JPH0331762A - Method for decomposing solid sample - Google Patents
Method for decomposing solid sampleInfo
- Publication number
- JPH0331762A JPH0331762A JP16533889A JP16533889A JPH0331762A JP H0331762 A JPH0331762 A JP H0331762A JP 16533889 A JP16533889 A JP 16533889A JP 16533889 A JP16533889 A JP 16533889A JP H0331762 A JPH0331762 A JP H0331762A
- Authority
- JP
- Japan
- Prior art keywords
- combustion
- section
- solid sample
- gas
- 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.)
- Pending
Links
- 239000007787 solid Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000002485 combustion reaction Methods 0.000 claims abstract description 65
- 239000007789 gas Substances 0.000 claims abstract description 35
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 16
- 239000011261 inert gas Substances 0.000 claims abstract description 15
- 230000008016 vaporization Effects 0.000 claims description 30
- 238000009834 vaporization Methods 0.000 claims description 27
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 18
- 229910001882 dioxygen Inorganic materials 0.000 claims description 18
- 238000002844 melting Methods 0.000 claims description 10
- 230000008018 melting Effects 0.000 claims description 10
- 238000001816 cooling Methods 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 3
- 239000001301 oxygen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 238000001704 evaporation Methods 0.000 abstract 4
- 238000012790 confirmation Methods 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- 239000004449 solid propellant Substances 0.000 abstract 1
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 14
- 238000010521 absorption reaction Methods 0.000 description 11
- 239000010453 quartz Substances 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 10
- 229910052786 argon Inorganic materials 0.000 description 7
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- 239000011593 sulfur Substances 0.000 description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
- 238000003780 insertion Methods 0.000 description 4
- 230000037431 insertion Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 3
- 229910052794 bromium Inorganic materials 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 239000004071 soot Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 101100020289 Xenopus laevis koza gene Proteins 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 238000010000 carbonizing Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000000567 combustion gas Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- -1 polybutylene terephthalate Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- YPNVIBVEFVRZPJ-UHFFFAOYSA-L silver sulfate Chemical compound [Ag+].[Ag+].[O-]S([O-])(=O)=O YPNVIBVEFVRZPJ-UHFFFAOYSA-L 0.000 description 1
- 229910000367 silver sulfate Inorganic materials 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000004454 trace mineral analysis Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
Landscapes
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、固体試料を段階的に完全に燃焼分解させ、ガ
ス分析装置に供給可能な形態に変換する方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for completely combusting and decomposing a solid sample in stages and converting it into a form that can be supplied to a gas analyzer.
（従来の技術）
従来、固体試料中の窒素や硫黄などの元素を分析する方
法は、固体試料の分解燃焼による生成ガスを回収し、該
ガス成分をそれぞれの分析器で分析する手法がとられて
いる。第２図は、固体試料の分解装置の概念図である。(Prior Art) Conventionally, the method of analyzing elements such as nitrogen and sulfur in a solid sample has been to recover the gas produced by decomposition and combustion of the solid sample, and analyze the gas components using respective analyzers. ing. FIG. 2 is a conceptual diagram of a solid sample decomposition device.
この装置は、ガス供給口１がら不活性ガスを、ガス供給
口６から酸素ガスをそれぞれ流し、加熱炉８を８５０〜
９００℃に温度コントロールしておき、予め、試料用ボ
ート（以下単にボートという）３を秤量し、これに固体
試料を入れて＋ｑび秤量した後、挿入口２より石英管４
内に挿入し、加熱炉８の人口５まで該ボートを移動し、
この位置で固体試料の揮発・分解状態を観察しながら、
加熱炉の余熱によって徐々に揮発させ、その後、ボート
３を加熱炉８の中央の燃焼部７まで移動させ、しばらく
その状態を保持した後、ガス供給口１から供給する不活
性ガスを酸素ガスに切り換えて燃焼分解させ、ガス供給
口６から供給される酸素ガスにより、最終的に完全燃焼
させる。燃焼生成ガスは燃焼管４の出口に接続された吸
収瓶９の吸収液に捕捉される。この吸収液は種々の検出
手段、例えばイオンクロマト法、滴定法等の手段により
目的物質の検出が行われる。In this device, an inert gas is supplied through a gas supply port 1, and oxygen gas is supplied through a gas supply port 6, and a heating furnace 8 is
The temperature is controlled at 900°C, a sample boat (hereinafter simply referred to as a boat) 3 is weighed, a solid sample is placed in it and weighed, and then the quartz tube 4 is inserted through the insertion port 2.
