JPH0532700B2 - - Google Patents
Info
- Publication number
- JPH0532700B2 JPH0532700B2 JP58118682A JP11868283A JPH0532700B2 JP H0532700 B2 JPH0532700 B2 JP H0532700B2 JP 58118682 A JP58118682 A JP 58118682A JP 11868283 A JP11868283 A JP 11868283A JP H0532700 B2 JPH0532700 B2 JP H0532700B2
- Authority
- JP
- Japan
- Prior art keywords
- graphite crucible
- sample
- inert gas
- gas atmosphere
- powder 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.)
- Expired - Lifetime
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 46
- 229910002804 graphite Inorganic materials 0.000 claims description 46
- 239000010439 graphite Substances 0.000 claims description 46
- 239000000843 powder Substances 0.000 claims description 28
- 239000007789 gas Substances 0.000 claims description 18
- 239000011261 inert gas Substances 0.000 claims description 18
- 238000007872 degassing Methods 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 2
- 238000011002 quantification Methods 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 238000005259 measurement Methods 0.000 description 13
- 239000002184 metal Substances 0.000 description 4
- 239000012159 carrier gas Substances 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 238000004445 quantitative analysis Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000003780 insertion Methods 0.000 description 2
- 230000037431 insertion Effects 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000001304 sample melting Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/20—Metals
- G01N33/202—Constituents thereof
- G01N33/2022—Non-metallic constituents
- G01N33/2025—Gaseous constituents
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
Description
【発明の詳細な説明】
本発明は、不活性ガス雰囲気中で一対の電極間
に黒鉛るつぼを設置し、これら両電極に電圧を印
加して前記黒鉛るつぼを高温に加熱して脱ガスを
行ない、その後、黒鉛るつぼに金属等の粉粒体試
料を挿入し、再び不活性ガス雰囲気中で前記黒鉛
るつぼを加熱して試料を融解し、その試料から抽
出される成分ガスの定量をおこなう方法における
黒鉛るつぼの二次脱ガスを実施することを特徴と
する粉粒体試料の定量方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention involves installing a graphite crucible between a pair of electrodes in an inert gas atmosphere, applying a voltage to both electrodes, heating the graphite crucible to a high temperature, and degassing the crucible. Thereafter, a powder sample of metal or the like is inserted into a graphite crucible, the graphite crucible is heated again in an inert gas atmosphere to melt the sample, and the component gases extracted from the sample are quantified. The present invention relates to a method for quantifying a powder sample, which is characterized by performing secondary degassing of a graphite crucible.
まず、従来の定量装置ならびにその定量方法に
つき、第１図をもとに説明すると、図中１と２は
一対の電極で、これら電極１，２間には黒鉛るつ
ぼ４が設置されている。１４は黒鉛るつぼ４の上
方に配設された試料ホルダで、このホルダ１４は
ケーシング１５内に回転自在に支持されている。
ケーシング１５には開閉自在なシヤツタ１６が設
けられ、前記ケーシング１５内部ならびに黒鉛る
つぼ４周囲が不活性のキヤリアガスで満たされる
ように構成されている。このように構成された定
量装置は、るつぼ４の脱ガスを行ない、ついでシ
ヤツタ１６を開けて試料ホルダ１４内に定量の金
属試料１３を挿入し、シヤツタ１６を閉じた後、
試料ホルダ１４を回転させて金属試料１３をるつ
ぼ４に落下、挿入するのであるが、金属試料１３
がバリ片のある切粉や粉粒体のような特殊なもの
であると、該試料１３が試料ホルダ１４に引つ掛
かつたり付着したり、あるいはホルダ１４外に落
下したりして、確実にその全量を黒鉛るつぼ４に
挿入することができない難点があつた。このよう
な事態が生ずれば、正確なガス測定ができないば
かりか、場合によつては異常分析結果の原因とも
なる。また、シヤツタ１６を開閉して金属試料１
３をホルダ１４に挿入する際、シヤツタ１６のシ
ール１７に付着して不良を招くおそれすらあつ
た。 First, a conventional quantitative device and its quantitative method will be explained with reference to FIG. 1. In the figure, 1 and 2 are a pair of electrodes, and a graphite crucible 4 is installed between these electrodes 1 and 2. Reference numeral 14 denotes a sample holder disposed above the graphite crucible 4, and this holder 14 is rotatably supported within the casing 15.
