JPH09257899A - Hermetically sealable sample tube for measuring nuclear magnetic resonance - Google Patents
Hermetically sealable sample tube for measuring nuclear magnetic resonanceInfo
- Publication number
- JPH09257899A JPH09257899A JP8093265A JP9326596A JPH09257899A JP H09257899 A JPH09257899 A JP H09257899A JP 8093265 A JP8093265 A JP 8093265A JP 9326596 A JP9326596 A JP 9326596A JP H09257899 A JPH09257899 A JP H09257899A
- Authority
- JP
- Japan
- Prior art keywords
- inner plug
- sample tube
- main body
- hole
- insertion piece
- 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.)
- Granted
Links
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- Sampling And Sample Adjustment (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は広い圧力範囲及び温
度範囲において使用可能な気密性核磁気共鳴測定用試料
管に関する。The present invention relates to a sample tube for hermetic nuclear magnetic resonance measurement which can be used in a wide pressure range and a wide temperature range.
【０００２】[0002]
【従来の技術】核磁気共鳴は試料の同定および状態や物
性を解明する極めて有力な手段であり、通常、円筒状の
試料管を強磁場の中で高速回転させながら測定を行う。
空気中での取り扱いが困難な試料では気密性を有する試
料管が必要とされる。また、触媒などの研究では反応条
件に近い状態で測定を行うため、常圧下の他、減圧や加
圧下でも、広い温度範囲において気密性を保つことが要
求される。従来、気密性を必要とする測定では、（１）
ガラス管中に試料を封入し、これを保護管に入れて測定
する方法、（２）押し込み式樹脂製栓がついた試料管を
用いる方法があった。しかし、（１）の方法ではガラス
をバーナーによって封じきるため試料が熱的に不安定な
場合は採用できないし、ガラス管を軸対称性を保って封
じきるのが難しく安定な高速回転性が得られない。ま
た、（１）（２）の双方とも加圧状態では使用できない
し、特に（２）の場合では温度変化が大きい場合はそれ
に栓部が耐えられないので広い温度範囲での測定は不可
能である。特に、反応状態にある試料の測定は、その反
応機構の解明、それを手がかりとした新たな産業技術の
創出に極めて有効な方法であるが、従来の技術では反応
に伴う試料管内の圧力や温度の大きな変動に試料管又は
栓が耐えられず、測定はほとんど不可能である。2. Description of the Related Art Nuclear magnetic resonance is an extremely powerful means for identifying a sample and elucidating its state and physical properties. Usually, a measurement is performed while a cylindrical sample tube is rotated at a high speed in a strong magnetic field.
For a sample that is difficult to handle in air, an airtight sample tube is required. Further, in research on catalysts and the like, since measurement is performed under conditions close to the reaction conditions, it is required to maintain airtightness over a wide temperature range not only under normal pressure but also under reduced or increased pressure. Conventionally, in measurements requiring airtightness, (1)
There are a method of enclosing a sample in a glass tube and placing it in a protective tube for measurement, and (2) a method of using a sample tube with a push-in resin stopper. However, in the method (1), since the glass is sealed by a burner, it cannot be used when the sample is thermally unstable, and it is difficult to seal the glass tube while maintaining the axial symmetry, and stable high-speed rotation is obtained. I can't. In addition, both (1) and (2) cannot be used in a pressurized state, and especially in the case of (2), when the temperature change is large, the stopper cannot withstand the temperature change, so that measurement over a wide temperature range is impossible. is there. In particular, the measurement of a sample in a reaction state is an extremely effective method for elucidating the reaction mechanism and creating a new industrial technology using it as a clue, but with the conventional technology, the pressure and temperature in the sample tube accompanying the reaction The sample tubes or stoppers cannot withstand large fluctuations in, and measurement is almost impossible.
【０００３】[0003]
【発明が解決しようとする課題】触媒開発や物性研究に
おいては、減圧から加圧までの種々の圧力下で冷却ある
いは加熱を含む広い温度範囲において物質の特性を解明
するための核磁気共鳴測定をする必要がある。しかし、
前述のように軸対称性と気密性を保った試料管の作成に
ついての問題がある。このため、特に広い圧力及び温度
範囲で使用できる試料管の開発が望まれている。In the development of catalysts and research on physical properties, nuclear magnetic resonance measurements for elucidating the properties of materials in a wide temperature range including cooling or heating under various pressures from decompression to pressurization are carried out. There is a need to. But,
As described above, there is a problem in preparing a sample tube that maintains axial symmetry and airtightness. Therefore, development of a sample tube that can be used particularly in a wide pressure and temperature range is desired.
