JP3321382B2 - Sample introduction device for heating device - Google Patents
Sample introduction device for heating deviceInfo
- Publication number
- JP3321382B2 JP3321382B2 JP05650297A JP5650297A JP3321382B2 JP 3321382 B2 JP3321382 B2 JP 3321382B2 JP 05650297 A JP05650297 A JP 05650297A JP 5650297 A JP5650297 A JP 5650297A JP 3321382 B2 JP3321382 B2 JP 3321382B2
- Authority
- JP
- Japan
- Prior art keywords
- sample container
- sample
- heating device
- handle
- elastic portion
- 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.)
- Expired - Lifetime
Links
- 238000010438 heat treatment Methods 0.000 title claims description 77
- 229920000642 polymer Polymers 0.000 claims description 26
- 150000003377 silicon compounds Chemical class 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 4
- 239000011247 coating layer Substances 0.000 claims description 2
- 238000000197 pyrolysis Methods 0.000 description 34
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 29
- 235000012239 silicon dioxide Nutrition 0.000 description 27
- 239000010453 quartz Substances 0.000 description 26
- 239000007789 gas Substances 0.000 description 15
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 10
- 239000010935 stainless steel Substances 0.000 description 10
- 229910001220 stainless steel Inorganic materials 0.000 description 10
- 238000004458 analytical method Methods 0.000 description 6
- 239000012159 carrier gas Substances 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 230000001154 acute effect Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052697 platinum Inorganic materials 0.000 description 5
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 238000005979 thermal decomposition reaction Methods 0.000 description 3
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、高分子試料を加熱
することにより生成する気体から該高分子試料の組成ま
たは微細構造の分析を行う際に、該高分子試料を加熱装
置に導入する器具に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for introducing a polymer sample into a heating device when analyzing the composition or microstructure of the polymer sample from gas generated by heating the polymer sample. It is about.
【０００２】[0002]
【従来の技術】高分子試料を加熱したときに、該試料の
熱分解により、或いは該試料から脱着することにより得
られる気体成分をガスクロマトグラフ装置、質量分析装
置等の分析装置に導いて定性分析または定量分析して、
前記高分子試料の組成や微細構造の分析を行うことが知
られている。前記高分子試料の組成や微細構造の分析結
果は、品質管理、鑑識等にも用いられる。2. Description of the Related Art When a polymer sample is heated, a gas component obtained by thermal decomposition of the sample or by desorption from the sample is led to an analyzer such as a gas chromatograph device or a mass spectrometer for qualitative analysis. Or quantitative analysis,
It is known to analyze the composition and microstructure of the polymer sample. The analysis results of the composition and the fine structure of the polymer sample are also used for quality control, discrimination, and the like.
【０００３】前記高分子試料を加熱する加熱装置とし
て、例えば図６（ａ）示のように、石英熱分解管２１の
外周部にヒーター２２を備えるものが知られている。前
記石英熱分解管２１は縦型に配置されており、その上部
には石英熱分解管２１内にキャリヤガスを導入するガス
導入口２３を備えるキャリヤガス導入部材２４が装着さ
れ、さらにその上部開口部に試料サンプラー２５が嵌着
されて閉蓋される。前記試料サンプラー２５は、前記石
英熱分解管２１の内部に前記高分子試料を導入するもの
であってチャッキング手段２６を備えている。As a heating device for heating the polymer sample, for example, as shown in FIG. 6 (a), a device having a heater 22 on an outer peripheral portion of a quartz pyrolysis tube 21 is known. The quartz pyrolysis tube 21 is arranged vertically, and a carrier gas introduction member 24 having a gas introduction port 23 for introducing a carrier gas into the quartz pyrolysis tube 21 is mounted on an upper portion thereof. The sample sampler 25 is fitted to the section and the lid is closed. The sample sampler 25 is for introducing the polymer sample into the quartz pyrolysis tube 21 and has a chucking means 26.
【０００４】前記石英熱分解管２１は中空部２７を備
え、中空部２７の最下部には下方に行くほど細くなるロ
ート状部２８が設けられている。そして、ロート状部２
８の下端部は前記高分子試料の加熱により生成した気体
成分の導出口２９となっており、該導出口２９に図示し
ないガスクロマトグラフ装置、質量分析装置等の分析装
置が接続される。[0004] The quartz pyrolysis tube 21 has a hollow portion 27, and a funnel-shaped portion 28 that becomes thinner downward is provided at the lowermost portion of the hollow portion 27. And the funnel-shaped part 2
The lower end of 8 is an outlet 29 for a gas component generated by heating the polymer sample, and an analyzer (not shown) such as a gas chromatograph or a mass spectrometer is connected to the outlet 29.
【０００５】前記加熱装置に前記高分子試料を導入する
試料容器３１として、図７示のように、中空の有底円筒
状体の容器本体３２の外壁に、止め鉤３３が設けられた
柄部３４が溶接により取着されたものが知られている。
前記容器本体３２は直接試料と接触するので化学的活性
が低い白金により形成されているが、白金は高価である
ので、試料容器３１のコスト低減のために、試料と直接
に接触することのない柄部３４はステンレス等の安価な
金属で構成されている。As a sample container 31 for introducing the polymer sample into the heating device, as shown in FIG. 7, a handle portion having a hook 33 provided on the outer wall of a hollow cylindrical container body 32 with a bottom. It is known that 34 is attached by welding.
The container body 32 is made of platinum having a low chemical activity because it directly contacts the sample. However, since platinum is expensive, it does not come into direct contact with the sample in order to reduce the cost of the sample container 31. The handle 34 is made of an inexpensive metal such as stainless steel.
【０００６】前記従来の試料容器３１により、図６
（ａ）示の熱分解装置に試料を導入するときには、ま
ず、ガス導入口２３から石英熱分解管２１内にキャリヤ
ガスを流通させながら、ヒーター２２により石英熱分解
管２１内を５００〜８００℃程度に加熱する。そして、
試料容器３１の柄部３４を試料サンプラー２５のチャッ
キング手段２６でチャッキングし、試料サンプラー２５
を石英熱分解管２１に嵌着する。FIG. 6 shows the conventional sample container 31.
