JP6003233B2 - Sample processing method for fluorescent X-ray analysis - Google Patents

Sample processing method for fluorescent X-ray analysis Download PDF

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JP6003233B2
JP6003233B2 JP2012121995A JP2012121995A JP6003233B2 JP 6003233 B2 JP6003233 B2 JP 6003233B2 JP 2012121995 A JP2012121995 A JP 2012121995A JP 2012121995 A JP2012121995 A JP 2012121995A JP 6003233 B2 JP6003233 B2 JP 6003233B2
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山田　康治郎
康治郎 山田
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本発明は、微量の粉末試料を蛍光Ｘ線分析に供するための試料処理方法およびそれを用いた蛍光Ｘ線分析方法に関する。   The present invention relates to a sample processing method for subjecting a small amount of powder sample to fluorescent X-ray analysis and a fluorescent X-ray analysis method using the sample processing method.

従来、微量の粉末試料を蛍光Ｘ線分析に供するための試料処理方法としては、セルロースパウダーやホウ酸を基材として予備加圧成形しておき、その表面に粉末試料を載置するなどしてさらに加圧成形して分析試料とする方法（非特許文献１参照）や、高分子フィルムの表面に粉末試料を載置し加圧成形して分析試料とする方法（特許文献１参照）などがあり、基材だけでは成形性が不十分な場合には、例えばステアリン酸をバインダーとして混合する場合もある（特許文献２参照）。   Conventionally, as a sample processing method for subjecting a small amount of powder sample to fluorescent X-ray analysis, pre-press molding is performed using cellulose powder or boric acid as a base material, and the powder sample is placed on the surface thereof. Further, there are a method of forming an analysis sample by pressure molding (see Non-Patent Document 1), a method of placing a powder sample on the surface of a polymer film and molding the sample by pressure molding (see Patent Document 1), etc. If the moldability is insufficient with only the base material, for example, stearic acid may be mixed as a binder (see Patent Document 2).

特開２００６−７８３８６号公報JP 2006-78386 A 特開２０００−７４８５８号公報JP 2000-74858 A

中井泉編，「蛍光Ｘ線分析の実際」，初版，朝倉書店，２００５年１０月２０日，ｐ．７５−７７Izumi Nakai, “Practical X-ray fluorescence analysis”, first edition, Asakura Shoten, October 20, 2005, p. 75-77

しかし、従来用いられている基材、バインダー、高分子フィルムには、ホウ素、炭素、窒素、酸素などのいわゆる超軽元素が相当量含まれており、１次Ｘ線が照射されると蛍光Ｘ線を発生してそれが不純線となる。これに対し、粉末試料が体積で耳掻き約１杯以下、重量で約１０mg以下の微量である場合には、粉末試料から発生する蛍光Ｘ線が特に微弱で不純線の影響を受けやすく、それらの超軽元素を分析対象元素として蛍光Ｘ線分析を行うことが事実上不可能であった。また、高分子フィルムの表面に粉末試料を載置し加圧成形して分析試料とする方法では、粉末試料が約１０mg以下であると成形性が確保できず分析面積（成形後の粉末試料の面積）を広げることが困難な場合が多く、超軽元素に対する感度が低くなり、正確な蛍光Ｘ線分析を行えないこともあった。   However, conventionally used base materials, binders, and polymer films contain a considerable amount of so-called ultralight elements such as boron, carbon, nitrogen, and oxygen. When primary X-rays are irradiated, fluorescent X A line is generated and becomes an impure line. On the other hand, when the powder sample is a trace amount of about 1 cup or less of earpick by volume and about 10 mg or less by weight, the fluorescent X-ray generated from the powder sample is particularly weak and easily affected by impure lines. It was practically impossible to perform fluorescent X-ray analysis using ultra-light elements as analysis target elements. In addition, in the method of placing a powder sample on the surface of a polymer film and press-molding to make an analysis sample, if the powder sample is about 10 mg or less, the moldability cannot be secured and the analysis area (of the powder sample after molding) In many cases, it is difficult to widen the area), the sensitivity to ultra-light elements is lowered, and accurate X-ray fluorescence analysis may not be performed.