【０００４】本発明は上記の問題を解決し、取り扱いが
容易であり、かつ広い圧力範囲及び温度範囲での測定を
可能にする核磁気共鳴試料管を提供することを目的とす
る。An object of the present invention is to provide a nuclear magnetic resonance sample tube which solves the above problems, is easy to handle, and enables measurement in a wide pressure range and temperature range.
【０００５】[0005]
【課題を解決するための手段】上記の目的を達成するた
め本発明は、上端部が開放された筒状の管本体と、該管
本体の開放端から挿入されて装着される内栓と、前記管
本体及び内栓の間に介在するシールリングと、前記内栓
を前記管本体に固定するための挿入片及び密栓用ボルト
とを備えた気密性核磁気共鳴測定用試料管であって、前
記管本体は、側壁の上部付近において径方向に対向し少
なくとも一方が側壁を貫通している２つの切り欠き部を
有し、該切り欠き部より下方における内側面に係止用凸
部が設けられ、前記内栓は、前記切り欠き部より上下方
向に大きな径を有する横孔が側面を貫通し、該横孔から
上方に延び天面に達する縦孔が形成されており、前記横
孔は、該内栓が前記管本体に挿入されて前記係止用凸部
により位置決めされたときに、前記切り欠き部に臨み且
つ上端が該切り欠き部の上端より上方に位置するように
形成されており、前記挿入片は、前記２つの切り欠き部
に差し渡して装着することができ、装着時に上下方向に
向く雌ねじ付貫通孔を有しており、前記密栓用ボルト
は、上部にボルトヘッドを有し、下部は、前記内栓及び
挿入片が前記管本体に装着された状態で、前記内栓の縦
孔に緩く嵌まり前記挿入片の雌ねじ付貫通孔に雄ねじ部
が螺合し前記内栓の横孔の下面に達しうる径及び長さと
されていることを特徴とする気密性核磁気共鳴測定用試
料管を提供するものである。SUMMARY OF THE INVENTION In order to achieve the above object, the present invention provides a tubular pipe body having an open upper end, an inner plug inserted and mounted from an open end of the pipe body, A seal tube interposed between the tube main body and the inner plug, an airtight nuclear magnetic resonance measurement sample tube including an insert and a sealing bolt for fixing the inner plug to the tube main body, The tube main body has two notches radially opposed to each other in the vicinity of the upper part of the side wall and at least one of the notches penetrates the side wall, and a locking projection is provided on an inner surface below the notch. The inner plug has a lateral hole having a diameter larger in the vertical direction than the cutout portion penetrates a side surface, and a vertical hole extending upward from the lateral hole and reaching the top surface is formed, and the lateral hole is The inner plug is inserted into the pipe main body and positioned by the locking projection. Is formed so that the upper end faces the notch portion and the upper end is located above the upper end of the notch portion, and the insertion piece can be mounted across the two notch portions. Has a through-hole with a female thread that faces vertically when mounted, the sealing bolt has a bolt head on the upper part, and the lower part has the inner plug and the insertion piece mounted on the pipe body. Airtight, characterized in that it has a diameter and a length that can be loosely fitted in the vertical hole of the inner plug, and a male screw part can be screwed into the through hole with a female thread of the insert to reach the lower surface of the horizontal hole of the inner plug. The present invention provides a sample tube for measuring nuclear magnetic resonance.
【０００６】上記気密性核磁気共鳴測定用試料管は、前
述の内栓に変えて、前記管本体に挿入されて前記係止用
凸部により位置決めされたときに、天面が前記切り欠き
部より下方に位置する寸法とされた内栓を備えることが
できる。この場合、前記ボルトの下部は、前記内栓及び
挿入片が前記管本体に装着された状態で、前記挿入片の
雌ねじ付貫通孔に雄ねじ部が螺合し前記内栓の天面に達
し得る径及び長さとされる。When the sample tube for airtight nuclear magnetic resonance measurement is inserted into the tube main body instead of the inner plug and positioned by the locking projection, the top surface has the notch. An inner plug sized below may be provided. In this case, the lower part of the bolt can reach the top surface of the inner plug by screwing the male screw portion into the female-threaded through-hole of the insert while the inner plug and the insert are attached to the pipe body. Diameter and length.
