inductively coupled plasma emission spectrometry described in US Pat.
【０００３】しかしながら、この方法では試料の前処理
として全てを溶液化する為に液の液性・噴霧状態等に結
果が影響されたりまた操作性が非常に悪く、これらの分
析精度は装置の性能や測定条件によって大きく影響され
る。However, in this method, since all of the solution is converted into a solution as a pretreatment of the sample, the result is affected by the liquid properties and the spray state of the solution, and the operability is extremely poor. And measurement conditions.
【０００４】一方、溶液中の無機イオン元素の構成成分
元素分析法としては、キレート適定分析が知られている
が共存無機イオン元素等が多い場合分離が必要になった
り分離困難な場合は妨害が生じ正確な結果が得られな
い。[0004] On the other hand, as a method for elemental analysis of constituent elements of inorganic ion elements in a solution, chelate appropriate analysis is known. And accurate results cannot be obtained.
【０００５】このように、従来の技術では、無機イオン
交換体中の構成成分元素存在比を同時に、迅速に、精度
よく測定することは共存元素イオンによる妨害等の除去
のために分析に長時間を要するために困難であり、ま
た、試料を硝酸等の酸により溶解させる前処理が必要と
なるため操作性が悪いものであった。[0005] As described above, in the prior art, simultaneous, rapid and accurate measurement of the constituent element abundance in the inorganic ion exchanger requires a long time for analysis in order to remove interference or the like due to coexisting element ions. In addition, operability is poor because pretreatment for dissolving the sample with an acid such as nitric acid is required.
【０００６】[0006]
【発明が解決しようとする課題】本発明の目的は、無機
イオン交換体中の構成成分元素存在比を測定する際に、
従来の方法と同程度以上に正確に無機イオン交換体中の
構成成分元素存在比を測定でき、しかも共存無機イオン
元素が多い場合においても妨害を受けることなく、迅速
かつ簡便で正確に構成成分元素存在比を測定する方法を
提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to measure the ratio of constituent elements in an inorganic ion exchanger.
The component element abundance ratio in the inorganic ion exchanger can be measured more accurately than the conventional method, and even if there are many coexisting inorganic ion elements, it is quick, simple and accurate without any interference. An object of the present invention is to provide a method for measuring an abundance ratio.
【０００７】[0007]
【課題を解決するための手段】本発明者らは上記課題を
解決するために鋭意検討を重ねた結果、無機イオン交換
体中の含有成分元素の測定法において、無機イオン交換
体中の構成成分元素を内部標準元素とし、蛍光Ｘ線分析
装置を用い構成成分元素存在比を測定できることを見出
し、本発明を完成するに至った。Means for Solving the Problems The present inventors have conducted intensive studies in order to solve the above-mentioned problems, and as a result, in the method of measuring the constituent elements contained in the inorganic ion exchanger, Using the element as an internal standard element, it has been found that the constituent element abundance ratio can be measured using a fluorescent X-ray analyzer, and the present invention has been completed.
【０００８】以下、本発明を詳細に説明する。Hereinafter, the present invention will be described in detail.
【０００９】本発明の方法は、無機イオン交換体中の構
成成分元素の測定法において、無機イオン交換体中の構
成成分元素を内部標準元素とし、蛍光Ｘ線分析装置を用
い構成成分元素存在比を測定するものである。The method of the present invention is a method for measuring constituent elements in an inorganic ion exchanger, wherein the constituent elements in the inorganic ion exchanger are used as internal standard elements, and the ratio of constituent element abundance is determined using a fluorescent X-ray analyzer. Is measured.
【００１０】本発明の方法において分析に供せられる無
機イオン交換体とはイオン交換現象を示す無機物質をい
い、特に制限はなく、例えば、結晶性あるいは不定形の
アルミノケイ酸塩や、粘土鉱物、不溶性含水酸化物等が
挙げられ、これらは天然物であっても合成物であっても
よい。The inorganic ion exchanger used for analysis in the method of the present invention refers to an inorganic substance exhibiting an ion exchange phenomenon, and is not particularly limited. Examples thereof include a crystalline or amorphous aluminosilicate, a clay mineral, Examples include insoluble hydrated oxides, which may be natural products or synthetic products.
