CN107202858B - A kind of composite purification additive for direct mercury vapourmeter and its application in direct mercury vapourmeter - Google Patents
A kind of composite purification additive for direct mercury vapourmeter and its application in direct mercury vapourmeter Download PDFInfo
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- CN107202858B CN107202858B CN201710429606.0A CN201710429606A CN107202858B CN 107202858 B CN107202858 B CN 107202858B CN 201710429606 A CN201710429606 A CN 201710429606A CN 107202858 B CN107202858 B CN 107202858B
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- mercury vapourmeter
- composite purification
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- direct mercury
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- 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
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
- G01N2021/3107—Cold vapor, e.g. determination of Hg
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Abstract
It is as made from the raw material of following parts by weight the invention discloses a kind of composite purification additive for direct mercury vapourmeter: 30-40 parts of powdered whiting, 5-9 parts of line borate, 3-5 parts of nickel sesquioxide, 1-3 parts of tungsten carbide, 2 parts of graphene, 8-12 parts, -40 parts of carrier 30 as one kind of raising agent.The invention also discloses the application of the composite purification additive in direct mercury vapourmeter.Composite purification additive preparation process of the invention is simple, and purification efficiency is high, low in cost; direct mercury vapourmeter catalysing tube service life can effectively be extended, reduce smoke contamination, each components inside effective protection equipment; prolong the service life, reduces the maintenance cost of direct mercury vapourmeter.It does not need to improve equipment, technique, detection method in the composite purification additive use process, while the rate of recovery of mercury can also be improved, to improve the accuracy of the detection method.
Description
Technical field
The invention belongs to detection fields, and in particular to a kind of for the composite purification additive of direct mercury vapourmeter and its straight
Connect the application in mercury vapourmeter.
Background technique
Direct injected-cold-vapour atomic absorption method measurement mercury content is not necessarily to sample treatment, and directly sample is sent into instrument,
Under the load of oxygen stream, sample is dried, and is then thermal decomposited；Product after thermal decomposition enters catalysing tube, halogen therein and
For nitrogen oxysulfide by Catalyst Adsorption, mercury is reduced into mercury atom, and mercuryvapour is changed pipe together and collects the complete gold amalgam reaction of progress,
Subsequent high temperature parsing；The mercury finally parsed at 254nm wavelength with Cold-Atom Absorption Spectrometry for Determining in absorption cell, thus
Time saving simply without reagent contamination and environmental pollution, high sensitivity, accuracy are good, and execute Environmental Protection in America EP7473 method.Each
The samples such as kind sample such as coal fly ash, coke, combustion residue, soil, organic matter, food, Atmospheric particulates, environmental sample, mineral products
Middle Mercury Determination has been shown in document report or issuing standard, thus this kind of inspection technology is applied widely in a variety of industries,
Only in quality inspection and inspection and quarantine system, MILSTONE company, import Italy and the direct mercury vapourmeter of LEMAN company, the U.S. are close over 2 years
Hundred, it is mainly used in the inspection of import and field of circulation coal, the large mineral products of import and other imports.
Currently, import equipment consumptive material is expensive, and one is urged during direct injected-cold atomic absorption mercury spectrometry
Change nearly 4,000 yuan of pipe, there are the higher problems of consumables cost.Sample such as coal, copper concentrate, the zinc lead concentrate of sulphur are rich in detection
When, elemental sulfur and reduced sulfur therein will affect the test of instrument, the failure of accelerator activator.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides sulphur and halogens, nitrogen oxides in a kind of reduction thermal decomposition product
Content extends the composite purification additive for direct mercury vapourmeter of the service life of catalysing tube.
The present invention also provides the application of the composite purification additive in direct mercury vapourmeter.
The present invention is achieved through the following technical solutions:
A kind of composite purification additive for direct mercury vapourmeter, is as made from the raw material of following parts by weight: heavy carbon
Sour calcium 30-40 parts, 5-9 parts of line borate, 3-5 parts of nickel sesquioxide, 1-3 parts of tungsten carbide, 2 parts of graphene, 8-12 parts of raising agent, load
30-40 parts of body.
Described, raising agent is made from the weight ratio of silicon powder and paper mill sludge ash according to 1:1.5-2.
Described, carrier is made from the weight ratio of kaolin, corundum and diatomite according to 1:0.8-1:1-1.5.
Described, paper mill sludge ash is powder obtained by paper mill sludge is burned at 750 DEG C, and the screening of 200 meshes tails over and is less than
10%.
A kind of application for the composite purification additive of direct mercury vapourmeter in direct mercury vapourmeter, composite purification additive
After mixing with sample, it adds in direct mercury vapourmeter and is detected, operated according to operating instruction.
Described, the weight ratio of composite purification additive and sample is 1-50:100.
Described, sample is high sulfur fossil or coal.
Composite purification additive of the invention, is as made from following methods:
1) each raw material is crushed to 200 mesh, by powdered whiting, line borate, nickel sesquioxide, tungsten carbide, stone after crushing
Black alkene and raising agent are uniformly mixed, and obtain initial material；
2) initial material is added in carrier, is uniformly mixed, obtains powder；
3) powder is roasted at 650 DEG C 5h, can be prepared by composite purification additive.
