JPH063352A - Metallic pyrolysis tube for analyzing oxygen and its pyrolysis method - Google Patents
Metallic pyrolysis tube for analyzing oxygen and its pyrolysis methodInfo
- Publication number
- JPH063352A JPH063352A JP16301492A JP16301492A JPH063352A JP H063352 A JPH063352 A JP H063352A JP 16301492 A JP16301492 A JP 16301492A JP 16301492 A JP16301492 A JP 16301492A JP H063352 A JPH063352 A JP H063352A
- Authority
- JP
- Japan
- Prior art keywords
- tube
- pyrolysis
- metal
- oxygen
- sample
- 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 239000001301 oxygen Substances 0.000 title claims abstract description 47
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 47
- 238000000197 pyrolysis Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004458 analytical method Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 28
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 16
- 239000001307 helium Substances 0.000 claims abstract description 9
- 229910052734 helium Inorganic materials 0.000 claims abstract description 9
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 8
- DSVGQVZAZSZEEX-UHFFFAOYSA-N [C].[Pt] Chemical compound [C].[Pt] DSVGQVZAZSZEEX-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000006229 carbon black Substances 0.000 claims abstract description 7
- 239000002775 capsule Substances 0.000 claims abstract description 5
- 230000003647 oxidation Effects 0.000 claims abstract description 4
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims description 44
- 239000002184 metal Substances 0.000 claims description 44
- 239000000523 sample Substances 0.000 claims description 16
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 239000000538 analytical sample Substances 0.000 claims description 4
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 150000002927 oxygen compounds Chemical class 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims 1
- 150000002894 organic compounds Chemical class 0.000 abstract description 20
- 238000003556 assay Methods 0.000 abstract 2
- 239000012070 reactive reagent Substances 0.000 abstract 2
- 239000007789 gas Substances 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000000956 alloy Substances 0.000 description 7
- 229910045601 alloy Inorganic materials 0.000 description 7
- 229910002804 graphite Inorganic materials 0.000 description 7
- 239000010439 graphite Substances 0.000 description 7
- 229910052697 platinum Inorganic materials 0.000 description 7
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 4
- RLFWWDJHLFCNIJ-UHFFFAOYSA-N Aminoantipyrine Natural products CN1C(C)=C(N)C(=O)N1C1=CC=CC=C1 RLFWWDJHLFCNIJ-UHFFFAOYSA-N 0.000 description 3
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 3
- VEQOALNAAJBPNY-UHFFFAOYSA-N antipyrine Chemical compound CN1C(C)=CC(=O)N1C1=CC=CC=C1 VEQOALNAAJBPNY-UHFFFAOYSA-N 0.000 description 3
- 229960001948 caffeine Drugs 0.000 description 3
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 229960005222 phenazone Drugs 0.000 description 3
- 230000035945 sensitivity Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000011733 molybdenum Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910002065 alloy metal Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000003869 coulometry Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VMWYVTOHEQQZHQ-UHFFFAOYSA-N methylidynenickel Chemical compound [Ni]#[C] VMWYVTOHEQQZHQ-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、酸素分析用金属製熱
分解管とこれを用いた熱分解方法に関するものである。
さらに詳しくは、この発明は、有機元素微量分析法の分
野における酸素分析法に関するものであり、有機化合物
中の酸素元素を精密に定量するための、新しい熱分解管
とこれを用いた熱分解方法に関するものであって、基礎
有機化学の分野における精密分析から有機化学工業（主
として医薬品）などにおける品質管理等まで広範囲に寄
与するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a metal pyrolysis tube for oxygen analysis and a pyrolysis method using the same.
More specifically, the present invention relates to an oxygen analysis method in the field of organic element trace analysis method, and a new pyrolysis tube and a pyrolysis method using the same for accurately quantifying oxygen element in an organic compound. It contributes to a wide range from precision analysis in the field of basic organic chemistry to quality control in the organic chemical industry (mainly pharmaceuticals).