When a sample is introduced into the pyrolysis apparatus shown in FIG. 3A, first, the carrier 22 is circulated through the quartz pyrolysis tube 21 by the heater 22 at 500 to 800 ° C. while flowing the carrier gas from the gas inlet 23 into the pyrolysis tube 21. Heat to about. And
The handle 34 of the sample container 31 is chucked by the chucking means 26 of the sampler 25, and the sampler 25 is chucked.
Is fitted to the quartz pyrolysis tube 21.
【０００７】次に、チャッキング手段２６を操作してチ
ャッキングを解除すると、図６（ｂ）示のように、試料
容器３１が自重により自然落下して石英熱分解管２１内
に試料が導入される。このとき、石英熱分解管２１は前
記のように５００〜８００℃程度に加熱されているの
で、前記試料は瞬間的に熱分解され、或いは該試料に含
まれる成分の一部が瞬間的に熱脱着される。そして、前
記熱分解または熱脱着により生成した気体成分が、前記
キャリヤガスにより前記分析装置（図示せず）に導入さ
れ、分析が行われる。Next, when the chucking is released by operating the chucking means 26, the sample container 31 falls naturally by its own weight and the sample is introduced into the quartz pyrolysis tube 21 as shown in FIG. Is done. At this time, since the quartz pyrolysis tube 21 is heated to about 500 to 800 ° C. as described above, the sample is instantaneously pyrolyzed, or a part of the components contained in the sample is instantaneously heated. Desorbed. Then, the gas component generated by the thermal decomposition or thermal desorption is introduced into the analyzer (not shown) by the carrier gas, and is analyzed.
【０００８】前記加熱装置では、分析が終了すると、図
６（ｃ）示のように、試料サンプラー２５を石英熱分解
管２１から取り外し、先端に鉤部３５が設けられた試料
容器回収器具３６を石英熱分解管２１の上部から挿入し
て、試料容器回収器具３６の鉤部３５を試料容器３１の
柄部３４に設けられた止め鉤３３に引掛けて引上げるこ
とにより、試料容器３１が回収される。In the heating device, when the analysis is completed, as shown in FIG. 6C, the sample sampler 25 is detached from the quartz pyrolysis tube 21 and a sample container collecting instrument 36 provided with a hook 35 at the tip is removed. The sample container 31 is recovered by being inserted from the upper part of the quartz pyrolysis tube 21 and hooking the hook 35 of the sample container collecting device 36 on the hook 33 provided on the handle 34 of the sample container 31 and pulling up. Is done.
【０００９】しかしながら、石英熱分解管２１の外周部
には前記のようにヒーター２２が備えられていて、前記
試料容器回収器具３６の鉤部３５を試料容器３１の柄部
３４に設けられた止め鉤３３に引掛ける作業は目視する
ことができず、手さぐりで行わなければならないので、
高度の熟練を要するとの不都合がある。However, the heater 22 is provided on the outer peripheral portion of the quartz pyrolysis tube 21 as described above, and the hook 35 of the sample container collecting device 36 is fixed to the stopper provided on the handle 34 of the sample container 31. Since the work hooked on the hook 33 cannot be seen and must be performed by hand,
There is a disadvantage that it requires a high degree of skill.
【００１０】また、前記従来の試料容器３１は、前述の
ように白金製の容器本体３２にステンレス製の柄部３４
が溶接されているので、繰り返し使用すると、石英熱分
解管２１内の５００〜８００℃という高温環境下におけ
る容器本体３２と柄部３４との膨張係数の相違から、両
者が剥離することがあるという問題がある。前記問題を
解決するために、容器本体３２に柄部３４を備えず、容
器本体３２のみにより試料容器を構成することが考えら
れるが、このような試料容器では石英熱分解管２１内に
導入する際に前記試料サンプラー２５のチャッキング手
段２６にチャッキングすることができず、また、分析終
了後に石英熱分解管２１内から回収することが非常に困
難になるという不都合がある。As described above, the conventional sample container 31 has a stainless steel handle 34 attached to a platinum container main body 32.
Are welded, so that if they are used repeatedly, they may peel off from each other due to the difference in the expansion coefficient between the container body 32 and the handle 34 in a high-temperature environment of 500 to 800 ° C. in the quartz pyrolysis tube 21. There's a problem. In order to solve the above-mentioned problem, it is conceivable that a sample container is constituted only by the container main body 32 without providing the handle portion 34 in the container main body 32. In this case, the chucking means 26 of the sampler 25 cannot be chucked, and it is very difficult to recover the sample sampler 25 from the quartz pyrolysis tube 21 after the analysis.
【００１１】[0011]
【発明が解決しようとする課題】本発明は、かかる不都
合を解消して、高温環境下で支障なく使用することがで
き、取り扱いが容易な加熱装置用試料導入器具を提供す
ることを目的とする。SUMMARY OF THE INVENTION An object of the present invention is to provide a sample introduction instrument for a heating apparatus which can be used in a high-temperature environment without difficulty and which can be easily handled. .
【００１２】[0012]
【課題を解決するための手段】かかる目的を達成するた
めに、本発明の加熱装置用試料導入器具は、高分子試料
を加熱して気体を生成させることにより該高分子試料の
分析を行う際に、該高分子試料を加熱装置に導入する器
具であって、該高分子試料を収容して該加熱装置に導入
する試料容器と、該試料容器を該加熱装置に導入するた
めの柄部を備え該試料容器を着脱自在に保持する試料容
器導入具と、該加熱装置に導入された該試料容器に到達
可能な長さの柄部を備え、該試料容器を着脱自在に保持
する試料容器回収具とからなることを特徴とする。In order to achieve the above object, a sample introduction instrument for a heating apparatus according to the present invention is used for analyzing a polymer sample by heating the polymer sample to generate a gas. An instrument for introducing the polymer sample into a heating device, comprising a sample container for accommodating the polymer sample and introducing into the heating device, and a handle for introducing the sample container into the heating device. A sample container introduction tool for detachably holding the sample container, and a sample container recovery device having a handle portion long enough to reach the sample container introduced into the heating device, and detachably holding the sample container. And a tool.