本発明は前記従来の問題に鑑みてなされたもので、微量の粉末試料についてホウ素、炭素、窒素または酸素を分析対象元素として蛍光Ｘ線分析を行うことを可能とする試料処理方法およびそれを用いた蛍光Ｘ線分析方法を提供することを目的とする。   The present invention has been made in view of the above-described conventional problems, and uses a sample processing method that enables X-ray fluorescence analysis of a very small amount of powder sample using boron, carbon, nitrogen or oxygen as an analysis target element, and the method. It is an object to provide a fluorescent X-ray analysis method.

前記目的を達成するために、本発明の第１構成は、微量の粉末試料を蛍光Ｘ線分析するための試料処理方法であって、フッ化リチウム粉末からなる基材と、ホウ素、炭素、窒素および酸素のうちの少なくとも１つを含む粉末のバインダーとを、バインダーの含有率が０wt％よりも大きく５０wt％以下になるように混合した混合した混合基材の表面を押し固め、その混合基材の表面に粉末試料を載置して加圧成形し、混合基材と粉末試料とを一体化して分析試料とする。   In order to achieve the above object, a first configuration of the present invention is a sample processing method for fluorescent X-ray analysis of a small amount of powder sample, and a substrate made of lithium fluoride powder, boron, carbon, nitrogen And a powdered binder containing at least one of oxygen and the mixed base material mixed so that the binder content is more than 0 wt% and not more than 50 wt%, and the mixed base material is compacted A powder sample is placed on the surface of the substrate and pressure-molded, and the mixed base material and the powder sample are integrated into an analysis sample.

第１構成の試料処理方法で使用する混合基材には、ホウ素、炭素、窒素および酸素のうち少なくとも１つが、バインダーの成分として含まれているが、混合基材に含まれるフッ素からの蛍光Ｘ線の測定強度を利用した補正により、不純線の影響を除去できる。したがって、微量の粉末試料についてホウ素、炭素、窒素または酸素を分析対象元素として蛍光Ｘ線分析を行うことが可能となる。   The mixed base material used in the sample processing method of the first configuration contains at least one of boron, carbon, nitrogen and oxygen as a component of the binder, but the fluorescence X from fluorine contained in the mixed base material The correction using the measured intensity of the line can remove the influence of the impure line. Therefore, it becomes possible to perform fluorescent X-ray analysis on a very small amount of powder sample using boron, carbon, nitrogen or oxygen as an analysis target element.

本発明の第２構成は、第１構成の試料処理方法で作製した分析試料に１次Ｘ線を照射し、発生する蛍光Ｘ線の強度を測定して、粉末試料中の各元素の含有率を求める蛍光Ｘ線分析方法であって、分析対象元素に、ホウ素、炭素、窒素および酸素のうちの少なくとも１つが含まれている。この分析方法では、分析試料の作製に用いたバインダーに含まれる、フッ素以外の元素を補正対象元素とし、あらかじめ、分析試料の作製に用いた混合基材のみを加圧成形したブランク試料について、補正対象元素とフッ素の蛍光Ｘ線の強度を測定し、フッ素の測定強度に対する補正対象元素の測定強度の強度比を求めておく。そして、粉末試料中の補正対象元素の含有率を求める際には、分析試料についてのフッ素の測定強度に前記強度比を乗じて不純線強度とし、分析試料についての補正対象元素の測定強度から前記不純線強度を差し引いて補正する。   In the second configuration of the present invention, the analysis sample produced by the sample processing method of the first configuration is irradiated with primary X-rays, the intensity of the generated fluorescent X-rays is measured, and the content of each element in the powder sample X-ray fluorescence analysis method for obtaining the above, wherein the analysis target element contains at least one of boron, carbon, nitrogen and oxygen. In this analysis method, correction is performed on a blank sample in which only the mixed base material used for the preparation of the analysis sample is pressure-molded in advance, with elements other than fluorine included in the binder used for the preparation of the analysis sample as correction target elements. The intensity of the fluorescent X-rays of the target element and fluorine is measured, and the intensity ratio of the measured intensity of the correction target element to the measured intensity of fluorine is obtained. Then, when determining the content of the correction target element in the powder sample, the measurement ratio of fluorine for the analysis sample is multiplied by the intensity ratio to obtain the impure line intensity, and the measurement intensity of the correction target element for the analysis sample is calculated from the measurement intensity of the correction target element. Correct by subtracting the impure line intensity.