【０００７】[0007]
【発明の実施の形態】以下、本発明の実施の形態につき
添付図面を参照しつつ説明する。気密性核磁気共鳴試料
管は図１に示されるように、試料管本体１、Ｏ−リング
２、内栓３、密栓用ボルト４、挿入片５を備えている。
図２から図４に試料管本体の正面図、平面図と縦断面
図、図８に雌ネジが切られている挿入片の平面図を示
す。試料管本体１は一方が閉鎖された円筒管である。試
料管本体１の閉鎖された底部１１には試料管を空気の吹
き付けによって回転させるために必要なタービン状の回
転子を装着するための受け口１５が設られている。Embodiments of the present invention will be described below with reference to the accompanying drawings. As shown in FIG. 1, the airtight nuclear magnetic resonance sample tube includes a sample tube main body 1, an O-ring 2, an inner plug 3, a sealing bolt 4, and an insertion piece 5.
2 to 4 show a front view, a plan view and a longitudinal sectional view of the sample tube main body, and FIG. 8 shows a plan view of an insertion piece with a female screw cut. The sample tube main body 1 is a cylindrical tube whose one end is closed. The closed bottom 11 of the sample tube main body 1 is provided with a receiving port 15 for mounting a turbine-like rotor necessary for rotating the sample tube by blowing air.
【０００８】しかし、試料管本体底部１１を加工して回
転子の形状にすることもでき、回転力付与のための他の
構造とすることもできる。試料管本体の内部側面には段
差を設け環状の係止用凸部１６として内栓を支える。However, the sample tube main body bottom portion 11 can be processed into a rotor shape, and another structure for imparting a rotational force can be employed. A step is provided on the inner side surface of the sample tube main body to support the inner plug as an annular locking projection 16.
【０００９】内栓３と本体内面とのシールはＯ−リング
２等のシールリングを係止用凸部と内栓との間に介在さ
せて内栓を試料管に固定するには、試料管内面に雌ネジ
を切り、雄ネジを設けた内栓を上方から螺入して固定す
ることも考えられるが、試料管がセラミックス製である
場合、加工性が悪い材料で形成されていると、そのよう
な構造は採用し難い。そこで試料管本体上方の側壁１３
に、雌ネジ５１を切った挿入片５を差し渡すための切り
欠き部１４（この例では貫通孔）を２ヶ所に設ける。To seal the inner plug 3 from the inner surface of the main body, a seal ring such as an O-ring 2 is interposed between the locking projection and the inner plug to fix the inner plug to the sample tube. It is also conceivable to cut the female screw on the surface and screw in the inner plug provided with the male screw from above to fix it.However, when the sample tube is made of ceramic, if the sample tube is formed of a material with poor workability, Such a structure is difficult to adopt. Therefore, the side wall 13 above the sample tube main body
In addition, cutouts 14 (through holes in this example) for inserting the insertion pieces 5 with the female screws 51 are provided at two places.
【００１０】内栓３は、この例では、図５から図７に示
されるように、切り欠き部１４より上下方向に大きな径
を有する横孔３１が側面を貫通し、横孔３１から上方に
延び天面３３に達する縦孔３２が形成されており、横孔
３１は、内栓３が管本体１に挿入されて係止用凸部１６
により位置決めされたときに、切り欠き部１４に臨み且
つ上端が切り欠き部１４の上端より上方に位置するよう
に形成されている。In this example, as shown in FIGS. 5 to 7, the inner plug 3 has a lateral hole 31 having a larger diameter in the vertical direction than the cutout portion 14 penetrates the side surface, and extends upward from the lateral hole 31. A vertical hole 32 extending to the top surface 33 is formed, and the horizontal hole 31 is formed by inserting the inner plug 3 into the pipe main body 1 and holding the locking projection 16.
When it is positioned by the notch, it is formed so as to face the notch 14 and the upper end is located above the upper end of the notch 14.
【００１１】試料管各部分の材質の選定には測定核種に
よって制約が加えられ、通常はバックグラウンド信号が
小さい材質が選定される。一般的に望ましい材質とし
て、例えば、試料管本体１にはジルコニア、アルミナ、
窒化珪素、窒化アルミナ等の磁性を示さないセラミック
スが挙げられるが、Kel-F 等の高分子化合物を使用でき
る場合もある。内栓には試験管本体と同じく磁性を示さ
ないジルコニア、アルミナ、窒化珪素、窒化アルミナ等
のセラミックスを使用することができる。シールリング
は、一般的な材質のものを使用できるが、例えばフッ素
シリコンゴム等の温度特性の良好なゴム製のものが有利
に使用できる。雌ネジ５１を切った挿入片５の材質とし
ては、マコール等のセラミックやベスペル等の高分子素
材が挙げられる。ボルト４の材質としては、常磁性でな
い種々のものが使用でき、例えばベスペル、マコール等
のような高分子素材やセラミックを使用することができ
る。The selection of the material of each part of the sample tube is restricted by the nuclide to be measured, and usually a material having a small background signal is selected. As a generally desirable material, for example, zirconia, alumina,
Ceramics that do not exhibit magnetism, such as silicon nitride and alumina nitride, may be mentioned. In some cases, polymer compounds such as Kel-F may be used. As the inner plug, ceramics such as zirconia, alumina, silicon nitride, and alumina nitride which do not show magnetism like the test tube body can be used. The seal ring can be made of a general material, but a rubber material having good temperature characteristics, such as fluorine silicon rubber, can be advantageously used. Examples of the material of the insertion piece 5 in which the female screw 51 is cut include a ceramic material such as Macor and a polymer material such as Vespel. Various materials that are not paramagnetic can be used as the material of the bolt 4, and for example, a polymer material such as Vespel, Macor, or the like, or ceramic can be used.