and move the boat to population 5 of heating furnace 8,
While observing the volatilization and decomposition state of the solid sample at this position,
It is gradually volatilized by the residual heat of the heating furnace, and then the boat 3 is moved to the combustion part 7 in the center of the heating furnace 8, and after maintaining that state for a while, the inert gas supplied from the gas supply port 1 is converted into oxygen gas. The gas is switched to combustion and decomposition, and is finally completely combusted by the oxygen gas supplied from the gas supply port 6. The combustion product gas is captured in an absorption liquid in an absorption bottle 9 connected to the outlet of the combustion tube 4. The target substance in this absorption liquid is detected by various detection means such as ion chromatography and titration.
（発明が解決しようとする課題）
−１−、記の固体試料の分解方法では、高温に保持され
た加熱炉の人口に、固体試料を収容したボートをゆっく
りと近付け、試料の揮発・分解状態を観察しながら、加
熱炉中に固体試料を移動する時期を判断するという、分
析者の経験に依存して分析が行われていた。この分析操
作が少しでも早すぎると不完全燃焼を起こし、固体試料
中の目的成分を回収することができない。また、多ｊｉ
１の試寥ｌを」二３己の分角り方法で処理することは、
」−記の分析操作が一層複雑になり、不完全燃焼を避け
ることが極めて難しい。従って、微量分析への適用が困
難であった。(Problems to be Solved by the Invention) In the method for decomposing a solid sample described in -1-, a boat containing a solid sample is slowly brought close to a heating furnace maintained at a high temperature, and the sample is in a state of volatilization and decomposition. Analyzes depend on the experience of the analyst to determine when to move the solid sample into the heating furnace while observing the If this analysis operation is performed even slightly too quickly, incomplete combustion will occur, making it impossible to recover the target component in the solid sample. Also, many
Processing the first trial using my own method is,
”-The analytical operations described above become even more complicated, and it is extremely difficult to avoid incomplete combustion. Therefore, it has been difficult to apply it to trace analysis.
本発明は、」−記の欠点を解消し、多量の固体試料を完
全に分解燃焼させることができる分解方法を堤供しよう
とするものである。The present invention aims to solve the above drawbacks and provide a decomposition method that can completely decompose and burn a large amount of solid samples.
（課題を解決するための手段）
本発明は、固体試料を段階的に分解し、燃焼生成ガスを
回収する方法において、固体試料を分解装置の気化部に
セットし、該気化部に続く燃焼部に酸素ガスを流しなが
ら、燃焼操作の最高温度に保持し、まず、該気化室に不
活性ガスを流しながら、」１記の固体、、ｔ： ｊ’ｌ
をその融点ないし融点より５０℃高い温度まで、比較的
高い昇温速度で加熱し、必要に応じて、該温度に一定時
間保持した後、−に記昇湿速度より緩やかな昇温速度で
加熱を続け、その間、燃焼部における揮発成分の燃焼の
終ｒを確認した後、」−配気化部に供給する不活性ガス
を酸素ガスに切り換えて、不揮発成分を徐々に分解し、
最終的に試料を完全に燃焼させた後、」ユ記気化部にｔ
ｌｌび不活性ガスを供給して室温まで冷却することを特
徴とする固体試料の分解方法である。(Means for Solving the Problems) The present invention provides a method for decomposing a solid sample in stages and recovering combustion generated gas, in which a solid sample is set in a vaporization section of a decomposition device, and a combustion section following the vaporization section is provided. While flowing oxygen gas into the chamber, the temperature is maintained at the maximum temperature for combustion operation, and first, while flowing an inert gas into the vaporization chamber, the solid of ``1'', t: j'l
to its melting point or a temperature 50°C higher than the melting point at a relatively high rate of temperature increase, and if necessary, after holding at that temperature for a certain period of time, heat at a rate of temperature increase slower than the rate of humidity increase described in -. In the meantime, after confirming the completion of combustion of volatile components in the combustion section, the inert gas supplied to the air distribution section is switched to oxygen gas to gradually decompose the non-volatile components,
Finally, after completely burning the sample, the
This is a method for decomposing a solid sample, which is characterized by supplying an inert gas and cooling it to room temperature.