Beneficial effects of the present invention:
Composite purification additive preparation process of the invention is simple, and purification efficiency is high, low in cost, can effectively extend straight
Mercury vapourmeter catalysing tube service life is connect, smoke contamination is reduced, each components inside effective protection equipment prolong the service life, drop
The maintenance cost of low direct mercury vapourmeter.Do not needed in the composite purification additive use process to equipment, technique, detection method into
Row improves, while can also improve the rate of recovery of mercury, to improve the accuracy of the detection method.
Specific embodiment
Below with reference to embodiment, the present invention will be further described.
The raw materials used in the present invention is market purchase gained.
Embodiment 1
A kind of composite purification additive for direct mercury vapourmeter, is as made from the raw material of following parts by weight: heavy carbon
40 parts of sour calcium, 5 parts of line borate, 3 parts of nickel sesquioxide, 1 part of tungsten carbide, 2 parts of graphene, 12 parts of raising agent, carrier 30 as one kind part.
Described, raising agent is made from the weight ratio of silicon powder and paper mill sludge ash according to 1:1.5.
Described, carrier is made from the weight ratio of kaolin, corundum and diatomite according to 1:1:1.
Described, paper mill sludge ash is powder obtained by paper mill sludge is burned at 750 DEG C, and the screening of 200 meshes tails over and is less than
10%.
A kind of application for the composite purification additive of direct mercury vapourmeter in direct mercury vapourmeter, composite purification additive
After mixing with sample, it adds in direct mercury vapourmeter and is detected, operated according to operating instruction.
Described, the weight ratio of composite purification additive and sample is 50:100.
Described, sample is high sulfur fossil or coal.
The composite purification additive of the present embodiment, is as made from following methods:
1) each raw material is crushed to 200 mesh, by powdered whiting, line borate, nickel sesquioxide, tungsten carbide, stone after crushing
Black alkene and raising agent are uniformly mixed, and obtain initial material；
2) initial material is added in carrier, is uniformly mixed, obtains powder；
3) powder is roasted at 650 DEG C 5h, can be prepared by composite purification additive.
It is demonstrated experimentally that the clearing machine and sample to be tested equal proportion are used in mixed way, catalysis tube lifetime 1.5 can be extended again with
On, 95% or more is reached to sulphur in thermal decomposition product and halogen, nox purification rate, hence it is evident that improve the rate of recovery of mercury, simultaneously
Reduce smoke contamination, each components inside effective protection equipment extend complete machine service life, reduce the maintenance of direct mercury vapourmeter at
This.
Embodiment 2
A kind of composite purification additive for direct mercury vapourmeter, is as made from the raw material of following parts by weight: heavy carbon
35 parts of sour calcium, 7 parts of line borate, 4 parts of nickel sesquioxide, 2 parts of tungsten carbide, 2 parts of graphene, 10 parts of raising agent, 35 parts of carrier.
Described, raising agent is made from the weight ratio of silicon powder and paper mill sludge ash according to 1:1.8.
Described, carrier is made from the weight ratio of kaolin, corundum and diatomite according to 1:0.9:1.3.
Described, paper mill sludge ash is powder obtained by paper mill sludge is burned at 750 DEG C, and the screening of 200 meshes tails over and is less than
10%.
A kind of application for the composite purification additive of direct mercury vapourmeter in direct mercury vapourmeter, composite purification additive
After mixing with sample, it adds in direct mercury vapourmeter and is detected, operated according to operating instruction.
Described, the weight ratio of composite purification additive and sample is 30:100.
Described, sample is high sulfur fossil or coal.
Remaining is the same as embodiment 1.
It is demonstrated experimentally that the clearing machine and sample to be tested equal proportion are used in mixed way, catalysis tube lifetime 1.5 can be extended again with
On, 90% or more is reached to sulphur in thermal decomposition product and halogen, nox purification rate, hence it is evident that improve the rate of recovery of mercury, simultaneously
Reduce smoke contamination, each components inside effective protection equipment extend complete machine service life, reduce the maintenance of direct mercury vapourmeter at
This.
Embodiment 3
A kind of composite purification additive for direct mercury vapourmeter, is as made from the raw material of following parts by weight: heavy carbon
30 parts of sour calcium, 9 parts of line borate, 5 parts of nickel sesquioxide, 3 parts of tungsten carbide, 2 parts of graphene, 8 parts of raising agent, 40 parts of carrier.
Described, raising agent is made from the weight ratio of silicon powder and paper mill sludge ash according to 1:2.
Described, carrier is made from the weight ratio of kaolin, corundum and diatomite according to 1:0.8:1.5.
Described, paper mill sludge ash is powder obtained by paper mill sludge is burned at 750 DEG C, and the screening of 200 meshes tails over and is less than
10%.
A kind of application for the composite purification additive of direct mercury vapourmeter in direct mercury vapourmeter, composite purification additive
After mixing with sample, it adds in direct mercury vapourmeter and is detected, operated according to operating instruction.
Described, the weight ratio of composite purification additive and sample is 1:100.
Described, sample is high sulfur fossil or coal.
