CN104713966A - Thermal desorption and sampling device for methyl mercury - Google Patents
Thermal desorption and sampling device for methyl mercury Download PDFInfo
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- CN104713966A CN104713966A CN201510126439.3A CN201510126439A CN104713966A CN 104713966 A CN104713966 A CN 104713966A CN 201510126439 A CN201510126439 A CN 201510126439A CN 104713966 A CN104713966 A CN 104713966A
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Abstract
The invention discloses a thermal desorption and sampling device for methyl mercury. The thermal desorption and sampling device comprises a flow meter and a thermal desorption device, wherein the thermal desorption device comprises a heating coil, a heating power supply, a heating switch and a heating power supply and voltage regulator; when an experiment for determining the content of the methyl mercury is carried out, an argon bottle is firstly opened; argon enters the lower end of the flow meter through a PFA gas pipeline, then flows out from the upper end of the flow meter, and enters a methyl mercury-enriched Tenax adsorption pipe through the PFA gas pipeline; and the heating coil sleeves the adsorption pipe. According to the thermal desorption and sampling device, carrier gas flow control and heating desorption devices are integrated; the thermal desorption and sampling device is simple in structure and convenient to operate; thermal desorption and sampling operation on the methyl mercury are greatly simplified; experiment efficiency is improved; and compared with devices with the similar functions, the thermal desorption and sampling device is extremely low in construction cost.
Description
Technical field
The present invention relates to a kind of chemical analysis apparatus, particularly relate to a kind of methyl mercury thermal desorption sampling device.
Background technology
In the analytical approach of methyl mercury, high performance liquid chromatography (HPLC) or vapor-phase chromatography (GC) is generally adopted to be separated.HPLC can reach good separating effect, but due to the dilution of mobile phase, often causes higher detection limit, usually adopts the method for liquid-liquid extraction or Solid-Phase Extraction to carry out enrichment to sample, complex operation.GC easily and the method coupling such as purge and trap (P & T), solid-phase microextraction (SPME), has the advantages such as Matrix effects is little, easy and simple to handle, has very high sensitivity simultaneously.
For the sample tests of trace methyl mercury content, external many employing aqueous phases ethylize and derive-purge and trap technology, first the method carries out ethylation reaction to sample solution, the methyl mercury in solution and inorganic mercury is made to be converted into volatile Methylethyl mercury and dimethylmercury, then from aqueous solution, stripping is out them to use nitrogen, with the enrichment of Tenax adsorption tube, then heat Tenax pipe release organic mercury and enter the separation that gas chromatographic column realizes different alkyl mercury, final high temperature pyrolysis alkyl mercury is Elemental Mercury, detects with cold-atomic fluorescence mercury meter.The method is simple to operate, highly sensitive, greatly reduces the Matrix effects produced in analytic process.
Existing thermal desorption sampling device improves from the injection port of gas chromatograph often, complex structure; Adsorption tubes used etc. are the special part of specific chromatogram, expensive; Under injection port is in higher temperature all the time, operation inconvenience.The thermal desorption sampling device of import methyl mercury analyser is expensive, and is an ingredient of set of equipments, can not dismantle and control separately, thus cannot realize the coupling with miscellaneous equipment.
Summary of the invention
Technical matters to be solved by this invention is controlled by carrier gas flux and adds thermal analysis apparatus integration, can use online with all kinds of gas chromatograph easily, structure is simple, easy to operate, the Thermal desorption of methyl mercury and sample introduction operation are simplified greatly, improve conventional efficient, compared with the device of similar function, this apparatus cost is extremely cheap.
