CN109696377A - The method of building sample cell gas atmosphere, sample analysis method and analysis instrument under gas atmosphere - Google Patents
The method of building sample cell gas atmosphere, sample analysis method and analysis instrument under gas atmosphere Download PDFInfo
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- CN109696377A CN109696377A CN201710996426.0A CN201710996426A CN109696377A CN 109696377 A CN109696377 A CN 109696377A CN 201710996426 A CN201710996426 A CN 201710996426A CN 109696377 A CN109696377 A CN 109696377A
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- 238000004458 analytical method Methods 0.000 title claims abstract description 60
- 238000000034 method Methods 0.000 title claims abstract description 34
- 238000012284 sample analysis method Methods 0.000 title claims abstract description 9
- 238000012360 testing method Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 16
- 238000001514 detection method Methods 0.000 claims abstract description 16
- 238000009835 boiling Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 242
- 239000012159 carrier gas Substances 0.000 claims description 28
- 230000001105 regulatory effect Effects 0.000 claims description 28
- 238000002441 X-ray diffraction Methods 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000006200 vaporizer Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 7
- 230000001276 controlling effect Effects 0.000 claims description 4
- 238000004080 punching Methods 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 18
- 239000013078 crystal Substances 0.000 abstract description 7
- 230000009849 deactivation Effects 0.000 abstract description 3
- 238000009472 formulation Methods 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000005457 optimization Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 169
- 239000002808 molecular sieve Substances 0.000 description 20
- 239000007788 liquid Substances 0.000 description 18
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 13
- 239000003795 chemical substances by application Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000001483 high-temperature X-ray diffraction Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 8
- 238000011160 research Methods 0.000 description 8
- 238000010998 test method Methods 0.000 description 8
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 238000011065 in-situ storage Methods 0.000 description 7
- 238000004364 calculation method Methods 0.000 description 6
- 238000003889 chemical engineering Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000005259 measurement Methods 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000010926 purge Methods 0.000 description 4
- 239000013068 control sample Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000003570 air Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011066 ex-situ storage Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000006199 nebulizer Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- 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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/20—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/02—Mechanical
- G01N2201/023—Controlling conditions in casing
- G01N2201/0231—Thermostating
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/31—Accessories, mechanical or electrical features temperature control
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention provides a kind of analysis instruments of sample under the sample analysis method and detection gas atmosphere under method for constructing sample cell gas atmosphere, gas atmosphere.The method of building sample cell gas atmosphere of the invention, it include: that the gas for constructing sample cell gas atmosphere is input in sample cell, the inner wall temperature for controlling sample cell is test temperature, and the outside wall temperature for controlling sample cell is higher than the boiling point of the gas, lower than the safe operating temperature of detection unit component in the affiliated analysis instrument of sample cell.Analysis method and instrument of the invention is able to detect the sample under the conditions of high-temperature gas atmosphere, particularly suitable for detecting the changing rule of catalysis material crystal structure under high temperature thermal and hydric environment, come deactivation prob and formulation optimization problem during the industry park plan of Study of Catalyst.
Description
Technical field
The present invention relates to a kind of sample analysis method, in particular to a kind of method for constructing sample cell gas atmosphere, in the gas
Sample analysis method under body atmosphere.
Background technique
From the 1960s, gradually become catalyst, catalyst by the silica-alumina material of representative of molecular sieve type materials
One of the main component of carrier, adsorbent etc..However, these are using silica-alumina material as the catalyst and catalysis of carrier and framework material
Material requires the harsh high temperature hydrothermal condition of experience in actual use, and the lattice collapse temperature of catalyst and catalysis material is got over
Height, crystal phase are more stable, and thermal stability is better.So researchers tie catalyst and catalysis material under hydrothermal conditions
The changing rule of structure has carried out many researchs, and what people generallyd use at present is the evaluation that non-in-situ method carries out hydrothermal stability,
That is: different time, different temperatures are carried out to catalyst and catalysis material first with hydro-thermal process furnace that is dedicated or voluntarily assembling
High-temperature water heat treatment, then sample is cooled to room temperature again, using prolonged drying and steam-laden adsorption treatment
Afterwards, it is put into polycrystal powder X-ray diffractometer (XRD) and carries out crystal structure analysis, to judge its crystal structure whether by broken
Bad or generation significant change, calculates cell parameter and crystallinity.It can be seen that the shortcomings that this method, is: although (1) urging
Agent and catalysis material have passed through the processing of high temperature thermal and hydric environment, but when testing its crystal structure need room temperature,
Carried out under drying condition, it is completely different with the high temperature thermal and hydric environment of their actual use, it is difficult to complete reflection catalyst and
The change procedure and affecting laws of catalysis material structure feature in high temperature thermal and hydric environment, and these information are to catalyst and catalysis
The exploitation of material is of great significance；(2) heavy workload of this method needs a large amount of manual operation, and generally requires time-consuming
One day or more, preprocessing process it is complicated, and the disadvantages of there are complicated for operation, energy consumption is high, time-consuming and laborious.
