JP2002181743A - Method for preparing oil sample for fluorescent x-ray analysis - Google Patents
Method for preparing oil sample for fluorescent x-ray analysisInfo
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- JP2002181743A JP2002181743A JP2000374793A JP2000374793A JP2002181743A JP 2002181743 A JP2002181743 A JP 2002181743A JP 2000374793 A JP2000374793 A JP 2000374793A JP 2000374793 A JP2000374793 A JP 2000374793A JP 2002181743 A JP2002181743 A JP 2002181743A
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- Prior art keywords
- oil sample
- analyzed
- filtration
- filtration membrane
- additive
- Prior art date
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- Separation Using Semi-Permeable Membranes (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、添加剤を含む潤滑
油試料等の油試料を蛍光Ｘ線分析するための調製法に関
する。TECHNICAL FIELD The present invention relates to a preparation method for X-ray fluorescence analysis of an oil sample such as a lubricating oil sample containing an additive.
【０００２】[0002]
【従来の技術】従来より、油試料の含有成分、例えば潤
滑油試料に含まれる種々の添加剤元素の含有量を分析す
る方法として、ＩＣＰ発光分析と蛍光Ｘ線分析がある。2. Description of the Related Art Conventionally, ICP emission analysis and X-ray fluorescence analysis have been used as methods for analyzing the components contained in an oil sample, for example, the contents of various additive elements contained in a lubricating oil sample.
【０００３】[0003]
【発明が解決しようとする課題】ＩＣＰ発光分析では、
その原理から、ppb レベルの濃度の微量元素の分析が可
能であるが、Ｓについては検出感度不足から精度が悪
く、Ｎについては分析ができず、これらの非金属元素の
分析が不十分である。一方、蛍光Ｘ線分析では、その原
理から、非金属元素の分析も可能であるが、数百ppm レ
ベルの濃度のＢ、Ｎ等のいわゆる超軽元素（Ｍg よりも
軽い元素）や、その他の元素でも数ppm レベルの濃度の
微量元素からはごく微弱な蛍光Ｘ線しか得られず、それ
らの元素の分析が非常に困難である。したがって、いず
れの分析方法でも、非金属元素、超軽元素、微量元素の
すべてを適切に分析することはできない。SUMMARY OF THE INVENTION In ICP emission spectrometry,
From the principle, it is possible to analyze trace elements at the ppb level, but the accuracy of S is poor due to insufficient detection sensitivity, the analysis of N cannot be performed, and the analysis of these non-metal elements is insufficient. . On the other hand, in the fluorescent X-ray analysis, the analysis of nonmetallic elements is also possible from the principle, but so-called ultralight elements (elements lighter than Mg) such as B and N at a concentration of several hundred ppm level, and other elements. Only trace X-rays can be obtained from trace elements at a concentration of several ppm, and it is very difficult to analyze these elements. Therefore, none of the analysis methods can properly analyze all of the nonmetallic elements, ultralight elements, and trace elements.
【０００４】本発明は前記従来の問題に鑑みてなされた
もので、蛍光Ｘ線分析するのに十分な強度の蛍光Ｘ線が
得られるように、油試料に含まれる分析対象元素を濃縮
する調製法を提供することを目的とする。SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned conventional problems, and has been made to concentrate an element to be analyzed contained in an oil sample so as to obtain X-ray fluorescence having sufficient intensity for X-ray fluorescence analysis. The purpose is to provide the law.
【０００５】[0005]
【課題を解決するための手段】前記目的を達成するため
に、本願第１の発明に係る蛍光Ｘ線分析用の油試料の調
製法は、油試料に含まれる分析対象元素を濃縮して蛍光
Ｘ線分析するのに用いられる方法であって、ろ過膜を用
いて前記油試料を吸引ろ過または加圧ろ過し、前記分析
対象元素を含む成分を前記ろ過膜上に分離する。In order to achieve the above object, a method for preparing an oil sample for X-ray fluorescence analysis according to the first invention of the present application comprises concentrating an element to be analyzed contained in the oil sample to obtain a fluorescent light. A method used for X-ray analysis, wherein the oil sample is subjected to suction filtration or pressure filtration using a filtration membrane, and a component containing the element to be analyzed is separated on the filtration membrane.
【０００６】本願第１の発明によれば、油試料を吸引ろ
過または加圧ろ過して、分析対象元素を含む成分をろ過
膜上に分離するので、分析対象元素を迅速に濃縮でき、
蛍光Ｘ線分析するのに十分な強度の蛍光Ｘ線が得られ
る。According to the first aspect of the present invention, since the oil sample is subjected to suction filtration or pressure filtration to separate a component containing the element to be analyzed on the filtration membrane, the element to be analyzed can be rapidly concentrated.
X-ray fluorescence with sufficient intensity for X-ray fluorescence analysis is obtained.
【０００７】本願第２の発明に係る蛍光Ｘ線分析用の油
試料の調製法は、油試料に含まれる分析対象元素を濃縮
して蛍光Ｘ線分析するのに用いられる方法であって、加
圧した溶媒を用いる液相クロマトグラフィーにより、前
記分析対象元素を含む成分をろ過膜上に分離する。The method for preparing an oil sample for X-ray fluorescence analysis according to the second invention of the present application is a method used for concentrating an element to be analyzed contained in an oil sample and performing X-ray fluorescence analysis. The component containing the element to be analyzed is separated on a filtration membrane by liquid phase chromatography using a pressurized solvent.
【０００８】本願第２の発明によれば、液相クロマトグ
ラフィーにおいて溶媒を加圧して分析対象元素を含む成
分をろ過膜上に分離するので、分析対象元素を迅速に濃
縮でき、蛍光Ｘ線分析するのに十分な強度の蛍光Ｘ線が
得られる。According to the second aspect of the present invention, since the component containing the element to be analyzed is separated on the filtration membrane by pressurizing the solvent in liquid phase chromatography, the element to be analyzed can be rapidly concentrated, and the X-ray fluorescence analysis Fluorescent X-rays of sufficient intensity to obtain
【０００９】本願第３の発明に係る蛍光Ｘ線分析用の油
試料の調製法は、油試料に含まれる分析対象元素を濃縮
して蛍光Ｘ線分析するのに用いられる方法であって、加
圧した溶媒を用いる液相クロマトグラフィーにより前記
油試料から前記分析対象元素を含む成分を分離してカラ
ム充填剤に吸着させ、そのカラム充填剤を平板状に加圧
成形する。The method of preparing an oil sample for X-ray fluorescence analysis according to the third invention of the present application is a method used for concentrating an element to be analyzed contained in an oil sample and performing X-ray fluorescence analysis. The component containing the element to be analyzed is separated from the oil sample by liquid phase chromatography using a pressurized solvent, adsorbed to a column filler, and the column filler is pressed into a flat plate.
