JP4050577B2 - Mercury analyzer and sample changer used therefor - Google Patents
Mercury analyzer and sample changer used therefor Download PDFInfo
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- JP4050577B2 JP4050577B2 JP2002257618A JP2002257618A JP4050577B2 JP 4050577 B2 JP4050577 B2 JP 4050577B2 JP 2002257618 A JP2002257618 A JP 2002257618A JP 2002257618 A JP2002257618 A JP 2002257618A JP 4050577 B2 JP4050577 B2 JP 4050577B2
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- Prior art keywords
- sample
- mercury
- air
- changer
- sample changer
- 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.)
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- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 title claims description 62
- 229910052753 mercury Inorganic materials 0.000 title claims description 62
- 239000012159 carrier gas Substances 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims 1
- 238000010586 diagram Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 229910000497 Amalgam Inorganic materials 0.000 description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 3
- 229910052737 gold Inorganic materials 0.000 description 3
- 239000010931 gold Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
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- Sampling And Sample Adjustment (AREA)
Description
【０００１】
【発明の属する技術分野】
本発明は、試料中に含まれる水銀を分析する水銀分析装置およびこれに用いるサンプルチェンジャに関するものである。
【０００２】
【従来の技術および発明が解決しようとする課題】
一般に、水銀分析装置では、試料をセラミックや石英製の試料ボートに入れ、試料投入口から試料加熱炉の位置まで挿入し、例えばエアポンプによりエアのようなキャリアガスを流しながら、試料加熱炉で試料を加熱し、酸化促進炉で試料から発生した化合物水銀を０価の水銀に分解し、これを水銀捕集管で金アマルガムとして捕集する。次に、水銀捕集管を加熱し水銀を追い出し、これを原子吸光法などの方法で検出し測定する。この場合、通常エア（室内空気）には必ず水銀が存在するため、通常エアをキャリアガスとして用いる場合、水銀を除去するフィルタが必要であり、フィルタを通らない通常エアがキャリアガスに混ざらないよう、試料投入口に蓋を設けて、試料ボードを入れた後、蓋を閉める必要があった。こうした加熱気化水銀分析装置にサンプルチェンジャを接続する場合、自動的に蓋を開閉し、試料ボートを出し入れする必要があるが、通常エアが入り込まないように、厳密なシールを施す必要があり、蓋構造が複雑となる。
【０００３】
また、加熱気化金アマルガム法による水銀分析では、通常１試料に１０分くらい測定時間がかかる。したがって、水銀分析装置に試料を供給するために、例えば３０試料のサンプルチェンジャを使用し、最初にすべての試料を並べた場合、３０試料目は５時間後の測定となる。この場合、上述のとおり、通常エアには必ず水銀が存在するので、上記測定待ち時間に、この通常エア中の水銀により試料が汚染され、正確な分析ができない。
【０００４】
そこで、本発明の目的は、サンプルチェンジャ内部において測定待ち試料が汚染するのを防止すること、および水銀分析装置の試料投入口の蓋構造を不要とすることにある。
【０００５】
【課題を解決するための手段】
前記目的を達成するため、本発明にかかる水銀分析装置は、キャリアガスを流しながら試料を加熱して試料中に含まれる水銀を分析する水銀分析装置であって、通常エアに含まれる水銀をフィルタで除去した後のガスを供給する手段と、試料を分析する時間中、装置の蓋なし試料投入口から、装置内部の前記キャリアガス流量以上の流量の前記供給された水銀を除去したガスを注入して前記試料投入口から該ガスをあふれさせる手段とを有する。
【０００６】
本発明にかかる前記水銀分析装置用のサンプルチェンジャは、サンプルチェンジャ外部から通常エアを取り入れ、この通常エアに含まれる水銀をフィルタで除去した後のエアを供給する手段と、このエアをサンプルチェンジャ内部に放出してサンプルチェンジャ内部を当該水銀を含まないエアで充満させる手段とを有する。
【０００７】
【発明の実施の形態】
以下、本発明の一実施形態を図面に基づいて説明する。
図１は本発明の第１実施形態に係る水銀分析装置を示す構成図である。まず、水銀分析装置は、試料をセラミックや石英製の試料ボート１に入れ、試料投入口２から試料加熱炉の位置まで挿入し、エアポンプによる所定の流量（例えば０．５Ｌ／ｍｉｎ）のキャリアガス（例えば水銀を含まないエア）を流しながら、試料加熱炉で試料を加熱し、酸化促進炉で試料から発生した化合物水銀を０価の水銀に分解し、これを水銀捕集管で金アマルガムとして捕集する。次に、水銀捕集管を加熱し水銀を追い出し、これを検出器５により、原子吸光法などの方法で検出し測定する。なお、キャリアガスは酸素や窒素などであってもよい。
【０００８】
また、サンプルチェンジャは、上記の水銀分析装置と接続されて、これに試料を供給するもので、複数の試料ボード１を載置したターレットが支持軸回りに回転自在に支持されてなるサンプルチェンジャ本体６と、エア採取口７、水銀除去フィルタ８およびエアポンプ４と、水銀分析装置の試料投入口２に対向する位置で、試料ボード１をスライドさせて投入するスライダ９と、スライダに取り付けられて試料ボード１のうしろにエア吹出口を有するエア吹出手段とを備えている。エア採取口７から採取されたサンプルチェンジャ外部の通常エアは、水銀除去フィルタ８により水銀が除去された後に、エアポンプ４により、試料ボード１を試料投入口２に投入する際、所定のエア流量（例えば４Ｌ／ｍｉｎ）で試料投入口２に注入される。