To solve the above-mentioned problems, people carry out catalyst and catalysis using in-situ high temperature XRD (in situ HT-XRD)
The research of material hydrothermal stability.But it can only be in drying currently in situ HT-XRD Study of Catalyst and catalysis material
It is carried out in atmosphere, there is no the document report used in hydro-thermal atmosphere.
Summary of the invention
The invention proposes the sample analysis methods and detection gas under a kind of method for constructing sample cell gas atmosphere, gas atmosphere
The analysis instrument of sample under body atmosphere.
The method of building sample cell gas atmosphere of the invention, comprising: the gas for constructing sample cell gas atmosphere is input to sample
In product pond, control sample cell inner wall temperature be test temperature, control sample cell outside wall temperature be higher than the gas boiling point,
Lower than the safe operating temperature of detection unit component in the affiliated analysis instrument of sample cell.
The gas of the building sample cell gas atmosphere is the gas contacted under measuring temperature with sample.
It is gaseous gas under room temperature that the gas of the building gas atmosphere, which can be, is also possible under room temperature for liquid or consolidates
The gas of state can be air, oxygen, hydrogen, vapor etc..
When the gas of the building gas atmosphere is a variety of, the one or more of gas of the building gas atmosphere can be
Carrier gas, the carrier gas are usually inert gas and/or inactive gas, such as helium, argon gas, xenon, nitrogen, carbon dioxide.
When test is in the sample of thermal and hydric environment, i.e., in the sample that measurement is contacted with vapor, the building gas
The gas of atmosphere is vapor.
For some known analysis instruments, the safe operating temperature of detection unit component is lower, usually much
Lower than test temperature, thus some analysis instruments measuring temperature be higher than detection unit component safe operating temperature when, can not
Analysis operation is carried out, otherwise will lead to analysis instrument damage or is scrapped.
The method of building sample cell gas atmosphere of the invention can construct the gas atmosphere under room temperature for liquid or solid, in sample
It will not be condensed into liquid or solid in product pond and pipeline, establish stable gas atmosphere, be easily obtained accurate measurement result.
Sample analysis method under gas atmosphere of the invention, comprising: the gas atmosphere for constructing sample cell is examined using analysis instrument
Sample in sample pond.The method of the gas atmosphere of the building sample cell is the same as described above.
The analysis instrument can be XRD analysis instrument, infrared spectrum analyser or thermogravimetric analyzer.
It is preferred that constructing the gas atmosphere of vapor in sample cell, the outside wall temperature for controlling sample cell is higher than 100 DEG C, lower than sample
The safe operating temperature of detection unit component in the affiliated analysis instrument in product pond.
When the analysis instrument is XRD analysis instrument, the sample in water vapor gas atmosphere can be measured, particularly suitable for
Catalyst sample of the measurement under thermal and hydric environment.When constructing the gas atmosphere of vapor, sample cell outer wall and vapor are controlled
The temperature of intake pipeline can guarantee to construct stable steam atmosphere in sample cell in this way on the boiling point of water.It is described
The temperature of sample cell inner wall can control at 120 DEG C~1200 DEG C, preferably 200 DEG C~1000 DEG C, can measure sample and steam in water
It is the XRD diffraction maximum under thermal and hydric environment under gas atmosphere.The outside wall temperature of the sample cell is lower than the safety of XRD detection unit component
Operation temperature can control in 100 DEG C or more, 200 DEG C hereinafter, preferably 120 DEG C -150 DEG C.When carrying out XRD analysis, preferably
It is passed through carrier gas, carrier gas flux is preferably 5mL/min-1000mL/min, more preferable 50mL/min-300mL/min, and nebulizer gas pressure is excellent
It is selected as 0.05MPa-1.0MPa, more preferable 0.1MPa-0.3MPa.The flow of the vapor with liquid water be calculated as 1ml/min~
100ml/min, preferably 5ml/min~30ml/min.Sample preferred catalytic agent material to be analyzed, more preferable solid catalyst material
Material.It is preferred that being punched on sample to be analyzed, sample is punched on the circulating direction of gas more preferably in sample cell, aperture is excellent
It is selected as 0.01~2.0mm, more preferably 0.1~1mm.Sample can be kept complete, otherwise in water with steady air flow sample punching
Under vapor atmosphere and under larger pressure, sample is easy to damaged, fragmentation, influences measurement result.
Sample analysis method under gas atmosphere of the invention is able to detect the sample under the conditions of high-temperature gas atmosphere, particularly suitable for
The changing rule for detecting catalysis material crystal structure under high temperature thermal and hydric environment, comes during the industry park plan of Study of Catalyst
Deactivation prob and formulation optimization problem.