【００１０】本願第３の発明によれば、液相クロマトグ
ラフィーにおいて溶媒を加圧して用い、油試料から分析
対象元素を含む成分を分離してカラム充填剤に吸着さ
せ、そのカラム充填剤を平板状に加圧成形するので、分
析対象元素を迅速に濃縮でき、蛍光Ｘ線分析するのに十
分な強度の蛍光Ｘ線が得られる。According to the third aspect of the present invention, in a liquid phase chromatography, a solvent is used under pressure, a component containing an element to be analyzed is separated from an oil sample and adsorbed on a column packing material, and the column packing material is flattened. Since the pressure is formed into a shape, the element to be analyzed can be rapidly concentrated, and fluorescent X-rays having sufficient intensity for fluorescent X-ray analysis can be obtained.
【００１１】[0011]
【発明の実施の形態】以下、本発明の実施形態の方法に
ついて、潤滑油試料中の添加剤元素や摩耗粉元素を蛍光
Ｘ線分析するために濃縮する手法の一例として、説明す
る。まず、第１実施形態の方法では、図１のように、フ
ラスコ（ブフナーフラスコ）１にゴム栓２およびガラス
摺り合わせを介して漏斗３をシールして取り付け、漏斗
３の注入口に、メッシュ部材４を介して試料調整用ホル
ダー５を載置する。漏斗３、メッシュ部材４、試料調整
用ホルダー５の各間も、ゴム部材によりシールする。BEST MODE FOR CARRYING OUT THE INVENTION A method according to an embodiment of the present invention will be described below as an example of a technique for concentrating additive elements and wear powder elements in a lubricating oil sample for X-ray fluorescence analysis. First, in the method of the first embodiment, as shown in FIG. 1, a funnel 3 is sealed and attached to a flask (Buchner flask) 1 via a rubber stopper 2 and a glass rub, and a mesh member is inserted into an inlet of the funnel 3. The sample adjustment holder 5 is placed via the sample holder 4. The space between the funnel 3, the mesh member 4, and the sample adjustment holder 5 is also sealed with a rubber member.
【００１２】試料調整用ホルダー５には、ゴム膜、高分
子膜、ミリポアフィルターまたはろ紙の表面にポリメタ
クリレート（ＰＭＡ）を付着させたろ過膜６が張ってあ
る。ゴム膜としては、天然ゴム膜、Ｓi ゴム膜、ウレタ
ンゴム膜等を用いることができ、高分子膜としては、同
軸延伸、二軸延伸、イオンスパッタリング、ケミカルエ
ッチング等で多孔質化された高分子膜を用いることがで
きる。特に、東燃タピルス（株）より商品名「ＳＥＰＥ
ＬＡ」で発売されている二軸延伸高分子膜が好ましく、
ここではそれを用いる。The sample adjusting holder 5 has a rubber membrane, a polymer membrane, a millipore filter, or a filter membrane 6 in which polymethacrylate (PMA) is adhered to the surface of a filter paper. As the rubber film, a natural rubber film, a Si rubber film, a urethane rubber film, or the like can be used. As the polymer film, a polymer film made porous by coaxial stretching, biaxial stretching, ion sputtering, chemical etching, or the like can be used. A membrane can be used. In particular, the brand name "SEPE" from Tonen Tapils
LA "is preferably a biaxially stretched polymer membrane,
Here we use it.
【００１３】ポリメタクリレートは、例えば以下のよう
にして付着させることができる。市販の二軸延伸高分子
膜を５０×５０ｍｍに切り出して吸引ろ過器に取り付
け、その上に０．３％のポリメタクリレートを１ｍｌ滴
下して吸引ろ過し、乾燥空気を流して溶媒を完全に除去
して、吸引ろ過器から取り外す。このように、市販のろ
過膜の表面にポリメタクリレートを付着させる前処理に
より、ろ過膜の孔径を調整できるとともに、ろ過膜の溶
媒に対する強度や機械的強度を増大させることができ
る。ポリメタクリレートを付着させたろ過膜６におい
て、ろ過膜６が通過させる分子の分子量は、捕捉すべき
添加剤または摩耗粉の分子量よりも小さくなるよう設定
し、１３００以下にある。通過させる分子の分子量での
設定に代えて、ろ過膜６が多数有する孔の直径を２００
〜８００Åの範囲内に設定することもできる（平均的な
孔径は３００〜５００Åである）。なお、ポリメタクリ
レートを付着させる代わりに、ろ過膜に極性をもたせる
ように改造してイオン交換により分析対象元素を含む成
分を分離濃縮することもできる。The polymethacrylate can be deposited, for example, as follows. A commercially available biaxially stretched polymer membrane is cut into 50 × 50 mm, attached to a suction filter, 1 ml of 0.3% polymethacrylate is dropped thereon, suction filtered, and dry air is flowed to completely remove the solvent. And remove it from the suction filter. As described above, by the pretreatment of attaching polymethacrylate to the surface of a commercially available filtration membrane, the pore size of the filtration membrane can be adjusted, and the strength of the filtration membrane with respect to the solvent and the mechanical strength can be increased. In the filtration membrane 6 to which polymethacrylate is adhered, the molecular weight of the molecules passed through the filtration membrane 6 is set to be smaller than the molecular weight of the additive or wear powder to be captured, and is 1300 or less. Instead of setting the molecular weight of the molecules to be passed, the diameter of the pores of the filtration membrane 6 is set to 200
It can also be set in the range of Å800 ° (average pore size is 300〜500 °). Instead of attaching polymethacrylate, the filtration membrane may be modified so as to have polarity, and components containing the element to be analyzed may be separated and concentrated by ion exchange.
【００１４】そして、所定量の潤滑油試料７および適量
の溶媒８をろ過膜６に注ぐとともに、フラスコ１の吸引
口１ａから、例えば蛍光Ｘ線分析装置付属の真空ポンプ
およびアスピレーターで排気して、吸引ろ過を行う。溶
媒８を用いるのは、吸引ろ過をより迅速に行うためであ
り、溶媒８としては、トルエン、メタノール、ペンタ
ン、ヘキサン、ヘプタン、オクタン、石油エーテル、ア
セトンまたはそれらを混合したものを用いることができ
る。特に、ヘキサンとイソオクタンを３対７で混合した
ものが、油除去率、分散性（ろ過膜上に捕捉したものが
均等に分散する状態）等の効果において好ましく、ここ
ではこの混合溶媒８を用いる。Then, a predetermined amount of the lubricating oil sample 7 and an appropriate amount of the solvent 8 are poured into the filtration membrane 6 and evacuated from the suction port 1a of the flask 1 by, for example, a vacuum pump and an aspirator attached to a fluorescent X-ray analyzer. Perform suction filtration. The solvent 8 is used in order to perform suction filtration more quickly. As the solvent 8, toluene, methanol, pentane, hexane, heptane, octane, petroleum ether, acetone, or a mixture thereof can be used. . In particular, a mixture of hexane and isooctane at a ratio of 3: 7 is preferable in terms of effects such as an oil removal rate and dispersibility (a state in which the substance captured on the filtration membrane is uniformly dispersed), and the like. .