The present invention counts spinner-type flowmeter for technical scheme that technical solution problem is taked is to provide flow, it regulates argon flow amount by flowmeter knob, flowmeter is arranged on the anterior aluminium sheet of methyl mercury thermal desorption sampling device, lower end connects PFA gas piping through after anterior aluminium sheet, then through methyl mercury thermal desorption sampling device rear portion aluminium sheet, aluminium sheet both sides all use Teflon to cross wall interface, connect PFA gas piping, be then connected with argon bottle by the second pipe interface;
The upper end of flowmeter connects PFA gas piping through after anterior aluminium sheet, then through aluminium sheet on the left of methyl mercury thermal desorption sampling device, aluminium sheet both sides, left side all use Teflon to cross wall interface, and the first gas piping interface connects PFA gas piping, is then connected with Tenax adsorption tube; Tenax adsorption tube is by two the adsorption tube support supports being fixed on both sides, methyl mercury thermal analysis apparatus top;
Thermal analysis apparatus comprises heater coil, heating power supply heating power supply, heater switch and heating power supply voltage regulator, and wherein, heater switch is single two countdown switch; Wherein, heating power supply draws two electric wires, is connected with heater switch through anterior aluminium sheet, draws two electric wires in addition draw as wire and plug from methyl mercury thermal desorption sampling device rear portion aluminium sheet from heater switch;
Methyl mercury thermal desorption sampling device base plate is installed heating power supply and heating power supply voltage regulator, two electric wires are drawn in heating power supply voltage regulator one end, pass from the front portion of methyl mercury thermal desorption sampling device upper position, connect heater coil, the other end is connected with heating power supply, heating power supply voltage regulator has a knob for regulating heating power supply voltage.
Good effect of the present invention is:
Carrier gas flux can control and add thermal analysis apparatus integration by invention, the online use with all kinds of gas chromatograph can be realized, structure is simple, easy to operate, the Thermal desorption of methyl mercury and sample introduction operation are simplified greatly, improve conventional efficient, compared with the device of similar function, this apparatus cost is extremely cheap;
In the present invention, the temperature of heater coil is by heater switch (single two countdown switch) and heating power supply voltage regulator co-controlling, and coil temperature is controlled at 180 DEG C ~ 200 DEG C.The methyl mercury that air-flow after this device carries parsing enters gas chromatographic column and Cold Atomic Fluorescent Mercury detecting device, and can complete the test job of methyl mercury, test process is simply efficient.
Accompanying drawing explanation
Fig. 1 is inner side pipeline schematic diagram of the present invention;
Fig. 2 is inside top pipeline schematic diagram of the present invention;
Fig. 3, Fig. 4 and Fig. 5 are respectively the surface structure schematic diagram at front, side and the back side.
Wherein: 1-heating power supply voltage regulator knob, 2-flowmeter knob, 3-first gas piping interface, 4-heater coil, 5-flowmeter, 6-heater switch, 7-wire and plug, 8-second gas piping interface, 9-adsorption tube support, 10-heating power supply voltage regulator, 11-heating power supply, 12-shell, the anterior aluminium sheet of 13-, 14-rear portion aluminium sheet, aluminium sheet on the left of 15-, 16-electric wire, 17-gas piping, 18-Tenax adsorption tube.
Specific implementation method
Below in conjunction with accompanying drawing 1-5, technical scheme of the present invention is described further.
As Fig. 1-5, the invention provides a kind of methyl mercury thermal desorption sampling device, comprise flowmeter 5, thermal analysis apparatus and shell 12, described thermal analysis apparatus comprises heater coil 4, heating power supply 11, heater switch 6 and heating power supply voltage regulator 10, wherein, heater switch 6 is single two countdown switch.
Described flowmeter 5 is spinner-type flowmeter, argon flow amount can be regulated by flowmeter knob 2, flowmeter 5 is arranged on the anterior aluminium sheet 13 of methyl mercury thermal desorption sampling device, lower end connects 1/8 inch of PFA gas piping through after anterior aluminium sheet 13, then through methyl mercury thermal desorption sampling device rear portion aluminium sheet 14, aluminium sheet both sides all use Teflon to cross wall interface, connect 1/8 inch of PFA gas piping 17, be then connected with argon bottle by 1/8 inch of PFA gas piping interface 3.
The upper end of flowmeter 5 connects 1/8 inch of PFA gas piping through after anterior aluminium sheet 13, then through aluminium sheet 15 on the left of methyl mercury thermal desorption sampling device, aluminium sheet both sides all use Teflon to cross wall interface to connect 1/8 inch of PFA gas piping 17 by 1/8 inch of PFA gas piping interface 3, be then connected with Tenax adsorption tube.Tenax adsorption tube is by 2 adsorption tube support 9 supports being fixed on both sides, device top.
