GB2223305A - Pre-injection water vapour differential thermal-analysis - Google Patents
Pre-injection water vapour differential thermal-analysis Download PDFInfo
- Publication number
- GB2223305A GB2223305A GB8816681A GB8816681A GB2223305A GB 2223305 A GB2223305 A GB 2223305A GB 8816681 A GB8816681 A GB 8816681A GB 8816681 A GB8816681 A GB 8816681A GB 2223305 A GB2223305 A GB 2223305A
- Authority
- GB
- United Kingdom
- Prior art keywords
- analysis
- differential thermal
- sample
- water vapor
- heat chamber
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
- G01N25/48—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation
- G01N25/4846—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample
- G01N25/4866—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity on solution, sorption, or a chemical reaction not involving combustion or catalytic oxidation for a motionless, e.g. solid sample by using a differential method
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
Differential thermal analysis is carried out with a test sample positioned in a heating chamber maintained under a 100% water vapour atmosphere.
Description
TITLE OF THE INVENTION
A method for pre-injection water vapor differential
thermal-analysis
BRIEF SUMMARY OF THE INVENTION
The present invention relates to differential thermal
analysis in which especially the characteristics of the
ultra-stabilized Y zeolite composition or a catalyst for
fluid catalytic cracking(F.C.C.) containing zeolite Y -necessitating a hydrothermal stability test is possible
to be easily and exactly analyzed.
To know a hydrothermal stability is necessary to a lot of
industrial products, and the ultra-stabilized Y zeolite
composition contained in a catalyst for F.C.C. is one of
the representatives. Such hydrothermal resistant materials were usually heated in water vapor for 6 - 16 hours, and methods for determining a disinegration of a crystal by
X-ray diffraction or nitrogen adsorption at about -1969C are usued. Therefore, several times of the determinations
at 750 - 810C had to be done in this method, and it took
a lot of times to determine.
On the other hand, a water vapor differential thermal
analysis unit is also developing, but an apparatus becomes on a large scale and very expensive because a process in which the whole determined part of an apparatus is filled with water vapor is used.
It is an object of the present invention to provide differential thermal analysis which solves the'above-mentioned problem, that is to say, around a heated part of a sample is changed to the condition of 100% water vapor atmosphere, so that an analysis apparatus does not become on a large scale, and the determination also becomes easy.
An object of the present invention is achieved by the following method.
A method for pre-injection water vapor differential thermal-analysis; which consists of constructing a bottom part of a heat chamber of a sample in a differential thermal-analysis unit by a refractory in which a coefficient of thermal expansion is almost same with an inner tube of an electric furnace for heating, penetrateing an injection pipe into a small crevice between the above-mentioned inner tube.and a circumference of the bottom part of a heat chamber of a sample with-inserting a thermocouple protective pipe into the bottom part of a heat chamber of a sample, inserting water into an injection pipe at a temperature of which intended peak by differential thermal-analysis appears, dischargeing water vapor into the above-mentioned heat chamber of a sample from the above-mentioned small crevice, and analyzing under the condition of an atmosphere of 1008 water vapor.
BRIEF DESCRIPTION OF THE DRAWINGS
Figure 1 shows a scheme explanation view of an apparatus which was used in an example of the present invention; and
Figure 2 shows a graph which is a result of an example of the present invention.
DETAILED DESCRIPTION OF THE INVENTION
The following detailed explanation is a method of the present invention.
In a method for differential thermal analysis, since the position of intended peak is almost observed at a limited point, a detection circuit of differential thermal-analysis is closed at a range of pertinent temperature before intended peak appears at a heating process, and for example, a few m2S of distilled water is injected to a heat chamber of a sample by using a micro quantitative pump etc. For example, considering with a case of that the amount of injected distilled water vapor is observed at a room temperature, and a injected distilled water becomes 50 - 500 times of water vapor for a volume of a heated part of a sample and surrounds a heated part of said sample. At a practical analysis, a program heating circuit is kept definite temperature rise or a definite temperature at the time of injecting.The distribution of ununiform temperature which originates to thermal impact accompanies an injection is solved before intended peak appears, and even minute peak is enough determined.