【００１５】この吸引ろ過により、潤滑油試料７中の基
油７ａだけが溶媒８に溶けて低粘度の溶液となって、ろ
過膜６を通過してフラスコ１内に溜まり、図２のよう
に、ろ過膜６上に添加剤７ｂが分離される。すなわち、
試料調整用ホルダー５のろ過膜６上に、添加剤７ｂが濃
縮されて塗布された状態になるので、この試料調整用ホ
ルダー５に下方からベース部材８を取り付けてろ過膜６
および添加剤７ｂを持ち上げ、試料測定用ホルダー９と
する。この試料測定用ホルダー９を蛍光Ｘ線分析装置の
試料台に載置すれば、上方から添加剤７ｂに１次Ｘ線１
０を照射して発生する蛍光Ｘ線１１の強度を測定するこ
とができる。なお、ここでは、分析対象元素を含む成分
が添加剤である場合について説明したが、分析対象元素
を含む成分が、摩耗粉である場合や、添加剤と摩耗粉の
両方である場合も、同様に分離できる。この点は、以下
の他の実施形態においても同様である。By this suction filtration, only the base oil 7a in the lubricating oil sample 7 is dissolved in the solvent 8 to form a low-viscosity solution, passes through the filtration membrane 6, and accumulates in the flask 1 as shown in FIG. The additive 7b is separated on the filtration membrane 6. That is,
Since the additive 7b is concentrated and applied on the filtration membrane 6 of the sample adjustment holder 5, the base member 8 is attached to the sample adjustment holder 5 from below and the filtration membrane 6 is removed.
Then, the additive 7b is lifted to be the sample measuring holder 9. When this sample measuring holder 9 is placed on the sample stage of the fluorescent X-ray analyzer, the primary X-rays 1
The intensity of the fluorescent X-ray 11 generated by irradiating 0 can be measured. Here, the case where the component containing the element to be analyzed is an additive has been described, but the same applies to the case where the component containing the element to be analyzed is wear powder or when both the additive and the wear powder are present. Can be separated. This is the same in other embodiments described below.
【００１６】このように、第１実施形態の方法によれ
ば、潤滑油等の油試料７を吸引ろ過して、添加剤等の分
析対象元素を含む成分７ｂをろ過膜６上に分離するの
で、分析対象元素を迅速に濃縮でき、分析対象元素が、
１００〜５００ppm の濃度のＢ、Ｎ等のいわゆる超軽元
素や、その他の元素で数ppm レベルの濃度の微量元素で
あっても、蛍光Ｘ線分析するのに十分な強度の蛍光Ｘ線
１１が得られる。しかも、分析対象元素を含む成分７ｂ
がろ過膜６上に薄膜状かつ平坦に塗布された状態になる
ので、散乱線の発生を抑制でき、蛍光Ｘ線分析のＳＮ比
をいっそう高めることができる。As described above, according to the method of the first embodiment, the oil sample 7 such as a lubricating oil is suction-filtered, and the component 7b containing the element to be analyzed such as an additive is separated on the filtration membrane 6. , The element to be analyzed can be rapidly concentrated,
Even so-called ultra-light elements such as B and N having a concentration of 100 to 500 ppm, and trace elements having a concentration of several ppm as other elements, fluorescent X-rays 11 having sufficient intensity for fluorescent X-ray analysis can be obtained. can get. Moreover, the component 7b containing the element to be analyzed
Is thinly and flatly applied on the filtration membrane 6, so that the generation of scattered radiation can be suppressed and the SN ratio of the fluorescent X-ray analysis can be further increased.
【００１７】次に、本発明の第２実施形態の方法では、
図３のように、シリンジ（注射器）１２に所定量の潤滑
油試料７および適量の溶媒８を吸引し、シリンジ１２の
先に、ろ過膜６を組み込んだろ過カートリッジ１３を取
り付け、シリンジ１２内の溶液７，８を押し出すことに
より加圧ろ過する。ろ過膜６、溶媒８は、第１実施形態
と同様のものを用いることができる。加圧ろ過の結果、
図４のように、ろ過膜６上に添加剤７ｂが分離される。
すなわち、ろ過カートリッジ１３のろ過膜６上に、添加
剤７ｂが濃縮されて塗布された状態になるので、このろ
過カートリッジ１３を分解してろ過膜６を取り出し、上
面照射の場合は、図５のように、通常用いられる試料ホ
ルダー１４に組み込んで、蛍光Ｘ線分析装置の試料台に
載置すれば、上方から添加剤７ｂに１次Ｘ線１０を照射
して発生する蛍光Ｘ線１１の強度を測定することができ
る。ろ過膜６上に付着した捕捉物（添加剤７ｂ）が、粘
性が高く、少量の場合には、下方から添加剤７ｂに１次
Ｘ線１０を照射する下面照射も可能である。Next, in the method according to the second embodiment of the present invention,
As shown in FIG. 3, a predetermined amount of the lubricating oil sample 7 and an appropriate amount of the solvent 8 are sucked into a syringe (syringe) 12, and a filtration cartridge 13 having the filtration membrane 6 incorporated therein is attached to the tip of the syringe 12. The solutions 7 and 8 are filtered under pressure by extruding. As the filtration membrane 6 and the solvent 8, the same one as in the first embodiment can be used. As a result of pressure filtration,
As shown in FIG. 4, the additive 7b is separated on the filtration membrane 6.
That is, since the additive 7b is concentrated and applied on the filtration membrane 6 of the filtration cartridge 13, the filtration cartridge 13 is disassembled and the filtration membrane 6 is taken out. As described above, by incorporating the sample into a commonly used sample holder 14 and placing it on the sample stage of the fluorescent X-ray analyzer, the intensity of the fluorescent X-ray 11 generated by irradiating the additive 7b with the primary X-ray 10 from above is generated. Can be measured. When the trapped substance (additive 7b) attached to the filtration membrane 6 has a high viscosity and a small amount, lower surface irradiation in which the additive 7b is irradiated with the primary X-ray 10 from below can be performed.