【００１３】本発明の加熱装置用試料導入器具によれ
ば、前記試料容器は前記試料容器導入具に保持されるこ
とにより、該試料容器導入具の柄部を用いて、前記従来
の試料容器と同様にして前記加熱装置内に導入される。
また、分析終了後には、前記試料容器回収具を前記加熱
装置内に挿入し、前記加熱装置内に導入された試料容器
を保持して引き上げることにより、該試料容器が容易に
回収される。According to the sample introduction device for a heating device of the present invention, the sample container is held by the sample container introduction device, so that the conventional sample container can be connected to the conventional sample container using the handle of the sample container introduction device. It is similarly introduced into the heating device.
After the analysis, the sample container collecting tool is inserted into the heating device, and the sample container introduced into the heating device is held and pulled up, whereby the sample container is easily collected.
【００１４】前記試料容器導入具は、前記柄部の先端
に、前記試料容器に圧接することにより変形され該変形
の復元力により該試料容器に圧着して該試料容器を保持
する弾性部を備えることを特徴とする。前記試料容器導
入具によれば、前記柄部の先端に備えられた弾性部が、
前記試料容器に圧接することにより変形され、該変形が
復元しようとする際に働く復元力により該試料容器に圧
着するので、前記試料容器を容易に保持することができ
る。The sample container introduction tool has an elastic portion at the tip of the handle portion, which is deformed by being pressed against the sample container and is pressed against the sample container by a restoring force of the deformation to hold the sample container. It is characterized by the following. According to the sample container introduction tool, the elastic portion provided at the tip of the handle portion,
The sample container is deformed by being pressed against the sample container, and is pressed against the sample container by a restoring force that is exerted when the deformation attempts to recover, so that the sample container can be easily held.
【００１５】また、前記試料容器回収具は、前記柄部の
先端に、前記試料容器に圧接することにより変形され該
変形の復元力により該試料容器に圧着して該試料容器を
保持する弾性部を備えることを特徴とする。前記試料容
器回収具によれば、前記柄部の先端に備えられた弾性部
が、前記試料容器に圧接することにより変形され、該変
形が復元しようとする際に働く復元力により該試料容器
に圧着して該試料容器を保持する。従って、前記試料容
器回収具は、前記加熱装置内に導入された試料容器に圧
接することにより、容易に該試料容器を保持することが
でき、何ら熟練を要することなく前記加熱装置内に導入
された試料容器の回収を行うことができる。Further, the sample container collecting tool is deformed by being pressed against the sample container at the tip of the handle, and is elastically held on the sample container by a restoring force of the deformation to hold the sample container. It is characterized by having. According to the sample container collection tool, the elastic portion provided at the tip of the handle is deformed by pressing against the sample container, and the elastic force provided to the sample container by a restoring force acting when the deformation is restored. The sample container is pressed and held. Therefore, the sample container collection tool can easily hold the sample container by pressing against the sample container introduced into the heating device, and can be introduced into the heating device without any skill. The collected sample container can be collected.
【００１６】また、前記試料容器回収具は、前記柄部の
先端を、前記加熱装置に導入された前記試料容器に圧接
可能に位置決めする位置決め手段を備えることを特徴と
する。前記加熱装置では、前記試料容器回収具を該加熱
装置に挿入して前記試料容器を回収する作業は目視する
ことができず、手さぐりで行わなければならないが、前
記位置決め手段を備えることにより、前記柄部の先端が
前記加熱装置に導入された前記試料容器に圧接可能に位
置決めされるので、前記柄部の先端を前記試料容器に容
易に圧接することができる。Further, the sample container collecting tool is provided with positioning means for positioning the tip of the handle so as to be able to press against the sample container introduced into the heating device. In the heating device, the operation of inserting the sample container collection tool into the heating device and collecting the sample container is not visible and must be performed by hand, but by providing the positioning means, Since the tip of the handle is positioned so as to be able to press against the sample container introduced into the heating device, the tip of the handle can be easily pressed against the sample container.
【００１７】また、本発明の加熱装置用試料導入器具に
おいて、前記試料容器は従来の試料容器本体と同様に白
金により形成されていてもよいが、白金は前記のような
高温環境下にある前記熱分解管内では、塩酸と反応して
塩化白金を生成したり、白金自体の触媒作用により酸素
または水の存在下に他の化合物と反応することがあり、
繰り返し使用したときに分析誤差の要因になる虞れがあ
る。そこで、本発明の加熱装置用試料導入器具では、前
記試料容器は表面に珪素化合物からなる被覆層を形成し
たものであることを特徴とする。In the sample introduction device for a heating apparatus according to the present invention, the sample container may be formed of platinum similarly to a conventional sample container main body. In the pyrolysis tube, it may react with hydrochloric acid to produce platinum chloride, or may react with other compounds in the presence of oxygen or water due to the catalytic action of platinum itself,
When used repeatedly, it may cause analysis errors. Therefore, in the sample introduction device for a heating device according to the present invention, the sample container has a coating layer made of a silicon compound formed on a surface thereof.
【００１８】前記珪素化合物は、実質的に化学的活性が
ないので、他の化合物と反応する虞れがない。従って、
前記試料容器の表面を前記珪素化合物で被覆することに
より、該試料容器と高分子試料との反応を防止すること
ができる。Since the silicon compound has substantially no chemical activity, there is no fear of reacting with other compounds. Therefore,
By coating the surface of the sample container with the silicon compound, a reaction between the sample container and the polymer sample can be prevented.
【００１９】[0019]
【発明の実施の形態】次に、添付の図面を参照しながら
本発明の実施の形態についてさらに詳しく説明する。図
１（ａ）は本実施形態の加熱装置用試料導入器具を構成
する試料容器の底部側から見た斜視図、図１（ｂ）は図
１（ａ）のＩ−Ｉ線断面図であり、図２は本実施形態の
加熱装置用試料導入器具を構成する試料容器導入具の説
明図であり、図３は本実施形態の加熱装置用試料導入器
具を構成する試料容器導入具の説明図であり、図４は本
実施形態の加熱装置用試料導入器具の使用方法を示す説
明的断面図であり、図５は本実施形態の加熱装置用試料
導入器具を構成する試料容器導入具の他の態様の説明図
及びその使用方法を示す説明的断面図である。Next, embodiments of the present invention will be described in more detail with reference to the accompanying drawings. FIG. 1A is a perspective view of a sample container constituting the sample introduction device for a heating device according to the present embodiment, as viewed from the bottom side, and FIG. 1B is a cross-sectional view taken along line II of FIG. 1A. FIG. 2 is an explanatory view of a sample container introducing tool constituting the heating device sample introducing device of the present embodiment, and FIG. 3 is an explanatory diagram of a sample container introducing device constituting the heating device sample introducing device of the present embodiment. FIG. 4 is an explanatory cross-sectional view illustrating a method of using the sample introduction device for a heating device according to the present embodiment. FIG. FIG. 4 is an explanatory view of the embodiment and an explanatory sectional view showing a method of using the same.
