CN104330379B - The preparation method and device of a kind of normal concentration arsenic trioxide gas - Google Patents
The preparation method and device of a kind of normal concentration arsenic trioxide gas Download PDFInfo
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- CN104330379B CN104330379B CN201410613003.2A CN201410613003A CN104330379B CN 104330379 B CN104330379 B CN 104330379B CN 201410613003 A CN201410613003 A CN 201410613003A CN 104330379 B CN104330379 B CN 104330379B
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Abstract
The present invention relates to a kind of preparation method of normal concentration arsenic trioxide gas, the method is comprised the steps of：(1) sample cell of a three-stage is selected, the sample cell has the first chamber of rods arranged in horizontal line, second chamber and the 3rd chamber successively, wherein being equipped with the window of permeable to infrared spectrum signal between two of the sample cell and first chamber and second chamber and second chamber and the 3rd chamber between；(2) three chambers of the sample cell are vacuumized, and nitrogen and arsenic trioxide is added in second chamber and three chambers are sealed；Then, the sample cell is integrally heated to making the arsenic trioxide in second chamber be gasified totally；Wherein, the addition of nitrogen and arsenic trioxide meets in the second chamber, and pressure in second chamber is a standard atmospheric pressure after arsenic trioxide is gasified totally.Pond body is separated into three independent chambers by the sample cell the invention further relates to realize the three-stage of the above method, the sample cell by four windows.
Description
Technical field
Tested the present invention relates to the chemically or physically property by means of measure material or analysis of material, and in particular to test
With the preparation method and device of sample.
Background technology
The existing forms of the arsenic of arsenic-containing gold concentrate smelting process have material impact, roasting process to gold yield and quality
Arsenic is volatilized with the gaseous state of arsenic trioxide when middle oxygen is insufficient, and arsenic is deposited with the solid states of diarsenic pentoxide when oxygen is abundant
The arsenate of the difficult volatilization of the generation such as the di-iron trioxide in, diarsenic pentoxide with slag, lead oxide, can cause the secondary of gold
Parcel, reduces the quantum of output and quality of gold.Therefore, the concentration of arsenic trioxide gas in roaster is accurately monitored in real time,
Based Intelligent Control for arsenic-containing gold concentrate smelting process is significant.
Arsenic trioxide is noxious material, and temperature is solid-state when being less than 200 DEG C.Traditional extraction-type measuring method sampling is surveyed
Amount and pretreatment need the regular hour, it is impossible to realize real-time monitoring；Sampling process can cause the absorption of arsenic trioxide, it is impossible to
Realize accurate measurement.Infrared spectrum technology has non-cpntact measurement, and measurement sensitivity is high, the features such as fast response time, Ke Yishi
The accurate real time on-line monitoring of existing arsenic trioxide.But, it is necessary to use concentration known during using ft-ir measurement, temperature,
The arsenic trioxide gas of pressure is demarcated and calibrated to measuring apparatus, but known temperature is obtained in reality, and the three of pressure
It is highly difficult to aoxidize two arsenic normal concentration gases.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of normal concentration arsenic trioxide gas.
Another technical problem to be solved by this invention is to provide a kind of device for realizing the above method.
Technical proposal that the invention solves the above-mentioned problems is as follows：
A kind of preparation method of normal concentration arsenic trioxide gas, the method is comprised the steps of：
(1) selecting the sample cell of a three-stage, the sample cell has the first chamber of rods arranged in horizontal line, second chamber successively
With the 3rd chamber, wherein between two of the sample cell and first chamber and second chamber and second chamber and the 3rd chamber it
Between be equipped with the window of permeable to infrared spectrum signal；
(2) three chambers of the sample cell are vacuumized, and nitrogen and arsenic trioxide is added simultaneously in second chamber
Three chambers of sealing；Then, the sample cell is integrally heated to making the arsenic trioxide in second chamber be gasified totally；
Wherein, in the second chamber nitrogen and arsenic trioxide addition meet, arsenic trioxide be gasified totally after second chamber
Interior pressure is a standard atmospheric pressure.
A kind of sample cell of the three-stage for realizing the above method, it is characterised in that the sample cell includes the pond body of a tubular,
Two of the pond body is respectively equipped with one only through the window of infrared spectroscopy signals, and middle part is provided with two and only passes through infrared spectrum
The window of signal；Pond body is separated into three independent chambers by four described windows, forms first chamber, second chamber and the
Three chambers.