【０００９】
試料を分析する時間中、つまり、水銀分析装置のエアポンプ３が動作している間、水銀分析装置のキャリアガスのエア流量（０．５Ｌ／ｍｉｎ）より多く、試料投入口２へ所定のエア流量（４Ｌ／ｍｉｎ）の水銀を除去したエアを流すことにより、試料投入口２から例えば３．５Ｌ／ｍｉｎの当該エアがあふれることとなり、試料投入口２から水銀を含む通常エアが入り込むことを防止することができる。したがって、本発明は、従来のように、試料投入口に厳密なシールを施した蓋を設けて開閉させなくとも、フィルタを通らない通常エアがキャリアガスに混ざることがないから、試料投入口に蓋を設ける必要がなくなる。
【００１０】
図２は本発明の第２実施形態に係る水銀分析装置用のサンプルチェンジャを示す構成図である。このサンプルチェンジャは、水銀分析装置に試料を供給するために、複数の試料ボード１を載置したターレットが支持軸回りに回転自在に支持されてなるサンプルチェンジャ本体６と、エア採取口７、水銀除去フィルタ８、エアポンプ４およびエア吹出口１０とを備えている。
【００１１】
エア採取口７から採取されたサンプルチェンジャ外部の通常エアは、水銀除去フィルタ８により水銀が除去された後、エアポンプ４により所定のエア流量でエア吹出口１０からサンプルチェンジャ内に放出される。これにより、サンプルチェンジャ内は水銀のないエアで充満するので、サンプルチェンジャ外部から通常エアがサンプルチェンジャ内に入り込まないから、測定待ちの試料が通常エア中の水銀により汚染するのを防止できる。
【００１２】
なお、第１実施形態の水銀分析装置のサンプルチェンジャにおいて、第２実施形態のようにサンプルチェンジャ内を水銀のないエアで充満するようにしてもよい。
【図面の簡単な説明】
【図１】本発明の第１実施形態に係る水銀分析装置とこれに用いるサンプルチェンジャを示す構成図である。
【図２】第２実施形態に係る水銀分析装置用のサンプルチェンジャを示す構成図である。
【符号の説明】
１…試料ボート、２…試料投入口、３、４…エアポンプ、５…検出器、７…エア採取口、８…水銀除去フィルタ。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a mercury analyzer for analyzing mercury contained in a sample and a sample changer used therefor.
[0002]
[Background Art and Problems to be Solved by the Invention]
In general, in a mercury analyzer, a sample is put into a sample boat made of ceramic or quartz, inserted from the sample inlet to the position of the sample heating furnace, and the sample is sampled in the sample heating furnace while flowing a carrier gas such as air by an air pump. Is heated, the compound mercury generated from the sample in the oxidation promotion furnace is decomposed into zero-valent mercury, and this is collected as gold amalgam in a mercury collecting tube. Next, the mercury collecting tube is heated to drive out mercury, which is detected and measured by a method such as atomic absorption. In this case, mercury is always present in normal air (room air), so when using normal air as a carrier gas, a filter that removes mercury is required, so that normal air that does not pass through the filter is not mixed with the carrier gas. It was necessary to provide a lid at the sample inlet and close the lid after inserting the sample board. When connecting a sample changer to such a heat-vaporizing mercury analyzer, it is necessary to automatically open and close the lid and put the sample boat in and out, but it is usually necessary to provide a strict seal to prevent air from entering the lid. The structure becomes complicated.
[0003]
Further, in the mercury analysis by the heat vaporized gold amalgam method, it usually takes about 10 minutes for one sample. Therefore, in order to supply a sample to the mercury analyzer, for example, when a sample changer of 30 samples is used and all samples are first arranged, the 30th sample is measured after 5 hours. In this case, as described above, since mercury is always present in normal air, the sample is contaminated by mercury in the normal air during the measurement waiting time, and accurate analysis cannot be performed.