【００２０】本実施形態の加熱装置用試料導入器具は、
図１示の試料容器１と、図２示の試料容器導入具２と、
図３示の試料容器回収具３とからなる。本実施形態の加
熱装置用試料導入器具は、図４（ａ）示のような加熱装
置に使用することができる。図４（ａ）示の加熱装置
は、それ自体公知のシングルショット用縦型小型加熱炉
型の熱分解装置であり、その構成は図６（ａ）示の加熱
装置と全く同一であるので、同一の符号を付して説明を
省略する。The sample introduction instrument for a heating device according to the present embodiment comprises:
A sample container 1 shown in FIG. 1, a sample container introduction tool 2 shown in FIG.
The sample container collection tool 3 shown in FIG. The sample introduction instrument for a heating device of the present embodiment can be used for a heating device as shown in FIG. The heating device shown in FIG. 4 (a) is a well-known single-shot vertical small heating furnace type pyrolysis device, and its configuration is exactly the same as the heating device shown in FIG. 6 (a). The same reference numerals are given and the description is omitted.
【００２１】試料容器１は、例えば図１（ａ）示のよう
に、円筒状の胴部４とその底面に連接される略四角錐台
形状の底部５とからなり、底部５の最下部には長方形状
の底面５ａが形成されている。また、試料容器１の内部
には、図１（ｂ）示のように、前記胴部４及び底部５の
形状に沿って中空部６が形成されており、該中空部６に
高分子試料を収容するようになっている。As shown in FIG. 1A, for example, the sample container 1 comprises a cylindrical body 4 and a substantially truncated pyramid-shaped bottom 5 connected to the bottom thereof. Has a rectangular bottom surface 5a. As shown in FIG. 1B, a hollow portion 6 is formed inside the sample container 1 along the shape of the body portion 4 and the bottom portion 5, and a polymer sample is placed in the hollow portion 6. It is designed to accommodate.
【００２２】本実施形態の試料容器１は、例えばステン
レス等の基材表面が溶融シリカ、シリコン等の珪素化合
物の薄膜で被覆された構成となっている。ステンレスは
化学的活性が比較的高いが、その表面を化学的に実質的
に不活性である前記珪素化合物の薄膜で被覆して、前記
加熱装置内の高温環境下で前記高分子試料が加熱されて
生成する気体成分と反応しないようにすることにより、
試料容器１の基材として使用することができる。The sample container 1 of this embodiment has a structure in which the surface of a base material such as stainless steel is coated with a thin film of a silicon compound such as fused silica or silicon. Stainless steel has relatively high chemical activity, but its surface is coated with a thin film of the silicon compound that is chemically substantially inactive, and the polymer sample is heated under a high temperature environment in the heating device. By not reacting with the gas component generated by
It can be used as a base material of the sample container 1.
【００２３】前記珪素化合物の薄膜は、例えば、減圧下
にモノシラン（ＳｉＨ4 ）を気相熱分解し、試料容器１
の表面にモノシランの分解生成物である金属シリコン
（Ｓｉ）の薄膜を蒸着させる化学蒸着（ＣＶＤ）法によ
り形成することができる。前記ＣＶＤ法によれば、試料
容器１の表面に蒸着された金属シリコンが試料容器１の
基材であるステンレスとの間に超薄膜合金を形成し、そ
の最表面層に二酸化珪素（ＳｉＯ2 ）層が形成される。The silicon compound thin film is formed, for example, by subjecting monosilane (SiH 4 ) to a gas phase pyrolysis under reduced pressure to obtain a sample container 1.
Can be formed by a chemical vapor deposition (CVD) method in which a thin film of metallic silicon (Si), which is a decomposition product of monosilane, is deposited on the surface of the substrate. According to the CVD method, the metal silicon deposited on the surface of the sample container 1 forms an ultra-thin alloy with the stainless steel that is the base material of the sample container 1, and silicon dioxide (SiO 2 ) is formed on the outermost surface layer. A layer is formed.
【００２４】試料容器導入具２はステンレスからなり、
例えば図２（ａ）示のように、試料容器１を前記加熱装
置に導入する柄部７の先端に、柄部７から二股に分岐す
る弾性部８ａを備える。弾性部８ａの先端は柄部７との
間に試料容器１の胴部４の外壁を挿入できる間隔を存し
て柄部７から離間しており、弾性部８ａの中央部には柄
部７との間に試料容器１の胴部４の外壁を挟持して保持
する保持部９ａが設けられている。The sample container introduction tool 2 is made of stainless steel,
For example, as shown in FIG. 2A, an elastic portion 8a that branches from the handle 7 into two branches is provided at the tip of the handle 7 for introducing the sample container 1 into the heating device. The tip of the elastic portion 8a is separated from the handle 7 with an interval allowing the outer wall of the body 4 of the sample container 1 to be inserted between the handle 7 and the handle 7. The handle 7 has a central portion of the elastic portion 8a. A holding portion 9a for holding the outer wall of the body portion 4 of the sample container 1 is provided therebetween.
