JPH03235039A - Infrared spectrophotometer - Google Patents
Infrared spectrophotometerInfo
- Publication number
- JPH03235039A JPH03235039A JP2029641A JP2964190A JPH03235039A JP H03235039 A JPH03235039 A JP H03235039A JP 2029641 A JP2029641 A JP 2029641A JP 2964190 A JP2964190 A JP 2964190A JP H03235039 A JPH03235039 A JP H03235039A
- Authority
- JP
- Japan
- Prior art keywords
- belt
- infrared
- sample
- specimen
- absorption spectrum
- 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
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 19
- 238000000862 absorption spectrum Methods 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 5
- 239000000523 sample Substances 0.000 claims description 17
- 239000012141 concentrate Substances 0.000 claims description 7
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 3
- 239000012488 sample solution Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 abstract description 11
- 238000005259 measurement Methods 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 7
- 239000012299 nitrogen atmosphere Substances 0.000 abstract description 2
- 230000005855 radiation Effects 0.000 abstract 1
- 230000003252 repetitive effect Effects 0.000 abstract 1
- 230000035945 sensitivity Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000012468 concentrated sample Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001028 reflection method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Landscapes
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は赤外分光光度計に関し、さらに詳しくは高速液
体クロマトグラフに付設して用いられ、難揮発性物質の
分子構造を分析する赤外分光光度計に関する。[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to an infrared spectrophotometer, and more specifically, an infrared spectrophotometer that is used attached to a high-performance liquid chromatograph to analyze the molecular structure of a hardly volatile substance. Regarding spectrophotometers.
［従来の技術］
難揮発性物質を含む混合物の同定を行う場合、高速液体
クロマトグラフによって各成分の分離を行った後、赤外
分光光度８寸や核磁気共鳴装置を用いて分子構造の解析
を行う。従来は、高速液体クロマトグラフを用いて各成
分の分取を行い、溶媒を加熱・除去したうえでセルに試
料を塗布したり、ＫＢｒ粉末に滴下して拡散反射法によ
って赤外吸収スペクトルの測定を行っていた。[Conventional technology] When identifying a mixture containing difficult-to-volatile substances, each component is separated using high-performance liquid chromatography, and then the molecular structure is analyzed using infrared spectroscopy or nuclear magnetic resonance. I do. Conventionally, each component was separated using a high-performance liquid chromatograph, the solvent was heated and removed, and then the sample was applied to a cell, or it was dropped onto KBr powder and the infrared absorption spectrum was measured using the diffuse reflection method. was going on.
近年、装置の簡略化が進むに伴って、高速液体クロマト
グラフと赤外分光光度計の一体化が試みられている。そ
の方式としては、高速液体クロマトグラフからの流路を
直接赤外分光光度ｔ１の７０液体セルへ接続し、リアル
タイムで透過法により赤外吸収スペクトルを得る方法か
ある。また、高速液体クロマトグラフからの分離溶出物
をＫＢｒ結晶板に自動捕集し、これを赤外分光光度計に
移して測定する方法もある。この方法では、高速液体ク
ロマトグラフからの分離溶出物をＫＢｒ結晶を用いた円
板上の捕集板に回転させながら捕集する。溶媒は、温め
られたＮ２カス雰囲気中で蒸発させるため、分離された
試料のみが円弧上のトレースとして残る。この捕集板を
ビームコンデンサに取り付け、回転させなから順次透過
法で測定する。In recent years, as equipment has become simpler, attempts have been made to integrate a high-performance liquid chromatograph and an infrared spectrophotometer. One method for this is to directly connect a flow path from a high performance liquid chromatograph to a 70 liquid cell with an infrared spectrophotometer t1, and obtain an infrared absorption spectrum in real time by a transmission method. There is also a method in which the separated eluate from the high performance liquid chromatograph is automatically collected on a KBr crystal plate and then transferred to an infrared spectrophotometer for measurement. In this method, the separated eluate from a high-performance liquid chromatograph is collected while rotating on a collecting plate on a disk using KBr crystals. Since the solvent is evaporated in a heated N2 gas atmosphere, only the separated sample remains as a trace on an arc. This collection plate is attached to a beam condenser, and measurements are made sequentially using the transmission method without rotating it.
［発明が解決しようとする課題１
しかしながら、このような高速液体クロマトグラフに接
続して用いられる赤外分光光度調のうち、直接溶出物を
フロー液体セルへ流す方式による装置では、多量の溶媒
も混入する可能性かあり、試料か微量な場合には試料の
スペクトルを得ることができない。また、分離溶出物を
捕集板に捕集する方式による装置では、ＫＢｒ結晶を用
いているため溶媒に水を使用覆ることは不可能であり、
そのため分離できる試料にも制限かあるし、この方法で
は高速液体クロマトグラフ装置との一体化もなされ得な
い。[Problem to be Solved by the Invention 1] However, among the infrared spectrophotometers used in connection with such high-performance liquid chromatographs, in devices that directly flow the eluate into a flow liquid cell, a large amount of solvent is There is a possibility of contamination, and if the sample is in trace amounts, it is not possible to obtain a spectrum of the sample. In addition, in a device that collects the separated eluate on a collection plate, it is impossible to use water as a solvent because KBr crystals are used.