第２構成の蛍光Ｘ線分析方法では、第１構成の試料処理方法で微量の粉末試料を処理するので、使用する混合基材には、ホウ素、炭素、窒素および酸素のうち少なくとも１つが、バインダーの成分として含まれているが、混合基材に含まれるフッ素からの蛍光Ｘ線の測定強度を利用した補正により、不純線の影響を除去できる。したがって、微量の粉末試料についてホウ素、炭素、窒素または酸素を分析対象元素とすることが可能となる。   In the fluorescent X-ray analysis method of the second configuration, since a small amount of powder sample is processed by the sample processing method of the first configuration, at least one of boron, carbon, nitrogen, and oxygen is included in the binder used as a binder. Although it is contained as a component, it is possible to remove the influence of impure lines by correction using the measured intensity of fluorescent X-rays from fluorine contained in the mixed base material. Therefore, boron, carbon, nitrogen or oxygen can be used as an analysis target element for a very small amount of powder sample.

本発明の第１実施形態の試料処理方法により表面を押し固めた混合基材を示す側面図である。It is a side view which shows the mixing base material which the surface was pressed and solidified by the sample processing method of 1st Embodiment of this invention. 同方法により表面に粉末試料を載置した混合基材を示す側面図である。It is a side view which shows the mixing base material which mounted the powder sample on the surface by the same method. 同方法により作製した分析試料を示す側面断面図である。It is side surface sectional drawing which shows the analysis sample produced by the same method. 本発明の第２実施形態の蛍光Ｘ線分析方法において用いるブランク試料を示す側面図である。It is a side view which shows the blank sample used in the fluorescent X ray analysis method of 2nd Embodiment of this invention. 同方法において用いる蛍光Ｘ線分析装置を示す概略図である。It is the schematic which shows the fluorescent X ray analyzer used in the same method.

以下、本発明の第１実施形態の試料処理方法について、図にしたがって説明する。この方法は、微量の粉末試料を蛍光Ｘ線分析するための試料処理方法であって、まず、図１に示すように、フッ化リチウム粉末からなる基材と、粉末のバインダーとを混合した約５ｇの混合基材３ｂを、周知の加圧成形機を用いて手動による低い圧力で予備加圧成形することにより、混合基材３ｂを例えば直径４０mmの円板状に成形して、表面を押し固める。ここで、バインダーは、ホウ素、炭素、窒素および酸素のうちの少なくとも１つを含んでおり、例えばSpectro Blend （商品名。組成はＣ１９Ｈ３８ＯＮで表される）であって、混合基材３ｂにおけるバインダーの含有率は、０wt％よりも大きく５０wt％以下であり、２０wt％以下が好ましく、例えば１０wt％である。バインダーとしては、Spectro Blendの他に、例えば組成がＣ１３Ｈ１４Ｏ４またはＨ３ＢＯ３で表されるものであってもよく、基材と同様にフッ素を含むものであってもよい。 Hereinafter, the sample processing method of the first embodiment of the present invention will be described with reference to the drawings. This method is a sample processing method for fluorescent X-ray analysis of a very small amount of powder sample. First, as shown in FIG. 1, a base material made of lithium fluoride powder and a powder binder are mixed. 5 g of the mixed base material 3b is pre-press-molded at a low manual pressure using a known pressure molding machine, thereby forming the mixed base material 3b into a disk shape having a diameter of, for example, 40 mm, and pressing the surface. Solidify. Here, the binder contains at least one of boron, carbon, nitrogen and oxygen, for example, Spectro Blend (trade name; composition is represented by C 19 H 38 ON), The binder content in 3b is greater than 0 wt% and not more than 50 wt%, preferably not more than 20 wt%, for example, 10 wt%. As the binder, in addition to Spectro Blend, for example, the composition may be represented by C 13 H 14 O 4 or H 3 BO 3 , and may contain fluorine in the same manner as the base material.