（作用）
第１図は、本発明を実施するための分解装置の概念図で
ある。この装置は、気化部５に昇温パターンをプログラ
ムすることのできる加熱炉ｌＯと燃焼部７に８５０〜９
００℃の燃焼温度を保持することのできる加熱炉８をイ
ーｆし、石英管４がそれらを貞通させたものであり、気
化部５の上流にガス供給口ｌと試料挿入口２を設け、気
化部用の加熱炉１０には冷却装置１１及び加熱炉コント
ロール装置１２が付設されている。また、燃焼部７には
酸素ガス供給１」６が設けられ、燃焼部の下流には燃焼
生成ガスを捕捉するための吸収瓶９が接続されている。(Operation) FIG. 1 is a conceptual diagram of a disassembly apparatus for carrying out the present invention. This device has a heating furnace lO in which a temperature increase pattern can be programmed in the vaporization part 5, and a combustion part 7 in which the
A heating furnace 8 capable of maintaining a combustion temperature of 00° C. is installed, and a quartz tube 4 is made to pass through them, and a gas supply port 1 and a sample insertion port 2 are provided upstream of the vaporization section 5. A cooling device 11 and a heating furnace control device 12 are attached to the heating furnace 10 for the vaporizing section. Further, the combustion section 7 is provided with an oxygen gas supply 1'' 6, and an absorption bottle 9 for capturing combustion generated gas is connected downstream of the combustion section.
固体試料の分解方法の手順を説明すると、ガス供給［コ
１から石英管４にアルゴン等の不活性ガスを流し、燃焼
部の加熱炉８を燃焼湿度に保持し、供給１１６から酸素
ガスを供給し、加熱炉８の温度を安定させてから、燃焼
生成ガスを捕捉するための吸収液を適用収容した吸収瓶
９を、石英管４の出１コに接続する。次に、固体試料を
ボート３にＩ・ｒ呈して挿入口２から石英管４内に挿入
し、該ボートを気化部５に移動する。加熱炉１０のコン
トロール装置Ｉ２に対し、打潟パターンのプログラムを
セットし、スタートボタンを押して４温を開始する。固
体試料の融点若しくは融点より５０℃高い温度まで比較
的急な昇温速度で気化部５を加熱し、その後は比較的緩
やかな昇温速度で加熱する。昇温速度は、分解対象であ
る固体試料によって異なるが、固体試料の融点ないし融
点より５０″Ｃ高い温度まで加熱する時の昇温速度は、
５０〜ｂ
〜ｂ
温速度は、前段の昇温速度より小さい昇温速度で、例え
ば、５〜ｂ
気化部５で気化されたガスは、燃焼部７に送られ、ガス
供給口６からの酸素ガスにより燃焼される。燃焼生成ガ
スは燃焼部から吸収瓶９に送られ捕捉される。燃焼部に
おいて、揮発性成分の燃焼の終了を確認してから、ガス
供給口１からの不活性ガスを酸素ガスに切り換え、ボー
ト３内の不揮発性成分を完全に燃焼させる。固体試料か
らの揮発性成分の抜けは、燃焼部の炎の消失を目視する
ことにより、容易に確認することができる。固体試料が
完全に燃焼したことを確認してから、加熱炉１０の加熱
を停止し、ガス供給口１から再び不活性ガスを流し、加
熱炉１０の冷却装置１１を作動させて気化部５内の温度
を室温まで下げ、試料挿入１コ２に該ボート３を戻して
分析を終了する。To explain the steps of the method for decomposing a solid sample, an inert gas such as argon is flowed from the gas supply 1 to the quartz tube 4, the heating furnace 8 in the combustion section is maintained at combustion humidity, and oxygen gas is supplied from the supply 116. After stabilizing the temperature of the heating furnace 8, an absorption bottle 9 containing an absorption liquid for trapping combustion generated gas is connected to one outlet of the quartz tube 4. Next, the solid sample is transferred to the boat 3 and inserted into the quartz tube 4 through the insertion port 2, and the boat is moved to the vaporization section 5. A program for the wafer pattern is set in the control device I2 of the heating furnace 10, and the start button is pressed to start 4-heating. The vaporization section 5 is heated at a relatively rapid rate of temperature increase to the melting point of the solid sample or a temperature 50° C. higher than the melting point, and then heated at a relatively slow rate of temperature increase. The rate of temperature increase varies depending on the solid sample to be decomposed, but the rate of temperature increase when heating to the melting point of the solid sample or a temperature 50"C higher than the melting point is:
