JPS6367133B2 - - Google Patents
Info
- Publication number
- JPS6367133B2 JPS6367133B2 JP7914082A JP7914082A JPS6367133B2 JP S6367133 B2 JPS6367133 B2 JP S6367133B2 JP 7914082 A JP7914082 A JP 7914082A JP 7914082 A JP7914082 A JP 7914082A JP S6367133 B2 JPS6367133 B2 JP S6367133B2
- Authority
- JP
- Japan
- Prior art keywords
- mercury
- mercury concentration
- way
- gas
- collection
- 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
Links
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 68
- 229910052753 mercury Inorganic materials 0.000 claims description 68
- 239000010453 quartz Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 8
- 239000010931 gold Substances 0.000 claims description 6
- 229910052737 gold Inorganic materials 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 229910000497 Amalgam Inorganic materials 0.000 claims description 4
- 238000002485 combustion reaction Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000007789 gas Substances 0.000 description 24
- 238000005259 measurement Methods 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 5
- 238000000354 decomposition reaction Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000007257 malfunction Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002516 radical scavenger Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/12—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using combustion
Description
【発明の詳細な説明】
本発明は、特定化学物質に関する水銀の濃度測
定及び作業環境に関する空気中の水銀濃度測定に
於いて、ガス化水銀を金アマルガム法により固体
捕集した後、捕集部を強熱して捕集水銀を再びガ
ス化し、水銀濃度計ガスセルに導入するための水
銀濃度測定装置内の再ガス化部の改良に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION In the measurement of the concentration of mercury related to a specific chemical substance and the concentration of mercury in the air related to a working environment, the present invention collects gasified mercury as a solid by a gold amalgam method, and then collects it in a collection section. This invention relates to an improvement of a regasification section in a mercury concentration measuring device for igniting mercury to gasify the collected mercury again and introducing it into a mercury concentration meter gas cell.
水銀濃度測定に於けるいわゆる金アマルガム捕
集―冷原子吸光測定法は、水銀捕集管、例えば金
粉、金綿、金ワイヤー又は金塗着無機充填材等を
石英管に充填した捕集管に、ガス状水銀を導入し
て金アマルガム捕集した後、水銀捕集部を一気に
500℃乃至900℃に強熱して捕集水銀を再びガス化
し、冷原子吸光装置、いわゆる水銀濃度計のガス
セルを経由して廃棄される。 The so-called gold amalgam collection-cold atomic absorption spectrometry method for measuring mercury concentration uses a mercury collection tube, such as a quartz tube filled with gold powder, gold cotton, gold wire, or gold-coated inorganic filler. After introducing gaseous mercury and collecting gold amalgam, the mercury collection section is removed all at once.
The collected mercury is ignited to 500°C to 900°C to gasify it again, and is disposed of via the gas cell of a cold atomic absorption device, a so-called mercury concentration meter.
水銀の濃度は、水銀濃度計内ガスセルを水銀ガ
スが通過した際、水銀ランプの253.7nmの光の吸
光量から計測される。従来法によれば、捕集水銀
を再ガス化し、水銀濃度計内ガスセルを通過して
その水銀濃度が表示及び記録される瞬間に於い
て、捕集した水銀濃度が、先に作成しておく検量
線の範囲外である場合は、測定感度の切換え及び
記録倍率の切換え等の測定条件の調整操作を行う
余裕のないまま水銀ガスは廃棄される。又、再ガ
ス化以後の時点に於いて装置の誤動作や誤操作そ
の他何等かの突発事故が発生した場合に於いて
も、濃度検知が行われないまま水銀ガスは廃棄さ
れ、分析検体又は捕集水銀を消耗する。 The concentration of mercury is measured from the amount of light absorbed at 253.7 nm from a mercury lamp when mercury gas passes through the gas cell in the mercury concentration meter. According to the conventional method, at the moment when the collected mercury is regasified, passes through the gas cell in the mercury concentration meter, and the mercury concentration is displayed and recorded, the collected mercury concentration is first created. If it is outside the range of the calibration curve, the mercury gas is discarded without having time to adjust the measurement conditions, such as changing the measurement sensitivity and recording magnification. In addition, even in the event of equipment malfunction, erroneous operation, or any other unexpected accident after regasification, the mercury gas will be discarded without concentration detection, and the analysis sample or collected mercury will be disposed of without being detected. consume.
本発明は、１検体の水銀ガスについて測定条件
の調整を行いつつ繰返し濃度測定を行う水銀濃度
測定装置の発明である。 The present invention is an invention of a mercury concentration measuring device that repeatedly measures the concentration of one sample of mercury gas while adjusting measurement conditions.
本発明の具体例を図面に従い更に詳細に説明す
る。 Specific examples of the present invention will be explained in more detail with reference to the drawings.
