JPS62100649A - Flame analysis method and apparatus - Google Patents
Flame analysis method and apparatusInfo
- Publication number
- JPS62100649A JPS62100649A JP24216385A JP24216385A JPS62100649A JP S62100649 A JPS62100649 A JP S62100649A JP 24216385 A JP24216385 A JP 24216385A JP 24216385 A JP24216385 A JP 24216385A JP S62100649 A JPS62100649 A JP S62100649A
- Authority
- JP
- Japan
- Prior art keywords
- flame
- paper material
- porous paper
- liquid sample
- combustion chamber
- 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
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
Description
【発明の詳細な説明】
（イ）産業上の利用分野
この発明は、炎光分析法及び装置に関する。ざらに詳し
く【ま、液体クロマトグラフィの溶離液中の被検成分の
検出にイ４ ｆｌＪな炎光分析払及び装置に関する。DETAILED DESCRIPTION OF THE INVENTION (a) Field of Industrial Application This invention relates to a method and apparatus for flame analysis. In more detail, this article relates to a flame optical analyzer and apparatus for detecting analyte components in liquid chromatography eluents.
（ロ）従来の技術
液体クロア１へグラフィに上る溶離液中の被検成分の検
出には導電率を用いた方法、Ｕ Ｖ吸収を用いた方法、
Ｉｉ′１ｌｖｉ率を用いた方法、蛍光光度を用いた方法
などが知られている。(b) Conventional technology Methods using electrical conductivity, methods using UV absorption,
A method using the Ii′1lvi ratio, a method using fluorescence intensity, etc. are known.
（ハ）発明が解決しようとする問題点
しかしながら、リン化合物又ｔまイオウ化合物を被検対
象とする場合にはそれ自体のＵＶ吸収に基づく検出や屈
折率検出などが用いられているが、検出感度が不充分ひ
あると共に、ボ１賃の検出ではＵＶ吸収をしたない彼検
対τ土についての測定が不可能であるという問題かあっ
た。そのため、リン化合力のリン原子やイオウ化合物の
イオ・り原子に基づいて検出する方法も考えられ、例え
ば液体クロマ１〜グラフイの溶離液をＩ ＣＰ （Ｉｎ
ｄｕｃｅｄ ｃｏｕｐｌｅｄ ｐｌａｓｍａ）炎光分
析器に導ひいて分析することも考えられるが、分析コス
トが高く、感度も依然不充分であるという問題点があっ
た。(c) Problems to be solved by the invention However, when phosphorus compounds or sulfur compounds are to be tested, detection based on their own UV absorption or refractive index detection is used. In addition to insufficient sensitivity, there was also the problem that it was impossible to measure the UV-absorbing tau soil when detecting the volcanic acid. Therefore, a method of detection based on the phosphorus atom of the phosphorus compounding power or the sulfur atom of the sulfur compound is also considered.
Although it is conceivable to conduct the analysis using a flame analyzer (duced coupled plasma), there are problems in that the analysis cost is high and the sensitivity is still insufficient.
従って、溶離液中のリン化合物やイオウ化合物をそのリ
ン原子やイオウ原子に基づいて簡便に効率良く分析する
方法が望まれていた。Therefore, a method for easily and efficiently analyzing phosphorus compounds and sulfur compounds in eluents based on their phosphorus atoms and sulfur atoms has been desired.
この発明は、かかる状況に鑑みなされたものであり、こ
とに、液体クロマトグラフィからの溶離液中のリンやイ
オウ化合物の定量やリンやイオウの元素分析を簡便に行
ないうる炎光分析法を提供しようとするものである。The present invention has been made in view of the above circumstances, and particularly, it is an object of the present invention to provide a flame light analysis method that can easily quantify phosphorus and sulfur compounds in an eluent from liquid chromatography and perform elemental analysis of phosphorus and sulfur. That is.
（ニ）問題点を解決するための手段
かくしてこの発明によれば、帯状の多孔質紙材の長手方
向に液体試料を順次保持させ、この多孔質紙材を乾燥す
るか又は乾燥せずして炎光光度計のフレーム内にその長
手方向に連続的に供給することにより多孔質紙材の燃焼
及び液体試料中の被検成分の炎光分析を連続的に行なう
ことを特徴とする炎光分析法が提供される。(d) Means for Solving the Problems Thus, according to the present invention, liquid samples are sequentially held in the longitudinal direction of a strip-shaped porous paper material, and the porous paper material is dried or not dried. Flame light analysis characterized by continuously performing flame light analysis of combustion of porous paper material and test components in liquid samples by continuously supplying flame light into the frame of a flame photometer in its longitudinal direction. law is provided.
