JPH0371035A - Method for preparing hydrophobic sample - Google Patents
Method for preparing hydrophobic sampleInfo
- Publication number
- JPH0371035A JPH0371035A JP20732089A JP20732089A JPH0371035A JP H0371035 A JPH0371035 A JP H0371035A JP 20732089 A JP20732089 A JP 20732089A JP 20732089 A JP20732089 A JP 20732089A JP H0371035 A JPH0371035 A JP H0371035A
- Authority
- JP
- Japan
- Prior art keywords
- protective film
- sample
- analysis
- mgcl2
- powdery
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 8
- 230000002209 hydrophobic effect Effects 0.000 title abstract description 9
- 230000001681 protective effect Effects 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000005871 repellent Substances 0.000 claims abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 19
- 238000002441 X-ray diffraction Methods 0.000 abstract description 14
- 239000004215 Carbon black (E152) Substances 0.000 abstract description 9
- 229930195733 hydrocarbon Natural products 0.000 abstract description 9
- 150000002430 hydrocarbons Chemical class 0.000 abstract description 9
- -1 liquid paraffin Substances 0.000 abstract description 7
- 238000000862 absorption spectrum Methods 0.000 abstract description 5
- 239000011521 glass Substances 0.000 abstract description 5
- 239000012188 paraffin wax Substances 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 5
- 229940057995 liquid paraffin Drugs 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052799 carbon Inorganic materials 0.000 abstract description 2
- 239000001257 hydrogen Substances 0.000 abstract description 2
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 238000004876 x-ray fluorescence Methods 0.000 abstract description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 abstract 6
- 229910001629 magnesium chloride Inorganic materials 0.000 abstract 3
- 230000002940 repellent Effects 0.000 abstract 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract 1
- 229920005992 thermoplastic resin Polymers 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 16
- 239000003921 oil Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 239000004698 Polyethylene Substances 0.000 description 5
- 229920000573 polyethylene Polymers 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 238000004566 IR spectroscopy Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000005464 sample preparation method Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000538 analytical sample Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000004378 air conditioning Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000001028 reflection method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は大気中の水分により変化する材料を分析する
際の試料調製法に係り、特にＸ線回折や赤外分光分析等
に適用可能な試料調製法に関する。[Detailed Description of the Invention] [Industrial Application Field] This invention relates to a sample preparation method for analyzing materials that change due to atmospheric moisture, and is particularly applicable to X-ray diffraction, infrared spectroscopy, etc. Concerning sample preparation methods.
大気中の水分により潮解したり、水利反応などをおこす
材料は、物性の測定中に変化するためＸ線回折や赤外分
光分析等の測定をおこなうことができない。そのために
このような嫌水性材料を分析するには分析装置の試料室
内を乾燥状態にしたり、乾燥ガスを流したり、真空に引
いたりして分析試料ふん囲気中の水分を極力少なくする
方法がとられる。Materials that deliquesce due to moisture in the atmosphere or undergo water use reactions cannot be measured using X-ray diffraction or infrared spectroscopy because their physical properties change during measurement. Therefore, in order to analyze such hydrophobic materials, it is best to keep the sample chamber of the analyzer dry, run dry gas, or create a vacuum to minimize the amount of moisture in the atmosphere surrounding the sample to be analyzed. It will be done.
しかしながらこのような方法を実施するためには専用の
付属設備が必要であり、分析装置が大型化したり高価に
なったりする。このような付属装置は製造プロセスにお
ける品質管理などには有効であるが、汎用性を班悦する
Ｘ１ｆｉ！回折装置、蛍光ｘｉ分析装置α、赤外分光分
析計などにおいては実用的でない。However, in order to carry out such a method, dedicated auxiliary equipment is required, making the analytical device large and expensive. Such accessory devices are effective for quality control in the manufacturing process, but the X1fi! It is not practical in diffractometers, fluorescence xi analyzers α, infrared spectrometers, etc.
この発明は上述の点に鑑みてなされ、その目的とすると
ころは、嫌水性材料に対して迅速かつ簡便に適用でき、
目的とする分析の所要時間内において十分に安定な嫌水
性分析試料のｆｌ’ｌ製方法を提供することにある。This invention has been made in view of the above points, and its purpose is to be able to be quickly and easily applied to hydrophobic materials,
The object of the present invention is to provide a fl'l production method for a hydrophobic analysis sample that is sufficiently stable within the time required for the intended analysis.
上述の目的はこの発明によれば大気中の水分によって変
化する材料を分析する際の試料の調製方法φこおいて、
前記材料の表面（こはっ水性の保護膜を設けることによ
り達成される。According to the present invention, the above-mentioned purpose is to provide a method for preparing a sample when analyzing a material that changes due to moisture in the atmosphere.