It is equal in order to ensure the vacuum in first chamber and the 3rd chamber room, the sample cell of three-stage of the present invention
An improvement project be that pipe is communicated with the outside of described pond body, the communicating pipe is by first chamber and the 3rd chamber.
In order that the surrounding of the sample cell is heated evenly, another improvement of the sample cell of three-stage of the present invention
Scheme is that the described sample cell also resistance wire including heating, the resistance wire is wrapped on the outer wall of the pond body.
Standard items are needed to compare the collection of illustrative plates for obtaining standard items during due to using ft-ir measurement gas concentration, then
The absorbance of comparative sample and standard items determines the concentration of sample, and arsenic trioxide need 457.2 DEG C high temperature
Can gasify, therefore, it is difficult to obtain using the standard items of ft-ir measurement arsenic trioxide gas concentration.The present invention uses institute
Stating the sample cell of three-stage can not only readily obtain arsenic trioxide gas, and the second chamber in the middle part of the sample cell
Indoor pressure is a standard atmospheric pressure, and the Pressure, Concentration, Temperature of gas is also known, so the present invention is solved well
It is technical barrier that arsenic trioxide gas standard product are difficult to acquisition in the prior art.
Additionally, first chamber and the 3rd chamber that scheme of the present invention will be located at two are vacuumized, by second chamber two
The window of head is isolated from the outside, and not only can guarantee that the temperature of second chamber gas is uniform, and can avoid arsenic trioxide gas
Condensation is attached on window and influences to detect the transmitance of light, causes measured gas concentration value inaccurate.
Brief description of the drawings
Fig. 1 is a schematic diagram for specific embodiment of the sample cell of three-stage of the present invention.
Specific embodiment
First, the structure design of sample cell
Referring to Fig. 1, the pond body 1 of sample cell is the tubular structure of cylinder, and its two is respectively equipped with one only through infrared
The window 2 of spectral signal, middle part is provided with two only through the window 2 of infrared spectroscopy signals；Four described windows 2 are by tubular
Pond body 1 is separated into three independent cylindrical chamber, forms first chamber 7, the chamber 9 of second chamber 8 and the 3rd.
Referring to Fig. 1, in this example, the length L=100mm of second chamber 8, radius r=20mm.
Referring to Fig. 1, the outside of described pond body 1 is communicated with pipe 3, and the communicating pipe 3 is by the chamber 9 of first chamber 7 and the 3rd
Connection.
Referring to Fig. 1, described resistance wire 4 of the sample cell including heating, the resistance wire 4 is wrapped in the outer of the pond body 1
On wall.Herein it should be noted that when it is conductor to make the material of pond body 1, described resistance wire 4 can be arranged earthenware, to keep away
Exempt from short circuit, these general knowledge all known to a person of ordinary skill in the art.
Referring to Fig. 1, be additionally provided with two import and export 5 in described pond body 1, two import and export 5 respectively with the chamber of first chamber 7 and second
Room 8 connects, and every one or two imports and exports 5 is provided with stop valve 6.
2nd, the preparation of normal concentration arsenic trioxide gas
Three chambers of the sample cell shown in Fig. 1 are vacuumized, and nitrogen and arsenic trioxide are added in second chamber 8
And seal three chambers；Then, the sample cell is integrally heated to 470 DEG C, makes the arsenic trioxide in second chamber complete
Gasification.Wherein, the addition of nitrogen and arsenic trioxide meets in the second chamber 8, arsenic trioxide be gasified totally after the
Pressure in two chambers is a standard atmospheric pressure.
