CN105699160A - Method and device for removing trace mercury in carrier gas - Google Patents
Method and device for removing trace mercury in carrier gas Download PDFInfo
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- CN105699160A CN105699160A CN201610028891.0A CN201610028891A CN105699160A CN 105699160 A CN105699160 A CN 105699160A CN 201610028891 A CN201610028891 A CN 201610028891A CN 105699160 A CN105699160 A CN 105699160A
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- carrier gas
- trace
- mercury
- gas
- drying tube
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
Abstract
The invention discloses a method and device for removing trace mercury in carrier gas.The method comprises the steps that the carrier gas is fed into a container containing an acidic potassium permanganate solution, so that the trace zero-valent mercury in the carrier gas is oxidized into mercury ions by the acidic potassium permanganate solution to be retained in the container; after the carrier gas is dehumidified through a drying agent, extremely trace amount of gaseous-state element mercury in the carrier gas is removed through physical non-specific adsorption.The method and device have the advantages that the effect is good, using of the carrier gas is not influenced, no secondary pollution is generated, the device is small and exquisite, distribution is flexible, installation is convenient, no power is needed, and management is easy and are widely applied to the low-concentration mercury-containing sample analysis process in the fields of environmental monitoring, detecting on trace mercury in food and medicine, teaching and scientific researching and the like.
Description
Technical field
The present invention relates to a kind of method removing Trace Hg and device, especially remove method and the device of Trace Hg in carrier gas, belong to trace element detection analysis technical field。
Background technology
Hydrargyrum, as many commercial production, the indispensable material of scientific research, plays an important role in productive life。But, hydrargyrum has toxicity, can cause the pollution of environment, threatens human health。Since minamata disease event occurs in 50-60 in last century age Japan, Mercury In Environment problem has caused countries in the world to show great attention to。China is the first big country of the production of hydrargyrum, use, consumption and discharge in the world, therefore it is faced with huge environmental mercury pressure, brings environmental sample (water sample, earth sample, plant sample, animal sample), food samples, drug sample mercury content to analyze upsurge therewith。Along with development in science and technology, the analytical technology of hydrargyrum progressively moves towards the mercurous sample high precision of low concentration, high accuracy is analyzed, and at quality control procedure, in carrier gas (in mercurous sample detection analysis process use), the removal of Trace Hg plays most important effect, directly affect accuracy and the elaboration of the mercurous analysis of low concentration, for this, the nitrogen used in sample pretreatment process at present, the argon that instrument flow phase uses is highly purified, but owing to each production and processing links control of current hyperpure gas is not in place, still can be mixed into Trace Hg, so that affecting precision and the accuracy that the mercurous sample detection of low concentration is analyzed。
Summary of the invention
The technical problem to be solved is in that to provide a kind of and removes the method for Trace Hg in carrier gas and provide a kind of simultaneously and remove the device of Trace Hg in carrier gas, carrier gas is purified, thus improving precision and the accuracy that the mercurous sample detection of low concentration is analyzed。
For solving above-mentioned technical problem, the technical solution used in the present invention is as follows:
A kind of remove the method for Trace Hg in carrier gas, the method is first to send into carrier gas equipped with in the container of acid permanganate soln, make the trace nonvalent mercury in carrier gas be oxidized to mercury ion residue in container by acid permanganate soln, after then carrier gas drying agent being dehumidified, with gold sand, the gaseous elementary mercury of denier in carrier gas is passed through the non-obligate Adsorption of physics。
A kind of removing the device of Trace Hg in carrier gas, this device is by opaque casing and is arranged on the gas flowmeter in casing, oxic gas bubble vial, drying tube and gold amalgam pipe and constitutes；In oxic gas bubble vial built with acid permanganate soln, being filled with desiccant in drying tube, desiccant two ends block with silica wool, are filled with gold sand in gold amalgam pipe, and gold sand two ends block with silica wool；Being respectively provided on two sides with air inlet and venthole at casing, air inlet connects gas flowmeter, and gas flowmeter connects oxic gas bubble vial, and oxic gas bubble vial connects drying tube, and drying tube connects gold amalgam pipe, and gold amalgam pipe connects the venthole of casing。
Above-mentioned removes in carrier gas in the device of Trace Hg, and described casing is preferably PVC material, and oxic gas bubble vial is preferably Pyrex material, and drying tube is preferably Pyrex material。