Gas is arranged in the sample cell 1 in the analysis instrument of sample under detection gas atmosphere of the invention, including sample cell 1
Intake pipeline 21, temperature regulating device 3, temperature regulating device 3 can control the outer wall 11, inner wall 12, gas inlet pipe line of sample cell respectively
21 temperature.
It is preferred that gas output tube line 22 is arranged on the sample cell.
The gas inlet pipe line 21, gas output tube line 22 are used to input, export the building gas atmosphere in sample cell
Gas.
The gas of the building gas atmosphere can be one kind, be also possible to a variety of.When the gas of the building gas atmosphere is
When a variety of, multiple gases can be input in sample cell through a gas inlet pipe line 21, it is defeated that multiple gases also can be set
Enter pipeline 21 to input different gas respectively, gas mixer chamber 4 can also be set and be connected with sample cell, in gas mixer chamber 4
The upper multiple gas inlet pipe lines 21 of setting, so that different gas is mixed in gas mixer chamber 4, to input different gas.Institute
State and be preferably provided with baffle 41 in gas mixer chamber 4, the baffle 41 can for one or more, the baffle 41 enable into
The gas mixing entered in gas mixer chamber 4 is uniform.When the gas of the building gas atmosphere is a variety of, the building gas atmosphere
The one or more of gas can be carrier gas, and the carrier gas is usually inert gas and/or inactive gas, such as helium, argon
Gas, xenon, nitrogen, carbon dioxide.
The gas of the building gas atmosphere is the gas contacted under measuring temperature with sample, be can be under room temperature as gaseous state
Gas, be also possible under room temperature for liquid or solid gas, can be air, oxygen, hydrogen, vapor etc..
It is preferred that gas mixer chamber 4 is arranged on sample cell, the gas mixer chamber 4 passes through gas inlet pipe line 21 and sample
Pond is connected, and one or more gas input passages is arranged on gas mixer chamber 4, one or more of gas input passages can
It is sent into the gas mixer chamber 4 so that the gas of gas atmosphere will be constructed, finally enters sample cell.In the gas of the building gas atmosphere
It may include carrier gas, can not also include carrier gas, preferably include carrier gas.It is highly preferred that a load is arranged on gas mixer chamber 4
The gas input passage 6 of gas input channel 5, one building gas atmosphere.It is highly preferred that in the gas input passage of building gas atmosphere
Vaporizer 7 is set on 6.When construct under room temperature be liquid or solid gas atmosphere when, can by under the room temperature the liquid or
Solid is sent into vaporizer 7, is allowed to be converted into gas, be input in gas mixer chamber 4.It is preferred that controlling gas by temperature regulating device 3
The temperature of body mixing chamber 4.
Preferably, for easy to operate or quantitatively building gas atmosphere gas, each input of sample cell described above
Valve 8 is set on pipeline or input channel, can be set as needed the quantity of valve 8.It is preferred that in the gas inlet pipe line
21 and/or gas output tube line 22 on be arranged valve 8；It is preferred that being inputted in carrier gas input channel 5 and/or the gas for constructing gas atmosphere
Valve 8 is set on channel 6.
When gas output tube line 22 is arranged on the sample cell, can be arranged on the gas output tube line 22 cold
Solidifying room 9 can control the temperature of condensation chamber 9 under the boiling point of the gas of the building gas atmosphere in operation, can condense
Recycle the liquid or solid-state condensate of the gas of the building gas atmosphere.
Pressure control device, the internal pressure of the pressure control device pressure control control sample cell can be set on the sample cell.
Gas atmosphere can be constructed in sample cell of the invention, particularly suitable for being liquid or solid matter under building room temperature
Gas atmosphere.
The sample cell is placed among the analysis instrument or is connected with the analysis instrument.
The analysis instrument can be XRD analysis instrument, infrared spectrum analyser or thermogravimetric analyzer.When the analysis instrument is
When XRD analysis instrument, the sample in water vapor gas atmosphere can be measured.When constructing the gas atmosphere of vapor, sample is controlled
The temperature of pond outer wall and vapor intake pipeline can guarantee to construct stable water in sample cell in this way on the boiling point of water
Vapor atmosphere.The temperature of the sample cell inner wall can control at 120 DEG C~1200 DEG C, preferably 200 DEG C~1000 DEG C, can survey
Random sample product are the XRD diffraction maximum under thermal and hydric environment under steam atmosphere.The outside wall temperature of the sample cell can control 100
DEG C or more, 200 DEG C hereinafter, preferably 120 DEG C -150 DEG C, the outside wall temperature is lower than the safety operation of XRD detection unit component
Temperature.
In existing XRD analysis instrument, the gas atmosphere of vapor can not be constructed, and for XRD test, XRD sample
The temperature of pond inner wall can be set to high temperature, such as 800~1000 DEG C, and the temperature of outer wall does not allow more than in XRD analysis instrument
Otherwise the operating temperature of detection unit component can damage the normal work of XRD analysis instrument detection unit component, so that XRD analysis
Instrument breaks down or even scraps.