【００１１】アルミノケイ酸塩としては、ジュンウイリ
ーアンドサンズ、ニューヨークＮ．Ｙ（１９７４年）、
デイ・ダブリュ・ブレック（Ｄ．Ｗ．Ｂｒｅｃｋ）著の
「ゼオライトモレキュラーシーブ」で定義されるような
ゼオライトや、不定形のアルミノケイ酸塩が挙げられ
る。特にゼオライトとしては、フェリライト、フィリッ
プサイト、ソ−ダライト、カンクリナイト、エオリナイ
ト、オフレタイト、クリノプチロライト、グメリナイ
ト、チャバサイト、フォージャサイト、モルデナイト、
Ａ型ゼオライト、Ｘ型ゼオライト、Ｙ型ゼオライト、Ｌ
型ゼオライト、ベータ型ゼオライト、オメガ型ゼオライ
ト、ＺＳＭ−５等のゼオライトやメソポーラスモレキュ
ラーシーブを挙げることができ、これらのプロトン型
や、Ｌｉ、Ｍｇ、Ｃａ等のアルカリ金属塩、アルカリ土
類金属塩、及びこれらの水和物も用いられる。As aluminosilicates, Jun Wheelie and Sons, New York N.N. Y (1974),
Zeolite as defined in "Zeolite Molecular Sieve" by DW Breck, and amorphous aluminosilicate. Particularly as zeolites, ferrilite, phillipsite, sodalite, canclinite, aeolite, offretite, clinoptilolite, gmelinite, chabazite, faujasite, mordenite,
A-type zeolite, X-type zeolite, Y-type zeolite, L
Zeolite, beta zeolite, omega zeolite, zeolites such as ZSM-5 and mesoporous molecular sieves, and these proton types, and alkali metal salts such as Li, Mg and Ca, alkaline earth metal salts, And hydrates thereof.
【００１２】粘土鉱物としては、岩波書店発行、第４版
「理化学辞典」より定義されるようなものであり、さら
に具体的には、カオリナイト、ハロサイト、モンモリロ
ナイト、イライト、バーミキュライト、緑泥石などを挙
げることができ、これらのＬｉ、Ｍｇ、Ｃａ等のアルカ
リ金属塩、アルカリ土類金属塩、及びこれらの水和物も
用いられる。Clay minerals are those defined by Iwanami Shoten Publishing Co., Ltd., 4th edition, "The Dictionary of Physical and Chemical Sciences". More specifically, kaolinite, halosite, montmorillonite, illite, vermiculite, chlorite, etc. Examples thereof include alkali metal salts such as Li, Mg, and Ca, alkaline earth metal salts, and hydrates thereof.
【００１３】不溶性含水酸化物としては、金属の含水酸
化物、多価金属の酸性塩、不溶性のヘテロポリ塩、不溶
性ヘキサシアノ鉄酸塩などを挙げることができ、さらに
具体的には、シリカアルミナ、アルミナチタニア、リン
酸ジルコニウム、シリカチタニア等を挙げることがで
き、これらのＬｉ、Ｍｇ、Ｃａ等のアルカリ金属塩、ア
ルカリ土類金属塩、及びこれらの水和物も用いられる。Examples of the insoluble hydrated oxide include hydrated oxides of metals, acidic salts of polyvalent metals, insoluble heteropoly salts, insoluble hexacyanoferrates, and more specifically, silica alumina, alumina Examples thereof include titania, zirconium phosphate, and silica titania, and alkali metal salts such as Li, Mg, and Ca, alkaline earth metal salts, and hydrates thereof are also used.
【００１４】また、これらの無機イオン交換体は単独の
みならず、これらの２種以上の混合物であってもよい。These inorganic ion exchangers may be used alone or as a mixture of two or more of them.
【００１５】これらの内、測定精度や測定感度の面か
ら、各測定元素のピークのオーバーラップがなく測定精
度を向上させることができるためにアルミノケイ酸塩
が、さらに結晶性を有したゼオライトが好ましく用いら
れる。Of these, aluminosilicates are preferable, and zeolite having crystallinity is more preferable in terms of measurement accuracy and measurement sensitivity because the measurement accuracy can be improved without overlapping peaks of the respective measurement elements. Used.