【００１８】このように、第２実施形態の方法によれ
ば、潤滑油等の油試料７を加圧ろ過して、添加剤等の分
析対象元素を含む成分７ｂをろ過膜６上に分離するの
で、分析対象元素を迅速に濃縮でき、分析対象元素が、
１００〜５００ppm の濃度のＢ、Ｎ等のいわゆる超軽元
素や、その他の元素で数ppm レベルの濃度の微量元素で
あっても、蛍光Ｘ線分析するのに十分な強度の蛍光Ｘ線
１１が得られる。しかも、分析対象元素を含む成分７ｂ
がろ過膜６上に薄膜状かつ平坦に塗布された状態になる
ので、散乱線の発生を抑制でき、蛍光Ｘ線分析のＳＮ比
をいっそう高めることができる。As described above, according to the method of the second embodiment, the oil sample 7 such as a lubricating oil is filtered under pressure, and the component 7b containing the element to be analyzed such as an additive is separated on the filtration membrane 6. Therefore, the element to be analyzed can be concentrated quickly,
Even so-called ultra-light elements such as B and N having a concentration of 100 to 500 ppm, and trace elements having a concentration of several ppm as other elements, fluorescent X-rays 11 having sufficient intensity for fluorescent X-ray analysis can be obtained. can get. Moreover, the component 7b containing the element to be analyzed
Is thinly and flatly applied on the filtration membrane 6, so that the generation of scattered radiation can be suppressed and the SN ratio of the fluorescent X-ray analysis can be further increased.
【００１９】次に、本発明の第３実施形態の方法では、
図６のように、まず、シリンジ１２に所定量の潤滑油試
料７および適量の第１の溶媒８Ａを吸引し、シリンジ１
２の先に、カラム充填剤１５を詰めたカラムカートリッ
ジ１６を取り付け、シリンジ１２内の溶液７，８Ａを押
し出して、カラム充填剤１５に吸着させる。第１の溶媒
８Ａとしては、第１実施形態と同様のものを用いること
ができる。カラム充填剤１５としては、シリカゲル、フ
ロリジル（Ｍg ＯとＳi Ｏ2 ）、Ａl2Ｏ3 、イオン交換
樹脂、Ｓi Ｏ2 にＣ１８やＣ８を付加したもの、高分子
に極性を付加したもの等を用いることができ、ここでは
粉状のシリカゲルを用いる。これにより、潤滑油試料７
中の基油７ａを第１の溶媒８Ａに溶かして、洗い流すこ
とができる。Next, in the method according to the third embodiment of the present invention,
As shown in FIG. 6, first, a predetermined amount of the lubricating oil sample 7 and an appropriate amount of the first solvent 8A are sucked into the syringe 12, and the syringe 1
A column cartridge 16 packed with a column filler 15 is attached to the end of the column 2, and the solutions 7, 8A in the syringe 12 are extruded and adsorbed on the column filler 15. As the first solvent 8A, the same solvent as in the first embodiment can be used. The column packing material 15, silica gel, Florisil (Mg O and Si O 2), Al 2 O 3, ion exchange resins, obtained by adding the Si O 2 to C18 or C8, and the like obtained by adding a polarity polymer In this case, powdery silica gel is used. Thereby, the lubricating oil sample 7
The base oil 7a therein can be dissolved in the first solvent 8A and washed away.
【００２０】次に、シリンジ１２からいったんカラムカ
ートリッジ１６を取り外して、適量の第２の溶媒８Ｂを
吸引し、再度カラムカートリッジ１６を取り付け、シリ
ンジ１２内の第２の溶媒８Ｂを押し出す。第２の溶媒８
Ｂとしては、トルエンを用いることができる。これによ
り、潤滑油試料７中の添加剤７ｂのうちベンゼン環をも
つ第１種の添加剤７ｂ1 が第２の溶媒８Ｂに溶かし出さ
れるので、第１実施形態と同様の試料調整用ホルダー５
のろ過膜６上に採取し、８０℃で真空乾燥させて採取し
た溶液７ｂ1 ，８Ｂから第２の溶媒８Ｂを揮発させ、第
１種の添加剤７ｂ1 をろ過膜６上に分離する。すなわ
ち、試料調整用ホルダー５のろ過膜６上に、第１種の添
加剤７ｂ1 が濃縮されて塗布された状態になる。Next, once the column cartridge 16 is removed from the syringe 12, an appropriate amount of the second solvent 8B is sucked, the column cartridge 16 is attached again, and the second solvent 8B in the syringe 12 is pushed out. Second solvent 8
As B, toluene can be used. As a result, the first additive 7b1 having a benzene ring among the additives 7b in the lubricating oil sample 7 is dissolved out in the second solvent 8B, so that the sample adjusting holder 5 similar to the first embodiment is used.
The second solvent 8B is volatilized from the collected solutions 7b1 and 8B by vacuum drying at 80 ° C., and the first kind of additive 7b1 is separated on the filtration membrane 6. That is, the first additive 7b1 is concentrated and applied on the filtration membrane 6 of the sample preparation holder 5.
【００２１】次に、シリンジ１２からまたいったんカラ
ムカートリッジ１６を取り外して、適量の第３の溶媒８
Ｃを吸引し、再度カラムカートリッジ１６を取り付け、
シリンジ１２内の第３の溶媒８Ｃを押し出す。第３の溶
媒８Ｃとしては、メタノールを用いることができる。こ
れにより、潤滑油試料７中の添加剤７ｂのうち極性の強
い第２種の添加剤７ｂ2 が第３の溶媒８Ｃに溶かし出さ
れるので、新たな試料調整用ホルダー５のろ過膜６上に
採取し、８０℃で真空乾燥させて採取した溶液７ｂ2 ，
８Ｃから第３の溶媒８Ｃを揮発させ、第２種の添加剤７
ｂ2 をろ過膜６上に分離する。すなわち、試料調整用ホ
ルダー５のろ過膜６上に、第２種の添加剤７ｂ2 が濃縮
されて塗布された状態になる。Next, the column cartridge 16 is once again removed from the syringe 12 and an appropriate amount of the third solvent 8 is removed.
C is aspirated, and the column cartridge 16 is attached again,
The third solvent 8C in the syringe 12 is pushed out. As the third solvent 8C, methanol can be used. As a result, the second polar additive 7b2 of the additive 7b in the lubricating oil sample 7 is dissolved out into the third solvent 8C, and is collected on the filtration membrane 6 of the new sample adjusting holder 5. And dried under vacuum at 80 DEG C. to obtain a solution 7b2,
8C, the third solvent 8C is volatilized, and the second additive 7
b2 is separated on the filtration membrane 6. That is, the second additive 7b2 is concentrated and applied on the filtration membrane 6 of the sample preparation holder 5.