【０００２】[0002]
【従来の技術】周知の通り、酸素分析法については、１
９１０年頃から多数の文献が報告されている。それらの
骨子は、有機化合物の所要量を石英管または黒鉛管など
で作成した熱分解管内で、９００〜１３００℃に加熱
し、その熱分解生成物を白金炭素層またはカーボンブラ
ック層に移送させて、すべての酸素化合物を一酸化炭素
に（ＣＯ）に変換し、次いでＣＯを酸化層に移送して二
酸化炭素（ＣＯ2 ）に酸化したのち、ＣＯ2 の量を重量
法、クーロメトリー、熱伝導度法および赤外吸収法など
で検出して、酸素元素の含有率を測定するものである。
また、これらの基本的原理に基づく、数種類の酸素分析
計もすでに市販されている。2. Description of the Related Art As is well known, there are 1
Many documents have been reported since around 910. These skeletons are prepared by heating a required amount of an organic compound to 900 to 1300 ° C. in a pyrolysis tube made of a quartz tube or a graphite tube and transferring the pyrolysis product to a platinum carbon layer or a carbon black layer. After converting all oxygen compounds into carbon monoxide (CO) and then transferring CO to the oxidation layer to oxidize it into carbon dioxide (CO 2 ), the amount of CO 2 is determined by gravimetric method, coulometry, thermal conductivity. And the infrared absorption method to detect the oxygen element content.
Also, several types of oxygen analyzers based on these basic principles are already on the market.
【０００３】しかしながら、これらの従来の酸素分析法
の場合には、いずれも次のような問題点がある。 〈ａ〉一般に、酸素元素の分析値の精度が低く、正確さ
が得られない。特に、酸素含有率１０％以下の試料の分
析誤差が大きく、それは±０．５％を越えることがあ
る。 〈ｂ〉有機化合物の種類によって熱分解特性が異なるた
め、酸素の分析値の検出感度に差が認められる。 〈ｃ〉酸素元素が含まれていない有機化合物から、１〜
５％の酸素が検出されることがある。However, each of these conventional oxygen analysis methods has the following problems. <a> In general, the accuracy of the analysis value of oxygen element is low and accuracy cannot be obtained. In particular, the analysis error of a sample having an oxygen content of 10% or less is large, which may exceed ± 0.5%. <B> Since the thermal decomposition characteristics differ depending on the type of organic compound, there is a difference in the detection sensitivity of the analysis value of oxygen. <C> From an organic compound containing no oxygen element, 1 to
5% oxygen may be detected.
【０００４】以上のような理由から、酸素分析法は長年
にわたる経緯を経た現在も、日常分析法として広く普及
するまでに至っていない。For the above reasons, the oxygen analysis method has not been widely used as a daily analysis method even after many years.
【０００５】[0005]
【発明が解決しようとする課題】この発明の発明者は、
有機化合物中の酸素元素の精度および正確さの優れた日
常分析法を確立することを目的とし、従来の酸素分析法
について詳細な基礎的検討を行った。その結果、前述の
問題点はすべて熱分解管の材質とその熱分解方法に起因
していることを見出した。The inventor of the present invention is
For the purpose of establishing a routine analysis method with excellent accuracy and precision of oxygen elements in organic compounds, detailed basic studies were conducted on conventional oxygen analysis methods. As a result, they have found that all of the above problems are caused by the material of the pyrolysis tube and its pyrolysis method.
【０００６】そして、石英ガラス製、黒鉛製および金属
製などの各種の熱分解管を試作し、多数の有機化合物の
熱分解特性を検討した。また、それぞれの熱分解管を用
いて黒鉛るつぼ、ニッケルるつぼおよび白金るつぼなど
による最適な熱分解条件を評価した。この発明は、以上
の研究の成果から完成されたものであり、従来の酸素分
析法の問題点を改良し、酸素元素の分析値の精度および
正確さを大きく向上させることのできる新しい熱分解管
と熱分解方法を提供することを目的としている。[0006] Various pyrolysis tubes made of quartz glass, graphite, metal, etc. were prototyped and the pyrolysis characteristics of many organic compounds were examined. In addition, the optimum pyrolysis conditions using graphite crucible, nickel crucible and platinum crucible were evaluated using each pyrolysis tube. The present invention has been completed from the results of the above research, and is a new pyrolysis tube capable of improving the problems of the conventional oxygen analysis method and greatly improving the accuracy and precision of the oxygen element analysis value. And is intended to provide a pyrolysis method.
【０００７】[0007]
【課題を解決するための手段】この発明は、上記の課題
を解決するものとして、金属製外管と、金属製外管の一
端に挿着された試料投入口を有する金属製ランス管と、
金属製外管に内接して配設された金属製カートリッジ型
反応管および金属製カートリッジ型反応管に充填された
一酸化炭素生成用反応試薬から構成されたことを特徴と
する酸素分析用金属製熱分解管を提供する。In order to solve the above-mentioned problems, the present invention provides a metal outer tube, a metal lance tube having a sample inlet inserted at one end of the metal outer tube,
A metal for oxygen analysis, characterized by comprising a metal cartridge type reaction tube arranged inscribed in a metal outer tube and a reaction reagent for carbon monoxide generation filled in the metal cartridge type reaction tube Provide a pyrolysis tube.