第１図の１は酸素ガス供給口をもつ石英管と電
気炉で成り、分析試料を燃焼し、含有する水銀を
ガス化する分解炉、２は酸性ガス吸収剤、例えば
酸化カルシウム粉末を充填した石英管と電気ヒー
ターとで成り、分解ガス中の酸性ガスを捕捉除去
する捕捉管、３はガラス製蛇管とトラツプとでな
り、空冷による分解ガス中の生成水分の凝縮装置
であるが、他の凝縮法、列えば水冷コンデンサー
を使用しても良い。４及び５は、ガラス製の２通
路をもつ四方コツク（以下コツクという）から成
るガス導入経路変換のためのコツク、６は水銀捕
集剤を充填した石英管と電気炉及び冷却フアンと
で成る水銀ガス第１捕集部、７は、冷原子吸光装
置で成る水銀濃度計、８は水銀捕集剤を充填した
石英管と電気炉及び冷却フアンとで成る水銀ガス
第２捕集部、９は、廃棄水銀ガスを捕捉するため
の薬液、例えば過マンガン酸カリ水溶液を注入し
たガス洗浄ビンである。 1 in Figure 1 is a decomposition furnace consisting of a quartz tube with an oxygen gas supply port and an electric furnace, which burns the analysis sample and gasifies the mercury contained therein, and 2 is a decomposition furnace filled with an acidic gas absorbent, such as calcium oxide powder. A capture tube consisting of a quartz tube and an electric heater captures and removes the acidic gas in the decomposed gas, and 3 is a condensation device for water produced in the decomposed gas by air cooling, consisting of a glass corrugated tube and a trap. Condensation method, water-cooled condenser may be used. Numerals 4 and 5 are four-sided cots with two glass passages (hereinafter referred to as cots) for changing the gas introduction route, and 6 is a quartz tube filled with a mercury collector, an electric furnace, and a cooling fan. A first mercury gas collection section 7 is a mercury concentration meter consisting of a cold atomic absorption device; 8 is a second mercury gas collection section consisting of a quartz tube filled with a mercury scavenger, an electric furnace, and a cooling fan; 9 is a gas cleaning bottle filled with a chemical solution, such as an aqueous potassium permanganate solution, to capture waste mercury gas.
本発明によれば、水銀を含有する分析試料を石
英ボートに採り、分解炉１に挿入した後、酸素ガ
スを供給しつつ500℃乃至900℃に加熱し、有機物
を燃焼する。燃焼により生成する酸性ガス及び水
蒸気は捕捉管２及び凝縮装置３で各々捕捉除去さ
れる。 According to the present invention, an analysis sample containing mercury is taken in a quartz boat, inserted into the decomposition furnace 1, and then heated to 500°C to 900°C while supplying oxygen gas to burn the organic matter. Acid gas and water vapor generated by combustion are captured and removed by a capture tube 2 and a condensing device 3, respectively.
更に発生する水銀ガスは、コツク４を経て第１
捕集管６に至り捕集される。 Furthermore, the mercury gas generated passes through Kotoku 4 and is transferred to the first
It reaches the collection tube 6 and is collected.
試料の燃焼分解が終り、含有水銀の捕集が終了
した時、第１捕集管６を約500℃乃至900℃に一気
に加熱して捕集水銀を再ガス化し、コツク５を径
て水銀濃度計７に導入され、水銀濃度が測定され
る。 When the combustion decomposition of the sample is completed and the collection of the mercury contained is completed, the first collection tube 6 is heated at once to approximately 500°C to 900°C to regasify the collected mercury, and the mercury concentration is reduced through the tube 5. mercury concentration is measured.
水銀濃度ガスセルを通過したガス状水銀は、コ
ツク４を径て第２捕集管８に捕集されて第１回の
水銀濃度測定が終了する。 The gaseous mercury that has passed through the mercury concentration gas cell passes through the tank 4 and is collected in the second collection tube 8, thereby completing the first mercury concentration measurement.
次にコツク４及び５を回転して流路を変換した
後、第２捕集管８を500℃乃至900℃に一気に加熱
して捕集水銀をガス化するならば、水銀ガスはコ
ツク５を径て水銀濃度計７を通過して水銀濃度が
測定された後、コツク４を径て再び第１捕集管６
に捕集されて第２回の水銀濃度測定が終了する。 Next, after rotating the tubes 4 and 5 to change the flow path, if the second collection tube 8 is heated at once to 500°C to 900°C to gasify the collected mercury, the mercury gas will pass through the tube 5. After passing through the mercury concentration meter 7 and measuring the mercury concentration, it passes through the cot 4 and returns to the first collection tube 6.
The second mercury concentration measurement is completed.
以上の如く、装置のコツク４及び５の回転と、
水銀捕集管６及び８を交互に加熱する操作を必要
な限り行えば、１検体の試料について捕集水銀の
濃度を繰返し測定する事が出来る。濃度測定が終
了し水銀ガスを廃棄する際は、水銀捕集管６及び
８を同時に加熱し、コツク５を排出側となるよう
にすることにより、装置系内水銀ガスは洗ビン９
に至り排出・捕捉する事が出来る。 As mentioned above, the rotation of the tips 4 and 5 of the device,
By repeating the operation of heating the mercury collection tubes 6 and 8 alternately as long as necessary, the concentration of collected mercury can be repeatedly measured for one sample. When the concentration measurement is completed and the mercury gas is to be disposed of, the mercury collection tubes 6 and 8 are heated at the same time, and the mercury gas inside the device system is removed from the washing bottle 9 by heating the mercury collection tubes 6 and 8 so that the pot 5 is on the discharge side.