In aforesaid removal carrier gas in the device of Trace Hg, described oxic gas bubble vial, drying tube and gold amalgam pipe need to soak before the use in the salpeter solution of 20% > 24h, then clean up with the clean ultra-pure water without hydrargyrum, 500 DEG C of high temperature dry combustion methods after wrapping up with masking foil > 30min, use after cooling in cleaning is without the environment of hydrargyrum；Silica wool needs before using to use masking foil parcel, 500 DEG C of high temperature dry combustion methods > 30min, use after cooling in cleaning is without the environment of hydrargyrum。
Beneficial effect: compared with prior art, the present invention utilizes chemical oxidation and the principle of the non-obligate absorption of physics, the technical measures that acid potassium permanganate oxidation is combined with gold amalgam Adsorption Phase are adopted to remove Trace Hg in carrier gas, carrier gas is purified, improve precision and accuracy that the mercurous sample detection of low concentration is analyzed, in environmental monitoring, food and medicine, the field such as Trace Hg detection, teaching and scientific research is widely applied。
The major advantage of the present invention is as follows: (1) achieves the removal of Trace Hg in carrier gas, respond well, do not affect the use of carrier gas, non-secondary pollution, repeatable utilization after changing acid permanganate soln and gold amalgam pipe being added thermal purification, the feature there is sustainable purification, recycling。(2) device is small and exquisite, flexible arrangement, easy for installation, does not need power, and management is simple, is widely applied in environmental monitoring, food and medicine in the mercurous sample analysis process of field low concentration such as Trace Hg detection, teaching and scientific research。
Accompanying drawing explanation
Fig. 1 is assembly of the invention structural representation；
Fig. 2 is assembly of the invention principle schematic；
Fig. 3 is the structural representation of the oxic gas bubble vial of the present invention；
Fig. 4 is the structural representation of the drying tube of the present invention；
Fig. 5 is the structural representation of the gold amalgam pipe of the present invention。
Below in conjunction with the drawings and specific embodiments, the present invention is further illustrated。
Detailed description of the invention
Embodiment 1: as shown in Figure 1, by opaque casing 1 and be arranged on the gas flowmeter 2 in casing 1, oxic gas bubble vial 3, drying tube 4 and gold amalgam pipe 5 and constitute, casing 1 adopts PVC material manufacture, light tight, the potassium permanganate solution in oxic gas bubble vial 3 can be avoided to see photolysis, improve the continued oxidation ability of potassium permanganate。Gas flowmeter 2 is arranged on the inside dead ahead of casing 1, according to the manually adjustable carrier gas flux of practical measurement requirement。It is respectively provided on two sides with air inlet 10 and venthole 11 at casing 1, air inlet 10 connects gas flowmeter 2, and gas flowmeter 2 connects oxic gas bubble vial 3, and oxic gas bubble vial 3 connects drying tube 4, drying tube 4 connects gold amalgam pipe 5, and gold amalgam pipe 5 connects the venthole 11 of casing 1。As it is shown on figure 3, oxic gas bubble vial 3 is Pyrex material, in oxic gas bubble vial 3 built with acid potassium permanganate (saturated) solution 6。As shown in Figure 4, drying tube 4 is Pyrex material, desiccant 7 it is filled with in drying tube 4, desiccant 7 selects Germany to produce Sodalime(purchased from Sigma-Alorich company), the two ends of desiccant 7 block with silica wool 8, load good after pass into carrier gas and carry out sky and blow, by tiny fine particle stripping。As it is shown in figure 5, be filled with gold sand 9 in gold amalgam pipe 5, gold sand particle diameter is 60 orders, and gold sand 9 two ends block with silica wool 8。This device needs extremely strict quality control in installing and using process, must assure that and operate in cleaning is without the environment of hydrargyrum and avoid cross-contamination, oxic gas bubble vial 3, drying tube 4 and gold amalgam pipe 5 need to soak before the use in the salpeter solution of 20% > 24h, then clean up with the clean ultra-pure water without hydrargyrum, 500 DEG C of high temperature dry combustion methods in Muffle furnace after wrapping up with masking foil > 30min, use after cooling in cleaning is without the environment of hydrargyrum；Silica wool 8 needs before using to use masking foil parcel, 500 DEG C of high temperature dry combustion methods > 30min, use after cooling in cleaning is without the environment of hydrargyrum。
During use, air inlet 10 and gas flowmeter 2 is connected with carrier gas pipe 13,1L acid permanganate soln 6 is loaded in oxic gas bubble vial 3, put into casing 1 after connecting bubble bar and fix, then connecting drying tube 4 and gold amalgam pipe 5, the gas outlet carrier gas pipe 13 of gold amalgam pipe 5 is attached with the venthole 11 of casing 1。Carrier gas pipe 13 is Teflon material, it is necessary to soak in the salpeter solution of 20% > 24h, clean up with ultra-pure water, use after drying in cleaning is without the environment of hydrargyrum。Acid permanganate soln 6 in oxic gas bubble vial 3 to regularly replace, due to the mercury content of carrier gas, that gas makes consumption be difficult to is constant, color change generally according to solution judges whether to change acid permanganate soln 6, when namely replaceable after the lighter of solution。