Methyl mercury thermal desorption sampling device base plate is installed heating power supply 11 and heating power supply voltage regulator 10, two electric wires 16 are drawn in heating power supply voltage regulator 10 one end, pass from the front portion of methyl mercury thermal desorption sampling device upper position, connect heater coil 4, the other end is connected with heating power supply 11, heating power supply voltage regulator 10 has a knob, and this knob passes the left side aluminium sheet 15 of methyl mercury thermal desorption sampling device upper position, for regulating heating power supply voltage.Heating power supply 11 draws 2 electric wires 16 again, is connected with the heater switch 6 being positioned at apparatus platform position through anterior aluminium sheet 13, then draws 2 electric wires 16 from heater switch 6 again and draws as wire and plug from device rear portion aluminium sheet 14.Shell 12 is aluminum design, and it is installed for all parts and provides support.
When carrying out the experiment of methyl mercury assay, carry out according to following steps:
Step 1, open argon bottle, argon gas enters flowmeter 5 lower end through 1/8 inch of PFA gas piping 17, and adjust flux meter knob 2 makes argon flow amount control at 35mL/min;
Step 2, from flowmeter 5 upper end flow out enter through 1/8 inch of PFA gas piping 17 the Tenax adsorption tube 18 being enriched methyl mercury, adsorption tube overcoat heater coil 4, the temperature of heater coil is by heater switch 6 and heating power supply voltage regulator 10 co-controlling, by arranging the heater switch time, wherein the time is fixed as 30 seconds, regulate heating power supply voltage regulator knob 1, coil temperature is controlled at 180 DEG C ~ 200 DEG C.
Such setting can ensure that the methyl mercury in Tenax adsorption tube is resolved completely, can ensure that again the chromatographic peak shape of methyl mercury is symmetrical Gaussian distribution.
The methyl mercury that air-flow after this device carries parsing enters gas chromatographic column and Cold Atomic Fluorescent Mercury detecting device, can complete the test job of methyl mercury.
Although describe in detail invention has been in conjunction with the embodiments; but those skilled in the art are with being to be understood that; the present invention is not limited only to specific embodiment; on the contrary; do not exceeding the various corrections of the application's spirit and essence, distortion and replacement all drop among the protection domain of the application.
Claims (2)
1. a methyl mercury thermal desorption sampling device, comprises flowmeter (5), thermal analysis apparatus; It is characterized in that:
Flowmeter (5) is spinner-type flowmeter, it regulates argon flow amount by flowmeter knob (2), flowmeter (5) is arranged on the anterior aluminium sheet (13) of methyl mercury thermal desorption sampling device, lower end connects PFA gas piping (17) afterwards through anterior aluminium sheet (13), then through methyl mercury thermal desorption sampling device rear portion aluminium sheet (14), aluminium sheet both sides all use Teflon to cross wall interface, connect PFA gas piping (17) by the second pipe interface (8), be then connected with argon bottle;
The upper end of flowmeter (5) connects PFA gas piping (17) afterwards through anterior aluminium sheet (13), then through aluminium sheet (15) on the left of methyl mercury thermal desorption sampling device, aluminium sheet (15) both sides, left side all use Teflon to cross wall interface, first gas piping interface (3) connects PFA gas piping (17), is then connected with Tenax adsorption tube; Tenax adsorption tube is by two adsorption tube support (9) supports being fixed on both sides, methyl mercury thermal analysis apparatus top;
Thermal analysis apparatus comprises heater coil (4), heating power supply heating power supply (11), heater switch (6) and heating power supply voltage regulator (10), wherein, heater switch (6) is single two countdown switch; Wherein, heating power supply (11) draws two electric wires (16), be connected with heater switch (6) through anterior aluminium sheet (13), draw two electric wires (16) from heater switch (6) in addition and draw as wire and plug from methyl mercury thermal desorption sampling device rear portion aluminium sheet (14);
Methyl mercury thermal desorption sampling device base plate is installed heating power supply (11) and heating power supply voltage regulator (10), two electric wires (16) are drawn in heating power supply voltage regulator (10) one end, pass from the front portion of methyl mercury thermal desorption sampling device upper position, connect heater coil (4), the other end is connected with heating power supply (11), heating power supply voltage regulator (10) has a knob for regulating heating power supply voltage.