Analysis method and instrument of the invention is able to detect the sample under the conditions of high-temperature gas atmosphere, is catalyzed particularly suitable for detection
The changing rule of material crystal structure under high temperature thermal and hydric environment, carrys out the deactivation prob during the industry park plan of Study of Catalyst
With formulation optimization problem.
Methods and apparatus of the present invention can provide thermal and hydric environment and test method, tool in in-situ high temperature XRD test process
Have it is simple and efficient, low in cost, more close to industrial environment the advantages of, the rate of recovery of liquid water is up to 98%, and test result is quasi-
It is really reliable, expensive XRD is not adversely affected.
Detailed description of the invention
Fig. 1 is the schematic diagram of analysis instrument of the present invention.
Fig. 2 is the schematic diagram of analysis instrument of the present invention.
Fig. 3 is the schematic diagram of analysis instrument of the present invention.
Fig. 4 is the schematic diagram of analysis instrument of the present invention.
Fig. 5 is the schematic diagram of analysis instrument of the present invention.
Fig. 6 is the schematic diagram of analysis instrument of the present invention.
Fig. 7 is the schematic diagram of analysis instrument of the present invention.
Fig. 8 is the schematic diagram of analysis instrument of the present invention.
Fig. 9 is the XRD spectra of embodiment 1.
Figure 10 is the XRD spectra of comparative example 1.
Specific embodiment
Following embodiment is for tentatively illustrating the present invention, and its non-limiting range, in the various changes of the art, only
It falls within the spirit and scope of claims of the present invention, should be understood as constituting a part of the invention.
Fig. 1 is analysis instrument A of the invention, including sample cell therein 1, and gas inlet pipe is arranged in the sample cell 1
Line 21, temperature regulating device 3, temperature regulating device 3 can be controlled separately the temperature of the outer wall 11 of sample cell, inner wall 12, gas inlet pipe line 21
Degree.
Fig. 2 is analysis instrument A of the invention, including sample cell therein, the sample cell include sample cell shell 1, with
Gas inlet pipe line 21, the gas output tube line 22, temperature regulating device 3 of sample cell connection, temperature regulating device 3 can be controlled separately sample
The temperature of the outer wall 11 in pond, inner wall 12, gas inlet pipe line 21, gas output tube line 22.
Fig. 3 is analysis instrument A of the invention, including sample cell therein, the sample cell include sample cell shell 1, with
Gas inlet pipe line 21, the gas output tube line 22, temperature regulating device 3 of sample cell connection, temperature regulating device 3 can be controlled separately sample
The temperature of the outer wall 11 in pond, inner wall 12, gas inlet pipe line 21, gas output tube line 22；Setting gas mixer chamber 4 passes through gas
Intake pipeline 21 is connected with sample cell, and a carrier gas input channel 5, one building gas atmosphere are arranged on gas mixer chamber 4
Gas input passage 6.
Fig. 4 is analysis instrument A of the invention, including sample cell therein, the sample cell include sample cell shell 1, with
Gas inlet pipe line 21, the gas output tube line 22, temperature regulating device 3 of sample cell connection, temperature regulating device 3 can be controlled separately sample
The temperature of the outer wall 11 in pond, inner wall 12, gas inlet pipe line 21, gas output tube line 22；Setting gas mixer chamber 4 passes through gas
Intake pipeline 21 is connected with sample cell, and a carrier gas input channel 5, one building gas atmosphere are arranged on gas mixer chamber 4
Gas input passage 6；Baffle 41 is set in gas mixer chamber 4, so that gas mixing therein is uniform.
Fig. 5 is analysis instrument A of the invention, including sample cell therein, the sample cell include sample cell shell 1, with
Gas inlet pipe line 21, the gas output tube line 22, temperature regulating device 31,32 of sample cell connection, temperature regulating device 31 can be controlled respectively
The temperature of the outer wall 11 of sample cell processed, inner wall 12, gas inlet pipe line 21, temperature regulating device 32 can control gas mixer chamber 4
Temperature；Setting gas mixer chamber 4 is connected by gas inlet pipe line 21 with sample cell, and a load is arranged on gas mixer chamber 4
The gas input passage 6 of gas input channel 5, one building gas atmosphere.
Fig. 6 is analysis instrument A of the invention, including sample cell therein, the sample cell include sample cell shell 1, with
Gas inlet pipe line 21, the gas output tube line 22, temperature regulating device 3 of sample cell connection, temperature regulating device 3 can be controlled separately sample
The temperature of the outer wall 11 in pond, inner wall 12, gas inlet pipe line 21, gas output tube line 22；Setting gas mixer chamber 4 passes through gas
Intake pipeline 21 is connected with sample cell, and the gas input passage 5 of a building gas atmosphere is arranged on gas mixer chamber 4；In gas
Vaporizer 6 is set in body input channel 5.