【００２５】試料容器導入具２によれば、図２（ａ）に
仮想線示するように、柄部７と弾性部８ａとの間に試料
容器１の胴部４の外壁を圧接することにより、柄部７と
弾性部８ａとの間に前記胴部４の外壁が挿入される。こ
の結果、弾性部８ａが試料容器１の外方に向けて変形さ
れると共に、試料容器１の側に向けて復元しようとする
復元力が働き、該復元力により保持部９ａが柄部７との
間に胴部４の外壁を挟持して試料容器１に圧着し、これ
を保持する。According to the sample container introducing tool 2, the outer wall of the body 4 of the sample container 1 is brought into pressure contact between the handle 7 and the elastic portion 8a as shown by a virtual line in FIG. The outer wall of the body 4 is inserted between the handle 7 and the elastic portion 8a. As a result, the elastic portion 8a is deformed toward the outside of the sample container 1, and a restoring force for restoring toward the side of the sample container 1 acts. The outer wall of the body 4 is sandwiched between them and pressed against the sample container 1 and held.
【００２６】試料容器導入具２では、弾性部８ａは柄部
７に溶接により取着されているが、弾性部８ａと柄部７
とは共にステンレスであって同材料であるので、前記加
熱装置内の高温環境下でも互いに剥離する虞れがない。In the sample container introducing tool 2, the elastic portion 8a is attached to the handle 7 by welding.
Are both stainless steel and the same material, so that there is no fear that they are separated from each other even in a high temperature environment in the heating device.
【００２７】試料容器回収具３はステンレスからなり、
例えば図３（ａ）示のように、試料容器１が前記加熱装
置に導入されたときに該加熱装置内の試料容器１に到達
可能な長さの柄部１１の先端に、柄部１１の先端を菱形
状に折り曲げて形成された弾性部１２ａを備える。弾性
部１２ａは菱形の鋭角部を上下に鈍角部を左右に配置し
て、該鈍角部を保持部１３ａとしている。The sample container collection tool 3 is made of stainless steel,
For example, as shown in FIG. 3A, when the sample container 1 is introduced into the heating device, a tip of the handle portion 11 having a length that can reach the sample container 1 in the heating device is provided. It has an elastic portion 12a formed by bending the tip into a rhombus shape. The elastic portion 12a has a rhombic acute angle portion arranged vertically and an obtuse angle portion on the left and right, and the obtuse angle portion is used as a holding portion 13a.
【００２８】弾性部１２ａは図３（ａ）に仮想線示する
ように、試料容器１に圧接されることにより前記菱形の
鋭角部が試料容器１の内側に向けて変形され、試料容器
１に内嵌される。この結果、弾性部１２ａに試料容器１
の外側に向けて復元しようとする復元力が働き、該復元
力により前記保持部１３ａが試料容器１に圧着し、これ
を保持する。As shown by the imaginary line in FIG. 3A, the elastic portion 12a is pressed against the sample container 1 so that the diamond-shaped acute angle portion is deformed toward the inside of the sample container 1, and It is fitted inside. As a result, the sample container 1 is attached to the elastic portion 12a.
A restoring force is applied to the outside of the sample container, and the restoring force causes the holding portion 13a to be pressed against the sample container 1 and held.
【００２９】前記試料容器導入具２及び試料容器回収具
３は、化学的活性が比較的高いステンレスにより構成さ
れているので、前記加熱装置内の高温環境下で前記高分
子試料が加熱されて生成する気体成分と反応しないよう
に、その表面が化学的に実質的に不活性である前記珪素
化合物の薄膜で被覆されていることが好ましい。前記珪
素化合物の薄膜は、試料容器１の場合と同一のＣＶＤ法
により形成することができる。Since the sample container introducing tool 2 and the sample container collecting tool 3 are made of stainless steel having a relatively high chemical activity, the polymer sample is formed by heating the polymer sample in a high temperature environment in the heating device. It is preferable that the surface is coated with a thin film of the silicon compound which is substantially inert chemically so as not to react with a gas component to be generated. The silicon compound thin film can be formed by the same CVD method as in the case of the sample container 1.
【００３０】次に、本実施形態の加熱装置用試料導入器
具の使用方法について説明する。Next, a method of using the sample introduction instrument for a heating device according to the present embodiment will be described.
【００３１】前記加熱装置に高分子試料を導入するとき
には、まず、図４（ａ）示のように、ガス導入口２３か
ら石英熱分解管２１内にキャリヤガスを流通させなが
ら、ヒーター２２により石英熱分解管２１内を５００〜
８００℃程度に加熱する。そして、弾性部８ａにより試
料容器１に圧着してこれを保持している試料容器導入具
２の柄部７の上端を試料サンプラー２５のチャッキング
手段２６でチャッキングし、試料サンプラー２５を石英
熱分解管２１に嵌着する。When a polymer sample is introduced into the heating device, first, as shown in FIG. 4A, quartz is heated by a heater 22 while a carrier gas is passed from a gas inlet 23 into a quartz pyrolysis tube 21. 500- in the pyrolysis tube 21
Heat to about 800 ° C. Then, the upper end of the handle 7 of the sample container introduction tool 2 holding the sample container 1 is pressed by the chucking means 26 of the sample sampler 25, and the sample sampler 25 is heated with quartz. Fit into the disassembly tube 21.
【００３２】次に、チャッキング手段２６を操作してチ
ャッキングを解除すると、図４（ｂ）示のように、試料
容器１が自重により自然落下して石英熱分解管２１内に
試料が導入される。石英熱分解管２１内に導入された試
料容器１は、ロート状部２８上に載置されるが、試料容
器１の底部５は図１示のように長方形の底面５ａを備え
ているので、該底面５ａが前記ロート状部２８のテーパ
ー面に係合し、底面５ａとロート状部２８との間隙から
前記高分子試料の加熱により生成した気体成分を導出口
２９に導くことができる。Next, when the chucking is released by operating the chucking means 26, the sample container 1 falls naturally by its own weight and the sample is introduced into the quartz pyrolysis tube 21 as shown in FIG. Is done. The sample container 1 introduced into the quartz pyrolysis tube 21 is placed on the funnel-shaped portion 28. Since the bottom 5 of the sample container 1 has a rectangular bottom surface 5a as shown in FIG. The bottom surface 5a is engaged with the tapered surface of the funnel-shaped portion 28, and a gas component generated by heating the polymer sample can be guided to the outlet 29 from the gap between the bottom surface 5a and the funnel-shaped portion 28.