【００１６】測定にあたっての内部標準元素としては、
測定対象となる無機イオン交換体中の元素の内蛍光Ｘ線
分析装置を用いて測定することができるものであれば特
に限定されるものではないが、Ｓｉ元素やＡｌ元素、さ
らにＡｌ元素を含むことが特に好ましい。そして、無機
イオン交換体に含まれるＮａ元素、Ｋ元素などを測定し
て、内部標準元素とこれらの無機イオン交換体に含まれ
る任意の元素とのモル比を測定することができる。The internal standard elements for the measurement include:
The element in the inorganic ion exchanger to be measured is not particularly limited as long as it can be measured using a fluorescent X-ray analyzer, and includes an Si element, an Al element, and an Al element. Is particularly preferred. Then, by measuring the Na element, the K element, and the like contained in the inorganic ion exchanger, the molar ratio between the internal standard element and any element contained in these inorganic ion exchangers can be measured.
【００１７】ここで、測定対象となる無機イオン交換体
中の構成成分元素とこれとは異なる任意に選ばれる無機
イオン交換体中の構成成分元素とのモル比は、内部標準
元素のモル量の０．０００００１以上であることが好ま
しく、さらに０．０００１以上１００００００倍以下で
あることが好ましい。この範囲であれば、蛍光Ｘ線分析
装置の測定強度より速やかにかつ定量的に分析できるか
らである。Here, the molar ratio between the constituent element in the inorganic ion exchanger to be measured and the constituent element in the inorganic ion exchanger which is arbitrarily different from the above is determined by the molar amount of the internal standard element. It is preferably 0.000001 or more, and more preferably 0.0001 to 1,000,000 times. This is because within this range, the analysis can be performed more quickly and quantitatively than the intensity measured by the fluorescent X-ray analyzer.
【００１８】またこれらの無機イオン交換体はほとんど
が粉体であり、測定に際しては、これらの試料を加圧成
形できるものであれば特に制限されるものではない。例
えば、加圧成形の方法としてはブリケット法やガラスビ
ード法などがあるが、電動式試料成形機を用いて行うブ
リケット法では、リング法、ダイス法のいずれの方法も
本発明の方法に用いることができる。一方、ガラスビー
ド法では、溶融法、高周波加熱法のいずれの方法も本発
明の方法に用いることができるが、これらの方法のいず
れも溶融助剤を添加するため、含有成分元素が低含有成
分元素が希釈されることがあるため注意が必要である。
また、成形品の形状、大きさ、圧縮密度等は特に制限さ
れるものではないが、試料表面への汚染が少なく、ま
た、分析面が常に平滑面となるようにすることに注意す
る必要がある。Most of these inorganic ion exchangers are powders, and the measurement is not particularly limited as long as these samples can be molded under pressure. For example, as a method of pressure molding, there are a briquette method, a glass bead method, and the like. In a briquette method performed using an electric sample molding machine, any of a ring method and a die method may be used in the method of the present invention. Can be. On the other hand, in the glass bead method, any of the melting method and the high-frequency heating method can be used in the method of the present invention. Care must be taken because the elements may be diluted.
The shape, size, compression density, etc. of the molded product are not particularly limited, but care must be taken to minimize contamination on the sample surface and to ensure that the analysis surface is always smooth. is there.
【００１９】このようにして成形された成形体を蛍光Ｘ
線分析装置を用いて測定される。The molded body formed in this manner is treated with fluorescent X
It is measured using a line analyzer.
【００２０】本発明の方法において用いられる蛍光Ｘ線
分析装置については波長分散型蛍光Ｘ線分析装置で用い
られるものであれば特に制限されるものではない。The X-ray fluorescence analyzer used in the method of the present invention is not particularly limited as long as it is used in a wavelength dispersive X-ray fluorescence analyzer.
【００２１】これらの加圧成形・測定の方法を用いるこ
とで無機イオン交換体中の構成成分元素の存在比を測定
することができ、この結果から無機イオン交換体中の構
成成分元素を内部標準元素として測定することで無機イ
オン交換体中の構成成分元素の存在比を測定できるわけ
であるが、実際の測定にあたっては、各元素の分析値が
既知の無機イオン交換体を用い無機イオン交換体中の構
成成分元素を内部標準元素として測定し無機イオン交換
体中の構成成分元素の存在比を測定し、本発明の方法に
より得られた測定結果との関係を示す検量線を作成し、
無機イオン交換体中の構成成分元素の量が未知な場合に
適用できる。The abundance ratio of the constituent elements in the inorganic ion exchanger can be measured by using these pressure molding / measuring methods. From the results, the constituent elements in the inorganic ion exchanger can be determined by the internal standard. By measuring as an element, the abundance ratio of the constituent elements in the inorganic ion exchanger can be measured.However, in actual measurement, the inorganic ion exchanger using an inorganic ion exchanger whose analytical value of each element is known is used. The constituent elements in the inorganic ion exchanger were measured as internal standard elements to determine the abundance ratio of the constituent elements, and a calibration curve showing the relationship with the measurement results obtained by the method of the present invention was created.