【００１２】試料管に密栓をするための手順は次の通り
である。即ち、試料管本体１にＯ−リング２を入れ次に
内栓３をした後、雌ネジを切った挿入片５を試料管本体
１の上方側壁部１３にある孔１４に通して内栓３の上に
差し渡し、試料管上方からボルト４を挿入片３の雌ネジ
５１に螺入し、ボルト４先端を押し当てて内栓３を上方
から固定する。The procedure for sealing the sample tube is as follows. That is, after inserting the O-ring 2 into the sample tube main body 1 and then closing the inner plug 3, the internal threaded insertion piece 5 is passed through the hole 14 in the upper side wall 13 of the sample tube main body 1, and the inner plug 3 is inserted. Then, the bolt 4 is screwed into the female screw 51 of the insertion piece 3 from above the sample tube, and the tip of the bolt 4 is pressed to fix the inner plug 3 from above.
【００１３】試料管内を加圧又は減圧状態にする場合に
は、試料管を減圧又は加圧容器内に入れ、支持具により
固定する。容器には、加圧又は減圧状態を保ちつつ外部
から回転させることが可能なネジ回し用棒が支持具に対
して配置されており、この棒を密栓用ボルト４に係合さ
せてボルト４を回して加圧又は減圧状態の中で試料管を
密栓する。When the sample tube is to be pressurized or decompressed, the sample tube is placed in a depressurized or pressurized container and fixed by a support. A screwdriver rod that can be rotated from the outside while maintaining a pressurized or depressurized state is disposed on the container with respect to the support, and this rod is engaged with the sealing bolt 4 to remove the bolt 4. Turn to seal the sample tube in a pressurized or reduced pressure state.
【００１４】図９は、本発明にかかる気密性核磁気共鳴
測定用試料管の他の実施形態を示したものである。この
例においては、内栓３は縦孔及び横孔を有していない。
内栓３は、装着した状態で内栓３の天面３３が試料管本
体１の切り欠き１４よりも下方に位置するような寸法の
内栓を用い、装着時において挿入片５の差し渡しを妨げ
ないようにしている。内栓３の固定は、挿入片５に螺入
したボルト５の先端が内栓の天面３３を押圧することに
より行われる。他は、前述の例と同様である。FIG. 9 shows another embodiment of a sample tube for airtight nuclear magnetic resonance measurement according to the present invention. In this example, the inner plug 3 does not have a vertical hole and a horizontal hole.
The inner plug 3 has a size such that the top surface 33 of the inner plug 3 is positioned below the cutout 14 of the sample tube main body 1 in the mounted state, and prevents the insertion piece 5 from being passed over when mounted. I try not to. The inner plug 3 is fixed by the tip of the bolt 5 screwed into the insertion piece 5 pressing the top surface 33 of the inner plug. Others are the same as the above-mentioned example.
【００１５】また、図１及び図９に示されている実施形
態においては、環状の係止用凸部１６の上にシールリン
グを載せて内栓で下方へ押圧する構造となっているが、
内栓３の側面又は試料管本体１の側面に環状の凹所を形
成してシールリングを収容することにより両側面間でシ
ールを得るようにしてもよい。この場合、内栓３の取り
出し用係止部を内栓３の上部に設けることが望ましい。In the embodiment shown in FIGS. 1 and 9, the seal ring is placed on the annular locking projection 16 and pressed down by the inner plug.
An annular recess may be formed on the side surface of the inner plug 3 or the side surface of the sample tube main body 1 to accommodate a seal ring, thereby obtaining a seal between both side surfaces. In this case, it is desirable to provide a locking portion for taking out the inner plug 3 above the inner plug 3.