Fig. 7 is XRD analysis instrument A of the invention, including sample cell therein, the sample cell include sample cell shell 1,
Gas inlet pipe line 21, gas output tube line 22, the temperature regulating device 3 connecting with sample cell, temperature regulating device 3 can be controlled separately sample
The temperature of the outer wall 11 in product pond, inner wall 12, gas inlet pipe line 21, gas output tube line 22；Setting gas mixer chamber 4 passes through gas
Body intake pipeline 21 is connected with sample cell, and 5, the vapor inputs of a carrier gas input channel are arranged on gas mixer chamber 4
Channel 6；Valve 8 is set on each intake pipeline or input channel of sample cell.
Fig. 8 is XRD analysis instrument A of the invention, including sample cell therein, the sample cell include sample cell shell 1,
Gas inlet pipe line 21, gas output tube line 22, the temperature regulating device 3 connecting with sample cell, temperature regulating device 3 can be controlled separately sample
The temperature of the outer wall 11 in product pond, inner wall 12, gas inlet pipe line 21, gas output tube line 22；Setting gas mixer chamber 4 passes through gas
Body intake pipeline 21 is connected with sample cell, and 5, the vapor inputs of a carrier gas input channel are arranged on gas mixer chamber 4
Channel 6；Condenser 9 is set on the gas output tube line 22 of sample cell.
Embodiment 1:
Reagent and instrument: German Brooker company D8X x ray diffractometer x (XRD) transform sample cell therein as Fig. 5 institute
The sample cell shown；Compressed air, Research Institute of Petro-Chemical Engineering's Gas Plant, NaY molecular sieve is from middle Effect of Catalysis In Petrochemistry agent Shandong point
Company.
Sample preparation: according to Instrument Operating Manual or People's Republic of China (PRC) petrochemical industry standard SH/T0339-92
Method prepare the molecular sieve tabletting of NaY type, and with small needle bundle 5, hole, be packed on the sample holder of XRD, sample holder is then placed in
The sample cell 1 of Fig. 5 shown device is medium to be tested.
Test method: (1) sample is placed on bracket and is placed in sample cell 1；(2) temperature regulating device 31 and 32 is opened, is adjusted
The temperature of throttle body intake pipeline 21 and export pipeline 22 is 220~250 DEG C, the temperature of gas mixer chamber 4 is 350 DEG C, sample
The temperature of pond outer wall 11 is 120 DEG C；(3) carrier gas air is opened, pressure 0.13MPa, flow 200mL/min, carrier gas is from defeated
Enter channel 5 and sequentially enters gas mixer chamber 4, gas inlet pipe line 21, sample cell 1, gas output tube line 22；(4) temperature control is used
12 temperature of sample cell inner wall is warming up to 200 DEG C, 400 DEG C, 600 DEG C, 800 DEG C with the heating rate of 6 DEG C/min by device 32, upper
State the XRD spectra of temperature difference test sample；(5) it is logical that gas input is opened after the temperature of sample cell inner wall 12 reaches 500 DEG C
Liquid water is injected into the flow of 10mL/hr and is allowed to gasify at high temperature in gas mixer chamber 4 by road 6, and vapor is in carrier gas
Gas inlet pipe line 21, sample cell 1, gas output tube line 22 are sequentially entered under purging；(6) it is exported by gas output tube line 22
Vapor can use cooling device recovering liquid water, to save water resource；(7) sample test spectrogram is shown in Fig. 9；(8) according to SH/
Cell parameter calculation method described in T0339-92 calculates cell parameter, and the results are shown in Table 1.
Embodiment 2:
Reagent and instrument: German Brooker company D8X x ray diffractometer x (XRD) transform sample cell therein as Fig. 5 institute
The sample cell shown；Compressed air, Research Institute of Petro-Chemical Engineering's Gas Plant, NaY molecular sieve is from middle Effect of Catalysis In Petrochemistry agent Shandong point
Company.
Sample preparation: according to Instrument Operating Manual or People's Republic of China (PRC) petrochemical industry standard SH/T0339-92
Method prepare the molecular sieve tabletting of NaY type, and with small needle bundle 3, hole, be packed on the sample holder of XRD, sample holder is then placed in
The sample cell 1 of Fig. 5 shown device is medium to be tested.