この発明の最も特徴とりる点は、液体試お１を一種の帯
状の保持体に付着させて該保持体と共にフレーム（炎）
に導入して炎光分析を連続的に行なう点にある。なＪ３
、液体試料は乾燥後にフレームに導入されてもよい。The most characteristic feature of this invention is that the liquid sample 1 is attached to a kind of belt-shaped holder, and a flame (flame) is formed together with the holder.
The point is that flame light analysis can be performed continuously by introducing the Na J3
, the liquid sample may be introduced into the frame after drying.
上記帯状の多孔質紙材としては、通常の濾紙を用いるの
が適しているが、液体試料の含浸保持性が良好でかつフ
レーム内で容易に燃焼される紙材であれば使用可能であ
る。As the band-shaped porous paper material, it is suitable to use ordinary filter paper, but any paper material can be used as long as it has good impregnation retention properties for a liquid sample and is easily combusted within the flame.
この発明で用いる炎光光度計としては、燃焼゛卒内にバ
ーナ、受光器及び排出ガス手段を備えた通常のものを適
用することができ、これらはシングルフレーム型であっ
てもよくダブルフレーム型のものであってもよい。また
バーナは燃焼室の下方から挿設されたものでもよく、上
方から挿設されたものでもよい。フレーム用のガスとし
ては水素又はアルゴンを含む水素等を用いるのが適して
おり、受光器としては、例えば光電子増倍管を用いるの
が適している。As the flame photometer used in this invention, an ordinary flame photometer equipped with a burner, a light receiver, and an exhaust gas means in the combustion chamber can be applied, and these may be of a single frame type or a double frame type. It may be of. Further, the burner may be inserted from below or above the combustion chamber. As the gas for the flame, it is suitable to use hydrogen or hydrogen containing argon, and as the light receiver, it is suitable to use, for example, a photomultiplier tube.
フレーム内で発光する原子が複数種存在しうる場合には
、各発光スペクトルの特性波長を選択的に透過しうるフ
ィルタを受光面に備えた複数の受光器を設定しておくこ
とが好ましい。If there may be multiple types of atoms that emit light within the frame, it is preferable to set up a plurality of light receivers each having a filter on the light receiving surface that can selectively transmit the characteristic wavelength of each emission spectrum.
なお、分析時に上記帯状の多孔質紙材を、モータと１又
は複数のローうによって燃焼室外からフレームに連続的
に供給しうる搬送手段を付設することにより分析操作を
より簡便化することができる。従って、この発明は排ガ
ス口を有する燃焼室と、この燃焼室内に被検成分の気化
・燃焼用のフレームを設定しうるバーナと、該フレーム
からの発光強度検出用の受光器とを備え、該フレームの
設定領域に帯状の多孔質紙材を上記燃焼室外から長手方
向に連続して供給しうるローラ搬送手段を付設したこと
を特徴とする炎光分析装置をも提供するものである。こ
の際、帯状の多孔質紙材のフレーム設定領域内への供給
速度は２０〜５００侑／分程度とするのが適切である。The analysis operation can be further simplified by adding a conveyance means that can continuously supply the band-shaped porous paper material from outside the combustion chamber to the frame using a motor and one or more rows during analysis. . Therefore, the present invention includes a combustion chamber having an exhaust gas port, a burner in which a flame for vaporizing and burning a test component can be set, and a light receiver for detecting the intensity of light emitted from the flame. The present invention also provides a flame light analyzer characterized in that a roller conveying means is attached to a set area of the frame to continuously supply a strip of porous paper material from outside the combustion chamber in the longitudinal direction. At this time, it is appropriate that the feeding speed of the band-shaped porous paper material into the frame setting area is approximately 20 to 500 mm/min.
上記帯状の多孔質紙材へ液体クロマトグラフィのＦＪＭ
液をその溶出速度に対応して連続的に搬送方向に滴下等
により含浸保持させることにより、液体クロマトグラフ
ィの検出器として用いることができる。なお、フレーム
への１９人前に液体試料は乾燥されていてもよい。この
際、液体クロマトグラフィとのリンクは溶離液の溶出量
を制御することにより容易に行なえ、通常微小口径（０
，５ｍｍ以下）のカラムを用いた液体クロマトグラフを
用いればよく、帯状の多孔質紙材の大きさ、搬送速度等
を調整することにより例えば口ｉ￥ｌ 、 Ｏｍｍ程度
のミクロボアカラム等を用いた液体クロマトグラフと直
結可能である。FJM of liquid chromatography on the above band-shaped porous paper material
It can be used as a detector for liquid chromatography by continuously impregnating and retaining a liquid by dripping or the like in the transport direction in accordance with its elution rate. Note that the liquid sample may be dried before being placed in the frame. At this time, linking with liquid chromatography can be easily done by controlling the elution volume of the eluent, and usually has a micro diameter (0
It is sufficient to use a liquid chromatograph using a column with a diameter of 5 mm or less, and by adjusting the size of the porous paper strip, the conveyance speed, etc., it is possible to use a microbore column with a diameter of about 1,000 mm or less. It can be directly connected to a liquid chromatograph.