Therefore, there are limits to the samples that can be separated, and this method cannot be integrated with a high-performance liquid chromatography device.
本発明の目的は、以上述べたような従来の問題点を解消
し、混合物中の難揮発性物質の分子構造解析において、
高速液体クロマトグラフの分離溶媒の種類に拘わらず、
かつ高速液体クロマトグラフと一体型で容易に赤外吸収
スペクトルを１ｑることのできる赤外分光光度計を提供
することにある。The purpose of the present invention is to solve the above-mentioned conventional problems, and to solve the problems described above, and to
Regardless of the type of separation solvent used in high performance liquid chromatography,
Another object of the present invention is to provide an infrared spectrophotometer that is integrated with a high-performance liquid chromatograph and can easily measure an infrared absorption spectrum of 1q.
［課題を解決するための手段］
本発明は、高速液体クロマトグラフで分離・溶出した試
料液を加熱・濃縮して濃縮液とする加熱濃縮管と、前記
濃縮液中の試料の赤外吸収スペクトル測定を行う赤外分
光光度計本体からなり、前記加熱濃縮管は、試料液の加
熱手段と、濃縮液を噴霧覆−るノズルとを備え１．前記
赤外分光光度計本体は、鏡面加工を施されて移動可能な
ベルトと、該ベルト上に前記ノズルから噴霧された濃縮
物を乾固させる加熱手段と、前記ベルト上の試料の赤外
吸収スペクトル測定を行う測定手段とを備えてなること
を特徴とする赤外分光光度計である。[Means for Solving the Problems] The present invention provides a heating concentration tube that heats and concentrates a sample solution separated and eluted using a high-performance liquid chromatograph to obtain a concentrated solution, and an infrared absorption spectrum of a sample in the concentrated solution. 1. It consists of an infrared spectrophotometer main body for carrying out measurements, and the heating concentration tube is equipped with means for heating the sample liquid and a nozzle for spraying and covering the concentrated liquid. The infrared spectrophotometer main body includes a mirror-finished movable belt, a heating means for drying the concentrate sprayed from the nozzle onto the belt, and an infrared absorption means for the sample on the belt. The present invention is an infrared spectrophotometer characterized by comprising a measuring means for performing spectrum measurement.
［作用１
高速液体クロマトグラフ装置から分離・溶出した試料液
をそのまま加熱濃縮管に通すことにより、溶媒はある程
度蒸発し、濃縮された試料のみがノズルから噴射される
。噴射された試料は、鏡面加工を施したベルトに付着さ
せたのち、加熱手段、例えば加熱ヒータ内を通し乾固さ
せる。このベルトを試料の付着面が赤外光照射位置にく
るまで移動させて赤外光を照射し、赤外吸収スペクトル
測定を行う。これにより高速液体クロマトグラフと赤外
分光光度計を一体化でき、容易に難揮発性物質の赤外吸
収スペクトルを得ることができる。[Operation 1] By passing the sample liquid separated and eluted from the high-performance liquid chromatography device as it is through the heating concentration tube, the solvent is evaporated to some extent, and only the concentrated sample is injected from the nozzle. The sprayed sample is attached to a mirror-finished belt, and then passed through a heating means, such as a heater, to dry up. This belt is moved until the surface to which the sample is attached comes to the infrared light irradiation position, infrared light is irradiated, and an infrared absorption spectrum is measured. This allows a high-performance liquid chromatograph and an infrared spectrophotometer to be integrated, making it possible to easily obtain an infrared absorption spectrum of a hardly volatile substance.
［実施例］
以下、本発明の実施例について図面を参照して詳細に説
明する。[Example] Hereinafter, an example of the present invention will be described in detail with reference to the drawings.
第１図は本発明の一実施例を示す赤外分光光度計の概略
構成図でおる。本装置は、高速液体クロマトグラフ１に
接続した加熱濃縮管２および赤外分光光度計本体３より
なり、加熱濃縮管２は試料液を加熱する加熱手段（図示
せず）と、先端部には得られた濃縮液を後記するベルト
上釘噴霧するノズル４とを備えている。また赤外分光光
度計本体３は、鏡面加工されたベルト５と、該ベルト上
に噴霧された濃縮液を乾固させる加熱手段である加熱ヒ
ータ６と、乾固して得られる試料の赤外吸収スペクトル
測定を行う測定手段としての光源９、反射ミラー８ａ〜
８ｄおよび検出器１０を備えている。FIG. 1 is a schematic diagram of an infrared spectrophotometer showing an embodiment of the present invention. This device consists of a heating concentrator tube 2 connected to a high-performance liquid chromatograph 1 and an infrared spectrophotometer main body 3. The heating concentrator tube 2 has a heating means (not shown) for heating the sample liquid and It is equipped with a nozzle 4 for spraying the obtained concentrated liquid onto the belt, which will be described later. The infrared spectrophotometer main body 3 includes a mirror-finished belt 5, a heater 6 which is a heating means for drying the concentrated liquid sprayed onto the belt, and an infrared ray of the sample obtained by drying. A light source 9 and a reflecting mirror 8a as a measuring means for measuring an absorption spectrum.