Test method: (1) sample is placed on bracket and is placed in sample cell 1；(2) temperature regulating device 31 and 32 is opened, is adjusted
The temperature of throttle body intake pipeline 21 and export pipeline 22 is 150~170 DEG C, the temperature of gas mixer chamber 4 is 250 DEG C, sample
The temperature of pond outer wall 11 is 150 DEG C；(3) carrier gas air is opened, pressure 0.11MPa, flow 100mL/min, carrier gas is from defeated
Enter channel 5 and sequentially enters gas mixer chamber 4, gas inlet pipe line 21, sample cell 1, gas output tube line 22；(4) temperature control is used
12 temperature of sample cell inner wall is warming up to 200 DEG C, 400 DEG C, 600 DEG C, 800 DEG C with the heating rate of 6 DEG C/min by device 32, upper
State the XRD spectra of temperature difference test sample；(5) it is logical that gas input is opened after the temperature of sample cell inner wall 12 reaches 500 DEG C
Liquid water is injected into the flow of 12mL/hr and is allowed to gasify at high temperature in gas mixer chamber 4 by road 6, and vapor is in carrier gas
Gas inlet pipe line 21, sample cell 1, gas output tube line 22 are sequentially entered under purging；(6) it is exported by gas output tube line 22
Vapor can use cooling device recovering liquid water, to save water resource；(7) sample test spectrogram is shown in Fig. 9；(8) according to SH/
Cell parameter calculation method described in T0339-92 calculates cell parameter, and the results are shown in Table 1.
Embodiment 1 and embodiment 2 have been all made of device described in Fig. 5, as can be seen from Table 1 NaY cell parameter almost phase
Together, there is preferable repeatability and accuracy.
Comparative example 1
Reagent and instrument: German Brooker company D8X x ray diffractometer x (XRD)；Compressed air, petrochemical industry scientific research
Institute's Gas Plant, NaY molecular sieve come from middle Effect of Catalysis In Petrochemistry agent asphalt in Shenli Refinery.
Sample preparation: according to Instrument Operating Manual or People's Republic of China (PRC) petrochemical industry standard SH/T0339-92
Method prepare the molecular sieve tabletting of NaY type, and be fitted into band be commercialized high temperature furnace attachment XRD in test.
Test method: (1) since commercialized high temperature XRD can not be passed through vapor, so compressed air can only be passed through, press
Power is 0.11MPa, and gas flow is about 100mL/min；(2) 200 DEG C, 400 DEG C, 600 are warming up to the heating rate of 6 DEG C/min
DEG C, after 800 DEG C, test sample, XRD spectra are shown in Figure 10 respectively；(3) according to cell parameter calculating side described in SH/T0339-92
Method calculates cell parameter, and the results are shown in Table 1.
Commercialized in-situ high temperature XRD and test method are used in comparative example 1, it, can from table 1 to be tested under dry environment
To see, at 30 DEG C, 200 DEG C and 400 DEG C, the NaY molecular sieve cell parameter of comparative example 1 and the test acquisition of embodiment 1,2 is several
It is consistent；And Examples 1 and 2 described device and method start to be passed through vapor after 500 DEG C, NaY molecule in Examples 1 and 2
Sieve cell parameter is significantly less than the test result of comparative example 1, illustrates that device and method employed in Examples 1 and 2 produce
Apparent effect.
Embodiment 3:
Reagent and instrument: German Brooker company D8X x ray diffractometer x (XRD) transform sample cell therein as Fig. 6 institute
The sample cell shown；Compressed air comes from Research Institute of Petro-Chemical Engineering's Gas Plant, and PSRY molecular sieve is long from middle Effect of Catalysis In Petrochemistry agent
Ridge branch company.
Sample preparation: according to Instrument Operating Manual or People's Republic of China (PRC) petrochemical industry standard SH/T0339-92
Method preparation the molecular sieve tabletting of NaY type be packed on the sample holder of XRD with 5, stylus printer hole, sample holder is then placed in Fig. 6 institute
The sample cell 1 of showing device is medium to be tested.
Test method: (1) sample is placed on bracket and is placed in sample cell 1；(2) temperature regulating device 3 and vaporizer are opened
6, the temperature of regulating gas mixing chamber 4, gas inlet pipe line 21 and export pipeline 22 is 120~150 DEG C, the temperature of vaporizer 6
It is 250 DEG C, the temperature of sample cell outer wall 11 is 185 DEG C；(3) carrier gas air, pressure 0.15MPa, flow 150mL/ are opened
Min, it is defeated that carrier gas from input channel 5 sequentially enters vaporizer 6, gas mixer chamber 4, gas inlet pipe line 21, sample cell 1, gas
Pipeline 22 out；(4) using temperature regulating device 32 with the heating rate of 6 DEG C/min by 12 temperature of sample cell inner wall be warming up to 200 DEG C,
400 DEG C, 600 DEG C, 800 DEG C, in the XRD spectra of above-mentioned temperature difference test sample；(5) when the temperature of sample cell inner wall 12 reaches
After 350 DEG C, liquid water is injected into the flow of 20mL/hr and is allowed to gasify at high temperature in vaporizer 6, vapor is in carrier gas
Gas mixer chamber 4, gas inlet pipe line 21, sample cell 1, gas output tube line 22 are sequentially entered from vaporizer 6 under purging；(6)
In 800 DEG C of constant temperature 4hr, an XRD spectra is acquired every 30min；(7) after constant temperature again with 6 DEG C/min cool to 600 DEG C and
Room temperature acquires an XRD spectra again respectively；(8) cooling device recycling can use by the vapor that gas output tube line 22 exports
Liquid water, to save water resource；(9) cell parameter is calculated according to cell parameter calculation method described in SH/T0339-92, as a result
As shown in table 2.