This is achieved by providing a water-repellent protective film on the surface of the material.
はつ水性物′Ｑとしては炭化水素系油、流動パラフィン
、固形パラフィン、熱可朔性ブラステノクなどが用いら
れる。Ｘ線回折、蛍光Ｘ線分析、赤外分光分析の試料と
して利用される。As the water-repellent material 'Q, hydrocarbon oil, liquid paraffin, solid paraffin, thermoplastic Brastenok, etc. are used. It is used as a sample for X-ray diffraction, X-ray fluorescence analysis, and infrared spectroscopy.
保護膜が大気中の水分を遮断する。保護膜は主として炭
素、水素、酸素などからなり、蛍光Ｘ線分析を妨害しな
い（蛍光Ｘ森分析はこれら元素を検知できない）。保護
膜の示すＸ線回折線、赤外吸収スペクトルはデータ処理
によって差引くことができるし、また波長による弁別が
できるのでＸ線回折や赤外分光分析を妨害しない。A protective film blocks moisture from the atmosphere. The protective film mainly consists of carbon, hydrogen, oxygen, etc., and does not interfere with fluorescent X-ray analysis (fluorescent X-ray analysis cannot detect these elements). The X-ray diffraction line and infrared absorption spectrum shown by the protective film can be subtracted by data processing, and can be discriminated by wavelength, so they do not interfere with X-ray diffraction or infrared spectroscopic analysis.
次にこの発明の実施例を図面に基いて説明する。 Next, embodiments of the present invention will be described based on the drawings.
保護膜３八で被覆されガラス基板２上に固定される。こ
のような分析試料は次のようにして調製される。ｏ、４
ｇのＭｇＣ−０２の粉末がガラス基板２の凹部（１８ｆ
ｆｉ Ｘ ２０ａ＋ｉ Ｘ ０．５ｍＮ ）に載置され
る。次に高粘度の液状はっ水性物質である炭化水素系油
（高真空ポンプ泊、ネオバックＭＲ−２００■松材石油
研究所の商品名）がＭｇＣ−Ｃ２扮末上に０．０３ｇ滴
下されろ。炭化水素系油が均一に展開されるとＭｇＣ４
粉停表面が油で被覆され、大気中の水分が遮断される。It is covered with a protective film 38 and fixed onto the glass substrate 2. Such an analytical sample is prepared as follows. o, 4
The MgC-02 powder of
fi x 20a+i x 0.5 mN). Next, 0.03 g of hydrocarbon oil (high vacuum pump, Neovac MR-200, product name of Matsuzai Oil Research Institute), which is a highly viscous liquid water-repellent substance, is dropped onto the MgC-C2 powder. . When hydrocarbon oil is uniformly spread, MgC4
The powder stop surface is coated with oil, blocking moisture from the atmosphere.
第３図はＭｇｃ−０２の粉末Ｘ線回折線を示す線図で特
性線４は保護膜を有するＭｇＣ−Ｃ２の回折線、特性線
５は保護膜を有しないＭｇＣ，＃２の回折線である。Figure 3 is a diagram showing the powder X-ray diffraction lines of Mgc-02. Characteristic line 4 is the diffraction line of MgC-C2 with a protective film, and characteristic line 5 is the diffraction line of MgC, #2 without a protective film. be.
回折は回折角０度より走査される。保護膜を有する場合
はＭ ｇＣＩ３２の鋭い回折線が観測される。この回折
線はＪＣＰＤＳ標準カードの値と良く一致する。Diffraction is scanned from a diffraction angle of 0 degrees. When a protective film is provided, a sharp diffraction line of MgCI32 is observed. This diffraction line agrees well with the value of the JCPDS standard card.
保護膜は炭化水素系油であるのでＸ線回折線を示さない
。これに対し保護膜を有しない場合は吸湿によって回折
線がブロードになるとともに回折角０大きいところで回
折線が消滅している。条件は室温２３℃、相対湿度７０
％で行われた。この条件では１０〜２０分でＭｇｃ／？
２が潮解し、測定所要時間の４０分間の中に溶液化した
ことによる。保ｉ ｓを有するＭｇＣ−Ｃ２につきＸｉ
回折線の経時変化を測定すると、４８ ｈ後においても
Ｘ紐回折線に変化を生じない。炭化水素系油の他、＼流
動パラフィンや固形パラフィンを保護膜に用いることも
できる。固形パラフィンは加熱溶融したものをガラス基
板２の四部に滴下する。流動パラフィンと固形パラフィ
ンを用いた場合の安定性はそれぞれ９６ｈ、２ｎｄであ
った。Since the protective film is made of hydrocarbon oil, it does not show any X-ray diffraction lines. On the other hand, in the case where no protective film is provided, the diffraction lines become broader due to moisture absorption, and the diffraction lines disappear when the diffraction angle is 0 large. Conditions are room temperature 23℃, relative humidity 70
It was done in %. Under these conditions, Mgc/?