The casing 15 is provided with a shutter 16 that can be opened and closed, and is configured so that the inside of the casing 15 and the surrounding area of the graphite crucible 4 are filled with an inert carrier gas. The quantitative device configured in this manner degasses the crucible 4, then opens the shutter 16, inserts a quantitative amount of the metal sample 13 into the sample holder 14, and closes the shutter 16, then
The sample holder 14 is rotated to drop and insert the metal sample 13 into the crucible 4.
If the sample 13 is a special material such as chips or powder particles with burrs, the sample 13 may get caught or stick to the sample holder 14, or fall outside the holder 14, and However, there was a problem in that the entire amount could not be inserted into the graphite crucible 4. If such a situation occurs, not only will accurate gas measurement not be possible, but in some cases it may also cause abnormal analysis results. Also, open and close the shutter 16 to remove the metal sample 1.
3 into the holder 14, there was even a risk that it would adhere to the seal 17 of the shutter 16 and cause a defect.
本発明は、このような従来方法の難点を解消
し、常に定量の粉粒体試料を確実に黒鉛るつぼ内
に挿入し、かつ精度の高いガス分析を行なうこと
のできる新規で有用な定量方法を提供せんとする
ものである。 The present invention solves the difficulties of the conventional methods and provides a new and useful quantitative method that can always reliably insert a fixed amount of powder sample into a graphite crucible and perform highly accurate gas analysis. This is what we intend to provide.
本発明方法の実施の態様を第２図〜第４図にも
とづいて説明すると、図中１，２は上下一対の電
極で、それぞれ電源３に接続され、これら電極
１，２間には黒鉛るつぼ４が設置されている。上
方の電極１には、不活性のキアリアガス挿入用の
パイプ５と計測系６へのパイプ７が連通され、両
電極１，２を閉じた状態においては両電極１，２
が互いにシールされ、黒鉛るつぼ４が不活性ガス
雰囲気中に置かれるように構成されている。前記
計測系６はカラムまたは試薬８、除去試薬９、検
出器１０などからなり、この計測系６と上方電極
１との間のパイプ７には切換弁１１が介在されて
いて、上方電極１及び下方電極２内からのガスを
放出パイプ１２を介して系外へ放出したり、ある
いは計測系６に送り込んだり、択一的に切換え可
能に構成されている。 The embodiment of the method of the present invention will be explained based on FIGS. 2 to 4. In the figures, 1 and 2 are a pair of upper and lower electrodes, each connected to a power source 3, and a graphite crucible is connected between these electrodes 1 and 2. 4 are installed. A pipe 5 for inserting inert Chiaria gas and a pipe 7 to a measurement system 6 are connected to the upper electrode 1, and when both electrodes 1 and 2 are closed, both electrodes 1 and 2 are connected to each other.
are sealed together and the graphite crucible 4 is placed in an inert gas atmosphere. The measurement system 6 includes a column or reagent 8, a removal reagent 9, a detector 10, etc. A switching valve 11 is interposed in the pipe 7 between the measurement system 6 and the upper electrode 1. The gas from within the lower electrode 2 can be selectively discharged to the outside of the system via the discharge pipe 12 or sent to the measurement system 6.
次に、この装置を用いて粉粒体試料１３を定量
する方法について説明すると、まず、従来と同様
に、両電極１，２に電力を加えて、黒鉛るつぼ４
を不活性ガス雰囲気中で高温加熱し、るつぼ４の
脱ガスを行なう。この場合には切換弁１１によ
り、上方電極１及び下方電極２内からのガスを系
外に放出するようにしておく。次に、両電極１，
２を分離して黒鉛るつぼ４を不活性ガス雰囲気中
から取り出し、定量の粉粒体試料１３を挿入す
る。このように、不活性ガス雰囲気中から取り出
した黒鉛るつぼ４に粉粒体試料１３を直接挿入す
るものであるから、所望量の粉粒体試料１３を外
部に付着させたり落ちこぼしたりすることなく、
確実に正味量を挿入することができ、挿入時の定
量が正確におこなえるようになつた。その後、る
つぼ４を再び両電極１，２間に設置して、不活性
ガス雰囲気中に置くのである。 Next, to explain how to quantify the powder sample 13 using this device, first, as in the conventional method, power is applied to both electrodes 1 and 2, and the graphite crucible 4 is
is heated at high temperature in an inert gas atmosphere to degas the crucible 4. In this case, the gas from inside the upper electrode 1 and the lower electrode 2 is discharged to the outside of the system by the switching valve 11. Next, both electrodes 1,
2 is separated, the graphite crucible 4 is taken out from the inert gas atmosphere, and a fixed amount of the powder sample 13 is inserted. In this way, since the powder sample 13 is directly inserted into the graphite crucible 4 taken out from the inert gas atmosphere, the desired amount of powder sample 13 can be inserted without adhering to the outside or spilling. ,
It has become possible to reliably insert the net amount and accurately quantify the amount at the time of insertion. Thereafter, the crucible 4 is again placed between the electrodes 1 and 2 and placed in an inert gas atmosphere.