【０００８】また、この発明は、黒鉛るつぼおよび白金
るつぼなどを用いることなく、分析試料を上記の酸素分
析用金属製熱分解管の金属製カートリッジ型反応管内に
直接導入し、この反応管内に充填した一酸化炭素生成用
反応試薬の表面で直接接触熱分解する方法をも提供す
る。すなわち、たとえば図１に示したように、この発明
の金属製熱分解管は、ニッケルまたはその合金、白金ま
たはその合金、モリブデン、タングステン等の金属製外
管（１）に内接して、同様の金属または合金製の金属製
カートリッジ型反応管（３）を配設し、この反応管
（３）内には少量の一酸化炭素生成用反応試薬（白金炭
素、ニッケル、炭素、カーボンブラック等）（５）を充
填している。反応試薬（５）の出口側にはフィルター
（４）を配設し、一方、金属製外管（１）の一端には試
料投入口（６）を有する前記と同様の金属またはその合
金製の金属製ランス管（２）を挿着している。Further, according to the present invention, the analytical sample is directly introduced into the metal cartridge type reaction tube of the above-mentioned metal pyrolysis tube for oxygen analysis without using a graphite crucible and a platinum crucible, and the reaction tube is filled. There is also provided a method for direct catalytic thermal decomposition on the surface of the reaction reagent for producing carbon monoxide. That is, for example, as shown in FIG. 1, the metal pyrolysis tube of the present invention is inscribed in a metal outer tube (1) made of nickel or an alloy thereof, platinum or an alloy thereof, molybdenum, tungsten or the like, A metal or alloy metal cartridge type reaction tube (3) is arranged, and a small amount of a reaction reagent for producing carbon monoxide (platinum carbon, nickel, carbon, carbon black, etc.) ( 5) is filled. A filter (4) is provided on the outlet side of the reaction reagent (5), while a metal outer tube (1) has a sample inlet (6) at one end and is made of the same metal or alloy thereof as described above. A metal lance tube (2) is inserted.
【０００９】この金属製熱分解管を使用する時は、これ
を約１２００〜１３５０℃、より好適には１３００〜１
３２０℃に加熱し、ヘリウム等のキャリアーガス気流中
でランス管（２）の試料投入口（６）より、金属カプセ
ルに包み込んだ試料を投入する。ヘリウムの流量は、通
常、１５０〜２５０ｍｌ／ｍｉｎ程度、より好適には１
９０〜２１０ｍｌ／ｍｉｎとする。ヘリウムの他、キャ
リアーガスとして、アルゴン、窒素ガス等を用いてもよ
く、混合使用してもよい。ただ、ヘリウムがより好まし
い。なお、ヘリウムの流量は、一回の分析時間にも関係
するが、この発明の方法（迅速分析法）では約３分程度
でよい。試料カプセルは加熱されている白金炭素または
カーボンブラック等の反応試薬（５）の表面に落下し、
瞬間的に熱分解されると共に、定量的にＣＯを生成す
る。さらに、生成したＣＯをヘリウム等と共に熱分解管
から導出し、酸化管に移送してＣＯ2 に変換し、ＣＯ2
の濃度を検出して酸素の含有率を算出する。When the metal pyrolysis tube is used, it is heated to about 1200 to 1350 ° C., more preferably 1300 to 1 ° C.
It is heated to 320 ° C., and the sample encapsulated in a metal capsule is charged from the sample charging port (6) of the lance tube (2) in a carrier gas stream such as helium. The flow rate of helium is usually about 150 to 250 ml / min, and more preferably 1
90 to 210 ml / min. Other than helium, argon, nitrogen gas, or the like may be used as a carrier gas, or may be mixed and used. However, helium is more preferable. The flow rate of helium is related to one analysis time, but may be about 3 minutes in the method of the present invention (rapid analysis method). The sample capsule drops on the surface of the reaction reagent (5) such as heated platinum carbon or carbon black,
It is thermally decomposed instantaneously and CO is quantitatively produced. Furthermore, the generated CO derived from the pyrolysis tube with helium, and transferred to the oxidized tube was converted to CO 2, CO 2
The concentration of oxygen is detected to calculate the oxygen content.