【００２２】このようにして得られた各試料調整用ホル
ダー５に、上面照射の場合は、図２のように、下方から
ベース部材８を取り付けて試料測定用ホルダー９とし、
蛍光Ｘ線分析装置の試料台に載置すれば、上方から添加
剤７ｂ1 ，７ｂ2 に１次Ｘ線１０を照射して発生する蛍
光Ｘ線１１の強度を測定することができる。ろ過膜６上
に付着した捕捉物（添加剤７ｂ1 ，７ｂ2 ）が、粘性が
高く、少量の場合には、下方から添加剤７ｂ1 ，７ｂ2
に１次Ｘ線１０を照射する下面照射も可能である。In the case of upper surface irradiation, a base member 8 is attached from below to a sample measuring holder 9 as shown in FIG.
When placed on the sample table of the fluorescent X-ray analyzer, the intensity of the fluorescent X-rays 11 generated by irradiating the additives 7b1 and 7b2 with the primary X-rays 10 from above can be measured. The trapped substances (additives 7b1 and 7b2) adhering to the filtration membrane 6 are highly viscous, and when the amount is small, the additives 7b1 and 7b2 are added from below.
It is also possible to irradiate the bottom surface with primary X-rays 10.
【００２３】以上のように、第３実施形態の方法によれ
ば、液相クロマトグラフィーにおいて溶媒８を加圧して
潤滑油試料中の添加剤等の分析対象元素を含む成分７ｂ
を溶解させ、ろ過膜６上に採取し、溶媒８を揮発させて
分析対象元素を含む成分７ｂをろ過膜６上に分離するの
で、分析対象元素を迅速に濃縮でき、分析対象元素が、
１００〜５００ppm の濃度のＢ、Ｎ等のいわゆる超軽元
素や、その他の元素で数ppm レベルの濃度の微量元素で
あっても、蛍光Ｘ線分析するのに十分な強度の蛍光Ｘ線
１１が得られる。しかも、分析対象元素を含む成分７ｂ
がろ過膜６上に薄膜状かつ平坦に塗布された状態になる
ので、散乱線の発生を抑制でき、蛍光Ｘ線分析のＳＮ比
をいっそう高めることができる。さらに、分析対象元素
を含む成分７ｂを溶解する溶媒８Ｂ，８Ｃを複数種類用
いて繰り返し処理することにより、分析対象元素を含む
成分７ｂ1 ，７ｂ2 を分別することができ、蛍光Ｘ線分
析における共存元素の影響を軽減することもできる。As described above, according to the method of the third embodiment, the solvent 8 is pressurized in the liquid phase chromatography and the component 7b containing the element to be analyzed such as an additive in the lubricating oil sample is added.
Is dissolved, collected on the filtration membrane 6, and the solvent 8 is volatilized to separate the component 7b containing the element to be analyzed on the filtration membrane 6, so that the element to be analyzed can be rapidly concentrated, and the element to be analyzed is
Even so-called ultra-light elements such as B and N having a concentration of 100 to 500 ppm, and trace elements having a concentration of several ppm as other elements, fluorescent X-rays 11 having sufficient intensity for fluorescent X-ray analysis can be obtained. can get. Moreover, the component 7b containing the element to be analyzed
Is thinly and flatly applied on the filtration membrane 6, so that the generation of scattered radiation can be suppressed and the SN ratio of the fluorescent X-ray analysis can be further increased. Furthermore, the components 7b1 and 7b2 containing the element to be analyzed can be separated by repeatedly performing the treatment using a plurality of types of solvents 8B and 8C that dissolve the component 7b containing the element to be analyzed. Can be reduced.
【００２４】次に、本発明の第４実施形態の方法では、
図７のように、第３実施形態と同様のカラムカートリッ
ジ１６と、第２実施形態と同様のろ過カートリッジ１３
とを併用する。まず、シリンジ１２に所定量の潤滑油試
料７および適量の第１の溶媒８Ａを吸引し、シリンジ１
２の先に、カラム充填剤１５を詰めたカラムカートリッ
ジ１６を取り付け、シリンジ１２内の溶液７，８Ａを押
し出して、カラム充填剤１５に吸着させる。第１の溶媒
８Ａとしては、第１実施形態と同様のものを用いること
ができる。カラム充填剤１５としては、第３実施形態と
同様のものを用いることができる。これにより、潤滑油
試料７中の基油７ａを第１の溶媒８Ａに溶かして、洗い
流すことができる。ここまでは、ろ過カートリッジ１３
を用いず、第３実施形態の方法と同じである。Next, in the method according to the fourth embodiment of the present invention,
As shown in FIG. 7, a column cartridge 16 similar to the third embodiment and a filtration cartridge 13 similar to the second embodiment are used.
And are used together. First, a predetermined amount of the lubricating oil sample 7 and an appropriate amount of the first solvent 8A are sucked into the syringe 12, and the syringe 1
A column cartridge 16 packed with a column filler 15 is attached to the end of the column 2, and the solutions 7, 8A in the syringe 12 are extruded and adsorbed on the column filler 15. As the first solvent 8A, the same solvent as in the first embodiment can be used. As the column filler 15, the same one as in the third embodiment can be used. Thereby, the base oil 7a in the lubricating oil sample 7 can be dissolved in the first solvent 8A and washed away. Up to this point, the filtration cartridge 13
, And is the same as the method of the third embodiment.
【００２５】次に、シリンジ１２からいったんカラムカ
ートリッジ１６を取り外して、適量の第２の溶媒８Ｂを
吸引し、再度カラムカートリッジ１６を取り付け、さら
にカラムカートリッジ１６の先にろ過カートリッジ１３
を取り付けて、シリンジ１２内の第２の溶媒８Ｂを押し
出す。第２の溶媒８Ｂとしては、トルエンを用いること
ができる。これにより、潤滑油試料７中の添加剤７ｂの
うちベンゼン環をもつ第１種の添加剤７ｂ1 が第２の溶
媒８Ｂに溶かし出され、その溶液が加圧ろ過される。加
圧ろ過の結果、ろ過膜６上に第１種の添加剤７ｂ1 が分
離される。すなわち、ろ過カートリッジ１３のろ過膜６
上に、第１種の添加剤７ｂ1 が濃縮されて塗布された状
態になるので、このろ過カートリッジ１３を取り外す。Next, once the column cartridge 16 is removed from the syringe 12, an appropriate amount of the second solvent 8B is sucked, the column cartridge 16 is attached again, and the filtration cartridge 13
And extrudes the second solvent 8B in the syringe 12. As the second solvent 8B, toluene can be used. As a result, the first additive 7b1 having a benzene ring among the additives 7b in the lubricating oil sample 7 is dissolved in the second solvent 8B, and the solution is subjected to pressure filtration. As a result of the pressure filtration, the first type additive 7b1 is separated on the filtration membrane 6. That is, the filtration membrane 6 of the filtration cartridge 13
Since the first type additive 7b1 is concentrated and applied, the filter cartridge 13 is removed.