【００１６】また、図１及び図９に示されている実施形
態においては、試料管本体の２つの切り欠き部１４が共
に貫通孔とされているが、一方のみを貫通孔とし、他方
を試料管本体内面に形成した凹所とし、挿入片を貫通孔
から挿入して試料管本体内面の凹所に嵌めるようにする
こともできる。試料管本体１は、両端を開放して、両端
部に内栓３を取り付けるようにすることもできる。In the embodiment shown in FIGS. 1 and 9, the two notches 14 of the sample tube main body are both formed as through holes, but only one is formed as a through hole and the other is formed as a sample. The recess may be formed on the inner surface of the tube main body, and the insertion piece may be inserted through the through hole to fit into the recess on the inner surface of the sample tube main body. Both ends of the sample tube main body 1 can be opened, and inner plugs 3 can be attached to both ends.
【００１７】さらに、図１０に示されているように、試
料管の本体の内径を試料管の底から開放端までほぼ一定
とし、内栓を保持するための係止用凸部を環状突起１７
とすることにより、試料室を大きくすることもできる。Further, as shown in FIG. 10, the inside diameter of the main body of the sample tube is made substantially constant from the bottom to the open end of the sample tube, and the locking projection for holding the inner plug is provided with an annular projection 17.
By doing so, the sample chamber can be enlarged.
【００１８】[0018]
【実施例】実施例１ 試料管本体及び内栓をジルコニア、挿入片は
マコール、密栓用ボルトはベスペル、Ｏ−リングはフッ
素シリコンゴムを材質として試料管を制作した。試料管
の各所の寸法は次の通りである。 試料管本体内部にＯ−リングを入れ、次に内栓を入れ、
挿入片を試料管本体側面の孔及び内栓側面の横孔を通し
て入れ、上部から密栓用ボルトを挿入片の雌ネジに未シ
ール状態に軽くねじ込み、試料管を組み立てた。その後
真空容器に試料管を入れて支持具で固定し、試料管内部
を10-3 Torrの真空とした。真空容器には真空を保ちつ
つ外部から回転させることが可能なネジ回し用棒が支持
具に対向して配置されており、この棒を雄ネジに係合さ
せて雄ネジを回して真空中で試料管を密栓した。この試
料管を真空容器から出し、ドライアイス中で３時間放置
した後、ふたたび真空容器中に戻し真空中で開栓した
が、真空容器の真空度の悪化は検知されず試料管は低温
にあっても長時間真空を保つことが明らかとなった。 EXAMPLE 1 A sample tube was manufactured using zirconia as the sample tube main body and inner plug, Macor as the insert, Vespel as the sealing plug, and fluorine silicon rubber as the O-ring. The dimensions of each part of the sample tube are as follows. Put the O-ring inside the sample tube body, then put the inner stopper,
The insert was inserted through the hole on the side of the sample tube main body and the lateral hole on the side of the inner plug, and a sealing bolt was lightly screwed from above into the female screw of the insert in an unsealed state to assemble the sample tube. Thereafter, the sample tube was placed in a vacuum vessel and fixed with a support, and the inside of the sample tube was evacuated to 10 -3 Torr. A screwdriver rod that can be rotated from the outside while maintaining a vacuum in the vacuum container is arranged opposite the support, and this rod is engaged with a male screw and the male screw is turned to rotate in a vacuum. The sample tube was sealed. The sample tube was taken out of the vacuum container, left in dry ice for 3 hours, then returned to the vacuum container and opened in vacuum again. However, the deterioration of the vacuum degree of the vacuum container was not detected, and the sample tube was at a low temperature. However, it became clear that the vacuum was maintained for a long time.
【００１９】実施例２ 実施例１で制作した試料管本体
に水（０．１ml）を入れ前述と同様にしてＯ−リング、
内栓、挿入片、密栓用ボルトにより試料管を組み立て
て、ボルトを緊く締めて密栓した。これを真空容器中に
入れ真空容器内を真空（10-3 Torr）とした後、外部か
ら試料管を２００℃で１時間加熱したが真空容器の真空
度の悪化は検知されず、試料管は高温にあっても長時間
内部の圧力状態を保つことが明らかとなった。 Example 2 Water (0.1 ml) was placed in the sample tube body prepared in Example 1 and an O-ring was prepared in the same manner as described above.
A sample tube was assembled with an inner stopper, an insertion piece, and a sealing bolt, and the bolt was tightly closed to seal. This was placed in a vacuum vessel, and the inside of the vacuum vessel was evacuated (10 -3 Torr). Then, the sample tube was externally heated at 200 ° C. for 1 hour, but no deterioration in the degree of vacuum of the vacuum vessel was detected. It became clear that the internal pressure was maintained for a long time even at high temperatures.