【００３３】試料容器１が石英熱分解管２１内に導入さ
れると、石英熱分解管２１は前記のように５００〜８０
０℃程度に加熱されているので、試料容器１に収容され
ている高分子試料は瞬間的に熱分解され、或いは該試料
に含まれる成分の一部が瞬間的に熱脱着される。そし
て、前記熱分解または熱脱着により生成した気体成分
は、前記キャリヤガスにより導出口２９を介して前記分
析装置（図示せず）に導入され分析が行われる。When the sample container 1 is introduced into the quartz pyrolysis tube 21, the quartz pyrolysis tube 21 is 500 to 80 as described above.
Since the polymer sample is heated to about 0 ° C., the polymer sample contained in the sample container 1 is instantaneously thermally decomposed, or a part of components contained in the sample is instantaneously thermally desorbed. Then, the gas component generated by the thermal decomposition or thermal desorption is introduced into the analyzer (not shown) through the outlet port 29 by the carrier gas and analyzed.
【００３４】次に、前記分析が終了すると、図４（ｃ）
示のように、試料サンプラー２５を石英熱分解管２１か
ら取り外し、石英熱分解管２１の上部から試料容器回収
具３を挿入し、弾性部１２ａを試料容器１に圧接して内
嵌する。すると、弾性部１２ａが試料容器１に圧着して
試料容器１を保持するので、図４（ｄ）示のように、試
料容器回収具３を引上げることにより、試料容器１が回
収される。前記柄部１１は、加熱装置内の試料容器１に
到達可能な長さを備えているので、その上端部を把持す
ることにより、前記加熱装置の外部から前記操作を容易
に行うことができる。Next, when the above analysis is completed, FIG.
As shown, the sample sampler 25 is detached from the quartz pyrolysis tube 21, the sample container recovery tool 3 is inserted from above the quartz pyrolysis tube 21, and the elastic portion 12 a is pressed against the sample container 1 and fitted therein. Then, since the elastic portion 12a is pressed against the sample container 1 and holds the sample container 1, the sample container 1 is collected by pulling up the sample container collection tool 3 as shown in FIG. Since the handle 11 has a length that can reach the sample container 1 in the heating device, the operation can be easily performed from the outside of the heating device by gripping the upper end thereof.
【００３５】前記のように加熱装置内の試料容器１に試
料容器回収具３の弾性部１２ａを圧接するときに、前記
試料容器１には試料容器導入具２が取着されたままとな
っている。しかし、試料容器回収具３の弾性部１２ａは
前記菱形の鋭角部が下方に向けて配置されているので、
該鋭角部により試料容器１の胴部４の外壁に取着されて
いる試料容器導入具２を回避し、試料容器１の中央部に
挿入することができる。従って、試料容器導入具２が容
器回収具３により試料容器１を保持する障害となること
はない。As described above, when the elastic portion 12a of the sample container collecting tool 3 is pressed against the sample container 1 in the heating device, the sample container introducing tool 2 is still attached to the sample container 1. I have. However, the elastic portion 12a of the sample container collection tool 3 has the diamond-shaped acute angle portion directed downward,
The acute angle portion allows the sample container introducing tool 2 attached to the outer wall of the body portion 4 of the sample container 1 to be avoided and inserted into the central portion of the sample container 1. Therefore, the sample container introducing tool 2 does not become an obstacle for holding the sample container 1 by the container collecting tool 3.
【００３６】また、試料容器回収具３は、図５（ａ）示
のように、弾性部１２ａを前記加熱装置に導入された試
料容器１に圧接可能に位置決めするために、柄部１１に
形成された石英熱分解管２１よりわずかに小径のスプリ
ング部１４からなる位置決め手段を備えるものであって
もよい。スプリング部１４を備える試料容器回収具３
は、石英熱分解管２１に挿入したときにスプリング部１
４が石英熱分解管２１の内壁に接触して、弾性部１２ａ
が常に試料容器１に圧接可能に位置決めされる。従っ
て、図５（ｂ）示のように、弾性部１２ａを容易に試料
容器１に圧接して内嵌することができる。As shown in FIG. 5 (a), the sample container collecting tool 3 is formed on the handle 11 to position the elastic portion 12a so as to be able to press against the sample container 1 introduced into the heating device. It may be provided with a positioning means comprising a spring portion 14 having a slightly smaller diameter than the quartz pyrolysis tube 21 provided. Sample container recovery tool 3 having spring portion 14
When the spring part 1 is inserted into the quartz pyrolysis tube 21,
4 comes into contact with the inner wall of the quartz pyrolysis tube 21 and the elastic portion 12a
Is always positioned so as to be able to press against the sample container 1. Therefore, as shown in FIG. 5B, the elastic portion 12a can be easily pressed into contact with the sample container 1 and fitted therein.
【００３７】本実施形態では、弾性部８ａを備える試料
容器導入具２を用いているが、試料容器導入具２は図２
（ｂ）示の弾性部８ｂまたは図２（ｃ）示の弾性部８ｃ
を備えるものでもよい。In this embodiment, the sample container introduction tool 2 having the elastic portion 8a is used.
The elastic portion 8b shown in FIG. 2B or the elastic portion 8c shown in FIG.
May be provided.
【００３８】図２（ｂ）示の試料容器導入具２は、試料
容器１を加熱装置に導入する柄部７の先端に、菱形状に
折り曲げて形成された弾性部８ｂを備える。弾性部８ｂ
は図３（ａ）示の弾性部１２ａと同一の構成であり、菱
形の鋭角部を上下に鈍角部を左右に配置して、該鈍角部
を保持部９ｂとしている。弾性部８ｂは図２（ｂ）に仮
想線示するように、試料容器１に圧接されることによ
り、弾性部１２ａと同一の作用によりに試料容器１に内
嵌され、保持部９ｂが試料容器１に圧着し、これを保持
する。The sample container introduction tool 2 shown in FIG. 2 (b) has an elastic portion 8b formed in a rhombus shape at the tip of a handle 7 for introducing the sample container 1 into the heating device. Elastic part 8b
Has the same configuration as the elastic portion 12a shown in FIG. 3 (a), in which rhombic acute angles are arranged vertically and obtuse angles are arranged on the left and right, and the obtuse angles are used as holding portions 9b. The elastic portion 8b is pressed into contact with the sample container 1 as shown by the imaginary line in FIG. 2 (b), so that the elastic portion 8b is fitted inside the sample container 1 by the same action as the elastic portion 12a, and the holding portion 9b is 1 and hold it.