This is because 2 deliquesced and became a solution within the 40 minutes required for measurement. Xi for MgC-C2 with retention is
When measuring the change in the diffraction line over time, there was no change in the X-string diffraction line even after 48 hours. In addition to hydrocarbon oil, liquid paraffin or solid paraffin can also be used for the protective film. The solid paraffin is heated and melted and then dropped onto the four parts of the glass substrate 2. The stability when using liquid paraffin and solid paraffin was 96 hours and 2nd, respectively.
第２図はこの発明の異なる実施例に係る調製方法で作製
された嫌水性分析試料を示す断面図で、ＭｇＣＪｈ粉末
１をポリエチレン保護膜で被覆している。このような試
料は次のようにしてＵＮすることができる。加μｍ厚の
低密度ポリエチレンの膜がＭｇＣ，！３２粉体の上に載
置される。熱風がイ’ Ｉ＋エチレン膜にあてられ、１
２０℃の温度でポリエチレン膜が半溶状態にされる。こ
のとき軽く押圧することによりＭｇ（Ｊ２粉末をガラス
基板２上に固定することができる。FIG. 2 is a cross-sectional view showing a hydrophobic analysis sample prepared by a preparation method according to a different embodiment of the present invention, in which MgCJh powder 1 is coated with a polyethylene protective film. Such a sample can be UNed as follows. The micron-thick low-density polyethylene film is MgC,! 32 powder. Hot air is applied to the ethylene film, and 1
At a temperature of 20°C, the polyethylene film is brought into a semi-dissolved state. At this time, the Mg(J2 powder) can be fixed on the glass substrate 2 by pressing lightly.
第４図はポリエチレン保護膜を有するＭｇ（２）２分析
試料と保蝕膜のないＭｇＣ−８２分析試料の粉末Ｘｉ回
折線を示す線図である。特性線６は保護膜を有する場合
で矢印Ｐで示したピークはポリエチレン（５）
保護膜による回折線である。特性線５は保護膜を有しな
い場合である。ポリエチレンのピークはデータ処理で差
引くことができるし、またＭｇＣ−Ｃ２の回折線と重な
ることがないのでＭ ｇ Ｃ−０２の回折線を町
正確に実走することができる。FIG. 4 is a diagram showing powder Xi diffraction lines of an Mg(2)2 analysis sample with a polyethylene protective film and an MgC-82 analysis sample without a protective film. Characteristic line 6 is the case where a protective film is provided, and the peak indicated by arrow P is a diffraction line due to the polyethylene (5) protective film. Characteristic line 5 is the case without a protective film. The peak of polyethylene can be subtracted by data processing, and since it does not overlap with the diffraction line of MgC-C2, it is possible to accurately measure the diffraction line of MgC-02.
赤外吸収を示す分析試料についてはこれをシリコン基板
上に形成してＦＴ−ＩＲの透過法が適用でき、鏡面金属
板上に形成して反射法が適用することもできる。赤外吸
収スペクトルには保ｉｌｌの吸収スペクトルも含まれる
ので、データ処理により保護膜の吸収スペクトルを差引
くことができる。For an analysis sample exhibiting infrared absorption, it can be formed on a silicon substrate and the FT-IR transmission method can be applied, or it can be formed on a mirror-finished metal plate and the reflection method can be applied. Since the infrared absorption spectrum also includes the absorption spectrum of the protective film, the absorption spectrum of the protective film can be subtracted by data processing.