[0004]
Accordingly, an object of the present invention is to prevent contamination of a sample waiting for measurement inside the sample changer, and to eliminate the need for a lid structure for the sample inlet of the mercury analyzer.
[0005]
[Means for Solving the Problems]
In order to achieve the above object, a mercury analyzer according to the present invention is a mercury analyzer for analyzing mercury contained in a sample by heating the sample while flowing a carrier gas, and filtering mercury contained in normal air. means for supplying gas after removal in, during the time to analyze the sample, from the lid without sample slot of the device, the removal of the said supply mercury of the carrier gas flow rate or flow rate of the apparatus gas injection And means for overflowing the gas from the sample inlet .
[0006]
The sample changer for mercury analyzer according to the present invention, incorporating the normal air from the sample changer outside, means for supplying air after removal filter mercury contained in the normal air, inside the air sample changer And a means for filling the sample changer with air containing no mercury.
[0007]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, an embodiment of the present invention will be described with reference to the drawings.
FIG. 1 is a block diagram showing a mercury analyzer according to the first embodiment of the present invention. First, the mercury analyzer puts a sample in a sample boat 1 made of ceramic or quartz, inserts the sample from the
[0008]
The sample changer is connected to the above mercury analyzer and supplies a sample to the sample changer body. The sample changer body is configured such that a turret on which a plurality of sample boards 1 are mounted is rotatably supported around a support shaft. 6, an
[0009]
During the time to analyze the sample, that is, while the air pump 3 of the mercury analyzer is operating, the air flow rate of the carrier gas of the mercury analyzer is higher than the air flow rate (0.5 L / min), and a predetermined air flow rate to the
[0010]
FIG. 2 is a block diagram showing a sample changer for a mercury analyzer according to the second embodiment of the present invention. This sample changer has a sample changer main body 6 in which a turret on which a plurality of sample boards 1 are mounted is rotatably supported around a support shaft, an
[0011]
The normal air outside the sample changer collected from the
[0012]
In the sample changer of the mercury analyzer of the first embodiment, the sample changer may be filled with air without mercury as in the second embodiment.
[Brief description of the drawings]
FIG. 1 is a configuration diagram showing a mercury analyzer according to a first embodiment of the present invention and a sample changer used therefor.
FIG. 2 is a configuration diagram showing a sample changer for a mercury analyzer according to a second embodiment.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 ... Sample boat, 2 ... Sample inlet, 3, 4 ... Air pump, 5 ... Detector, 7 ... Air sampling port, 8 ... Mercury removal filter.
Claims (2)
通常エアに含まれる水銀をフィルタで除去した後のガスを供給する手段と、試料を分析する時間中、装置の蓋なし試料投入口から、装置内部の前記キャリアガス流量以上の流量の前記供給された水銀を除去したガスを注入して前記試料投入口から該ガスをあふれさせる手段とを有する水銀分析装置。 A mercury analyzer for analyzing mercury contained in a sample by heating the sample while flowing a carrier gas,
Means for supplying gas after removal of the mercury contained in the normal air filter, in time analyzing the sample, the lid without sample slot of the device, is the supply of the carrier gas flow rate or flow rate of the apparatus And a means for injecting a gas from which mercury has been removed to overflow the gas from the sample inlet .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002257618A JP4050577B2 (en) | 2002-09-03 | 2002-09-03 | Mercury analyzer and sample changer used therefor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2002257618A JP4050577B2 (en) | 2002-09-03 | 2002-09-03 | Mercury analyzer and sample changer used therefor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2004093484A JP2004093484A (en) | 2004-03-25 |
| JP4050577B2 true JP4050577B2 (en) | 2008-02-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2002257618A Expired - Fee Related JP4050577B2 (en) | 2002-09-03 | 2002-09-03 | Mercury analyzer and sample changer used therefor |
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| JP (1) | JP4050577B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4226049B1 (en) | 2007-08-27 | 2009-02-18 | 日本インスツルメンツ株式会社 | Mercury measuring device for measuring mercury in hydrocarbon-based samples |
| CN104807732A (en) * | 2015-05-06 | 2015-07-29 | 北京市环境保护监测中心 | System and method for measuring mercury in atmospheric particulates |
| CN105092866B (en) * | 2015-08-20 | 2017-05-10 | 长沙开元仪器股份有限公司 | Automatic mercury measurement device |
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2002
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| Publication number | Publication date |
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| JP2004093484A (en) | 2004-03-25 |
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