50~b~b The temperature rate is lower than the temperature increase rate of the previous stage, for example, 5~b The gas vaporized in the vaporization section 5 is sent to the combustion section 7, and the oxygen from the gas supply port 6 is Burned by gas. The combustion generated gas is sent from the combustion section to the absorption bottle 9 and captured. In the combustion section, after confirming the completion of combustion of the volatile components, the inert gas from the gas supply port 1 is switched to oxygen gas, and the nonvolatile components in the boat 3 are completely combusted. The removal of volatile components from the solid sample can be easily confirmed by visually observing the disappearance of the flame in the combustion section. After confirming that the solid sample has completely burned, the heating of the heating furnace 10 is stopped, the inert gas is supplied again from the gas supply port 1, and the cooling device 11 of the heating furnace 10 is activated to cool down the inside of the vaporization section 5. The temperature of the boat 3 is lowered to room temperature, and the boat 3 is returned to the sample insertion boat 1 2 to complete the analysis.
このように本発明では、固体試料の融点を１つの指標に
して、主に揮発性成分を分離する１１１１段を比較約２
な昇温パターンで短時間で′加熱骨Ｍし、後段は不揮発
性成分の不完全燃焼を避けるために比較的績やかな昇温
パターンで加熱し、燃焼部における揮発性成分の燃焼を
確認してから、気化部に酸素ガスを供給して不揮発成分
の燃焼を行うもので、固体試料の分解燃焼状態に合わせ
て段階的に燃焼させるため、例えば、ＩｇａＫの多量の
固体試料についても完全に燃焼分解させることができる
ようになった。また、気化部側熱炉を昇温パターンのプ
ログラムに従ってコントロールし、燃焼部の揮発性成分
の燃焼の終了をセンサー笠により検知して不活性ガスか
ら酸素ガスへの切り換えを行うことにより、分析操作を
自動化することが可能となった。In this way, in the present invention, the melting point of the solid sample is used as an indicator, and the 1111 stage, which mainly separates volatile components, is compared with about 2
The bones were heated in a short period of time with a moderate temperature increase pattern, and the latter stage was heated with a relatively gentle temperature increase pattern to avoid incomplete combustion of non-volatile components, and the combustion of volatile components in the combustion section was confirmed. After that, oxygen gas is supplied to the vaporization section to burn the non-volatile components.The combustion is performed in stages according to the decomposition and combustion state of the solid sample, so for example, even a large amount of solid sample of IgaK can be completely burned. Now it can be disassembled. In addition, the heating furnace on the vaporizing section side is controlled according to the temperature increase pattern program, and a sensor cap detects the end of combustion of volatile components in the combustion section, and the switch from inert gas to oxygen gas is performed. It has become possible to automate.
（実施例１）
第１図の装置を用い、三菱化成製高密度ポリエチレン（
商品名二ノパテブクＩ’：５３０Ｇ）を０．５ｇ石英製
ボートに採取し、次の燃焼条件で分解試験を行った。ま
ず、燃焼部に酸素ガスを３００ｍ１／ｓｉｎで導入し、
該燃焼部の加熱炉を８００℃に加熱して安定するのを待
って、気化部にアルゴンガスを４００ｍ１／鳳ｉｎで流
し、上記のボートを気化部にセットする。次いで、気化
部を第１段の昇温速度１５０℃／ｓｉｎで４９０℃まで
昇ｉＪ Ｌ／、６分間保持した後、第２段の昇温速度０
７５℃／ｓｉｎで８００℃まで昇温し、この間、７００
℃において揮発性成分の燃焼の終了を確認し、気化部へ
の供給ガスをアルゴンガスから３００ｍ１／ｓｉｎの酸
素ガスに切り換え、８００℃で２分間保持して固体試料
を燃焼させた。この間、ボート中に不完全燃焼を示すス
スの付着もなく、最終的に固体試料が完全に燃焼したこ
とも確認された。燃焼分解時間は全体で１５分であった
。(Example 1) Using the apparatus shown in Figure 1, high-density polyethylene manufactured by Mitsubishi Kasei (
0.5 g of Ninopate Buku I' (trade name: 530G) was collected in a quartz boat, and a decomposition test was conducted under the following combustion conditions. First, oxygen gas is introduced into the combustion section at a rate of 300 m1/sin,
After heating the heating furnace of the combustion section to 800° C. and waiting for it to stabilize, argon gas was flowed into the vaporization section at a rate of 400 ml/in, and the above-mentioned boat was set in the vaporization section. Next, the vaporizing section was raised to 490°C at a temperature increase rate of 150°C/sin in the first stage, and held for 6 minutes, and then the temperature increase rate in the second stage was increased to 0.