（ホ）作 用
この発明において、液体試料が保持された帯状の多孔質
紙材は、フレームに連続導入され、そこで多孔質紙材の
燃焼除去及び液体試料中の被検成分の気化・燃焼・発光
が行なわれ、この発光スペクトルの強度が受光器で検出
される。ことに、リン化合物を含む液体試料においては
、フレーム中でｌ−Ｉ Ｐ Ｏの分子５と尤に基づいて
リン元素の連続測定が容易に可能となる。そして、液体
クロマトグラフィの溶雛液をリアルタイムに帯状多孔Ｍ
ｔ（１材に連続的に保持してフレームに導入すること
により液体クロマトグラフィの検出器として好適に使用
できる。(E) Function In this invention, a strip-shaped porous paper material holding a liquid sample is continuously introduced into a frame, where the porous paper material is burned and removed, and the test component in the liquid sample is vaporized, burned, and Light is emitted, and the intensity of this emission spectrum is detected by a light receiver. Particularly, in liquid samples containing phosphorus compounds, continuous measurements of elemental phosphorus are easily possible based on molecules 5 of l-I PO in a flame. Then, the melt liquid of liquid chromatography is applied to the band-shaped porous M in real time.
It can be suitably used as a detector for liquid chromatography by continuously holding it in one material and introducing it into a frame.
なお、この発明の炎光分析装置は、液体クロマ［ヘグラ
フイの溶離液の連続検出のみならず単品の液体試ｒ１の
分析に用いることかできる。The flame light analyzer of the present invention can be used not only for the continuous detection of liquid chroma [hegraphy eluent] but also for the analysis of a single liquid sample r1.
（へ）実施例
発光光度肝ＧＣ−７ＡダブルフレームＦＰＤ（（（未島
）Ｐ製作新製）を改造して第１図及び第２図に示すごと
きこの５で明の方法を実施する炎光分析装置（１）を設
定した。図に示すように炎光分析装置（１）は、バーナ
（２）、光電子倍増管（３）及び４１Ｆ気口（４）を有
する燃焼室（９）を描え、バーナ（２により燃焼室（９
）内に設定されるフレーム（８）に、帯状の濾紙（５：
幅２〜３１１１１ｎ、良さ４０ｃ７１１）を長手方向に
供給するローラ搬送手段を付設してなり、該搬送手段は
、ガイド（６）、ローラ（刀及びローラ駆動用モータ（
７１）とから４７４成されてなる。(f) Example luminous intensity A flame light is implemented by modifying a liver GC-7A double frame FPD ((Newly manufactured by (Mishima) P) and implementing the Ming method in this 5 as shown in Figures 1 and 2. The analyzer (1) was set up.As shown in the figure, the flame analyzer (1) depicts a combustion chamber (9) with a burner (2), a photomultiplier tube (3) and a 41F air port (4). Well, the burner (2 causes the combustion chamber (9)
), a strip of filter paper (5:
It is equipped with a roller conveying means for feeding the material (width 2 to 31111n, height 40c711) in the longitudinal direction.
71) and 474.
」二記分析装置（１）を使用し、帯状の濾紙の長手方向
の２り所に １％リン酸３４をそれぞれ付香させて保持
さけ、室温でしばらく放置後、ｄ紙搬送（供給）速度４
５ ｎｕｎ ／分でフレームに連続導入した。Using the Analyzer (1) described in Section 2, add 1% phosphoric acid 34 to each of the two longitudinal locations of a band-shaped filter paper and hold it there. After leaving it at room temperature for a while, adjust the paper conveyance (feeding) speed. 4
The frame was continuously introduced at 5 nun/min.
なイｊ３バーブはシングルフレームとした。このｆｓ果
を第３図に示ず。Nai J3 Barb is a single frame. This fs result is not shown in Figure 3.
このように、瀘ｊｖ口こ保持されたリン酸に基づく２つ
の強い発光ピーク（ピークＡ及びＢ）がル２められる。Thus, two strong emission peaks (peaks A and B) due to the retained phosphoric acid are identified.