Referring to Fig. 1, make in second chamber 8 pressure for a standard atmospheric pressure, the i.e. computational methods of P=101325Pa such as
It is lower described：
(1) the volumetric concentration c that we preset the arsenic trioxide gas standard product for needing to obtain in advance as needed is
1000ppm, then the addition that can calculate arsenic trioxide according to following formula I is m=1.11mg：
In above formula (I), c is the volumetric concentration of the arsenic trioxide gas standard product that needs are obtained, c=1000ppm；M is
The molecular weight of arsenic trioxide, M=197.84；V is the volume of second chamber 8, V=π r2L=1.256 × 10-4m3；
(2) make：P1It is room temperature T1(T1=298K) under 8 in second chamber in nitrogen pressure, P2To be heated to T2Temperature (this
Example is 470 DEG C, i.e. 743.15K) afterwards 8 in second chamber in nitrogen pressure, P3To be heated to T2After temperature 8 in second chamber in
The pressure of arsenic trioxide gas, then then have
In above formula (II), due to the concentration of arsenic trioxide gas in 8 in second chamber be it is default, i.e., it is known, because
This can calculate P according to following formula (III)3=275.8Pa：
In above formula (III), c is the volumetric concentration of the arsenic trioxide gas standard product that needs are obtained, c=1000ppm；R is
Ideal gas constant, R=8.3145；T2It is the temperature of arsenic trioxide gas resulting after heating, T2=470 DEG C=
743.15K；Therefore, can be obtained by (II)：
From above-mentioned calculating, in this example, after second chamber 8 is vacuumized, as long as being added thereto to 4.05 × 105Pa's
The arsenic trioxide of nitrogen and 1.11mg, then sample cell is integrally heated to 470 DEG C, you can obtain standard atmospheric pressure
Normal concentration is the arsenic trioxide gas of 1000ppm.
Claims (4)
1. a kind of preparation method of normal concentration arsenic trioxide gas, the method is comprised the steps of：
(1) selecting the sample cell of a three-stage, the sample cell has the first chamber of rods arranged in horizontal line, second chamber and the successively
Three chambers, wherein between two of the sample cell and first chamber and second chamber and second chamber and the 3rd chamber between
It is provided with the window of permeable to infrared spectrum signal；
(2) three chambers of the sample cell are vacuumized, and nitrogen and arsenic trioxide is added in second chamber and is sealed
Three chambers；Then, the sample cell is integrally heated to making the arsenic trioxide in second chamber be gasified totally；Its
In, the addition of nitrogen and arsenic trioxide meets in the second chamber, arsenic trioxide be gasified totally after in second chamber
Pressure be a standard atmospheric pressure.
2. a kind of sample cell of the three-stage for realizing claim 1 methods described, it is characterised in that the sample cell includes a tubular
Pond body, two of the pond body is respectively equipped with one only through the window of infrared spectroscopy signals, and middle part is provided with two and only passes through
The window of infrared spectroscopy signals；Pond body is separated into three independent chambers by four described windows, forms first chamber, second
Chamber and the 3rd chamber.
3. the sample cell of three-stage according to claim 2, it is characterised in that be communicated with the outside of described pond body
Pipe, the communicating pipe is by first chamber and the 3rd chamber.
4. the sample cell of the three-stage according to Claims 2 or 3, it is characterised in that described sample cell also includes heating
Resistance wire, the resistance wire is wrapped on the outer wall of the pond body.
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| CN105158191B (en) * | 2015-09-01 | 2018-02-06 | 中国科学院合肥物质科学研究院 | The concentration detection apparatus of arsenic trioxide gas in the roaster of gold concentrate containing arsenic |
| CN105891139B (en) * | 2016-06-28 | 2020-09-01 | 中国科学院合肥物质科学研究院 | CO in steel rolling heating furnace2And CO gas detection device |
| CN110398403B (en) * | 2019-07-29 | 2022-05-17 | 华北电力大学（保定） | Preparation method and device of stable arsenic trioxide standard gas |
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| US7390346B2 (en) * | 2005-05-12 | 2008-06-24 | Praxair Technology, Inc. | System and apparatus for producing primary standard gas mixtures |
| CN100513375C (en) * | 2006-06-16 | 2009-07-15 | 中国石油化工股份有限公司 | Preparation process of standard acetaldehyde gas |
| CN101038245B (en) * | 2007-01-29 | 2010-09-08 | 西北大学 | Device and method for preparing calibrating gas |
| CN101713712A (en) * | 2008-10-06 | 2010-05-26 | 中国科学院大连化学物理研究所 | Dynamic preparation device for standard gas of solid-phase or liquid-phase compounds and application thereof |
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| 在线红外气体分析器的发展及工程应用研究;姜培刚;《分析仪器》;20091231(第6期);全文 * |
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