It is applicable when the amount of the constituent element in the inorganic ion exchanger is unknown.
【００２２】測定結果の計算については、ピーク分離、
検出手段により変わるものの、その量が計算できる方法
であれば特に限定されるものではない。ここでは、蛍光
Ｘ線より得られるピークについて、そのピークの高さ、
ピークの幅、面積等を通常用いられる方法により計算す
ることができる。さらに、蛍光Ｘ線より得られるピーク
位置を確認することで同定もできる。これらの蛍光Ｘ線
分析装置により得られたデータを蛍光Ｘ線分析装置に内
蔵あるいは外部に設置されたコンピュータ等の情報処理
装置により計算し処理して無機イオン交換体中の構成成
分元素の存在比として求めることもできる。For calculation of the measurement results, peak separation,
Although it depends on the detection means, the method is not particularly limited as long as the amount can be calculated. Here, regarding the peak obtained from the fluorescent X-ray, the height of the peak,
The peak width, area and the like can be calculated by a commonly used method. Further, identification can be performed by confirming the peak position obtained from the fluorescent X-ray. The data obtained by these X-ray fluorescence analyzers are calculated and processed by an information processing device such as a computer built in or external to the X-ray fluorescence analyzer, and the abundance ratio of the constituent elements in the inorganic ion exchanger is calculated. Can also be sought.
【００２３】本発明の方法は、無機イオン交換体中の構
成成分元素の測定を迅速かつ簡便で正確にすることが可
能になるものである。The method of the present invention makes it possible to quickly, simply and accurately measure constituent elements in an inorganic ion exchanger.
【００２４】[0024]
【実施例】以下、本発明を実施例を用いてさらに詳細に
説明するが、本発明はこれら実施例にのみ限定されるも
のではない。EXAMPLES Hereinafter, the present invention will be described in more detail with reference to examples, but the present invention is not limited to these examples.
【００２５】実施例１ 標準サンプルとしてＩＣＰによる湿式化学分析により求
められたシリカ・アルミ比（ＳｉＯ2／Ａｌ2Ｏ3；モル
比）及びナトリウム・アルミナ比（Ｎａ2Ｏ／Ａｌ2Ｏ3
モル比）の異なるゼオライト粉末Ａ、Ｂ、Ｃ、Ｄを塩ビ
樹脂リング（径：３０ｍｍ、厚み：５ｍｍ）を用いて電
動式試料成形機により１５ｔ加重で３０秒加圧すること
でそれぞれの成形体を得た。Example 1 A silica-aluminum ratio (SiO 2 / Al 2 O 3 ; molar ratio) and a sodium-alumina ratio (Na 2 O / Al 2 O 3 ) determined by wet chemical analysis using ICP as standard samples
Zeolite powders A, B, C, and D having different molar ratios) are pressed by a motor-driven sample molding machine using a PVC resin ring (diameter: 30 mm, thickness: 5 mm) with a load of 15 t for 30 seconds to form each compact. Obtained.
【００２６】このようにして得た成形体に対して蛍光Ｘ
線分析装置（波長分散型、理学電気工業製、型式：ＲＩ
Ｘ―２１００）を用いて構成成分元素の分析を行った。
表１には湿式化学分析によるＳｉＯ2／Ａｌ2Ｏ3モル比
及び蛍光Ｘ線分析によるＳｉＯ2とＡｌ2Ｏ3のピーク強
度の比（測定強度比）を、表２には湿式化学分析による
Ｎａ2Ｏ／Ａｌ2Ｏ3モル比及び蛍光Ｘ線分析によるＮａ2
ＯとＡｌ2Ｏ3のピーク強度の比（測定強度比）をそれぞ
れ示した。これらの標準サンプルはあらかじめ湿式化学
分析により求めており、蛍光Ｘ線分析測定により得られ
るピーク強度とは比例関係にはあるが、ここではゼオラ
イトに構成されるＡｌ2Ｏ3を内部標準元素とした内部標
準法により適宜計算し検量線を作成した。The molded product obtained in this manner was subjected to fluorescent X
X-ray analyzer (wavelength dispersion type, manufactured by Rigaku Denki Kogyo, model: RI
X-2100) was used to analyze constituent elements.