【００２０】実施例３ 実施例１で制作した試料管本体
に固体粉末試料（０．３g）をいれ、同様にしてＯ−リ
ング、内栓、挿入片、密栓用ボルトにより試料管を組み
立て、密栓用ボルトを緊く締めて密栓した。これに市販
の核磁気共鳴測定用試料管に使用するタービン状回転子
を試料管下部に装着し、この試料管を核磁気共鳴測定装
置の試料室に入れ圧搾空気を吹き付けて試料管を回転さ
せ約６５００Ｈｚ±２Ｈｚの安定した回転速度を得るこ
とができた。また、通常の測定条件では、試料から13C,
1Hのバックグランドが観測されず、使用した材質が、
13C, 1Hの測定に適していると言える。 Example 3 A solid powder sample (0.3 g) was placed in the sample tube main body produced in Example 1, and a sample tube was assembled in the same manner using an O-ring, an inner plug, an insert, and a sealing bolt, and the sealing tube was sealed. The bolt was tightened tightly and sealed. A turbine-like rotor used for a commercially available sample tube for nuclear magnetic resonance measurement is attached to the lower part of the sample tube, and the sample tube is put into the sample chamber of the nuclear magnetic resonance measurement apparatus, and compressed air is blown to rotate the sample tube. A stable rotation speed of about 6500 Hz ± 2 Hz could be obtained. Under normal measurement conditions, 13 C,
No background of 1 H was observed, and the material used was
It can be said that it is suitable for measurement of 13 C and 1 H.
【００２１】[0021]
【発明の効果】本発明にかかる気密性核磁気共鳴測定用
試料管においては、挿入片が試料管本体の切り欠き部に
差し渡されて装着されるので管本体に対し上下方向に移
動せず、その固定状態の挿入片に密栓用ボルトが螺入さ
れて内栓を上方から押し付けて係止用凸部との間で内栓
を保持する。従って、測定中に内栓が試料管の軸線方向
に移動することがなく、減圧状態から加圧状態までの広
い圧力範囲で長時間気密性を保つことができる。特に、
これまでできなかった、加圧状態での核磁気共鳴測定が
可能となる点で有利である。In the sample tube for airtight nuclear magnetic resonance measurement according to the present invention, the insertion piece is attached to the notch portion of the sample tube body so as not to move vertically with respect to the tube body. A sealing plug bolt is screwed into the fixed insertion piece, and the inner plug is pressed from above to hold the inner plug with the locking projection. Therefore, the inner plug does not move in the axial direction of the sample tube during the measurement, and airtightness can be maintained for a long time in a wide pressure range from a reduced pressure state to a pressurized state. Especially,
This is advantageous in that a nuclear magnetic resonance measurement in a pressurized state, which has been impossible so far, can be performed.
【００２２】また、この気密性保持のための構造に関
し、試料管本体は上部に切り欠き部及び係止用凸部を設
けるという単純な構造とし、さらに該切り欠き、挿入
片、密栓用ボルト及び係止用凸部で内栓を保持する構成
とすることにより、内栓の形状の単純化を可能とした。
これにより、試料管内部の温度状態の影響を最も受ける
試料管本体及び内栓を、セラミック等のように耐熱性及
び低磁性の点で優れるが加工性の悪い材料で構成するこ
とを容易にした。従って、その材料の選択により低温か
ら高温に至る広い温度範囲に耐えることができる試料管
を実現することができる。Further, with respect to the structure for maintaining the airtightness, the sample tube main body has a simple structure in which a notch and a locking projection are provided on the upper part, and the notch, the insertion piece, the sealing bolt and By adopting a configuration in which the inner plug is held by the locking projection, the shape of the inner plug can be simplified.
Thereby, it is easy to configure the sample tube main body and the inner plug, which are most affected by the temperature state inside the sample tube, from a material excellent in heat resistance and low magnetism, such as ceramic, but poor in workability. . Therefore, a sample tube that can withstand a wide temperature range from a low temperature to a high temperature can be realized by selecting the material.
【００２３】また、本発明にかかる内栓を使用すること
により、試料管を封じきる必要がなくいため試料管の密
閉及び開封時の作業効率が向上する。Further, by using the inner plug according to the present invention, it is not necessary to completely seal the sample tube, so that the work efficiency at the time of sealing and opening the sample tube is improved.
【図１】本発明にかかる気密性核磁気共鳴測定用試料管
の１例の縦断面図である。FIG. 1 is a longitudinal sectional view of an example of a sample tube for airtight nuclear magnetic resonance measurement according to the present invention.
【図２】図１に示されている試料管本体の正面図であ
る。FIG. 2 is a front view of the sample tube main body shown in FIG.