Comparative example 2
Reagent and instrument: German Brooker company D8X x ray diffractometer x (XRD), band high temperature furnace attachment；Compressed air comes from
Research Institute of Petro-Chemical Engineering's Gas Plant, PSRY molecular sieve come from middle Effect of Catalysis In Petrochemistry agent Chang Ling branch company.
Sample preparation: according to Instrument Operating Manual or People's Republic of China (PRC) petrochemical industry standard SH/T0339-92
Method prepare the molecular sieve tabletting of NaY type, be packed into XRD it is medium to be tested.
Test method: (1) since commercialized high temperature XRD can not be passed through vapor, so compressed air can only be passed through, press
Power is 0.15MPa, and gas flow is about 150mL/min；(2) using with the identical temperature program(me) of embodiment 3 to sample into
Row heating, constant temperature and cooling processing, and XRD spectra is acquired under identical temperature and time；(3) according in SH/T0339-92
The cell parameter calculation method calculates cell parameter, and the results are shown in Table 2.
Embodiment 3 uses methods and apparatus of the present invention, is tested under thermal and hydric environment, and comparative example 2 is then normal
Rule commercialization in-situ high temperature XRD is tested in dry conditions, it can be seen that it is bright to reduce amplitude for molecular sieve cell parameter in embodiment 3
It is aobvious to increase, it is completely the same with notional result.
Embodiment 4:
Reagent and instrument: German Brooker company D8X x ray diffractometer x (XRD) transform sample cell therein as Fig. 5 institute
The sample cell shown；Compressed air comes from Research Institute of Petro-Chemical Engineering's Gas Plant, and DASY molecular sieve is long from middle Effect of Catalysis In Petrochemistry agent
Ridge branch company.
Sample preparation: according to Instrument Operating Manual or People's Republic of China (PRC) petrochemical industry standard SH/T0339-92
Method preparation the molecular sieve tabletting of NaY type be packed on the sample holder of XRD with 5, stylus printer hole, sample holder is then placed in Fig. 5 institute
The sample cell 1 of showing device is medium to be tested.
Test method: (1) sample is placed on bracket and is placed in sample cell 1；(2) temperature regulating device 31 and 32 is opened, is adjusted
The temperature of throttle body intake pipeline 21 and export pipeline 22 is 280~320 DEG C, the temperature of gas mixer chamber 4 is 360 DEG C, sample
The temperature of pond outer wall 11 is 110 DEG C；(3) carrier gas air is opened, pressure 0.10MPa, flow 500mL/min, carrier gas is from defeated
Enter channel 5 and sequentially enters gas mixer chamber 4, gas inlet pipe line 21, sample cell 1, gas output tube line 22；(4) temperature control is used
After 12 temperature of sample cell inner wall is warming up to 800 DEG C with the heating rate of 6 DEG C/min by device 32, with the flow of 100mL/hr by liquid
State water, which is injected into, to be allowed to gasify at high temperature in gas mixer chamber 4, and vapor sequentially enters gas input under the purging of carrier gas
Pipeline 21, sample cell 1, gas output tube line 22；(5) in 800 DEG C of constant temperature 5hr, an XRD spectra is acquired every 60min；(6)
Cooling device recovering liquid water can use by the vapor that gas output tube line 22 exports, to save water resource；(7) according to
Cell parameter calculation method described in SH/T0339-92 calculates cell parameter, and the results are shown in Table 3, within time-consuming 9h.
Comparative example 3
Reagent and instrument: Dutch Panaco Xpert type X-ray diffractometer (XRD), DASY molecular sieve come from middle Effect of Catalysis In Petrochemistry
Agent Chang Ling branch company.
Sample preparation and processing method: according to institute in People's Republic of China (PRC) petrochemical industry standard SH/T10339-92
Method for making sample, serial hydrothermal pretreatment process, test process and cell parameter calculation method, measurement and the calculating Y type molecule stated
Cell parameter is sieved, the results are shown in Table 3, time-consuming about 72h.
Comparative example 3 is using currently used standard method, after the hydro-thermal process that ex situ is first carried out to molecular sieve, so
Carry out XRD test again afterwards, time-consuming is up to 72h, and embodiment 4 can be obtained within 9h using apparatus and method of the present invention with
The identical test result of comparative example 3, test accuracy is high, the time is few.