しかし、このとき、脱ガス時に活性化された黒
鉛るつぼ４を大気中に取り出しているのでO2や
H2Oなどが付着しており、そのまま加熱した場
合には、そのO2やH2Oなどが粉粒体試料１３か
らの抽出成分ガスに混入して計測系６に送られる
ことになる。そうすると、測定すべきＯやＨのブ
ランク値が上昇したり、Ｎ測定へのクロマイトグ
ラフ上への影響が生じて正確なガス測定ができな
くなるばかりか、酸化試薬などの劣化速度を速め
るなど種々の不都合が生ずる。 However, at this time, since the graphite crucible 4 activated during degassing is taken out into the atmosphere, O 2 and
If H 2 O or the like is attached and the sample is heated as it is, the O 2 or H 2 O will be mixed into the extracted component gas from the powder sample 13 and sent to the measurement system 6 . If this happens, the blank values of O and H to be measured will increase, and the N measurement will be affected on the chromatograph, making accurate gas measurement impossible. This will cause inconvenience.
そこで、本発明による試料定量方法では、再び
不活性ガス雰囲気中で黒鉛るつぼ４を加熱する際
に、粉粒体試料１３が融解する前に、第４図に示
すように、粉粒体試料１３から測定すべき成分ガ
スが抽出しない程度の低温度で黒鉛るつぼ４を加
熱して二次脱ガスを行ない、上方電極１及び下方
電極２内からのガスを系外に放出させるようにし
たのである。そして、その後、所定の高温度で黒
鉛るつぼ４を加熱して粉粒体試料１３を融解して
その成分ガスを計測系６へ送ることにより、所望
通りの精度の高いガス測定を行ない得るのであ
る。 Therefore, in the sample quantitative method according to the present invention, when the graphite crucible 4 is heated again in an inert gas atmosphere, the powder sample 13 is heated as shown in FIG. 4 before the powder sample 13 is melted. Secondary degassing is performed by heating the graphite crucible 4 at a temperature low enough to prevent the component gases to be measured from being extracted from the graphite crucible 4, thereby releasing the gas from the upper electrode 1 and the lower electrode 2 to the outside of the system. . Thereafter, by heating the graphite crucible 4 at a predetermined high temperature to melt the powder sample 13 and sending its component gas to the measurement system 6, it is possible to perform highly accurate gas measurements as desired. .
この二次脱ガスは、試料融解時よりも相対的に
低い温度、すなわち、例えば50〜100℃の温度で
最大数分間行なう。これにより、前述したよう
に、粉粒体試料１３から成分ガスを発生させるこ
となく、黒鉛るつぼ４に付着した大気中成分のみ
を除去することができる。なお、その際に少量の
キヤリアガスを供給すればより効果的に付着成分
を除去することができる。ちなみに、かかる脱ガ
ス方法とは別に、多量のキヤリアガスを用いたパ
ージによる付着成分除去法もあるが、その除去効
果は十分ではなく、かつコスト高となる等の難点
があり、本実施例の方法には及ぶべくもない。 This secondary degassing is performed at a temperature relatively lower than that during sample melting, ie, for example, at a temperature of 50 to 100° C. for a maximum of several minutes. Thereby, as described above, only the atmospheric components adhering to the graphite crucible 4 can be removed without generating component gases from the powder sample 13. Note that if a small amount of carrier gas is supplied at this time, the adhered components can be removed more effectively. Incidentally, apart from such a degassing method, there is also a method for removing adhered components by purging using a large amount of carrier gas, but the removal effect is not sufficient and there are drawbacks such as high cost. There's no way it can reach that.