8d and a detector 10.
高速液体クロマトグラフ１から分離・溶出された試料液
は加熱濃縮管２を通り、その中に設置された加熱装置に
より、溶媒をある程度蒸発させる。The sample liquid separated and eluted from the high performance liquid chromatograph 1 passes through the heating concentration tube 2, and the solvent is evaporated to some extent by a heating device installed therein.
濃縮された試料のみをノズル４から一定速度で回転して
いるベルト５に噴射して付着させる。ベルト５の回転速
度は流量に合わせ任意に設定することか可能である。付
着した試料は加熱ヒータ６内を通すことにより乾固させ
る。この時に気化された溶媒、および加熱ヒータ６から
発生する熱は、ファン７によって装置外部へ除去される
。また、赤外分光光度計本体３内は窒素雰囲気としてお
く。Only the concentrated sample is injected from a nozzle 4 onto a belt 5 rotating at a constant speed and deposited thereon. The rotational speed of the belt 5 can be arbitrarily set according to the flow rate. The adhered sample is passed through the heater 6 to dry up. At this time, the vaporized solvent and the heat generated from the heater 6 are removed to the outside of the apparatus by the fan 7. Further, the inside of the infrared spectrophotometer main body 3 is kept in a nitrogen atmosphere.
試料付着面が赤外光照射位置に達した時点で、高感度反
射法により赤外吸収スペクトルの測定が可能となる。ベ
ルト５は取り外しが可能であるため、測定後洗浄し、繰
り返して測定を行うことが可能である。以上のようにし
て、難揮発性物質を含む混合物の分離成分の赤外吸収ス
ペクトルを得ることができる。When the sample-attached surface reaches the infrared light irradiation position, it becomes possible to measure the infrared absorption spectrum using the high-sensitivity reflection method. Since the belt 5 is removable, it can be washed after measurement and measurements can be repeated. In the manner described above, an infrared absorption spectrum of a separated component of a mixture containing a hardly volatile substance can be obtained.
［発明の効果］
以上説明したように、本発明による赤外分光光度計を用
いれば、迅速に、かつ容易に混合物中の難揮発性物質の
赤外吸収スペクトルを得ることが可能である。また、高
速液体クロマトグラフで使用する溶媒に水が用いられて
いても測定が可能なので、測定対象物質か広範なものと
なる等の効果を有する。[Effects of the Invention] As explained above, by using the infrared spectrophotometer according to the present invention, it is possible to quickly and easily obtain an infrared absorption spectrum of a hardly volatile substance in a mixture. Furthermore, since measurement is possible even when water is used as a solvent in a high-performance liquid chromatograph, it has the advantage that a wide range of substances can be measured.
第１図は本発明の一実施例の概略構成図でおる。 １・・・高速液体クロマトグラフ ２・・・加熱濃縮管 ３・・・赤外分光光度計本体 FIG. 1 is a schematic diagram of an embodiment of the present invention. 1...High performance liquid chromatograph 2... Heating concentration tube 3...Infrared spectrophotometer body
Claims (1)
を加熱・濃縮して濃縮液とする加熱濃縮管と、前記濃縮
液中の試料の赤外吸収スペクトル測定を行う赤外分光光
度計本体からなり、前記加熱濃縮管は、試料液の加熱手
段と、濃縮液を噴霧するノズルとを備え、前記赤外分光
光度計本体は、鏡面加工を施されて移動可能なベルトと
、該ベルト上に前記ノズルから噴霧された濃縮物を乾固
させる加熱手段と、前記ベルト上の試料の赤外吸収スペ
クトル測定を行う測定手段とを備えてなることを特徴と
する赤外分光光度計。(1) From a heating concentrator tube that heats and concentrates the sample solution separated and eluted by high-performance liquid chromatography to make a concentrate, and an infrared spectrophotometer body that measures the infrared absorption spectrum of the sample in the concentrate. The heating concentrator tube includes a means for heating the sample liquid and a nozzle for spraying the concentrate, and the infrared spectrophotometer body includes a mirror-finished movable belt and a movable belt on the belt. An infrared spectrophotometer comprising: heating means for drying the concentrate sprayed from the nozzle; and measuring means for measuring the infrared absorption spectrum of the sample on the belt.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2029641A JPH03235039A (en) | 1990-02-13 | 1990-02-13 | Infrared spectrophotometer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2029641A JPH03235039A (en) | 1990-02-13 | 1990-02-13 | Infrared spectrophotometer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03235039A true JPH03235039A (en) | 1991-10-21 |
Family
ID=12281710
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2029641A Pending JPH03235039A (en) | 1990-02-13 | 1990-02-13 | Infrared spectrophotometer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03235039A (en) |
-
1990
- 1990-02-13 JP JP2029641A patent/JPH03235039A/en active Pending
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