【００２６】次に、シリンジ１２からまたいったんカラ
ムカートリッジ１６を取り外して、適量の第３の溶媒８
Ｃを吸引し、再度カラムカートリッジ１６を取り付け、
さらにカラムカートリッジ１６の先に新たなろ過カート
リッジ１３を取り付けて、シリンジ１２内の第３の溶媒
８Ｃを押し出す。第３の溶媒８Ｃとしては、メタノール
を用いることができる。これにより、潤滑油試料７中の
添加剤７ｂのうち極性の強い第２種の添加剤７ｂ2 が第
３の溶媒８Ｃに溶かし出され、その溶液が加圧ろ過され
る。加圧ろ過の結果、ろ過膜６上に第２種の添加剤７ｂ
2 が分離される。すなわち、ろ過カートリッジ１３のろ
過膜６上に、第２種の添加剤７ｂ2 が濃縮されて塗布さ
れた状態になるので、このろ過カートリッジ１３を取り
外す。Next, the column cartridge 16 is once again removed from the syringe 12 and an appropriate amount of the third solvent 8 is removed.
C is aspirated, and the column cartridge 16 is attached again,
Further, a new filtration cartridge 13 is attached to the end of the column cartridge 16 to push out the third solvent 8C in the syringe 12. As the third solvent 8C, methanol can be used. As a result, the second polar additive 7b2 of the additive 7b in the lubricating oil sample 7 is dissolved in the third solvent 8C, and the solution is filtered under pressure. As a result of pressure filtration, the second type additive 7b
2 is separated. That is, the second type of additive 7b2 is concentrated and applied on the filtration membrane 6 of the filtration cartridge 13, so that the filtration cartridge 13 is removed.
【００２７】このようにして得られた各ろ過カートリッ
ジ１３を、図４のように分解してろ過膜６を取り出し、
上面照射の場合は、図５のように、通常用いられる試料
ホルダー１４に組み込んで、蛍光Ｘ線分析装置の試料台
に載置すれば、上方から添加剤７ｂ1 ，７ｂ2 に１次Ｘ
線１０を照射して発生する蛍光Ｘ線１１の強度を測定す
ることができる。ろ過膜６上に付着した捕捉物（添加剤
７ｂ1 ，７ｂ2 ）が、粘性が高く、少量の場合には、下
方から添加剤７ｂ1 ，７ｂ2 に１次Ｘ線１０を照射する
下面照射も可能である。Each of the filtration cartridges 13 thus obtained is disassembled as shown in FIG.
In the case of top-side irradiation, as shown in FIG. 5, by incorporating the sample into a commonly used sample holder 14 and placing it on a sample table of a fluorescent X-ray analyzer, the primary X-rays are added to the additives 7b1 and 7b2 from above.
The intensity of the fluorescent X-ray 11 generated by irradiating the line 10 can be measured. When the trapped substances (additives 7b1 and 7b2) attached to the filtration membrane 6 are high in viscosity and small, it is possible to irradiate the additives 7b1 and 7b2 with the primary X-rays 10 from below. .
【００２８】以上のように、第４実施形態の方法によれ
ば、液相クロマトグラフィーにおいて溶媒８を加圧して
潤滑油試料中の添加剤等の分析対象元素を含む成分７ｂ
を溶解させて採取し、その溶液を加圧ろ過して分析対象
元素を含む成分７ｂをろ過膜６上に分離するので、分析
対象元素を迅速に濃縮でき、分析対象元素が、１００〜
５００ppm の濃度のＢ、Ｎ等のいわゆる超軽元素や、そ
の他の元素で数ppm レベルの濃度の微量元素であって
も、蛍光Ｘ線分析するのに十分な強度の蛍光Ｘ線１１が
得られる。しかも、分析対象元素を含む成分７ｂがろ過
膜６上に薄膜状かつ平坦に塗布された状態になるので、
散乱線の発生を抑制でき、蛍光Ｘ線分析のＳＮ比をいっ
そう高めることができる。さらに、分析対象元素を含む
成分７ｂを溶解する溶媒８Ｂ，８Ｃを複数種類用いて繰
り返し処理することにより、分析対象元素を含む成分７
ｂ1 ，７ｂ2 を分別することができ、蛍光Ｘ線分析にお
ける共存元素の影響を軽減することもできる。なお、こ
こでは溶媒８Ｂ，８Ｃを除去するのに加圧ろ過を用いた
が、第１実施形態の方法のように吸引ろ過を用いてもよ
い。さらに、第３実施形態の方法では、溶媒８Ｂ，８Ｃ
を揮発させて除去したが、加圧または吸引ろ過を併せて
用いてもよい。As described above, according to the method of the fourth embodiment, in the liquid phase chromatography, the solvent 8 is pressurized and the component 7b containing the element to be analyzed such as an additive in the lubricating oil sample is added.
Is dissolved and collected, and the solution is subjected to pressure filtration to separate the component 7b containing the element to be analyzed on the filtration membrane 6, so that the element to be analyzed can be rapidly concentrated, and the element to be analyzed is 100 to 100%.
Even with so-called ultra-light elements such as B and N at a concentration of 500 ppm, and other trace elements at a concentration of several ppm, fluorescent X-rays 11 having sufficient intensity for fluorescent X-ray analysis can be obtained. . In addition, since the component 7b containing the element to be analyzed is thinly and flatly applied on the filtration membrane 6,
The generation of scattered radiation can be suppressed, and the SN ratio of the fluorescent X-ray analysis can be further increased. Furthermore, by repeatedly using a plurality of types of solvents 8B and 8C that dissolve the component 7b containing the element to be analyzed, the component 7
b1 and 7b2 can be separated, and the influence of coexisting elements in X-ray fluorescence analysis can be reduced. Here, pressure filtration is used to remove the solvents 8B and 8C, but suction filtration may be used as in the method of the first embodiment. Further, in the method of the third embodiment, the solvents 8B, 8C
Was removed by volatilization, but pressure or suction filtration may be used in combination.
【００２９】次に、本発明の第５実施形態の方法では、
図６の第３実施形態の方法と同様に、まず、シリンジ１
２に所定量の潤滑油試料７および適量の溶媒８を吸引
し、シリンジ１２の先に、カラム充填剤１５を詰めたカ
ラムカートリッジ１６を取り付け、シリンジ１２内の溶
液７，８を押し出して、カラム充填剤１５に吸着させ
る。溶媒８としては、第１実施形態と同様のものを用い
ることができる。カラム充填剤１５としては、第３実施
形態と同様のものを用いることができる。これにより、
潤滑油試料７中の基油７ａを溶媒８に溶かして、洗い流
すことができる。ここまでは、第３実施形態の方法と同
じである。Next, in the method according to the fifth embodiment of the present invention,
As in the method of the third embodiment shown in FIG.