【００３９】また、図２（ｃ）示試料容器導入具２は、
試料容器１を加熱装置に導入する柄部７の先端に、三叉
になった弾性部８ｃを備える。弾性部８ｃは三叉の先端
部が試料容器１に外嵌されるように外方に拡がっている
と共に、中央部に試料容器１に圧着してこれを保持する
保持部９ｃが設けられている。弾性部８ｃは、図２
（ｃ）に仮想線示するように、試料容器１に圧接するこ
とにより試料容器１に外嵌され、試料容器１の外方に向
けて変形される。この結果、試料容器１に外嵌された弾
性部８ｃに試料容器１の側に向けて復元しようとする復
元力が働き、該復元力により保持部９ｃが外側から押さ
え込むようにして試料容器１に圧着し、これを保持す
る。The sample container introduction tool 2 shown in FIG.
At the tip of the handle 7 for introducing the sample container 1 into the heating device, a trifurcated elastic portion 8c is provided. The elastic portion 8c is extended outward so that the tip of the three-pronged end is fitted to the sample container 1, and a holding portion 9c is provided at the center of the elastic portion 8c for pressing and holding the sample container 1. The elastic portion 8c is shown in FIG.
As shown by an imaginary line in (c), by being pressed against the sample container 1, it is fitted to the sample container 1 and deformed outward of the sample container 1. As a result, a restoring force is applied to the elastic portion 8c externally fitted to the sample container 1 so as to restore the sample container 1 toward the sample container 1, and the holding portion 9c is pressed from the outside by the restoring force. Crimp and hold.
【００４０】図２（ｃ）示の試料容器導入具２によれ
ば、保持部９ｃが試料容器１に３点で圧着するので、試
料容器１を安定して保持できる。弾性部８ｃは、柄部７
に溶接により取着されているが、弾性部８ｃと柄部７と
は共にステンレスであって同材料であるので、前記加熱
装置内の高温環境下でも互いに剥離する虞れがない。According to the sample container introducing tool 2 shown in FIG. 2C, the holding portion 9c is pressed against the sample container 1 at three points, so that the sample container 1 can be stably held. The elastic portion 8c is
However, since the elastic portion 8c and the handle portion 7 are both made of stainless steel and made of the same material, there is no possibility that they are separated from each other even in a high-temperature environment in the heating device.
【００４１】また、本実施形態では、弾性部１２ａを備
える試料容器回収具３を用いているが、試料容器回収具
３は図３（ｂ）示の弾性部１２ｂを備えるものでもよ
い。Further, in this embodiment, the sample container collecting tool 3 having the elastic portion 12a is used, but the sample container collecting device 3 may have the elastic portion 12b shown in FIG. 3B.
【００４２】図３（ｂ）示の試料容器回収具３は、試料
容器１が加熱装置に導入されたときに該加熱装置内の試
料容器１に到達可能な長さの柄部１１の先端に、三叉に
なった弾性部１２ｂを備える。弾性部１２ｂは図２
（ｃ）示の弾性部８ｃと同一の構成であり、三叉の先端
部が試料容器１に外嵌されるように外方に拡がっている
と共に、中央部に試料容器１に圧着してこれを保持する
保持部１３ｂが設けられている。弾性部１２ｂは図３
（ｂ）に仮想線示するように、試料容器１に圧接される
ことにより、弾性部８ｃと同一の作用によりに試料容器
１に外嵌され、保持部１３ｂが試料容器１に圧着し、こ
れを保持する。The sample container collecting tool 3 shown in FIG. 3B is provided at the tip of a handle 11 having a length that can reach the sample container 1 in the heating device when the sample container 1 is introduced into the heating device. , And a three-pronged elastic portion 12b. The elastic part 12b is shown in FIG.
(C) has the same configuration as the elastic portion 8c shown in the drawing, and has a three-pronged end that extends outward so as to be fitted to the sample container 1 and that is pressed against the sample container 1 at the center and is A holding section 13b for holding is provided. The elastic part 12b is shown in FIG.
As shown by the phantom line in (b), by being pressed against the sample container 1, it is fitted onto the sample container 1 by the same action as the elastic portion 8 c, and the holding portion 13 b is pressed against the sample container 1, Hold.
【００４３】本実施形態の加熱装置用試料導入器具は、
前記弾性部８ａ，８ｂ，８ｃのいずれかを備える試料容
器導入具２と、前記弾性部１２ａまたは１２ｂを備える
試料容器回収具３とを適宜組み合わせて使用することが
できる。The sample introduction instrument for a heating device according to the present embodiment
The sample container introduction tool 2 having any one of the elastic portions 8a, 8b, and 8c and the sample container collection tool 3 having the elastic portion 12a or 12b can be used in appropriate combination.
【００４４】また、本実施形態では、前記加熱装置用試
料導入器具をシングルショット用縦型小型加熱炉型の熱
分解装置に使用するものとして説明しているが、前記加
熱装置用試料導入器具はダブルショット用の熱分解装置
に使用することもでき、また縦型小型加熱炉型の熱分解
装置に変えて、フィラメント型またはキュリーポイント
型の熱分解装置に使用することもできる。Further, in the present embodiment, the sample introduction device for the heating device is described as being used for a single-shot type vertical small heating furnace type pyrolysis device. It can be used for a double-shot pyrolysis device, and can be used for a filament type or Curie point type pyrolysis device instead of a vertical small heating furnace type pyrolysis device.
【図１】本発明に係る加熱装置用試料導入器具を構成す
る試料容器の底部側から見た斜視図及び縦断面図。FIG. 1 is a perspective view and a vertical sectional view of a sample container constituting a sample introduction device for a heating device according to the present invention, as viewed from the bottom side.
【図２】本発明に係る加熱装置用試料導入器具を構成す
る試料容器導入具の斜視図。FIG. 2 is a perspective view of a sample container introduction tool constituting the sample introduction tool for a heating device according to the present invention.