ところで、上述のような二次脱ガスをおこなう
場合において、測定すべきガスがＨの場合には二
次脱ガスの際に、粉粒体試料１３から、このＨが
H2として抽出されてしまう場合がある。しかし、
黒鉛るつぼ４に付着したH2Oは、そのままH2O
として抽出されるので、二次脱ガスの際、その抽
出ガスをそのまま計測系６に送るようにしてい
る。かくすれば、計測系６の試薬８において、黒
鉛るつぼ４から抽出されたH2Oが除去されるの
で、検出器１０で粉粒体試料１３からのH2を確
実に測定することができる。よつて、この測定値
に粉粒体試料１３の融解時に測定したH2の値を
加算することにより、粉粒体試料１３から抽出さ
れたH2の真の値を測定することができるのであ
る。 By the way, when performing secondary degassing as described above, if the gas to be measured is H, this H is removed from the powder sample 13 during the secondary degassing.
It may be extracted as H 2 . but,
The H 2 O attached to the graphite crucible 4 remains as H 2 O.
Therefore, during secondary degassing, the extracted gas is directly sent to the measurement system 6. In this way, H 2 O extracted from the graphite crucible 4 is removed in the reagent 8 of the measurement system 6, so that the detector 10 can reliably measure H 2 from the powder sample 13. Therefore, by adding the H 2 value measured when the powder sample 13 is melted to this measurement value, the true value of H 2 extracted from the powder sample 13 can be measured. .
以上の説明から明らかなように、本発明による
試料定量方法では、まず、黒鉛るつぼを不活性ガ
ス雰囲気中から取り出し可能に構成するととも
に、不活性ガス雰囲気中で前記黒鉛るつぼの脱ガ
スをおこなつた後に、前記黒鉛るつぼを不活性ガ
ス雰囲気中から取り出してその黒鉛るつぼ自体に
直接粉粒体試料を挿入するようにしたので、粉粒
体試料を外部に付着させたり落ちこぼしたりする
ことなく、確実に正味量をその黒鉛るつぼに挿入
することができる。つまり、粉粒体試料の正確な
挿入時定量が可能となつた。 As is clear from the above description, in the method for quantifying a sample according to the present invention, first, a graphite crucible is configured to be removable from an inert gas atmosphere, and the graphite crucible is degassed in an inert gas atmosphere. After that, the graphite crucible is taken out of the inert gas atmosphere and the powder sample is directly inserted into the graphite crucible itself, so the powder sample does not stick to the outside or fall out. It is possible to ensure that a net amount is inserted into the graphite crucible. In other words, it has become possible to accurately quantify the powder sample at the time of insertion.
そして、上述の脱ガス後に、再び不活性ガス雰
囲気中でその黒鉛るつぼを加熱する際に、前記粉
粒体試料が融解する前に、その粉粒体試料から成
分ガスを発生させることなく前記黒鉛るつぼの付
着成分を除去するべく、50℃〜100℃の低温で前
記黒鉛るつぼを加熱する二次脱ガスをおこなうよ
うにしたので、粉粒体試料の挿入時に、前記黒鉛
るつぼに付着したO2やH2O等の大気中成分を効
果的に除去することができ、前述した粉粒体試料
の正確な挿入時定量と相まつて、精度の高い成分
ガスの定量が可能となつた。 After the above-mentioned degassing, when the graphite crucible is heated again in an inert gas atmosphere, the graphite crucible is heated without generating any component gas from the powder sample before the powder sample melts. In order to remove the components adhering to the crucible, secondary degassing was performed by heating the graphite crucible at a low temperature of 50°C to 100°C, so when the powder sample was inserted, the O 2 adhering to the graphite crucible was removed. It is possible to effectively remove atmospheric components such as and H 2 O, and in combination with the above-mentioned accurate quantification when inserting a powder sample, it has become possible to quantify component gases with high precision.
第１図は従来の定量装置の概略図、第２図、第
３図は本発明の方法を説明するための定量装置の
概略図、第４図は本発明の方法を示すグラフであ
る。
１，２……電極、４……黒鉛るつぼ、１３……
粉粒体試料。
FIG. 1 is a schematic diagram of a conventional quantitative device, FIGS. 2 and 3 are schematic diagrams of a quantitative device for explaining the method of the present invention, and FIG. 4 is a graph showing the method of the present invention. 1, 2... Electrode, 4... Graphite crucible, 13...
Powder sample.