Table 1 shows the molar ratio of SiO 2 / Al 2 O 3 by wet chemical analysis and the ratio of the peak intensity of SiO 2 to Al 2 O 3 (measured intensity ratio) by X-ray fluorescence analysis. Table 2 shows the ratio by wet chemical analysis. Na 2 O / Al 2 O 3 molar ratio and Na 2 by X-ray fluorescence analysis
The ratios of the peak intensities of O and Al 2 O 3 (measured intensity ratios) are shown. These standard samples have been determined in advance by wet chemical analysis and have a proportional relationship with the peak intensity obtained by the fluorescent X-ray analysis measurement. Here, Al 2 O 3 constituted by zeolite was used as the internal standard element. A calibration curve was prepared by appropriately calculating according to the internal standard method.
【００２７】[0027]
【表１】 [Table 1]
【００２８】[0028]
【表２】 [Table 2]
【００２９】表１、表２より明らかなように上記記載の
方法によれば、無機イオン交換体中の構成成分元素のモ
ル比として、無機イオン交換体中の構成成分元素である
Ａｌ2Ｏ3を内部標準元素とし、これとＳｉＯ2やＮａ2Ｏ
との測定強度比は湿式化学分析によるモル比とは直線性
が良く、両者によい相関性があることが分かった。As is clear from Tables 1 and 2, according to the method described above, the molar ratio of the constituent elements in the inorganic ion exchanger is expressed as Al 2 O 3 which is the constituent element in the inorganic ion exchanger. Is used as an internal standard element, and SiO 2 or Na 2 O
The measured intensity ratio was well linear with the molar ratio obtained by wet chemical analysis, and it was found that there was a good correlation between the two.
【００３０】実施例２ 表１、表２で得られた検量線を用い、Ｅ、Ｆ、Ｇ、Ｈの
ゼオライトサンプルについて、湿式化学分析及び蛍光Ｘ
線分析の測定を行い、ＳｉＯ2／Ａｌ2Ｏ3モル比及びＮ
ａ2Ｏ／Ａｌ2Ｏ3モル比を求め、その結果を表３、表４
に示した。Example 2 Using the calibration curves obtained in Tables 1 and 2, samples of zeolite E, F, G and H were subjected to wet chemical analysis and fluorescence X
Line analysis was performed and the SiO 2 / Al 2 O 3 molar ratio and N
The a 2 O / Al 2 O 3 molar ratio was determined, and the results were shown in Tables 3 and 4.
It was shown to.
【００３１】[0031]
【表３】 [Table 3]
【００３２】[0032]
【表４】 [Table 4]
【００３３】表３、表４より明らかなように、湿式化学
分析及び蛍光Ｘ線分析の測定の結果はよい相関性を示し
ており、本発明の方法は無機イオン交換体中の構成成分
元素の存在比を正確に測定できることが分かった。As is clear from Tables 3 and 4, the results of the wet chemical analysis and the X-ray fluorescence analysis show good correlation, and the method of the present invention shows that the constituent elements in the inorganic ion exchanger were It was found that the abundance ratio could be measured accurately.
【００３４】実施例３ 標準サンプルとしてＩＣＰによる湿式化学分析により求
められたカリウム・アルミ比（Ｋ2Ｏ／Ａｌ2Ｏ3；モル
比）の異なるゼオライト粉末Ｉ、Ｊ、Ｋを塩ビ樹脂リン
グ（径：３０ｍｍ、厚み：５ｍｍ）を用いて電動式試料
成形機により１５ｔ加重で３０秒加圧することでそれぞ
れの成形体を得た。Example 3 As a standard sample, zeolite powders I, J and K having different potassium / aluminum ratios (K 2 O / Al 2 O 3 ; molar ratio) determined by wet chemical analysis by ICP were converted to a PVC resin ring (diameter). : 30 mm, thickness: 5 mm) and pressurized with a 15-t load for 30 seconds using an electric sample molding machine to obtain respective molded bodies.