【図３】本発明に係る加熱装置用試料導入器具を構成す
る試料容器導入具の斜視図。FIG. 3 is a perspective view of a sample container introducing tool constituting the heating device sample introducing tool according to the present invention.
【図４】本発明に係る加熱装置用試料導入器具の使用方
法を示す説明的断面図。FIG. 4 is an explanatory sectional view showing a method for using the sample introduction instrument for a heating device according to the present invention.
【図５】本発明に係る加熱装置用試料導入器具を構成す
る試料容器導入具の他の態様の斜視図及びその使用方法
を示す説明的断面図。FIG. 5 is a perspective view of another embodiment of the sample container introduction tool constituting the sample introduction tool for a heating device according to the present invention, and an explanatory sectional view showing a method of using the same.
【図６】従来の加熱装置用試料導入器具の使用方法を示
す説明的断面図。FIG. 6 is an explanatory sectional view showing a method of using a conventional sample introduction device for a heating device.
【図７】従来の加熱装置用試料導入器具を示す斜視図。FIG. 7 is a perspective view showing a conventional sample introduction device for a heating device.
１…試料容器、 ２…試料容器導入具、 ３…試料容器
回収具、 ７…柄部、８ａ，８ｂ，８ｃ…弾性部、 １
１…柄部、 １２ａ，１２ｂ…弾性部、 １４…位置決
め手段。DESCRIPTION OF SYMBOLS 1 ... sample container, 2 ... sample container introduction tool, 3 ... sample container collection tool, 7 ... handle part, 8a, 8b, 8c ... elastic part, 1
DESCRIPTION OF SYMBOLS 1 ... Handle part, 12a, 12b ... Elastic part, 14 ... Positioning means.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 柘植 新 愛知県尾張旭市北本地ケ原町３の12 (72)発明者 大谷 肇 愛知県名古屋市緑区篠の風３−252 滝 の水住宅９−304 (56)参考文献 特開 昭48−66497（ＪＰ，Ａ) 実開 昭55−127267（ＪＰ，Ｕ) 実公 昭36−3199（ＪＰ，Ｙ１) 実公 昭48−58822（ＪＰ，Ｙ１) (58)調査した分野(Int.Cl.7，ＤＢ名) G01N 30/06 G01N 27/62 G01N 1/22 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Tsuge Shin 12-12 Kitamotochigaharacho, Owariasahi-shi, Aichi Prefecture (72) Inventor Hajime Otani 3-252 Shinonokaze, Midori-ku, Nagoya-shi, Aichi 9- Waterfall Water House 9- 304 (56) References JP-A-48-66497 (JP, A) JP-A-55-127267 (JP, U) JP-A-36-3199 (JP, Y1) JP-A-48-58822 (JP, Y1) (58) Field surveyed (Int. Cl. 7 , DB name) G01N 30/06 G01N 27/62 G01N 1/22
Claims (3)
とにより該高分子試料の分析を行う際に、該高分子試料
を加熱装置に導入する器具であって、 該高分子試料を収容して該加熱装置に導入する試料容器
と、 該試料容器を該加熱装置に導入するための柄部を備え、
前記柄部の先端に、前記試料容器に圧接することにより
変形され該変形の復元力により該試料容器に圧着して該
試料容器を着脱自在に保持する弾性部を備える試料容器
導入具と、 該加熱装置に導入された該試料容器に到達可能な長さの
柄部を備え、前記柄部の先端に、前記試料容器に圧接す
ることにより変形され該変形の復元力により該試料容器
に圧着して該試料容器を着脱自在に保持する弾性部を備
える試料容器回収具とからなることを特徴とする加熱装
置用試料導入器具。1. An instrument for introducing a polymer sample into a heating device when the polymer sample is analyzed by heating the polymer sample to generate a gas. A sample container to be introduced into the heating device, and a handle for introducing the sample container into the heating device.
By pressing against the tip of the handle, the sample container
A sample container introduction tool having an elastic portion that is deformed and pressed against the sample container by a restoring force of the deformation to hold the sample container detachably; and a length that can reach the sample container introduced into the heating device. Having a handle portion, and press-contacting the tip of the handle portion with the sample container.
The sample container is deformed by the restoring force of the deformation.
Bei elastic portion for removably holding removably a sample vessel and pressed to
A sample introduction device for a heating device, comprising:
壁に接触して、前記弾性部が前記加熱装置に導入された
前記試料容器に圧接されるように位置決めする位置決め
手段を備えることを特徴とする請求項１記載の加熱装置
用試料導入器具。 2. The apparatus according to claim 2, wherein the sample container collecting tool is provided in the heating device.
2. The sample introduction device for a heating device according to claim 1, further comprising a positioning unit that positions the elastic portion so as to be in contact with the wall so as to be pressed against the sample container introduced into the heating device.
被覆層を形成したものであることを特徴とする請求項１
または請求項２記載の加熱装置用試料導入器具。 3. A process according to claim 1, wherein the sample container is obtained by forming a coating layer made of silicon compound on the surface
Or the sample introduction instrument for a heating device according to claim 2 .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05650297A JP3321382B2 (en) | 1997-03-11 | 1997-03-11 | Sample introduction device for heating device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05650297A JP3321382B2 (en) | 1997-03-11 | 1997-03-11 | Sample introduction device for heating device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10253606A JPH10253606A (en) | 1998-09-25 |
| JP3321382B2 true JP3321382B2 (en) | 2002-09-03 |
Family
ID=13028898
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP05650297A Expired - Lifetime JP3321382B2 (en) | 1997-03-11 | 1997-03-11 | Sample introduction device for heating device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3321382B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5868908B2 (en) * | 2013-07-23 | 2016-02-24 | フロンティア・ラボ株式会社 | Sample container |
| JP7350632B2 (en) * | 2019-11-18 | 2023-09-26 | 株式会社住化分析センター | Analysis methods and kits |
| CN113607800B (en) * | 2021-07-27 | 2023-08-25 | 中国计量科学研究院 | Rapid mass spectrum detection device and detection method for detecting rubber content in plants |
-
1997
- 1997-03-11 JP JP05650297A patent/JP3321382B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH10253606A (en) | 1998-09-25 |
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