The temperature was raised to 800°C at a rate of 75°C/sin, and during this time, the
After confirming the completion of combustion of the volatile components at 800° C., the gas supplied to the vaporization section was switched from argon gas to oxygen gas at 300 ml/sin, and the temperature was held at 800° C. for 2 minutes to burn the solid sample. During this time, there was no soot attached to the boat indicating incomplete combustion, and it was confirmed that the solid sample had finally been completely burned. The total combustion decomposition time was 15 minutes.
（実施例２）
第１図の装置を用い、水添ピッチ０．５ｇを石英製ボー
トに収容し、硫黄の分析を行った。(Example 2) Using the apparatus shown in FIG. 1, 0.5 g of hydrogenated pitch was placed in a quartz boat, and sulfur was analyzed.
まず、燃焼部に酸素ガスを３００■ｌ／ｓｉｎで導入し
、該燃焼部の加熱炉を９００℃に加熱して安定するのを
待って、気化部にアルゴンガスを４００ｓｌ／ｓｉｎで
流し、上記のボートを気化部にセ−ｙ）した。次いで、
気化部を第１段の昇温速度１５０℃／−１ｎで３７０℃
まで昇温し、第２段の昇温速度５℃／−ｉｎで５５０℃
まで昇温し、第３段の昇温速度２０℃／＋ｓｉｎで７０
０℃まで昇温し、第４段で昇温速度１００℃／ｇ＋ｉｎ
で９００℃まで昇温し、その温度で３分間保持して固体
試料を燃焼させた。この間、第２段でピッチが溶けて炭
化する状況が観察され、７００℃において揮発性成分の
燃焼の終了を確認し、気化部への供給ガスをアルゴンガ
スから酸素ガスに切り換えたところ、第３段で炭化物が
燃焼する状況が観察された。この間、ボート中に不完全
燃焼を示すススの付ｎもなく、最終的に固体試料が完全
に燃焼したことも確認された。石英管の下流に接続した
吸収瓶には、０．３％の過酸化水素溶液を１５ｍ１収容
して、燃焼生成ガスを吸収させ、該吸収液に水を加えて
を１００ｍ１に定容してイオンクロマトグラフで分析し
たところ、硫黄の含ｆｒ量は０．３７％であった。First, oxygen gas is introduced into the combustion section at 300 sl/sin, the heating furnace of the combustion section is heated to 900°C, wait until it becomes stable, argon gas is flowed into the vaporization section at 400 sl/sin, and the above A boat was placed in the vaporization section. Then,
The vaporization section was heated to 370°C at a heating rate of 150°C/-1n in the first stage.
The temperature was increased to 550°C at a heating rate of 5°C/-in in the second stage.
The temperature was raised to 70°C at the third stage heating rate of 20°C/+sin.
Raise the temperature to 0℃ and increase the temperature at the 4th stage to 100℃/g+in.
The temperature was raised to 900° C. and held at that temperature for 3 minutes to burn the solid sample. During this time, it was observed that the pitch was melting and carbonizing in the second stage, and after confirming that the combustion of volatile components had finished at 700°C, the gas supplied to the vaporization section was switched from argon gas to oxygen gas. A situation where carbide was burned in the stage was observed. During this time, there was no soot in the boat indicating incomplete combustion, and it was confirmed that the solid sample had finally been completely burned. An absorption bottle connected downstream of the quartz tube contains 15 ml of 0.3% hydrogen peroxide solution to absorb combustion generated gas, and water is added to the absorption liquid to make a constant volume of 100 ml to absorb ions. Chromatographic analysis showed that the sulfur content was 0.37%.