【００１０】[0010]
【作用】この発明の熱分解管および熱分解方法において
は、以下の通りの特徴のある作用が実現される。 <i> 熱分解システム中に石英管または黒鉛管などを用
いないため、これらの管から二次的に発生したＣＯに起
因する分析誤差はなくなり、酸素含有率１０％以下の試
料も優れた精度および正確さで定量できる。In the thermal decomposition tube and the thermal decomposition method of the present invention, the following characteristic operations are realized. <i> Since no quartz tube or graphite tube is used in the pyrolysis system, there is no analysis error due to CO generated secondarily from these tubes, and samples with oxygen content of 10% or less have excellent accuracy. And can be quantified with accuracy.
【００１１】<ii> 白金るつぼまたは黒鉛るつぼなどの
中で熱分解することなく、白金炭素またはカーボンブラ
ックなどの反応試薬表面で試料を接触熱分解させること
により、試料の分子構造に基づく熱分解特性に依存する
ことなく、種々の有機化合物を同一の条件下で熱分解さ
せ、ＣＯに変換することができる。 <iii> 従って、酸素含有率４％〜５％の各種の有機化
合物の検出感度が一定になり、酸素元素の分析値の精度
および正確さが著しく向上する。<Ii> Pyrolysis characteristics based on the molecular structure of the sample by catalytically decomposing the sample on the surface of a reaction reagent such as platinum carbon or carbon black without thermally decomposing in a platinum crucible or a graphite crucible. It is possible to thermally decompose various organic compounds under the same conditions and convert them into CO, without depending on. <iii> Therefore, the detection sensitivity of various organic compounds having an oxygen content of 4% to 5% becomes constant, and the accuracy and precision of the analysis value of oxygen element are significantly improved.
【００１２】[0012]
【実施例】以下に、実施例を示し、さらに詳しくこの発
明について説明する。すなわち、図１に例示した金属製
外管（１）、ランス管（２）およびカートリッジ型反応
管（３）のいずれもニッケル製の熱分解管を１３００℃
（±２．５℃）に保持して、分析試料搬送用のヘリウム
流量を２００ｍｌ／ｍｉｎに設定した。ついで、銀製の
カプセル中に有機化合物１．５〜１．７ｍｇを量りとっ
てシールしたのち、試料投入口（６）よりカートリッジ
型反応管（３）に配設充填した一酸化炭素生成用の白金
炭素からなる反応試薬（５）表面上に投入して熱分解し
た。熱分解管で生成したＣＯはＨｅと共に金属製熱分解
管から導出し、酸化管に導きＣＯ2 に酸化したのち、Ｃ
Ｏ2 の濃度を赤外吸収検出器で検出して有機化合物中の
酸素元素の含有率を算出した。The present invention will be described in more detail with reference to the following examples. That is, all of the metal outer tube (1), the lance tube (2) and the cartridge type reaction tube (3) illustrated in FIG.
The temperature was maintained at (± 2.5 ° C.) and the flow rate of helium for conveying the analytical sample was set to 200 ml / min. Then, 1.5 to 1.7 mg of the organic compound is weighed and sealed in a silver capsule, and then platinum for carbon monoxide generation is arranged and filled in the cartridge type reaction tube (3) through the sample inlet (6). The reaction reagent (5) made of carbon was put on the surface and thermally decomposed. The CO generated in the pyrolysis tube is led out from the metal pyrolysis tube together with He, is led to an oxidation tube and is oxidized to CO 2 , and then C
The concentration of O 2 was detected by an infrared absorption detector, and the content rate of oxygen element in the organic compound was calculated.
【００１３】以上の方法で、各種の有機化合物中の酸素
を７回連続して分析し、その分析結果の一部を表１に示
した。Oxygen in various organic compounds was continuously analyzed seven times by the above method, and a part of the analysis results is shown in Table 1.