【図３】図１に示されている試料管本体の平面図であ
る。FIG. 3 is a plan view of the sample tube main body shown in FIG. 1;
【図４】図１に示されている試料管本体の縦断面図であ
る。FIG. 4 is a longitudinal sectional view of the sample tube main body shown in FIG.
【図５】図１に示されている内栓の正面図である。FIG. 5 is a front view of the inner plug shown in FIG. 1;
【図６】図１に示されている内栓の平面図である。FIG. 6 is a plan view of the inner plug shown in FIG. 1;
【図７】図１に示されている内栓の縦断面図である。FIG. 7 is a longitudinal sectional view of the inner plug shown in FIG.
【図８】図１に示されている挿入片の平面図である。FIG. 8 is a plan view of the insertion piece shown in FIG. 1;
【図９】本発明にかかる気密性磁気共鳴測定用試料管の
他の１例を示す縦断面図である。FIG. 9 is a longitudinal sectional view showing another example of the sample tube for airtight magnetic resonance measurement according to the present invention.
【図１０】本発明にかかる気密性磁気共鳴測定用試料管
の他の１例を示す縦断面図である。FIG. 10 is a longitudinal sectional view showing another example of the sample tube for airtight magnetic resonance measurement according to the present invention.
１ 試料管本体 ２ Ｏ−リング ３ 内栓 ４ 密栓用ボルト ５ 挿入片 １１ 試料管本体底部 １３ 試料管本体上方側壁部 １４ 切り欠き １６ 係止用凸部 １７ 環状突起 ３１ 横孔 ３２ 縦孔 ３３ 天面 ５１ 雌ねじ REFERENCE SIGNS LIST 1 Sample tube main body 2 O-ring 3 Inner plug 4 Sealing bolt 5 Insertion piece 11 Sample tube main body bottom 13 Sample tube main body upper side wall 14 Notch 16 Locking projection 17 Annular projection 31 Side hole 32 Vertical hole 33 Top Face 51 female screw
Claims (2)
用ボルトとを備えた気密性核磁気共鳴測定用試料管であ
って、 前記管本体は、側壁の上部付近において径方向に対向し
少なくとも一方が側壁を貫通している２つの切り欠き部
を有し、該切り欠き部より下方における内側面に係止用
凸部が設けられ、 前記内栓は、前記切り欠き部より上下方向に大きな径を
有する横孔が側面を貫通し、該横孔から上方に延び天面
に達する縦孔が形成されており、前記横孔は、該内栓が
前記管本体に挿入されて前記係止用凸部により位置決め
されたときに、前記切り欠き部に臨み且つ上端が該切り
欠き部の上端より上方に位置するように形成されてお
り、 前記挿入片は、前記２つの切り欠き部に差し渡して装着
することができ、装着時に上下方向に向く雌ねじ付貫通
孔を有しており、 前記密栓用ボルトは、上部にボルトヘッドを有し、下部
は、前記内栓及び挿入片が前記管本体に装着された状態
で、前記内栓の縦孔に緩く嵌まり前記挿入片の雌ねじ付
貫通孔に雄ねじ部が螺合し前記内栓の横孔の下面に達し
うる径及び長さとされていることを特徴とする気密性核
磁気共鳴測定用試料管。1. A tubular main body having an open upper end, an inner plug inserted and mounted from an open end of the main body, a seal ring interposed between the main body and the inner plug, An airtight nuclear magnetic resonance measurement sample tube including an insertion piece for fixing the inner plug to the tube main body and a sealing bolt, wherein the tube main body is radially opposed near an upper portion of a side wall. At least one has two notches penetrating the side wall, and a locking projection is provided on an inner surface below the notch, and the inner plug is arranged in a vertical direction from the notch. A horizontal hole having a large diameter penetrates the side surface, and a vertical hole extending upward from the horizontal hole and reaching the top surface is formed. The horizontal hole is formed by inserting the inner plug into the tube main body and locking the horizontal hole. When it is positioned by the convex part, it faces the notch and the upper end The insertion piece is formed so as to be located above the upper end of the notch, and the insertion piece can be mounted across the two notches, and has a through-hole with a female screw that is vertically oriented at the time of mounting. The sealing bolt has a bolt head at an upper part, and the lower part is loosely fitted in a vertical hole of the inner plug in a state where the inner plug and the insertion piece are attached to the pipe main body. A sample tube for airtight nuclear magnetic resonance measurement, characterized in that the diameter and length are such that a male screw portion is screwed into a through hole with a female screw and can reach the lower surface of the lateral hole of the inner plug.