同時に、従来の有機元素分析法（Ｄ本化学会編「実験化
学高座第１６巻有機化合物の分析方法Ｊ昭和３９年３月
１０１１発行）により、」二記水１おピッチの硫黄含有
量を分析した。銅粒を充填した吸収瓶を上記燃焼管の出
口に接続し、硫黄成分を硫酸銀として該銅粒に捕捉し、
東ｉｔ差測定により分析したところ、硫黄の含有量は０
３８％で、両者の測定値はよく一致していた。At the same time, the sulfur content of 1 pitch of water was analyzed using the conventional organic elemental analysis method (edited by the Chemical Society of Japan, "Jikken Kagaku Koza Vol. 16, Methods of Analyzing Organic Compounds J, Published March 1011, March 1960)". did. An absorption bottle filled with copper grains is connected to the outlet of the combustion tube, and the sulfur component is captured in the copper grains as silver sulfate,
When analyzed by TOIT difference measurement, the sulfur content was 0.
The two measurements were in good agreement at 38%.
（実施例３）
第１図の装置を用い、試料はバイエル社製ポカント４３
２５（ポリブチレンテレフタレート）を０．５１１ｇ石
英製ボートに収容し、次の燃焼部（’Ｉ＝で分解処理し
、燃焼生成ガスから臭素を分析した。まず、燃焼部に酸
素ガスを１５０ｍ１／ｓｉｎで導入し、該燃焼部の加熱
炉を９００℃に加熱して安定するのを待って、気化部に
アルゴンガスを２００ｍ１／ｓｉｎで流し、」二Ｊ己の
ボートを気化部にセットした。次いで、気化部を第１段
のシフ、 Ｎ速度１５０”Ｃ／ｓｉｎで４００℃まで昇
温し、６分間保持した後、第２段の昇温速度７５℃／ｓ
ｉｎで９００℃までＢ ｉシし、この間、７００℃にお
いて揮発性成分の燃焼の終了を確認し、気化部への供給
ガスをアルゴンガスから１５０ｍ１／ｓｉｎの酸素ガス
に切り換え、９００℃で３分１ｊｌ保持して固体試料を
燃焼させた。この間、ボート中に不完全燃焼を示すスス
の付着もなく、最終的に固体試料が完全に燃焼したこと
も確認された。石英管の下流に接続した吸収瓶には、０
．３％の過酸化水素を２０園１収容し、燃焼生成ガスを
吸収させ、該吸収液に水を加えてを１００ｓｌに定容し
てイオンクロマトグラフで臭素を検出した。その結果、
臭素の分析値は５．５８％であった。同時に同一試料を
従来の有機元素分析法である銅粒の！Ｉｔ ｌｉｔ増加
より求める方法で分析したところ、分析値は５．３７％
で両者の値はよく一致した。燃焼分解時間は全体で１８
分と短時間であった。(Example 3) Using the apparatus shown in Figure 1, the sample was Pocanto 43 manufactured by Bayer.
0.511 g of 25 (polybutylene terephthalate) was placed in a quartz boat and decomposed in the next combustion section ('I=), and bromine was analyzed from the combustion generated gas. First, oxygen gas was introduced into the combustion section at a rate of 150 m1/sin. After heating the heating furnace of the combustion section to 900°C and waiting for it to stabilize, argon gas was flowed into the vaporization section at a rate of 200 m1/sin, and two J's boats were set in the vaporization section. , the vaporization section was heated to 400°C at a first stage schiff, N rate of 150"C/sin, held for 6 minutes, and then heated at a second stage temperature increase rate of 75°C/s.