It can be discharged and captured.
本発明によれば、分析試料中の水銀濃度が先に
作製しておく検量線の範囲外であつた場合、更に
捕集管が加熱されてからの装置の誤動作又は誤操
作等突発事故が発生した場合に於いても、水銀ガ
スは廃棄される事なく別なる捕集管に捕集されて
いる。 According to the present invention, if the mercury concentration in the analysis sample is outside the range of the calibration curve prepared in advance, unexpected accidents such as equipment malfunction or erroneous operation may occur after the collection tube is further heated. In some cases, mercury gas is collected in a separate collection tube without being disposed of.
即ち分析試料を消耗する事なく、測定条件の変
更及び調整を行いつつ、１検体の水銀濃度を繰返
し測定する事が出来る。 That is, the mercury concentration of one sample can be repeatedly measured while changing and adjusting the measurement conditions without wasting the analysis sample.
第１図は本発明の水銀濃度測定装置の一例の系
路図を示したものである。
FIG. 1 shows a system diagram of an example of the mercury concentration measuring device of the present invention.
Claims (1)
度測定装置に於いて、一つの検体の水銀濃度を繰
り返し測定するために、検体燃焼部１から水銀ガ
スを第１の２通路をもつ四方コツク４を経て水銀
捕集剤を充填した石英管と電気炉及び冷却フアン
からなる第１捕集部６に導入する回路と、該第１
捕集部６より第２の２通路をもつ４方コツク５を
経て水銀濃度計７へ通ずる回路と、該水銀濃度計
７より再び第１の４方コツク４を経て次の水銀捕
集剤を充填した石英管と電気炉及び冷却フアンか
らなる第２捕集部８へ導入する回路と、第２捕集
部８から再び第２の四方コツク５及び水銀濃度計
７を経て、第１の四方コツク４へ通ずる回路を有
し、繰り返し水銀濃度を測定した後、第２の四方
コツク５により測定ずみの水銀を系外に排出でき
るような回路を有することを特徴とする水銀濃度
測定装置。1. In a mercury concentration measuring device using quartz tube combustion and gold amalgam collection, in order to repeatedly measure the mercury concentration of one specimen, mercury gas is passed from the specimen combustion section 1 to the first four-way pot 4 having two passages. A circuit to be introduced into the first collecting section 6 consisting of a quartz tube filled with a mercury collecting agent, an electric furnace, and a cooling fan;
A circuit leads from the collection section 6 to a mercury concentration meter 7 via a second four-way tank 5 having two passages, and from the mercury concentration meter 7, the next mercury collector is passed through the first four-way socket 4 again. A circuit is introduced into the second collection section 8 consisting of a filled quartz tube, an electric furnace, and a cooling fan, and then from the second collection section 8 again via the second four-way tank 5 and the mercury concentration meter 7, and then the first four-way A mercury concentration measuring device characterized in that it has a circuit leading to a pot 4, and after repeatedly measuring the mercury concentration, the measured mercury can be discharged out of the system by a second four-way pot 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7914082A JPS58196443A (en) | 1982-05-13 | 1982-05-13 | Mercury concentration measuring apparatus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7914082A JPS58196443A (en) | 1982-05-13 | 1982-05-13 | Mercury concentration measuring apparatus |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58196443A JPS58196443A (en) | 1983-11-15 |
| JPS6367133B2 true JPS6367133B2 (en) | 1988-12-23 |
Family
ID=13681650
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7914082A Granted JPS58196443A (en) | 1982-05-13 | 1982-05-13 | Mercury concentration measuring apparatus |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58196443A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20210043863A (en) | 2019-10-14 | 2021-04-22 | 주식회사 엘지화학 | Electrode slurry coating device and method forming active material double layers |
| KR20210045625A (en) | 2019-10-17 | 2021-04-27 | 주식회사 엘지화학 | Electrode slurry coating device and method forming active material double layers |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3540995B2 (en) * | 2000-09-08 | 2004-07-07 | 財団法人電力中央研究所 | Method and apparatus for continuous separation analysis of metallic mercury and water-soluble mercury in gas |
| CN110864946A (en) * | 2019-11-13 | 2020-03-06 | 清华大学 | Device and method for measuring mercury content in flue gas |
-
1982
- 1982-05-13 JP JP7914082A patent/JPS58196443A/en active Granted
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20210043863A (en) | 2019-10-14 | 2021-04-22 | 주식회사 엘지화학 | Electrode slurry coating device and method forming active material double layers |
| KR20210045625A (en) | 2019-10-17 | 2021-04-27 | 주식회사 엘지화학 | Electrode slurry coating device and method forming active material double layers |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58196443A (en) | 1983-11-15 |
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