用ボルトとを備えた気密性核磁気共鳴測定用試料管であ
って、 前記管本体は、側壁の上部付近において径方向に対向し
少なくとも一方が側壁を貫通している２つの切り欠き部
を有し、該切り欠き部より下方における内側面に係止用
凸部が設けられ、 前記内栓は、前記管本体に挿入されて前記係止用凸部に
より位置決めされたときに、天面が前記切り欠き部より
下方に位置する寸法とされており、 前記挿入片は、前記２つの切り欠き部に差し渡して装着
することができ、装着時に上下方向に向く雌ねじ付貫通
孔を有しており、 前記密栓用ボルトは、上部にボルトヘッドを有し、下部
は、前記内栓及び挿入片が前記管本体に装着された状態
で、前記挿入片の雌ねじ付貫通孔に雄ねじ部が螺合し前
記内栓の天面に達し得る径及び長さとされていることを
特徴とする気密性核磁気共鳴測定用試料管。2. A tubular body having an open upper end, an inner plug inserted and mounted from an open end of the tube body, a seal ring interposed between the tube body and the inner plug, An airtight nuclear magnetic resonance measurement sample tube including an insertion piece for fixing the inner plug to the tube main body and a sealing bolt, wherein the tube main body is radially opposed near an upper portion of a side wall. At least one has two notches penetrating the side wall, and a locking projection is provided on an inner surface below the notch, and the inner plug is inserted into the pipe body and When positioned by the locking projection, the top surface has a size that is located below the notch, and the insertion piece can be mounted across the two notches, It has a through hole with a female thread that faces vertically when mounted. The sealing bolt has a bolt head at an upper part, and the lower part has a male screw part screwed into a female-threaded through-hole of the insertion piece in a state where the inner plug and the insertion piece are attached to the pipe main body. A sample tube for airtight nuclear magnetic resonance measurement, wherein the sample tube has a diameter and a length that can reach the top surface of the inner plug.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8093265A JP2829382B2 (en) | 1996-03-22 | 1996-03-22 | Sample tube for airtight nuclear magnetic resonance measurement |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8093265A JP2829382B2 (en) | 1996-03-22 | 1996-03-22 | Sample tube for airtight nuclear magnetic resonance measurement |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09257899A true JPH09257899A (en) | 1997-10-03 |
| JP2829382B2 JP2829382B2 (en) | 1998-11-25 |
Family
ID=14077656
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8093265A Expired - Lifetime JP2829382B2 (en) | 1996-03-22 | 1996-03-22 | Sample tube for airtight nuclear magnetic resonance measurement |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2829382B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010032223A (en) * | 2008-07-25 | 2010-02-12 | National Institute For Materials Science | Method for attaching liquid specimen to probe, liquid specimen container, and tool used for its use |
| JP2010145104A (en) * | 2008-12-16 | 2010-07-01 | National Institute For Materials Science | Mas sample tube |
| JP2011089861A (en) * | 2009-10-22 | 2011-05-06 | National Institute For Materials Science | Sealed mas test tube |
| JP2017125760A (en) * | 2016-01-14 | 2017-07-20 | 日本電子株式会社 | Nmr measuring probe |
| CN111721797A (en) * | 2020-07-03 | 2020-09-29 | 河北中烟工业有限责任公司 | Compaction sealing device for analyzing moisture of tobacco material by low-field nuclear magnetic resonance |
| CN114768904A (en) * | 2015-06-15 | 2022-07-22 | 诺雷尔公司 | Closure for nuclear magnetic resonance sample container with secondary locking seal and system |
-
1996
- 1996-03-22 JP JP8093265A patent/JP2829382B2/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010032223A (en) * | 2008-07-25 | 2010-02-12 | National Institute For Materials Science | Method for attaching liquid specimen to probe, liquid specimen container, and tool used for its use |
| JP2010145104A (en) * | 2008-12-16 | 2010-07-01 | National Institute For Materials Science | Mas sample tube |
| JP2011089861A (en) * | 2009-10-22 | 2011-05-06 | National Institute For Materials Science | Sealed mas test tube |
| CN114768904A (en) * | 2015-06-15 | 2022-07-22 | 诺雷尔公司 | Closure for nuclear magnetic resonance sample container with secondary locking seal and system |
| CN114768904B (en) * | 2015-06-15 | 2024-06-11 | 诺雷尔公司 | Closure and system for nuclear magnetic resonance sample container with secondary locking seal |
| JP2017125760A (en) * | 2016-01-14 | 2017-07-20 | 日本電子株式会社 | Nmr measuring probe |
| CN111721797A (en) * | 2020-07-03 | 2020-09-29 | 河北中烟工业有限责任公司 | Compaction sealing device for analyzing moisture of tobacco material by low-field nuclear magnetic resonance |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2829382B2 (en) | 1998-11-25 |
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