During this time, the completion of combustion of the volatile components was confirmed at 700°C, and the gas supplied to the vaporization section was switched from argon gas to oxygen gas at 150 m1/sin, and heated at 900°C for 3 minutes. The solid sample was burned by holding 1 jl. During this time, there was no soot attached to the boat indicating incomplete combustion, and it was confirmed that the solid sample had finally been completely burned. The absorption bottle connected downstream of the quartz tube contains 0
．． 3% hydrogen peroxide was placed in a container containing 20 liters of hydrogen peroxide to absorb combustion gas, water was added to the absorbent solution to make a constant volume of 100 sl, and bromine was detected using an ion chromatograph. the result,
The analytical value of bromine was 5.58%. At the same time, the same sample was analyzed using the conventional organic elemental analysis method of copper grains! When analyzed using the method calculated from It lit increase, the analysis value was 5.37%.
The two values were in good agreement. Total combustion decomposition time is 18
It took only a few minutes.
（発明の効果）
不発１１，１よ、］２記。構成、採用ｔ６ｏと（２孕り
、多量の固体試料を比較的短時間で完全に燃焼させるこ
とができ、その後の分析精度の向」−に大きく寄与する
ものである。(Effect of the invention) Misfire 11, 1,] 2. The configuration and adoption of this method make it possible to completely burn a large amount of solid samples in a relatively short period of time, greatly contributing to the improvement of subsequent analytical accuracy.
４、図面のｉｎ ｌｉｔな説明
第１図は本発明を実施するための固体試料分解装置の概
念図であり、第２図は従来の固体試料分解装置の概念図
である。4. In-lit explanation of the drawings FIG. 1 is a conceptual diagram of a solid sample decomposition apparatus for carrying out the present invention, and FIG. 2 is a conceptual diagram of a conventional solid sample decomposition apparatus.
１．６・・・ガス供給【」、３・・・試料用ボート。1.6...Gas supply ['', 3...Sample boat.
４・・・７１芙管、５・・・気化部、７・・・燃焼部。4...71 tubes, 5...vaporization section, 7...combustion section.
８．１０・・・加熱炉。8.10...Heating furnace.
Claims (1)
にセットし、該気化部に続く燃焼部に酸素ガスを流しな
がら、燃焼操作の最高温度に保持し、まず、該気化室に
不活性ガスを流しながら、上記の固体試料をその融点な
いし融点より５０℃高い温度まで、比較的高い昇温速度
で加熱し、必要に応じて、該温度に一定時間保持した後
、上記昇温速度より緩やかな昇温速度で加熱を続け、そ
の間、燃焼部における揮発成分の燃焼の終了を確認した
後、上記気化部に供給する不活性ガスを酸素ガスに切り
換えて、不揮発成分を徐々に分解し、最終的に試料を完
全に燃焼させた後、上記気化部に再び不活性ガスを供給
して室温まで冷却することを特徴とする固体試料の分解
方法。[Claims] In a method of decomposing a solid sample in stages and recovering combustion generated gas, the solid sample is set in a vaporization section of a decomposition device, and while oxygen gas is flowing into a combustion section following the vaporization section, While maintaining the maximum temperature of the combustion operation, first, while flowing an inert gas into the vaporization chamber, the above-mentioned solid sample is heated at a relatively high heating rate to its melting point or a temperature 50°C higher than the melting point, and as necessary. Accordingly, after maintaining the temperature for a certain period of time, heating is continued at a temperature increase rate slower than the above temperature increase rate, and after confirming the completion of combustion of the volatile components in the combustion section, the inert gas supplied to the vaporization section is The method is characterized in that the active gas is switched to oxygen gas to gradually decompose the non-volatile components, and after the sample is finally completely combusted, the inert gas is again supplied to the vaporization section to cool it to room temperature. Method for decomposing solid samples.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16533889A JPH0331762A (en) | 1989-06-29 | 1989-06-29 | Method for decomposing solid sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP16533889A JPH0331762A (en) | 1989-06-29 | 1989-06-29 | Method for decomposing solid sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0331762A true JPH0331762A (en) | 1991-02-12 |
Family
ID=15810440
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP16533889A Pending JPH0331762A (en) | 1989-06-29 | 1989-06-29 | Method for decomposing solid sample |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0331762A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012163545A (en) * | 2011-01-17 | 2012-08-30 | Ayako Sato | Low-temperature combustion type analysis and measurement system depending upon metal catalyst effect |