また、バーナをダブルフレームと覆ることによりＳ／Ｎ
比の向１−シ可能である。In addition, by covering the burner with a double frame, S/N
It is possible to change the ratio in either direction.
（ト）発明の効果
この発明によれば、液体り［］マトグラノイの溶離液中
の被検成分ことに種々のリン化合物やイオウ化合物を連
続的に検出することができる。そして、炎〉に光度に基
づいているためリン化合物やイオウ化合物中の各原子に
７・１応する出力がＩｒｌられ、感度、再現性′８し良
好で・ある。さらに、液体クロマトグラフィの検出器と
して分析コスト上充分に許容できるものである。(G) Effects of the Invention According to the present invention, various phosphorus compounds and sulfur compounds can be continuously detected among the test components in the eluate of liquid phosphorus. Since it is based on the luminous intensity of the flame, an output corresponding to 7.1 for each atom in a phosphorus compound or a sulfur compound is output, and the sensitivity and reproducibility are good. Furthermore, it is sufficiently acceptable in terms of analysis cost as a detector for liquid chromatography.
第１図は、この発明の方法を実施する装置の一実施例を
示す概略図、第２図は同じく要部構成説明図、第３図は
この発明の方法による分析結束をｊりｊ示するグラフで
ある。
（１）・・・・・・炎光分析装置、（２）・・・・・・
バーナ、（３）・・・・・光電子倍増管、（４）・・・
・・・排気口、（５）・・・・・・帯状の濾紙、（６）
・・・・・・ガイド、（刀・・・・・・１」−ラ、（ε
３）・・・・・・フレーム、（７１）・・・・・・ロー
ラ駆動用モータ。
笥 １ 図
第３図
崎閏（分）Fig. 1 is a schematic diagram showing an embodiment of an apparatus for carrying out the method of the present invention, Fig. 2 is also an explanatory diagram of the main part configuration, and Fig. 3 is a diagram illustrating an analysis method according to the method of the present invention. It is a graph. (1)・・・Flame light analyzer, (2)・・・・・・
Burner, (3)...Photomultiplier tube, (4)...
...exhaust port, (5) ...band-shaped filter paper, (6)
...Guide, (sword...1"-ra, (ε
3)...Frame, (71)...Roller drive motor. 1. Figure 3: Sakijyu (minute)
Claims (1)
させ、この多孔質紙材を乾燥するか又は乾燥せずして炎
光光度計のフレーム内にその長手方向に連続的に供給す
ることにより多孔質紙材の燃焼及び液体試料中の被検成
分の炎光分析を連続的に行なうことを特徴とする炎光分
析法。 ２、液体試料が、液体クロマトグラフィの溶離液である
特許請求の範囲第１項記載の分析法。 ３、被検成分が、リン化合物又はイオウ化合物である特
許請求の範囲第１項記載の分析法。 ４、排ガス口を有する燃焼室と、この燃焼室内に被検成
分の気化・燃焼用のフレームを設定しうるバーナと、該
フレームからの発光強度検出用の受光器とを備え、該フ
レームの設定領域に帯状の多孔質紙材を上記燃焼室外か
ら長手方向に連続して供給しうるローラ搬送手段を付設
したことを特徴とする炎光分析装置。[Claims] 1. A liquid sample is sequentially held in the longitudinal direction of a strip-shaped porous paper material, and the porous paper material is dried or not dried and placed in the frame of a flame photometer along its longitudinal direction. A flame light analysis method characterized in that combustion of porous paper material and flame light analysis of test components in a liquid sample are continuously performed by continuously supplying the material in a direction. 2. The analysis method according to claim 1, wherein the liquid sample is an eluent for liquid chromatography. 3. The analytical method according to claim 1, wherein the component to be tested is a phosphorus compound or a sulfur compound. 4. A combustion chamber having an exhaust gas port, a burner in which a flame for vaporizing and burning the test component can be set, and a light receiver for detecting the intensity of light emitted from the flame, and setting of the flame. 1. A flame light analysis device, characterized in that a roller conveying means is attached to the combustion chamber to continuously supply a strip of porous paper material from outside the combustion chamber in the longitudinal direction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24216385A JPS62100649A (en) | 1985-10-28 | 1985-10-28 | Flame analysis method and apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24216385A JPS62100649A (en) | 1985-10-28 | 1985-10-28 | Flame analysis method and apparatus |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS62100649A true JPS62100649A (en) | 1987-05-11 |
Family
ID=17085266
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24216385A Pending JPS62100649A (en) | 1985-10-28 | 1985-10-28 | Flame analysis method and apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62100649A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002003054A1 (en) * | 2000-06-30 | 2002-01-10 | Iatron Laboratories, Inc. | Hydrogen flame luminosity analyzer for thin-layer chromatograph, and hydrogen flame luminosity analyzing method |
| CN103575723A (en) * | 2013-11-14 | 2014-02-12 | 内蒙古第一机械集团有限公司 | Method for testing content of phosphorus in nickel-phosphorus alloy plating layer |
-
1985