【００１４】[0014]
【表１】 [Table 1]
【００１５】表１は、アンチピリン（Ｏ＝８．５％）お
よびカフェイン（Ｏ＝１６．４８％）など２種類の有機
化合物を各々７回連続分析した場合の分析値と、その統
計量を示したものである。アンチピリン（Ｏ＝８．５
％）の平均酸素含有率は８．５４２％で平均分析誤差
０．０４２％と僅かに多いのみで、ばらつきの範囲は
０．２０１％、標準偏差は０．０７０７、変動係数０．
８２８０％であり、カフェイン（Ｏ＝１６．４８％）の
平均酸素含有率は１６．５２７％で平均分析誤差０．０
４７％、ばらつきの範囲は０．２６０％、標準偏差は
０．０８５８、変動係数０．５１９０％である。Table 1 shows the analytical values and the statistical values when the two kinds of organic compounds such as antipyrine (O = 8.5%) and caffeine (O = 16.48%) were continuously analyzed 7 times each. It is shown. Antipyrine (O = 8.5
%), The average oxygen content is 8.542% and the average analysis error is 0.042%, which is slightly large. The range of variation is 0.201%, the standard deviation is 0.0707, and the coefficient of variation is 0.
8280%, the average oxygen content of caffeine (O = 16.48%) is 16.527%, and the average analysis error is 0.0.
47%, the range of variation is 0.260%, the standard deviation is 0.0858, and the coefficient of variation is 0.5190%.
【００１６】従って、酸素含有率１０％以下のアンチピ
リンにおいても酸素含有率１６．４８％のカフェインと
劣ることなくいずれも良好な精度で酸素の含有率を測定
することができた。もちろん、この発明の方法は、表１
に示した分析例のみに限定されるものでなく、表１に示
した有機化合物のほかに２０種類の有機化合物について
も、酸素の含有率を測定しているが、いずれも精度およ
び正確さのすぐれた分析値が得られている。Therefore, even with antipyrine having an oxygen content of 10% or less, the oxygen content could be measured with good accuracy without being inferior to that of caffeine having an oxygen content of 16.48%. Of course, the method of the present invention is described in Table 1.
The oxygen content is measured not only for the analysis examples shown in Table 1 but also for 20 kinds of organic compounds in addition to the organic compounds shown in Table 1. Excellent analytical values are obtained.
【００１７】[0017]
【発明の効果】以上詳細に説明したとおり、この発明で
は、分析機器から発生するＣＯに起因する分析誤差がな
いので、有機化合物中の酸素含有率の多少にかかわりな
く、特に酸素含有率１０％以下にあっても、有機化合物
中の酸素元素を従来の方法よりすぐれた精度および正確
さで定量することができる。また、試料を直接接触熱分
解するので試料の分子構造に基づく熱分解特性に依存す
ることなく、種々の有機化合物を同一の条件下で熱分解
してＣＯに変換できる。従って、酸素含有率４％〜５％
の種々の有機化合物の検出感度が一定になり、酸素元素
の分析値の精度および正確さが著しく向上する。このこ
とは、有機化合物の元素組成に関する正確な情報が得ら
れる。As described in detail above, according to the present invention, since there is no analytical error due to CO generated from the analytical instrument, the oxygen content in the organic compound is 10%, regardless of the oxygen content. Even in the following cases, the oxygen element in the organic compound can be quantified with higher accuracy and precision than the conventional method. Further, since the sample is directly catalytically pyrolyzed, various organic compounds can be pyrolyzed and converted to CO under the same conditions without depending on the pyrolysis characteristics based on the molecular structure of the sample. Therefore, the oxygen content is 4% to 5%
The detection sensitivities of the various organic compounds described above become constant, and the accuracy and precision of the analysis value of oxygen element are significantly improved. This gives accurate information on the elemental composition of organic compounds.
【図１】この発明の酸素分析用の金属製熱分解管の断面
図である。FIG. 1 is a sectional view of a metal pyrolysis tube for oxygen analysis of the present invention.