【００３５】このようにして得た成形体に対して蛍光Ｘ
線分析装置（波長分散型、理学電気工業製、型式：ＲＩ
Ｘ―２１００）を用いて構成成分元素の分析を行った。
表５には湿式化学分析によるＫ2Ｏ／Ａｌ2Ｏ3モル比及
び蛍光Ｘ線分析によるＫ2ＯとＡｌ2Ｏ3のピーク強度の
比（測定強度比）を示した。これらの標準サンプルはあ
らかじめ湿式化学分析により求めており、蛍光Ｘ線分析
測定により得られるピーク強度とは比例関係にはある
が、ここではゼオライトに構成されるＡｌ2Ｏ3を内部標
準元素とした内部標準法により適宜計算し検量線を作成
した。A fluorescent X was applied to the thus obtained molded body.
X-ray analyzer (wavelength dispersion type, manufactured by Rigaku Denki Kogyo, model: RI
X-2100) was used to analyze constituent elements.
Table 5 shows the molar ratio of K 2 O / Al 2 O 3 by wet chemical analysis and the ratio of the peak intensity of K 2 O to Al 2 O 3 (measured intensity ratio) by X-ray fluorescence analysis. These standard samples have been determined in advance by wet chemical analysis and have a proportional relationship with the peak intensity obtained by the fluorescent X-ray analysis measurement. Here, Al 2 O 3 constituted by zeolite was used as the internal standard element. A calibration curve was prepared by appropriately calculating according to the internal standard method.
【００３６】[0036]
【表５】 [Table 5]
【００３７】表５より明らかなように上記記載の方法に
よれば、無機イオン交換体中の構成成分元素のモル比と
して、無機イオン交換体中の構成成分元素であるＡｌ2
Ｏ3を内部標準元素とし、これとＫ2Ｏとの測定強度比は
湿式化学分析によるモル比とは直線性が良く、両者によ
い相関性があることが分かった。As apparent from Table 5, according to the method described above, the molar ratio of the constituent elements in the inorganic ion exchanger is expressed as Al 2 which is the constituent element in the inorganic ion exchanger.
O 3 was used as an internal standard element, and the measured intensity ratio between K 3 O and K 2 O was excellent in linearity with the molar ratio determined by wet chemical analysis, and it was found that there was a good correlation between the two.
【００３８】実施例４ 表５で得られた検量線を用い、Ｌ、Ｍのゼオライトサン
プルについて、湿式化学分析及び蛍光Ｘ線分析の測定を
行い、Ｋ2Ｏ／Ａｌ2Ｏ3モル比を求め、その結果を表６
に示した。Example 4 Using the calibration curves obtained in Table 5, the L and M zeolite samples were subjected to wet chemical analysis and X-ray fluorescence analysis to determine the K 2 O / Al 2 O 3 molar ratio. Table 6 shows the results.
It was shown to.
【００３９】[0039]
【表６】 [Table 6]
【００４０】表６より明らかなように、湿式化学分析及
び蛍光Ｘ線分析の測定の結果はよい相関性を示してお
り、本発明の方法は無機イオン交換体中の構成成分元素
の存在比を正確に測定できることが分かった。As is clear from Table 6, the results of the wet chemical analysis and the X-ray fluorescence analysis show a good correlation, and the method of the present invention determines the abundance ratio of the constituent elements in the inorganic ion exchanger. It turned out that it can be measured accurately.
【００４１】[0041]
【発明の効果】以上述べてきたように、本発明の方法に
よれば、無機イオン交換体中の構成成分元素存在比を測
定する際に、従来の方法と同程度以上に正確に無機イオ
ン交換体中の構成成分元素存在比を測定でき、しかも共
存無機イオン元素が多い場合においても妨害を受けるこ
となく、迅速かつ簡便で正確に構成成分元素存在比を測
定する利点がある。As described above, according to the method of the present invention, when measuring the abundance ratio of the constituent elements in the inorganic ion exchanger, the inorganic ion exchange is more accurately performed than the conventional method. There is an advantage that the component element abundance ratio in the body can be measured, and even if there are many coexisting inorganic ion elements, the component element abundance ratio is measured quickly, simply, and accurately without being hindered.
Claims (8)
Ｘ線分析装置を用いて測定することを特徴とする無機イ
オン交換体中の構成成分元素の存在比測定方法。1. A method for measuring the abundance ratio of constituent elements in an inorganic ion exchanger, wherein the constituent elements in the inorganic ion exchanger are measured using an X-ray fluorescence analyzer.