- 1985-10-28 JP JP24216385A patent/JPS62100649A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2002003054A1 (en) * | 2000-06-30 | 2002-01-10 | Iatron Laboratories, Inc. | Hydrogen flame luminosity analyzer for thin-layer chromatograph, and hydrogen flame luminosity analyzing method |
| JP2002014046A (en) * | 2000-06-30 | 2002-01-18 | Iatron Lab Inc | Luminous intensity analyzer and analyzing method of hydrogen frame for thin layer chromatograph |
| AU774468B2 (en) * | 2000-06-30 | 2004-07-01 | Lsi Medience Corporation | Hydrogen flame luminosity analyzer for thin-layer chromatograph, and hydrogen flame luminosity analyzing method |
| EP1296130A4 (en) * | 2000-06-30 | 2006-07-05 | Mitsubishi Kagaku Iatron Inc | Hydrogen flame luminosity analyzer for thin-layer chromatograph, and hydrogen flame luminosity analyzing method |
| JP4612936B2 (en) * | 2000-06-30 | 2011-01-12 | 三菱化学メディエンス株式会社 | Hydrogen flame photometric analyzer and hydrogen flame photometric analysis method for thin layer chromatography |
| CN103575723A (en) * | 2013-11-14 | 2014-02-12 | 内蒙古第一机械集团有限公司 | Method for testing content of phosphorus in nickel-phosphorus alloy plating layer |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Baker et al. | Atomic absorption and flame emission spectrometry | |
| US20110098962A1 (en) | Spectrometer, spectrometry, and spectrometry program | |
| US3661533A (en) | Adjustable apparatus for flame ionization and flame emission detection | |
| US4225235A (en) | Sample introduction system for flameless emission spectroscopy | |
| JPS62100649A (en) | Flame analysis method and apparatus | |
| US4008963A (en) | Method of and device for the analysis of samples by means of flameless atomic absorption spectroscopy | |
| Katskov et al. | Design, operation and analytical characteristics of the filter furnace, a new atomizer for electrothermal atomic absorption spectrometry | |
| US3504976A (en) | Process and apparatus for the detection of halogens | |
| Gough et al. | A non-dispersive atomic fluorescence spectrometer for the direct determination of metals | |
| JPH04216440A (en) | Apparatus and method for jetting compound into plasma for induction coupling type argon-plasma light-emitting spectrochemical analysis | |
| US5702954A (en) | Method to detect phosphorus | |
| Montaser et al. | Graphite braid atomizer for atomic absorption and atomic fluorescence spectrometry | |
| Ghauch et al. | Room temperature phosphorescence analyses of polycyclic aromatic hydrocarbons using an imaging sensing system combined with a bifurcated optical fiber and a cooled charge coupled device detector | |
| JP4612936B2 (en) | Hydrogen flame photometric analyzer and hydrogen flame photometric analysis method for thin layer chromatography | |
| Edel et al. | Simultaneous multielement determination in complex matrices using frequency-modulated electrothermal atomic absorption spectrometry | |
| US4162849A (en) | Selected element concentration for flameless atomic absorption spectroscopic measurements | |
| Gornushkin et al. | Use of laser-excited atomic fluorescence spectrometry with a novel diffusive graphite tube electrothermal atomizer for the direct determination of silver in sea water and in solid reference materials | |
| JP5114587B2 (en) | Apparatus and method for determining material properties using HPLC | |
| West | Atomic-fluorescence and atomic-absorption spectrometry for chemical analysis | |
| US5708507A (en) | Temperature resolved molecular emission spectroscopy of materials | |
| Hood et al. | Determination of sulfur-and phosphorus-containing compounds using metastable transfer emission spectrometry | |
| GB2114736A (en) | Transporting laser-vaporised sample material for analysis | |
| Black et al. | Atomic fluorescence spectrometry with continuous nebulization into a platinum furnace | |
| Karanassios et al. | Determination of mercury vapor in air using electrically heated, gold-coated wire-loops, in-torch vaporization sample introduction and inductively coupled plasma atomic emission spectrometry with photodiode array detection | |
| US20040266018A1 (en) | Hydrogen-flame photometric analyzer for thin-layer chromatograph and hydrogen-flame photometric analyzing method |