Remaining is the same as embodiment 1.
It is demonstrated experimentally that the clearing machine and sample to be tested equal proportion are used in mixed way, 1 times of tube lifetime of catalysis or more can be extended,
85% or more is reached to sulphur in thermal decomposition product and halogen, nox purification rate, hence it is evident that the rate of recovery for improving mercury reduces simultaneously
Smoke contamination, each components in effective protection equipment inside, extends complete machine service life, reduces the maintenance cost of direct mercury vapourmeter.
Claims (4)
1. a kind of composite purification additive for direct mercury vapourmeter, which is characterized in that be made by the raw material of following parts by weight
:
It is 30-40 parts of powdered whiting, 5-9 parts of line borate, 3-5 parts of nickel sesquioxide, 1-3 parts of tungsten carbide, 2 parts of graphene, loose
8-12 parts, -40 parts of carrier 30 as one kind of agent；
The raising agent is made from the weight ratio of silicon powder and paper mill sludge ash according to 1:1.5-2；
The carrier is made from the weight ratio of kaolin, corundum and diatomite according to 1:0.8-1:1-1.5；
The paper mill sludge ash is powder obtained by paper mill sludge is burned at 750 DEG C, and the screening of 200 meshes is tailed over less than 10%.
2. a kind of claim 1 is used for application of the composite purification additive of direct mercury vapourmeter in direct mercury vapourmeter, feature
It is, the composite purification additive and sample after mixing, are added in direct mercury vapourmeter and detected.
3. the application according to claim 2 in direct mercury vapourmeter, which is characterized in that the composite purification additive and
The weight ratio of sample is 1-50:100.
4. the application according to claim 2 in direct mercury vapourmeter, which is characterized in that the sample be high sulfur fossil or
Coal.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710429606.0A CN107202858B (en) | 2017-06-09 | 2017-06-09 | A kind of composite purification additive for direct mercury vapourmeter and its application in direct mercury vapourmeter |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710429606.0A CN107202858B (en) | 2017-06-09 | 2017-06-09 | A kind of composite purification additive for direct mercury vapourmeter and its application in direct mercury vapourmeter |
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| Publication Number | Publication Date |
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| CN107202858A CN107202858A (en) | 2017-09-26 |
| CN107202858B true CN107202858B (en) | 2019-06-18 |
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| CN201710429606.0A Expired - Fee Related CN107202858B (en) | 2017-06-09 | 2017-06-09 | A kind of composite purification additive for direct mercury vapourmeter and its application in direct mercury vapourmeter |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112747994A (en) * | 2020-12-25 | 2021-05-04 | 防城海关综合技术服务中心 | Sulfur-fixing agent for directly measuring mercury by solid sample introduction |
| CN113092658A (en) * | 2021-04-07 | 2021-07-09 | 防城海关综合技术服务中心 | Method for prolonging service life of solid sample introduction direct mercury detector consumable |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2024154C (en) * | 1989-08-31 | 1995-02-14 | Senshi Kasahara | Catalyst for reducing nitrogen oxides from exhaust gas |
| US5417948A (en) * | 1992-11-09 | 1995-05-23 | Japan Pionics Co., Ltd. | Process for cleaning harmful gas |
| CN1381596A (en) * | 2002-05-17 | 2002-11-27 | 长春市南湖稀土合金厂 | Moisture-proof acive lime as composite desulfurizing agent |
| CN101386785A (en) * | 2008-10-24 | 2009-03-18 | 中国科学院山西煤炭化学研究所 | Desulphurizer for high-sulphur coal coke making and preparation method and applications |
| CN105854831A (en) * | 2016-06-20 | 2016-08-17 | 浙江澄宇环保新材料股份有限公司 | Calcium carbonate compound for desulfurization and denitrification |
| CN106139849A (en) * | 2009-01-12 | 2016-11-23 | Ifp 新能源公司 | The sulfur-bearing that comprises in synthesis gas for removing, nitrogenous and containing the method for halogen impurities |
-
2017
- 2017-06-09 CN CN201710429606.0A patent/CN107202858B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2024154C (en) * | 1989-08-31 | 1995-02-14 | Senshi Kasahara | Catalyst for reducing nitrogen oxides from exhaust gas |
| US5417948A (en) * | 1992-11-09 | 1995-05-23 | Japan Pionics Co., Ltd. | Process for cleaning harmful gas |
| CN1381596A (en) * | 2002-05-17 | 2002-11-27 | 长春市南湖稀土合金厂 | Moisture-proof acive lime as composite desulfurizing agent |
| CN101386785A (en) * | 2008-10-24 | 2009-03-18 | 中国科学院山西煤炭化学研究所 | Desulphurizer for high-sulphur coal coke making and preparation method and applications |
| CN106139849A (en) * | 2009-01-12 | 2016-11-23 | Ifp 新能源公司 | The sulfur-bearing that comprises in synthesis gas for removing, nitrogenous and containing the method for halogen impurities |
| CN105854831A (en) * | 2016-06-20 | 2016-08-17 | 浙江澄宇环保新材料股份有限公司 | Calcium carbonate compound for desulfurization and denitrification |
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