次に、図２に示すように、混合基材３ｂの押し固められた表面の中央に、例えば体積で耳掻き約１杯、重量で約７mgの粉末試料３ａを載置する。そして、粉末試料３ａが混合基材３ｂの内部（深さ方向）に分散しないように、予定される蛍光Ｘ線分析での測定範囲（例えば直径１０mm）内で粉末試料３ａを混合基材３ｂの表面上で広げて、例えば５０〜１００MPa の高い圧力で十分に加圧成形し、図３に示すように、混合基材３ｂと粉末試料３ａとを一体化して円板状の分析試料３とする。このとき、粉末試料３ａは薄い円板状に成形されつつ混合基材３ｂに埋没して、露出した部分が円形になり、その直径は例えば約４mmである。   Next, as shown in FIG. 2, for example, about 1 cup of earpick by volume and about 7 mg by weight is placed on the center of the pressed surface of the mixed base material 3 b. And the powder sample 3a is mixed with the mixed sample 3b within the planned measurement range (for example, 10 mm in diameter) in the fluorescent X-ray analysis so that the powder sample 3a is not dispersed in the mixed substrate 3b (in the depth direction). Spread on the surface and sufficiently press-molded at a high pressure of, for example, 50 to 100 MPa, and as shown in FIG. 3, the mixed base material 3b and the powder sample 3a are integrated into a disc-shaped analysis sample 3. . At this time, the powder sample 3a is embedded in the mixed base material 3b while being formed into a thin disk shape, and the exposed portion becomes circular, and the diameter thereof is about 4 mm, for example.

第１実施形態の試料処理方法で使用する混合基材３ｂには、ホウ素、炭素、窒素および酸素のうち少なくとも１つが、バインダーの成分として含まれているが、後述するように、混合基材に含まれるフッ素からの蛍光Ｘ線の測定強度を利用した補正により、不純線の影響を除去できる。したがって、微量の粉末試料３ａについてホウ素、炭素、窒素または酸素（これら４元素の任意の組合せを含む）を分析対象元素として蛍光Ｘ線分析を行うことが可能となる。   The mixed base material 3b used in the sample processing method of the first embodiment includes at least one of boron, carbon, nitrogen, and oxygen as a component of the binder. By the correction using the measurement intensity of the fluorescent X-rays from the contained fluorine, the influence of the impure line can be removed. Therefore, it is possible to perform fluorescent X-ray analysis on a very small amount of the powder sample 3a using boron, carbon, nitrogen or oxygen (including any combination of these four elements) as an analysis target element.

次に、本発明の第２実施形態の蛍光Ｘ線分析方法について説明するが、それにあたり、まず、同方法において用いる蛍光Ｘ線分析装置について説明する。図５に示すように、この装置は、分析試料３が載置される試料台８と、分析試料３に１次Ｘ線２を照射するＸ線管などのＸ線源１と、分析試料３から発生する蛍光Ｘ線４の強度を測定する検出手段９と、検出手段９での測定強度に基づいて分析試料３の一部となった粉末試料３ａ（図３）中の各元素の含有率を算出するコンピュータなどの算出手段１０とを備えている。   Next, a fluorescent X-ray analysis method according to a second embodiment of the present invention will be described. First, a fluorescent X-ray analysis apparatus used in the method will be described. As shown in FIG. 5, this apparatus includes a sample stage 8 on which the analysis sample 3 is placed, an X-ray source 1 such as an X-ray tube that irradiates the analysis sample 3 with the primary X-ray 2, and the analysis sample 3. Content of each element in the powder sample 3a (FIG. 3) which became a part of the analysis sample 3 based on the intensity measured by the detection means 9 And calculating means 10 such as a computer for calculating.