2, a predetermined amount of a lubricating oil sample 7 and an appropriate amount of a solvent 8 are sucked, a column cartridge 16 filled with a column filler 15 is attached to the tip of the syringe 12, and the solutions 7, 8 in the syringe 12 are extruded. Adsorb to the filler 15. As the solvent 8, the same solvent as in the first embodiment can be used. As the column filler 15, the same one as in the third embodiment can be used. This allows
The base oil 7a in the lubricating oil sample 7 can be dissolved in the solvent 8 and washed away. Up to this point, the method is the same as that of the third embodiment.
【００３０】このカラムカートリッジ１６内のカラム充
填剤１５には、潤滑油試料７から分離された添加剤７ｂ
が高濃度で吸着しているので、第５実施形態の方法で
は、カラムカートリッジ１６を分解してカラム充填剤１
５を取り出し、平板状例えば円板状に加圧成形して、蛍
光Ｘ線分析用の試料とする。The column filler 15 in the column cartridge 16 contains the additive 7 b separated from the lubricating oil sample 7.
Is adsorbed at a high concentration. Therefore, in the method of the fifth embodiment, the column cartridge 16 is disassembled to
5 is taken out and molded under pressure into a flat plate, for example, a disk, to obtain a sample for X-ray fluorescence analysis.
【００３１】第５実施形態の方法によれば、液相クロマ
トグラフィーにおいて溶媒８を加圧して用い、潤滑油試
料等の油試料７から添加剤等の分析対象元素を含む成分
７ｂを分離してカラム充填剤１５に吸着させ、そのカラ
ム充填剤１５を平板状に加圧成形して蛍光Ｘ線分析用の
試料とするので、分析対象元素を迅速に濃縮でき、分析
対象元素が、１００〜５００ppm の濃度のＢ、Ｎ等のい
わゆる超軽元素や、その他の元素で数ppm レベルの濃度
の微量元素であっても、蛍光Ｘ線分析するのに十分な強
度の蛍光Ｘ線が得られる。According to the method of the fifth embodiment, in the liquid phase chromatography, the solvent 8 is used under pressure to separate the component 7b containing the element to be analyzed such as an additive from the oil sample 7 such as a lubricating oil sample. Since the sample is adsorbed to the column filler 15 and the column filler 15 is pressure-formed into a flat plate and used as a sample for X-ray fluorescence analysis, the element to be analyzed can be rapidly concentrated, and the element to be analyzed is 100 to 500 ppm. X-rays of sufficient intensity for X-ray fluorescence analysis can be obtained even with so-called ultra-light elements such as B and N at a concentration of, and trace elements at a concentration of several ppm in other elements.
【００３２】なお、第３ないし第５実施形態の方法にお
いて、カラム充填剤をシリンジの先端部に充填してフィ
ルターパッキン等で固定し、シリンジとカラムカートリ
ッジの一体型として用いることもできる。In the methods of the third to fifth embodiments, the syringe may be used as an integral unit of the syringe and the column cartridge by filling the tip of the syringe with the column filler and fixing it with a filter packing or the like.
【００３３】[0033]
【発明の効果】以上詳細に説明したように、本発明の蛍
光Ｘ線用の油試料の調製法によれば、分析対象元素を迅
速に濃縮でき、分析対象元素が、１００〜５００ppm の
濃度のＢ、Ｎ等のいわゆる超軽元素や、その他の元素で
数ppm レベルの濃度の微量元素であっても、蛍光Ｘ線分
析するのに十分な強度の蛍光Ｘ線が得られる。As described above in detail, according to the method for preparing an oil sample for X-ray fluorescence of the present invention, the element to be analyzed can be rapidly concentrated, and the element to be analyzed has a concentration of 100 to 500 ppm. Even with so-called ultra-light elements such as B and N, and other elements such as trace elements having a concentration of several ppm, X-rays with sufficient intensity for X-ray fluorescence analysis can be obtained.
【図１】本発明の第１実施形態の蛍光Ｘ線用の油試料の
調製法において、ろ過膜を用いて油試料を吸引ろ過する
様子を示す概略断面図である。FIG. 1 is a schematic cross-sectional view showing a state in which an oil sample is suction-filtered using a filtration membrane in a method for preparing an oil sample for fluorescent X-rays according to a first embodiment of the present invention.
【図２】同調製法によりろ過膜上に分離した分析対象元
素を含む成分を、蛍光Ｘ線分析する様子を示す概略断面
図である。FIG. 2 is a schematic cross-sectional view showing a state in which a component containing an element to be analyzed separated on a filtration membrane by the same preparation method is subjected to fluorescent X-ray analysis.
【図３】本発明の第２実施形態の蛍光Ｘ線用の油試料の
調製法において、ろ過膜を用いて油試料を加圧ろ過する
様子を示す概略断面図である。FIG. 3 is a schematic cross-sectional view showing a state where an oil sample is subjected to pressure filtration using a filtration membrane in a method for preparing an oil sample for fluorescent X-rays according to a second embodiment of the present invention.
【図４】同調製法により分析対象元素を含む成分をろ過
膜上に分離した様子を示す概略断面図である。FIG. 4 is a schematic cross-sectional view showing a state where components including an element to be analyzed are separated on a filtration membrane by the same preparation method.
【図５】同調製法によりろ過膜上に分離した分析対象元
素を含む成分を、蛍光Ｘ線分析する様子を示す概略断面
図である。FIG. 5 is a schematic cross-sectional view showing a state in which a component containing an element to be analyzed separated on a filtration membrane by the same preparation method is subjected to fluorescent X-ray analysis.
【図６】本発明の第３実施形態の蛍光Ｘ線用の油試料の
調製法において、液相クロマトグラフィーにより分析対
象元素を含む成分をろ過膜上に採取する様子を示す概略
断面図である。FIG. 6 is a schematic cross-sectional view showing how a component containing an element to be analyzed is collected on a filtration membrane by liquid chromatography in a method for preparing an oil sample for X-ray fluorescence according to a third embodiment of the present invention. .
【図７】本発明の第４実施形態の蛍光Ｘ線用の油試料の
調製法において、液相クロマトグラフィーにより分析対
象元素を含む成分を溶媒に溶解させて採取し、加圧ろ過
する様子を示す概略断面図である。FIG. 7 shows a state in which a component containing an element to be analyzed is dissolved in a solvent by liquid phase chromatography, collected and filtered under pressure in the method for preparing an oil sample for X-ray fluorescence according to the fourth embodiment of the present invention. FIG.