１ 金属製外管 ２ 金属製ランス管 ３ 金属製カートリッジ型反応管 ４ フィルター ５ 反応試薬 ６ 試料投入口 1 metal outer tube 2 metal lance tube 3 metal cartridge type reaction tube 4 filter 5 reaction reagent 6 sample inlet
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成４年８月７日[Submission date] August 7, 1992
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】０００８[Correction target item name] 0008
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【０００８】また、この発明は、黒鉛るつぼおよび白金
るつぼなどを用いることなく、分析試料を上記の酸素分
析用金属製熱分解管の金属製カートリッジ型反応管内に
直接導入し、この反応管内に充填した一酸化炭素生成用
反応試薬の表面で直接接触熱分解する方法をも提供す
る。すなわち、たとえば図１に示したように、この発明
の金属製熱分解管は、ニッケルまたはその合金、白金ま
たはその合金、モリブデン、タングステン等の金属製外
管（１）に内接して、同様の金属または合金製の金属製
カートリッジ型反応管（３）を配設し、この反応管
（３）内には少量の一酸化炭素生成用反応試薬（白金炭
素、ニッケル炭素、カーボンブラック等）（５）を充填
している。反応試薬（５）の出口側にはフィルター
（４）を配設し、一方、金属製外管（１）の一端には試
料投入口（６）を有する前記と同様の金属またはその合
金製の金属製ランス管（２）を挿着している。Further, according to the present invention, the analytical sample is directly introduced into the metal cartridge type reaction tube of the above-mentioned metal pyrolysis tube for oxygen analysis without using a graphite crucible and a platinum crucible, and the reaction tube is filled. There is also provided a method for direct catalytic thermal decomposition on the surface of the reaction reagent for producing carbon monoxide. That is, for example, as shown in FIG. 1, the metal pyrolysis tube of the present invention is inscribed in a metal outer tube (1) made of nickel or an alloy thereof, platinum or an alloy thereof, molybdenum, tungsten or the like, A metal cartridge type reaction tube (3) made of metal or alloy is arranged, and a small amount of a reaction reagent for producing carbon monoxide (platinum carbon, nickel carbon , carbon black, etc.) (5) is provided in the reaction tube (3). ) Is filled. A filter (4) is provided on the outlet side of the reaction reagent (5), while a metal outer tube (1) has a sample inlet (6) at one end and is made of the same metal or alloy thereof as described above. A metal lance tube (2) is inserted.
Claims (4)
された試料投入口を有する金属製ランス管と、金属製外
管に内接して配設された金属製カートリッジ型反応管お
よび金属製カートリッジ型反応管に充填された一酸化炭
素生成用反応試薬から構成されたことを特徴とする酸素
分析用熱分解管。1. A metal outer tube, a metal lance tube having a sample inlet inserted at one end of the metal outer tube, and a metal cartridge type reaction arranged inscribed in the metal outer tube. A pyrolysis tube for oxygen analysis, comprising a tube and a reaction reagent for producing carbon monoxide filled in a metal cartridge type reaction tube.
るいはカーボンブラックのいずれかであることを特徴と
する請求項１の酸素分析用熱分解管。2. The pyrolysis tube for oxygen analysis according to claim 1, wherein the reaction reagent for producing carbon monoxide is either platinum carbon or carbon black.
化炭素に変換し、この一酸化炭素を酸化管に移送し二酸
化炭素に酸化してその濃度を検出して酸素の含有率を算
出する方法において、分析試料を酸素分析用金属製熱分
解管の金属製カートリッジ型反応管内に直接導入してこ
の反応管内に充填した一酸化炭素生成用反応試薬の表面
で直接接触熱分解させることを特徴とする酸素分析用熱
分解方法。3. An oxygen content is calculated by thermally decomposing an analytical sample to convert an oxygen compound into carbon monoxide, transferring this carbon monoxide to an oxidation tube, oxidizing it to carbon dioxide, and detecting its concentration. In the method described above, the analysis sample is directly introduced into the metal cartridge-type reaction tube of the metal pyrolysis tube for oxygen analysis, and direct catalytic thermal decomposition is carried out on the surface of the reaction reagent for carbon monoxide generation filled in the reaction tube. Characteristic thermal decomposition method for oxygen analysis.
ウム気流で搬送して金属製カートリッジ型反応管内に直
接投入することを特徴とする請求項３に記載の方法。4. The method according to claim 3, wherein the analysis sample is wrapped in a metal capsule, conveyed by a helium flow, and directly introduced into a metal cartridge type reaction tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16301492A JP3205594B2 (en) | 1992-06-22 | 1992-06-22 | Metal pyrolysis tube for oxygen analysis and its pyrolysis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16301492A JP3205594B2 (en) | 1992-06-22 | 1992-06-22 | Metal pyrolysis tube for oxygen analysis and its pyrolysis method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH063352A true JPH063352A (en) | 1994-01-11 |
| JP3205594B2 JP3205594B2 (en) | 2001-09-04 |
Family
ID=15765559
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16301492A Expired - Fee Related JP3205594B2 (en) | 1992-06-22 | 1992-06-22 | Metal pyrolysis tube for oxygen analysis and its pyrolysis method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3205594B2 (en) |
-
1992
- 1992-06-22 JP JP16301492A patent/JP3205594B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JP3205594B2 (en) | 2001-09-04 |
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