検出手段９は、分析試料３から発生する蛍光Ｘ線４を分光する分光素子５と、分光された蛍光Ｘ線６ごとにその強度を測定する検出器７で構成される。なお、分光素子５を用いずに、エネルギー分解能の高い検出器を検出手段としてもよい。また、分析試料３に１次Ｘ線２を照射する際には、所定の寸法形状のマスク孔を有するマスクで分析試料３の表面を覆う等の周知技術により、分析試料３の一部となった粉末試料３ａ（図３）が露出している部分に集中的に照射するようにする。   The detection means 9 includes a spectroscopic element 5 that separates the fluorescent X-rays 4 generated from the analysis sample 3 and a detector 7 that measures the intensity of each spectroscopic fluorescent X-ray 6. In addition, it is good also as a detection means not using the spectroscopic element 5, but a detector with high energy resolution. Further, when the analysis sample 3 is irradiated with the primary X-ray 2, the analysis sample 3 becomes a part of the analysis sample 3 by a known technique such as covering the surface of the analysis sample 3 with a mask having a mask hole having a predetermined size and shape. The exposed powder sample 3a (FIG. 3) is irradiated intensively.

第２実施形態の蛍光Ｘ線分析方法は、第１実施形態の試料処理方法で作製した分析試料３に対し、上述した蛍光Ｘ線分析装置を用いて、１次Ｘ線２を照射し、発生する蛍光Ｘ線４の強度を測定して、粉末試料３ａ中の各元素の含有率を求める蛍光Ｘ線分析方法であって、分析対象元素に、ホウ素、炭素、窒素および酸素のうちの少なくとも１つが含まれている。   The fluorescent X-ray analysis method of the second embodiment is generated by irradiating the analysis sample 3 produced by the sample processing method of the first embodiment with the primary X-ray 2 using the fluorescent X-ray analyzer described above. Is a fluorescent X-ray analysis method for determining the content of each element in the powder sample 3a by measuring the intensity of the fluorescent X-ray 4 that includes at least one of boron, carbon, nitrogen and oxygen One is included.

この分析方法では、分析試料３の作製に用いたバインダーに含まれる、フッ素以外の元素を補正対象元素とする。この例では、Spectro Blend であるバインダーの主成分すなわち炭素を補正対象元素とする。また、あらかじめ、分析試料３の作製に用いた混合基材のみを例えば５０〜１００MPa の高い圧力で十分に加圧成形して、図４に示すような円板状のブランク試料１３を作製し、上述した図５の蛍光Ｘ線分析装置を用いて、炭素（補正対象元素）とフッ素の蛍光Ｘ線４の強度をそれぞれ測定し、フッ素の測定強度ＩF0に対する炭素の測定強度ＩC0の強度比ＩC0／ＩF0をあらかじめ求めて算出手段１０に記憶させておく。   In this analysis method, an element other than fluorine contained in the binder used for producing the analysis sample 3 is used as a correction target element. In this example, the main component of the binder which is Spectro Blend, that is, carbon is used as the correction target element. Further, in advance, only the mixed base material used for the preparation of the analytical sample 3 is sufficiently press-molded at a high pressure of, for example, 50 to 100 MPa, to produce a disc-shaped blank sample 13 as shown in FIG. Using the fluorescent X-ray analyzer of FIG. 5 described above, the intensities of carbon (correction target element) and fluorine fluorescent X-ray 4 are measured, respectively, and the intensity ratio IC0 / of the measured intensity ICO of carbon to the measured intensity IF0 of fluorine. IF0 is obtained in advance and stored in the calculation means 10.