６…ろ過膜、７…油試料（潤滑油試料）、７ｂ…分析対
象元素を含む成分（添加剤または摩耗粉）、８…溶媒、
１５…カラム充填剤。6: filtration membrane, 7: oil sample (lubricating oil sample), 7b: component containing the element to be analyzed (additive or wear powder), 8: solvent,
15 ... Column packing material.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｇ０１Ｎ 33/30 Ｇ０１Ｎ 33/30 Ｆターム(参考） 2G001 AA01 BA04 CA01 GA01 JA12 KA01 LA04 MA02 MA04 RA01 RA20 2G052 AA08 AD29 AD52 BA22 CA03 CA11 CA13 EA02 EA03 EA17 ED01 ED03 GA19 JA09 JA13 JA16 4D006 GA06 KA02 KB12 MA06 MA22 MB05 MC37X MC68X PA02 PB13 PB70 PC38 4D017 AA04 BA05 CA05 CB01 DA03 DB02 EA05 ──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) G01N 33/30 G01N 33/30 F-term (Reference) 2G001 AA01 BA04 CA01 GA01 JA12 KA01 LA04 MA02 MA04 RA01 RA20 2G052 AA08 AD29 AD52 BA22 CA03 CA11 CA13 EA02 EA03 EA17 ED01 ED03 GA19 JA09 JA13 JA16 4D006 GA06 KA02 KB12 MA06 MA22 MB05 MC37X MC68X PA02 PB13 PB70 PC38 4D017 AA04 BA05 CA05 CB01 DA03 DB02 EA05
Claims (5)
て蛍光Ｘ線分析するのに用いられる前記油試料を調製す
る方法であって、 ろ過膜を用いて前記油試料を吸引ろ過または加圧ろ過
し、前記分析対象元素を含む成分を前記ろ過膜上に分離
する蛍光Ｘ線分析用の油試料の調製法。1. A method for preparing an oil sample to be used for X-ray fluorescence analysis by concentrating an element to be analyzed contained in an oil sample, wherein the oil sample is subjected to suction filtration or filtration using a filtration membrane. A method for preparing an oil sample for X-ray fluorescence analysis, comprising filtering under pressure and separating a component containing the element to be analyzed on the filtration membrane.
て蛍光Ｘ線分析するのに用いられる前記油試料を調製す
る方法であって、 加圧した溶媒を用いる液相クロマトグラフィーにより、
前記分析対象元素を含む成分をろ過膜上に分離する蛍光
Ｘ線分析用の油試料の調製法。2. A method for preparing an oil sample which is used for concentrating an element to be analyzed contained in the oil sample and performing X-ray fluorescence analysis, wherein the oil sample is subjected to liquid phase chromatography using a pressurized solvent.
A method for preparing an oil sample for X-ray fluorescence analysis, wherein the component containing the element to be analyzed is separated on a filtration membrane.
あり、 前記分析対象元素を含む成分が前記添加剤または摩耗粉
であり、 前記ろ過膜が、ゴム膜、高分子膜、ミリポアフィルター
またはろ紙の表面にポリメタクリレートを付着させたも
のであり、 前記ろ過膜が通過させる分子の分子量が、１３００以下
にある蛍光Ｘ線分析用の油試料の調製法。3. The filter membrane according to claim 1, wherein the oil sample is a lubricating oil sample containing an additive or wear powder, the component containing the element to be analyzed is the additive or wear powder, Is a rubber membrane, a polymer membrane, Millipore filter or filter paper with polymethacrylate adhered to the surface thereof. The molecular weight of the molecule passed through the filtration membrane is 1300 or less. Preparation method.
あり、 前記分析対象元素を含む成分が前記添加剤または摩耗粉
であり、 前記ろ過膜が、ゴム膜、高分子膜、ミリポアフィルター
またはろ紙の表面にポリメタクリレートを付着させたも
のであり、 前記ろ過膜が多数有する孔の直径が、２００〜８００Å
の範囲内にある蛍光Ｘ線分析用の油試料の調製法。4. The filter membrane according to claim 1, wherein the oil sample is a lubricating oil sample containing an additive or wear powder, the component containing the element to be analyzed is the additive or wear powder, Are those obtained by attaching polymethacrylate to the surface of a rubber membrane, a polymer membrane, a millipore filter or a filter paper, and the diameter of a large number of pores of the filtration membrane is 200 to 800 mm.
Preparation of an oil sample for X-ray fluorescence analysis within the range of
て蛍光Ｘ線分析するのに用いられる前記油試料を調製す
る方法であって、 加圧した溶媒を用いる液相クロマトグラフィーにより前
記油試料から前記分析対象元素を含む成分を分離してカ
ラム充填剤に吸着させ、そのカラム充填剤を平板状に加
圧成形する蛍光Ｘ線分析用の油試料の調製法。5. A method for preparing an oil sample used for X-ray fluorescence analysis by concentrating an element to be analyzed contained in an oil sample, wherein the oil sample is subjected to liquid phase chromatography using a pressurized solvent. A method for preparing an oil sample for X-ray fluorescence analysis, comprising separating a component containing the element to be analyzed from a sample, adsorbing the component on a column filler, and pressing the column filler into a flat plate under pressure.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000374793A JP3590836B2 (en) | 2000-12-08 | 2000-12-08 | Preparation of oil sample for X-ray fluorescence analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000374793A JP3590836B2 (en) | 2000-12-08 | 2000-12-08 | Preparation of oil sample for X-ray fluorescence analysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2002181743A true JP2002181743A (en) | 2002-06-26 |
| JP3590836B2 JP3590836B2 (en) | 2004-11-17 |
Family
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000374793A Expired - Fee Related JP3590836B2 (en) | 2000-12-08 | 2000-12-08 | Preparation of oil sample for X-ray fluorescence analysis |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005321207A (en) * | 2004-05-06 | 2005-11-17 | Nikko Materials Co Ltd | Sample holder for x-ray fluorescence analyses, and preparing method of sample |
| JP2006029864A (en) * | 2004-07-13 | 2006-02-02 | Hitachi Constr Mach Co Ltd | Fluorescent x-ray analyzing method of very small amount of element in water, and column and system used therein |
-
2000
- 2000-12-08 JP JP2000374793A patent/JP3590836B2/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005321207A (en) * | 2004-05-06 | 2005-11-17 | Nikko Materials Co Ltd | Sample holder for x-ray fluorescence analyses, and preparing method of sample |
| JP4549728B2 (en) * | 2004-05-06 | 2010-09-22 | 日鉱金属株式会社 | Sample for X-ray fluorescence analysis |
| JP2006029864A (en) * | 2004-07-13 | 2006-02-02 | Hitachi Constr Mach Co Ltd | Fluorescent x-ray analyzing method of very small amount of element in water, and column and system used therein |
| JP4523805B2 (en) * | 2004-07-13 | 2010-08-11 | 中部キレスト株式会社 | X-ray fluorescence analysis method for trace elements in water, column and system used in the method |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3590836B2 (en) | 2004-11-17 |
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