Operation principle: as shown in Figure 2, carrier gas 12(argon or nitrogen) first pass around after gas flowmeter 2 regulates the flow velocity of carrier gas and enter in oxic gas bubble vial 3, the acid permanganate soln 6 in the oxidized bubble bottle 3 of trace nonvalent mercury in carrier gas is oxidized to mercury ion residue in oxic gas bubble vial 3, then carrier gas enters in drying tube 4, enter after drying agent 7 dehumidifying in gold amalgam pipe 5, the gaseous elementary mercury of denier in carrier gas can be passed through the non-obligate Adsorption of physics by the gold sand 9 loaded in gold amalgam pipe 5, thus reaching to purify the purpose of carrier gas。
Embodiments of the present invention are not limited to above-described embodiment, and the various changes made under the premise without departing from present inventive concept belong within protection scope of the present invention。
Claims (4)
1. remove the method for Trace Hg in carrier gas for one kind, it is characterized in that: first carrier gas is sent into equipped with in the container of acid permanganate soln, make the trace nonvalent mercury in carrier gas be oxidized to mercury ion residue in container by acid permanganate soln, after then carrier gas drying agent being dehumidified, with gold sand, the gaseous elementary mercury of denier in carrier gas is passed through the non-obligate Adsorption of physics。
2. remove the device of Trace Hg in carrier gas for one kind, it is characterised in that: this device is by opaque casing (1) and is arranged on the gas flowmeter (2) in casing (1), oxic gas bubble vial (3), drying tube (4) and gold amalgam pipe (5) and constitutes；In oxic gas bubble vial (3) built with acid permanganate soln (6), desiccant (7) it is filled with in drying tube (4), desiccant (7) two ends block with silica wool (8), are filled with gold sand (9) in gold amalgam pipe (5), and gold sand (9) two ends block with silica wool (8)；It is respectively provided on two sides with air inlet (10) and venthole (11) at casing (1), air inlet (10) connects gas flowmeter (2), gas flowmeter (2) connects oxic gas bubble vial (3), oxic gas bubble vial (3) connects drying tube (4), drying tube (4) connects gold amalgam pipe (5), and gold amalgam pipe (5) connects the venthole (11) of casing (1)。
3. the device of Trace Hg in removal carrier gas according to claim 2, it is characterised in that: described casing (1) is PVC material, and oxic gas bubble vial (3) is Pyrex material, and drying tube (4) is Pyrex material。
4. the device of Trace Hg in removal carrier gas according to claim 2, it is characterized in that: described oxic gas bubble vial (3), drying tube (4) and gold amalgam pipe (5) need to soak before the use in the salpeter solution of 20% 24h, then clean up with the clean ultra-pure water without hydrargyrum, 500 DEG C of high temperature dry combustion methods after wrapping up with masking foil > 30min, use after cooling in cleaning is without the environment of hydrargyrum；Silica wool (8) needs before using to use masking foil parcel, 500 DEG C of high temperature dry combustion methods > 30min, use after cooling in cleaning is without the environment of hydrargyrum。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610028891.0A CN105699160A (en) | 2016-01-18 | 2016-01-18 | Method and device for removing trace mercury in carrier gas |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610028891.0A CN105699160A (en) | 2016-01-18 | 2016-01-18 | Method and device for removing trace mercury in carrier gas |
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| CN105699160A true CN105699160A (en) | 2016-06-22 |
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| CN201610028891.0A Pending CN105699160A (en) | 2016-01-18 | 2016-01-18 | Method and device for removing trace mercury in carrier gas |
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Cited By (4)
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| CN108956238A (en) * | 2018-09-12 | 2018-12-07 | 河南理工大学 | A kind of separation of Hg in natural gas, purification system and method |
| CN109253994A (en) * | 2018-10-31 | 2019-01-22 | 中国石油天然气股份有限公司 | A kind of oil-gas-source mercury isotope detection method and device |
| US10816532B2 (en) | 2018-10-31 | 2020-10-27 | Petrochina Company Limited | Methods and devices for detecting mercury isotopes in crude oil |
| US11119084B2 (en) | 2018-10-31 | 2021-09-14 | Petrochina Company Limited | Methods and devices for detecting mercury isotopes in natural gas |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108956238A (en) * | 2018-09-12 | 2018-12-07 | 河南理工大学 | A kind of separation of Hg in natural gas, purification system and method |
| CN109253994A (en) * | 2018-10-31 | 2019-01-22 | 中国石油天然气股份有限公司 | A kind of oil-gas-source mercury isotope detection method and device |
| AU2019202479B1 (en) * | 2018-10-31 | 2020-04-30 | Petrochina Company Limited | Methods and Devices for detecting mercury isotopes in oil-gas sources |
| US10816532B2 (en) | 2018-10-31 | 2020-10-27 | Petrochina Company Limited | Methods and devices for detecting mercury isotopes in crude oil |
| CN109253994B (en) * | 2018-10-31 | 2021-05-28 | 中国石油天然气股份有限公司 | Oil and gas source mercury isotope detection method and device |
| US11119085B2 (en) | 2018-10-31 | 2021-09-14 | Petrochina Company Limited | Methods and devices for detecting mercury isotopes in oil-gas sources |
| US11119084B2 (en) | 2018-10-31 | 2021-09-14 | Petrochina Company Limited | Methods and devices for detecting mercury isotopes in natural gas |
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