(unit is 1 molecular sieve NaY cell parameter test result of table)
| Temperature/DEG C | Embodiment 1 | Embodiment 2 | Comparative example 1 |
| 30 | 24.599 | 24.613 | 24.617 |
| 200 | 24.728 | 24.721 | 24.720 |
| 400 | 24.758 | 24.762 | 24.768 |
| 600 | 24.742 | 24.745 | 24.769 |
| 800 | 24.727 | 24.727 | 24.741 |
| 800-30min | -- | -- | 24.717 |
| 800-60min | -- | -- | 24.716 |
(unit is 2 molecular sieve PSRY cell parameter test result of table)
| Temperature/DEG C | Comparative example 2 | Embodiment 3 |
| 30 | 24.520 | 24.515 |
| 200 | 24.548 | 24.528 |
| 400 | 24.524 | 24.501 |
| 600 | 24.528 | 24.461 |
| 800 | 24.372 | 24.325 |
| 800-30min | 24.344 | 24.298 |
| 800-60min | 24.330 | 24.287 |
| 800-90min | 24.330 | 24.275 |
| 800-120min | 24.330 | 24.272 |
| 800-150min | 24.325 | 24.264 |
| 800-180min | 24.325 | 24.25 |
| 800-210min | 24.325 | 24.24 |
| 800-240min | 24.325 | 24.246 |
| 600 | 24.339 | 24.25 |
| 50 | 24.351 | 24.27 |
(unit is 3 molecular sieve DASY cell parameter test result of table)
| Treatment conditions | Comparative example 3 | Embodiment 4 |
| 30℃ | 2.4488 | 2.4440 |
| 800 DEG C of constant temperature 1h | 2.4304 | 2.4336 |
| 800 DEG C of constant temperature 2h | 2.4321 | 2.4320 |
| 800 DEG C of constant temperature 3h | 2.4275 | 2.4302 |
| 800 DEG C of constant temperature 4h | 2.4273 | 2.4286 |
| 800 DEG C of constant temperature 5h | 2.4273 | 2.4271 |
Claims (17)
1. a kind of method for constructing sample cell gas atmosphere, comprising: the gas for constructing sample cell gas atmosphere is input in sample cell,
The inner wall temperature for controlling sample cell is test temperature, and the outside wall temperature for controlling sample cell is higher than the boiling point of the gas, lower than sample
The safe operating temperature of detection unit component in the affiliated analysis instrument in product pond.
2. the sample analysis method under a kind of gas atmosphere, comprising: the gas atmosphere of sample cell is constructed using method of claim 1 method,
Utilize the sample in analysis instrument test sample pond.
3. analysis method according to claim 2, which is characterized in that the analysis instrument is XRD analysis instrument, infrared analysis
Instrument or thermogravimetric analyzer.
4. analysis method described in accordance with the claim 3, which is characterized in that construct the gas atmosphere of vapor, control in sample cell
The outside wall temperature of sample cell processed is higher than 100 DEG C, lower than the safety operation temperature of detection unit component in the affiliated analysis instrument of sample cell
Degree.
5. analysis method according to claim 4, which is characterized in that the analysis instrument is XRD analysis instrument, controls sample
The temperature of pond outer wall and vapor intake pipeline controls the temperature of sample cell inner wall 120 DEG C~1200 on the boiling point of water
℃。
6. analysis method according to claim 5, which is characterized in that be passed through carrier gas when carrying out XRD analysis.
7. analysis method according to claim 6, which is characterized in that sample to be analyzed is that catalyst material is (preferably solid
Body catalyst material).
8. analysis method according to claim 7, which is characterized in that punching is (preferably in sample on sample to be analyzed
Sample is punched on the circulating direction of gas in pond).
9. the analysis instrument of sample under a kind of detection gas atmosphere, including sample cell (1), defeated in the sample cell (1) setting gas
Enter pipeline (21), temperature regulating device (3), temperature regulating device (3) can control the outer wall (11) of sample cell, inner wall (12), gas respectively
The temperature of intake pipeline (21).
10. analysis instrument according to claim 9, which is characterized in that gas output tube is arranged on the sample cell (1)
Line (22).
11. analysis instrument according to claim 10, which is characterized in that gas mixer chamber is arranged on sample cell (1)
(4), the gas mixer chamber (4) is connected by gas inlet pipe line (21) with sample cell.
12. analysis instrument according to claim 11, which is characterized in that a carrier gas is arranged on gas mixer chamber (4)
Input channel (5), one building gas atmosphere gas input passage (6).
13. analysis instrument according to claim 12, which is characterized in that in the gas input passage (6) of building gas atmosphere
Upper setting vaporizer (7).
14. analysis instrument according to claim 13, which is characterized in that in the gas inlet pipe line (21) and/or gas
Valve (8) are set on body export pipeline (22).
15. analysis instrument according to claim 14, which is characterized in that be arranged on the gas output tube line (22) cold
Solidifying room (9).
16. according to analysis instrument described in one of claim 9~15, which is characterized in that the sample cell (1) is placed in described
It is connected among analysis instrument or with the analysis instrument.
17. analysis instrument according to claim 16, which is characterized in that the analysis instrument is XRD analysis instrument, infrared point
Analyzer or thermogravimetric analyzer.
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