そして、その蛍光Ｘ線分析装置を用いて、分析試料３について測定し、粉末試料３ａ中の炭素の含有率を求める際には、算出手段１０によって、分析試料３についてのフッ素の測定強度ＩF に前記強度比ＩC0／ＩF0を乗じて不純線強度ＩC0・ＩF ／ＩF0とし、分析試料３についての炭素の測定強度ＩC から前記不純線強度ＩC0・ＩF ／ＩF0を差し引いて補正する。つまり、補正後の分析試料３についての炭素の測定強度ＩCAは、ＩC −ＩC0・ＩF ／ＩF0で算出され、この補正後の測定強度ＩCAを分析試料３の一部となった粉末試料３ａから発生した炭素の蛍光Ｘ線４の強度とし、分析試料３からの他の元素の蛍光Ｘ線４の測定強度と併せ用いて、粉末試料３ａ中の各元素の含有率を求める。   Then, using the X-ray fluorescence analyzer, the analytical sample 3 is measured, and when the carbon content in the powder sample 3a is determined, the calculation means 10 determines the fluorine measurement intensity IF for the analytical sample 3. By multiplying the intensity ratio IC0 / IF0 to obtain an impure line intensity IC0 · IF / IF0, correction is performed by subtracting the impure line intensity IC0 · IF / IF0 from the measured intensity IC of carbon for the analysis sample 3. In other words, the measured carbon intensity ICA for the corrected analytical sample 3 is calculated as Ic-IC0.IF / IF0, and this corrected measured intensity ICA is generated from the powder sample 3a that is part of the analytical sample 3. The content of each element in the powder sample 3a is obtained by using the intensity of the fluorescent X-ray 4 of carbon and the measured intensity of the fluorescent X-ray 4 of other elements from the analysis sample 3.

第２実施形態の蛍光Ｘ線分析方法では、第１実施形態の試料処理方法で微量の粉末試料３ａを処理するので、使用する混合基材３ｂには、ホウ素、炭素、窒素および酸素のうち少なくとも１つが、バインダーの成分として含まれているが、上述したように、混合基材に含まれるフッ素からの蛍光Ｘ線４の測定強度ＩF0，ＩF を利用した補正により、不純線の影響を除去する。したがって、微量の粉末試料３ａについてホウ素、炭素、窒素または酸素（これら４元素の任意の組合せを含む）を分析対象元素とすることが可能となる。   In the fluorescent X-ray analysis method of the second embodiment, since a small amount of the powder sample 3a is processed by the sample processing method of the first embodiment, the mixed substrate 3b to be used includes at least one of boron, carbon, nitrogen, and oxygen. One is included as a component of the binder, but as described above, the influence of the impure line is removed by correction using the measured intensities IF0 and IF of the fluorescent X-ray 4 from the fluorine contained in the mixed base material. . Therefore, boron, carbon, nitrogen, or oxygen (including any combination of these four elements) can be used as an analysis target element for a very small amount of the powder sample 3a.

２ １次Ｘ線
３ 分析試料
３ａ 粉末試料
３ｂ 混合基材
４ 蛍光Ｘ線 2 Primary X-ray 3 Analysis sample 3a Powder sample 3b Mixed base material 4 Fluorescent X-ray

Claims (1)

微量の粉末試料を蛍光Ｘ線分析するために処理する方法であって、
フッ化リチウム粉末からなる基材と、ホウ素、炭素、窒素および酸素のうちの少なくとも１つを含む粉末のバインダーとを、バインダーの含有率が０wt％よりも大きく５０wt％以下になるように混合した混合基材の表面を押し固め、
その混合基材の表面に粉末試料を載置して加圧成形し、混合基材と粉末試料とを一体化して分析試料とする試料処理方法。 A method for processing a small amount of powder sample for fluorescent X-ray analysis,
A base material made of lithium fluoride powder and a powder binder containing at least one of boron, carbon, nitrogen and oxygen were mixed so that the binder content was greater than 0 wt% and less than 50 wt%. Press and harden the surface of the mixed substrate,
A sample processing method in which a powder sample is placed on the surface of the mixed base material, press-molded, and the mixed base material and the powder sample are integrated into an analysis sample.
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