In a method of the present invention, tht circumference of a heated part of a sample is directly made to be 100* water vapor atmosphere after injection, and then, there is a case of that a heated water vapor is discharged into an outer part, but the open air is never fed into an inner part.
Example
The following explanation is an example of the present invention.
An apparatus used in the present example is reconstructed as shown in Figure 1, in which a bottom part (1) of a heat chamber of a sample which is the commercial differential thermal-analysis-group is changed to a refractory firebrick made by silica, and an injection pipe (2) which is discharged from a micro quantitative pump is penetrately connected with a space between a bottom part of an electric furnace which freely moves up and down and a part which supports an electric furnace of the body and is sealed by a silicon rubber plate for the purpose of venting water minuteness.That is to say, an inner tube (3) is made with a marketing-typed quart: glass in which a coeffiCient of thermal expansion is almost the same with a bottom part (1) of said refractory firebrick made by silica, the above-mentioned injection tube (2) is penetrated into a small crevice between an inner tube (3) and a bottom part (1) a volume is made to be small by inserting a pin (5) made by stainless steel from an upper position to a water vapor effluent-opening (4) of an upper part, and the inflow into a heat chamber is prevented.
The material of a pin (5) has to have a large degree of thermal conductivity and excellent corrosion resistance, and is not particularly limited, and a thickness in which the drop of water leaked from an inner part of said water vapor effluent-opening (4) does not flow is desirable as a thickness of a pin.
In Figure 1, (6) is a calorific body for heating, (v) is-a thermocouple protective pipe, (8) is a sample, and (9 ) is a standard sample.
Usingvan apparatus shown in Figure 1, the results of each analysis- are shown in Figure 2 in cases of that an injection of the present invention is done and an injection of the present invention is not done.
That is to say, reference sample JRC-Z-HY4.8 in Catalyst
Society of Japan are used in a graph shown in Figure 2.
The disintegration temperature of sample without injection was 1019 0C with a heating rate of 10 C/mlnute. In the results of 1, 2, 3, 4, 5 and tome of injection, each disintegration temperature was 976, 969, 967, 966, 966 and 966eC, respectively. From these results, it is presumed that a disintegration temperature of this sample by a differential thermal-analysis in 100% water Vapor atmosphere is 9660C with a heating rate of 100C/minute.
As mentioned in the above, according to the present invention, the determination of hydrothermal stability at a high temperature of a sample is also to be done by injecting each samples at proper temperature which are possible to predist in advance, and a method of the present invention is able to be done by an apparatus in which one part usual differential thermal-analysis system is reorganized somewhat.
Claims (1)
- A method for pre-injection water vapor differential thermal-analysis; which consists of constructing a bottom part of a heat chamber of a sample in a differential thermal-analysis unit by a refractory in which a coefficient of thermal expansion is almost same with an inner tube of an electric furnace for heating, penetrateing an injection pipe into a small crevice between the above-mentioned inner tube and a circumference of the bottom part of a heat chamber of a sample with inserting a thermocouple protective pipe into the bottom part of a heat chamber of a sample, inserting water into an injection pipe at a temperature of which intended peak by differential thermal-analysis appears, dischargeing water vapor into the above-mentioned heat chamber of a sample from the above-mentioned small crevice, and analyzing under the condition of an atmosphere of 100% water vapor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB8816681A GB2223305A (en) | 1988-07-13 | 1988-07-13 | Pre-injection water vapour differential thermal-analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB8816681A GB2223305A (en) | 1988-07-13 | 1988-07-13 | Pre-injection water vapour differential thermal-analysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB8816681D0 GB8816681D0 (en) | 1988-08-17 |
| GB2223305A true GB2223305A (en) | 1990-04-04 |
Family
ID=10640384
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8816681A Withdrawn GB2223305A (en) | 1988-07-13 | 1988-07-13 | Pre-injection water vapour differential thermal-analysis |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB2223305A (en) |
-
1988
- 1988-07-13 GB GB8816681A patent/GB2223305A/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| GB8816681D0 (en) | 1988-08-17 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| WAP | Application withdrawn, taken to be withdrawn or refused ** after publication under section 16(1) |