2. the sample injection method of methyl mercury thermal desorption sampling device according to claim 1, is characterized in that, the method is carried out according to following steps:
Step 1, open argon bottle, argon gas enters flowmeter (5) lower end through PFA gas piping (17), and adjust flux meter knob (2) makes argon flow amount control at 35mL/min;
Step 2, argon gas flow out from flowmeter (5) upper end and enter through PFA gas piping (17) the Tenax adsorption tube (18) being enriched methyl mercury, adsorption tube overcoat heater coil (4), the temperature of heater coil is by heater switch (6) and heating power supply voltage regulator (10) co-controlling, by arranging the heater switch time, wherein the time is fixed as 30 seconds, regulate heating power supply voltage regulator knob (1), coil temperature is controlled at 180 DEG C ~ 200 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510126439.3A CN104713966B (en) | 2015-03-23 | 2015-03-23 | Methyl mercury thermal desorption sampling device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510126439.3A CN104713966B (en) | 2015-03-23 | 2015-03-23 | Methyl mercury thermal desorption sampling device |
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| CN104713966A true CN104713966A (en) | 2015-06-17 |
| CN104713966B CN104713966B (en) | 2016-11-30 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104819885A (en) * | 2015-05-13 | 2015-08-05 | 河南理工大学 | Thermal analysis device of elemental mercury in gold amalgam adsorption tube |
| CN106442811A (en) * | 2016-09-18 | 2017-02-22 | 中国海洋大学 | Thermal desorption, gas-phase separation and thermal cracking system based on ethylation derivation of methyl mercury |
| CN106644664A (en) * | 2017-01-06 | 2017-05-10 | 中国海洋大学 | Thermal desorption-gas phase separation-thermal pyrolysis system based on phenylated derived organic mercury |
| CN108333380A (en) * | 2018-01-25 | 2018-07-27 | 北京普立泰科仪器有限公司 | A kind of automatic sampling apparatus and its automatic sampling method |
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| CN1707259A (en) * | 2004-06-04 | 2005-12-14 | 中国科学院大连化学物理研究所 | Apparatus used for solid absorption stirrer thermal analyzer |
| US20060088442A1 (en) * | 2004-10-26 | 2006-04-27 | The Regents Of The University Of California | Chemical thermal desorption system |
| CN203606200U (en) * | 2013-12-05 | 2014-05-21 | 中国科学院大连化学物理研究所 | Rapid thermal desorption sampling device |
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2015
- 2015-03-23 CN CN201510126439.3A patent/CN104713966B/en not_active Expired - Fee Related
Patent Citations (3)
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| CN1707259A (en) * | 2004-06-04 | 2005-12-14 | 中国科学院大连化学物理研究所 | Apparatus used for solid absorption stirrer thermal analyzer |
| US20060088442A1 (en) * | 2004-10-26 | 2006-04-27 | The Regents Of The University Of California | Chemical thermal desorption system |
| CN203606200U (en) * | 2013-12-05 | 2014-05-21 | 中国科学院大连化学物理研究所 | Rapid thermal desorption sampling device |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104819885A (en) * | 2015-05-13 | 2015-08-05 | 河南理工大学 | Thermal analysis device of elemental mercury in gold amalgam adsorption tube |
| CN106442811A (en) * | 2016-09-18 | 2017-02-22 | 中国海洋大学 | Thermal desorption, gas-phase separation and thermal cracking system based on ethylation derivation of methyl mercury |
| CN106442811B (en) * | 2016-09-18 | 2019-03-05 | 中国海洋大学 | Based on the derivative methyl mercury Thermal desorption-gas phase separation-thermal splitting system that ethylizes |
| CN106644664A (en) * | 2017-01-06 | 2017-05-10 | 中国海洋大学 | Thermal desorption-gas phase separation-thermal pyrolysis system based on phenylated derived organic mercury |
| CN106644664B (en) * | 2017-01-06 | 2019-05-10 | 中国海洋大学 | One kind is based on the derivative organic mercury Thermal desorption-gas phase separation-thermal splitting system of phenylating |
| CN108333380A (en) * | 2018-01-25 | 2018-07-27 | 北京普立泰科仪器有限公司 | A kind of automatic sampling apparatus and its automatic sampling method |
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| CN104713966B (en) | 2016-11-30 |
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Granted publication date: 20161130 Termination date: 20200323 |