標準とすることを特徴とする請求項１に記載の無機イオ
ン交換体中の構成成分元素の存在比測定方法。2. The method according to claim 1, wherein the constituent elements in the inorganic ion exchanger are used as an internal standard.
ことを特徴とする請求項１又は請求項２に記載の無機イ
オン交換体中の構成成分元素の存在比測定方法。3. The method according to claim 1, wherein the inorganic ion exchanger is an aluminosilicate.
を特徴とする請求項３に記載の無機イオン交換体中の構
成成分元素の存在比測定方法。4. The method according to claim 3, wherein the inorganic ion exchanger is zeolite.
アルミニウム（Ａｌ）を内部標準とすることを特徴とす
る請求項２〜４のいずれかに記載の無機イオン交換体中
の構成成分元素の存在比測定方法。5. A constituent element in an inorganic ion exchanger according to claim 2, wherein aluminum (Al) which is a constituent element in the inorganic ion exchanger is used as an internal standard. Abundance ratio measurement method.
アルミニウムを内部標準として測定し、さらにナトリウ
ム（Ｎａ）、カリウム（Ｋ）及び珪素（Ｓｉ）からなる
群より選ばれる１種以上の元素を測定して、その対応す
るＮａ2Ｏ／Ａｌ2Ｏ3、Ｋ2Ｏ／Ａｌ2Ｏ3及びＳｉＯ2／
Ａｌ2Ｏ3からなる群より選ばれる１種以上のモル比を求
めることを特徴とする請求項５に記載の無機イオン交換
体中の構成成分元素の存在比測定方法。6. An inorganic ion exchanger in which aluminum as a constituent element is measured as an internal standard, and one or more elements selected from the group consisting of sodium (Na), potassium (K) and silicon (Si). Are measured to determine the corresponding Na 2 O / Al 2 O 3 , K 2 O / Al 2 O 3 and SiO 2 /
Abundance ratio measurement method for a component element of the inorganic ion exchanger in claim 5, wherein the determination of the one or more molar ratio selected from the group made of Al 2 O 3.
より無機イオン交換体中の構成成分元素の存在比を求め
ることを特徴とする請求項１〜６のいずれかに記載の無
機イオン交換体中の構成成分元素の存在比測定方法。7. The inorganic ion exchange according to claim 1, wherein an abundance ratio of the constituent elements in the inorganic ion exchanger is determined from a peak obtained by using an X-ray fluorescence analyzer. Method for measuring abundance ratio of constituent element in body.
を情報処理装置により処理して無機イオン交換体中の構
成成分元素の存在比を求めることを特徴とする請求項７
に記載の無機イオン交換体中の構成成分元素の存在比測
定方法。8. The method according to claim 7, wherein a peak obtained by using an X-ray fluorescence analyzer is processed by an information processor to determine the abundance ratio of the constituent elements in the inorganic ion exchanger.
4. The method for measuring the abundance ratio of constituent elements in an inorganic ion exchanger according to the above.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13307798A JPH11326246A (en) | 1998-05-15 | 1998-05-15 | Method for measuring abundance of constitutive component element in inorganic ion exchanger |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13307798A JPH11326246A (en) | 1998-05-15 | 1998-05-15 | Method for measuring abundance of constitutive component element in inorganic ion exchanger |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11326246A true JPH11326246A (en) | 1999-11-26 |
Family
ID=15096317
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13307798A Pending JPH11326246A (en) | 1998-05-15 | 1998-05-15 | Method for measuring abundance of constitutive component element in inorganic ion exchanger |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11326246A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010506176A (en) * | 2006-11-02 | 2010-02-25 | エフ．ホフマン−ラ ロシュ アーゲー | Method for preparing microporous crystals and conjugates thereof |
| JP2017058362A (en) * | 2015-09-15 | 2017-03-23 | 住友金属鉱山株式会社 | X-ray fluorescence analysis sample preparation method |
-
1998
- 1998-05-15 JP JP13307798A patent/JPH11326246A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010506176A (en) * | 2006-11-02 | 2010-02-25 | エフ．ホフマン−ラ ロシュ アーゲー | Method for preparing microporous crystals and conjugates thereof |
| JP2017058362A (en) * | 2015-09-15 | 2017-03-23 | 住友金属鉱山株式会社 | X-ray fluorescence analysis sample preparation method |
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