| JP2013173116A (en) * | 2012-02-27 | 2013-09-05 | Sumitomo Osaka Cement Co Ltd | Apparatus and method for removing volatile substance |
| JP2015210111A (en) * | 2014-04-24 | 2015-11-24 | 株式会社三菱化学アナリテック | Nitrogen analysis method |
| JP2016003896A (en) * | 2014-06-14 | 2016-01-12 | 佐藤 綾子 | Heat separation type ch analysis measurement system in transparent heating furnace |
| JP2017102101A (en) * | 2015-11-20 | 2017-06-08 | 株式会社日立ハイテクサイエンス | Evolved gas analysis device and evolved gas analysis method |
-
1989
- 1989-06-29 JP JP16533889A patent/JPH0331762A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012163545A (en) * | 2011-01-17 | 2012-08-30 | Ayako Sato | Low-temperature combustion type analysis and measurement system depending upon metal catalyst effect |
| JP2013173116A (en) * | 2012-02-27 | 2013-09-05 | Sumitomo Osaka Cement Co Ltd | Apparatus and method for removing volatile substance |
| JP2015210111A (en) * | 2014-04-24 | 2015-11-24 | 株式会社三菱化学アナリテック | Nitrogen analysis method |
| JP2016003896A (en) * | 2014-06-14 | 2016-01-12 | 佐藤 綾子 | Heat separation type ch analysis measurement system in transparent heating furnace |
| JP2017102101A (en) * | 2015-11-20 | 2017-06-08 | 株式会社日立ハイテクサイエンス | Evolved gas analysis device and evolved gas analysis method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Butcher | Recent advances in optical analytical atomic spectrometry | |
| Průša et al. | Ultratrace determination of tin by hydride generation in-atomizer trapping atomic absorption spectrometry | |
| Darke et al. | Review of solid sample introduction for plasma spectrometry and a comparison of results for laser ablation, electrothermal vaporization, and slurry nebulization | |
| US4916077A (en) | Method and apparatus for oxidative decomposition and analysis of a sample | |
| US4833322A (en) | Method and apparatus for analysis of material | |
| Levine et al. | Evaluation of a high-pressure, high-temperature microwave digestion system | |
| JPH0331762A (en) | Method for decomposing solid sample | |
| Frentiu et al. | Sono-induced cold vapour generation interfaced with capacitively coupled plasma microtorch optical emission spectrometry: Analytical characterization and comparison with atomic fluorescence spectrometry | |
| Lundgren et al. | A temperature-controlled graphite tube furnace for the determination of trace metals in solid biological tissue | |
| Krata et al. | Critical evaluation of analytical performance of atomic absorption spectrometry and inductively coupled plasma mass spectrometry for mercury determination | |
| JP2781013B2 (en) | Solid sample decomposition method | |
| Bazan | Enhancement of osmium detection in inductively coupled plasma atomic emission spectrometry | |
| JP2003302316A (en) | Oil analyzing-method and oil analyzer | |
| Tsalev et al. | Electrothermal atomisation atomic absorption spectrometric determination of inorganic and methylated arsenic after pre-concentration by hydride generation and trapping the hydrides in a cerium (IV)-iodide absorbing solution | |
| JP4849010B2 (en) | Method of burning sample for analysis | |
| JP2008298608A (en) | Method for combusting sample to be analyzed | |
| US5185268A (en) | Method for the determination of total nitrogen including adding an alkali metal halide or an alkaline earth metal halide to the sample | |
| Dědina | Nonplasma devices for atomization and detection of volatile metal species by atomic absorption and fluorescence | |
| JP2000002699A (en) | Analyzer for element in sample | |
| Kunwar et al. | Hot-injection procedures for the rapid analysis of biological samples by electrothermal atomic-absorption spectrometry | |
| Tessari et al. | Determination of subnanogram amounts of chromium in different matrices by flameless atomic-absorption spectroscopy | |
| JP2708236B2 (en) | Analysis of trace carbon, sulfur and phosphorus in metal samples | |
| Robinson et al. | Speciation of mercury compounds by differential atomization‐atomic absorption spectroscopy | |
| JPS6358160A (en) | Apparatus for measuring organocarbon | |
| Hinds et al. | Determination of trace metals in platinum by electrothermal atomic absorption spectrometry following a closed-vessel microwave dissolution procedure |