この発明によれば大気中の水分によって変化する材料を
分析する際の試料の調製方法において、前記材料の表面
にはっ水性の保護膜を設けるので大気中の水分が分析材
料と遮断され、安定したＸ線回折、蛍−ｘｘｉ分析、赤
外分光分析を行うことができる。またこの分析試料の調
製法は滴下あるいは刃口熱溶融といった簡易な方法で得
られる保護膜を用いるため、その調製に何らの熟練を要
しな（６）
い。さらにこの発明の調製方法を用いるときは大型のふ
ん囲気調整装置を心壁としなくなり、訝存のθ上用分析
装置に適用して嫌水材料につき種々の角度から物性解析
を進めることが可能となる。According to this invention, in a sample preparation method for analyzing a material that changes depending on moisture in the atmosphere, a water-repellent protective film is provided on the surface of the material, so moisture in the atmosphere is separated from the analysis material, making it stable. X-ray diffraction, fluorescence-xxi analysis, and infrared spectroscopy can be performed. Furthermore, since this analytical sample preparation method uses a protective film obtained by a simple method such as dripping or hot melting at the edge of the blade, no skill is required for its preparation (6). Furthermore, when using the preparation method of the present invention, a large-scale air conditioning device is no longer used as a core wall, and it can be applied to the existing θ analyzer to proceed with physical property analysis of hydrophobic materials from various angles. Become.
第１図はこの発明の実施例に係る調製方法で作製された
嫌水性分析試料を示す断面図、第２図はこの発明の異な
る実施例に係る。ｉｌ！ｌ製方法製作法された嫌水性分
析試料を示す断面図、＄３図は炭化水素系油を保護膜と
するＭｇＣ６２分析試料のＸ線回折線を保護膜を有しな
いＭｇＣ４分析試料のＸ線回折線と比較して示す線図、
第４図はボＩＪエチレンを保護膜とするＭｇｃ沼２分析
試料のＸ線回折線を保護膜を有しないＭｇｃ、ｇ２分析
試料のＸｉ回折蘇と比較して示す線図である。
１ ： ＭｇＣＡ２粉末、２ニガラス基板、（７）FIG. 1 is a sectional view showing a hydrophobic analysis sample prepared by a preparation method according to an embodiment of the present invention, and FIG. 2 is a cross-sectional view showing a different embodiment of the present invention. Il! 1 Production method A cross-sectional view showing the fabricated hydrophobic analysis sample. Figure 3 shows the X-ray diffraction lines of the MgC62 analysis sample with hydrocarbon oil as a protective film and the X-ray diffraction of the MgC4 analysis sample without a protective film. Line diagrams shown in comparison with lines,
FIG. 4 is a graph showing the X-ray diffraction lines of the Mgc Numa 2 analysis sample using BoIJ ethylene as a protective film in comparison with the Xi diffraction lines of the Mgc, G2 analysis sample without the protective film. 1: MgCA2 powder, 2-glass substrate, (7)
Claims (1)
試料の調製方法において、前記材料の表面にはっ水性の
保護膜を設けることを特徴とする嫌水性分析試料の調製
方法。1) A method for preparing a sample for analyzing a material that changes depending on moisture in the atmosphere, the method comprising providing a water-repellent protective film on the surface of the material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20732089A JPH0371035A (en) | 1989-08-10 | 1989-08-10 | Method for preparing hydrophobic sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20732089A JPH0371035A (en) | 1989-08-10 | 1989-08-10 | Method for preparing hydrophobic sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0371035A true JPH0371035A (en) | 1991-03-26 |
Family
ID=16537817
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20732089A Pending JPH0371035A (en) | 1989-08-10 | 1989-08-10 | Method for preparing hydrophobic sample |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0371035A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007152595A (en) * | 2005-11-30 | 2007-06-21 | Kubota Matsushitadenko Exterior Works Ltd | Decorative building board |
| CN104236972A (en) * | 2014-08-27 | 2014-12-24 | 胜科纳米（苏州）有限公司 | Preparation method and analysis method of aqueous samples |
| CN106769309A (en) * | 2016-12-20 | 2017-05-31 | 武汉科技大学 | The preparation method of the xrf analysis print combined based on foamed plastics |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5299885A (en) * | 1976-02-18 | 1977-08-22 | Toshiba Corp | Coating method for sample for x-ray analysis |
-
1989
- 1989-08-10 JP JP20732089A patent/JPH0371035A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5299885A (en) * | 1976-02-18 | 1977-08-22 | Toshiba Corp | Coating method for sample for x-ray analysis |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007152595A (en) * | 2005-11-30 | 2007-06-21 | Kubota Matsushitadenko Exterior Works Ltd | Decorative building board |
| CN104236972A (en) * | 2014-08-27 | 2014-12-24 | 胜科纳米（苏州）有限公司 | Preparation method and analysis method of aqueous samples |
| CN106769309A (en) * | 2016-12-20 | 2017-05-31 | 武汉科技大学 | The preparation method of the xrf analysis print combined based on foamed plastics |
| CN106769309B (en) * | 2016-12-20 | 2019-05-10 | 武汉科技大学 | Preparation method based on the xrf analysis print that foamed plastics combines |
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