Claims (1)
黒鉛るつぼを設置し、これら両電極に電圧を印加
し、前記黒鉛るつぼを高温に加熱して脱ガスをお
こなつた後、前記黒鉛るつぼ内に試料を挿入し、
再び不活性ガス雰囲気中で前記黒鉛るつぼを高温
で加熱し、前記試料から抽出される成分ガスの定
量をおこなう試料定量方法において、前記黒鉛る
つぼを不活性ガス雰囲気中から取り出し可能に構
成するとともに、不活性ガス雰囲気中で前記黒鉛
るつぼの脱ガスをおこなつた後に、前記黒鉛るつ
ぼを不活性ガス雰囲気中から取り出してその黒鉛
るつぼ自体に直接粉粒体試料を挿入し、再び不活
性ガス雰囲気中でその黒鉛るつぼを加熱する際
に、前記粉粒体試料が融解する前に、その粉粒体
試料から成分ガスを発生させることなく前記黒鉛
るつぼの付着成分を除去するべく、50℃〜100℃
の低温で前記黒鉛るつぼを加熱する二次脱ガスを
おこなうことを特徴とする黒鉛るつぼを用いた試
料定量方法。1. A graphite crucible is installed between a pair of electrodes provided in an inert gas atmosphere, a voltage is applied to both electrodes, the graphite crucible is heated to a high temperature and degassed, and then the inside of the graphite crucible is Insert the sample into the
In the sample quantification method of heating the graphite crucible at high temperature again in an inert gas atmosphere and quantifying the component gas extracted from the sample, the graphite crucible is configured to be removable from the inert gas atmosphere, and After degassing the graphite crucible in an inert gas atmosphere, the graphite crucible is taken out of the inert gas atmosphere, a powder sample is directly inserted into the graphite crucible itself, and the graphite crucible is placed in the inert gas atmosphere again. When heating the graphite crucible at 50°C to 100°C, in order to remove the components attached to the graphite crucible without generating component gas from the powder sample before the powder sample melts.
A method for quantifying a sample using a graphite crucible, characterized in that secondary degassing is performed by heating the graphite crucible at a low temperature of .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58118682A JPS608749A (en) | 1983-06-28 | 1983-06-28 | Quantitative analysis of sample such as metal using graphite crucible |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58118682A JPS608749A (en) | 1983-06-28 | 1983-06-28 | Quantitative analysis of sample such as metal using graphite crucible |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS608749A JPS608749A (en) | 1985-01-17 |
| JPH0532700B2 true JPH0532700B2 (en) | 1993-05-17 |
Family
ID=14742587
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58118682A Granted JPS608749A (en) | 1983-06-28 | 1983-06-28 | Quantitative analysis of sample such as metal using graphite crucible |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS608749A (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0620997Y2 (en) * | 1985-02-23 | 1994-06-01 | 株式会社堀場製作所 | Elemental analyzer for samples using crucible |
| JPH02234061A (en) * | 1989-03-08 | 1990-09-17 | Horiba Ltd | Extraction method for gas for analysis of sample |
| JPH0740027B2 (en) * | 1989-03-16 | 1995-05-01 | 株式会社堀場製作所 | Elemental analysis method |
| JP2949501B2 (en) * | 1989-03-29 | 1999-09-13 | 株式会社 堀場製作所 | Gas extractor for sample analysis |
| JP2856006B2 (en) * | 1992-11-13 | 1999-02-10 | 日本鋼管株式会社 | Trace oxygen analysis method for steel |
| EP4276458B1 (en) * | 2022-05-12 | 2024-05-01 | C. Gerhardt GmbH & Co. KG | Analytic device for elementary analysis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5227071A (en) * | 1975-08-27 | 1977-03-01 | Hitachi Ltd | Simple method of removing substances deposited on vessel walls |
| JPS55166044A (en) * | 1979-06-07 | 1980-12-24 | Oceanography Int Corp | Method of and apparatus for measuring whole organic carbon |
| JPS5640434A (en) * | 1979-09-08 | 1981-04-16 | Horiba Ltd | Graphite crucible |
-
1983
- 1983-06-28 JP JP58118682A patent/JPS608749A/en active Granted
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5227071A (en) * | 1975-08-27 | 1977-03-01 | Hitachi Ltd | Simple method of removing substances deposited on vessel walls |
| JPS55166044A (en) * | 1979-06-07 | 1980-12-24 | Oceanography Int Corp | Method of and apparatus for measuring whole organic carbon |
| JPS5640434A (en) * | 1979-09-08 | 1981-04-16 | Horiba Ltd | Graphite crucible |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS608749A (en) | 1985-01-17 |
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