WO1993003353A2 - Lösungskalorimetrie durch inkrementelle mischung - Google Patents
Lösungskalorimetrie durch inkrementelle mischung Download PDFInfo
- Publication number
- WO1993003353A2 WO1993003353A2 PCT/CH1992/000159 CH9200159W WO9303353A2 WO 1993003353 A2 WO1993003353 A2 WO 1993003353A2 CH 9200159 W CH9200159 W CH 9200159W WO 9303353 A2 WO9303353 A2 WO 9303353A2
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- reagent
- probe
- partial volume
- mixing
- measuring
- Prior art date
Links
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01K—MEASURING TEMPERATURE; MEASURING QUANTITY OF HEAT; THERMALLY-SENSITIVE ELEMENTS NOT OTHERWISE PROVIDED FOR
- G01K17/00—Measuring quantity of heat
-
- 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
Definitions
- the invention relates to a device for measuring calorimetric effects in solutions without using a calorimeter system in the conventional sense.
- the heat effect is measured in a semi-enclosed area at the point where two solutions are mixed.
- This new arrangement dispenses with the complex technical solutions that are customary for adiabatic or heat flow calorifiers. It is therefore a special feature of the described device that titrations can be carried out in any vessel without thermal insulation or cladding with thermocouples.
- thermally insulated containers have generally been used, in particular for t hermomet ri see titration and the resulting temperature change registered with increasing addition of reagent.
- an attempt is made to distribute the reaction energies in the system quickly and evenly by mixing them as effectively as possible.
- These compensation processes reduce the magnitude of the thermal effects, corresponding to the resulting dilution.
- the subject of the invention is now one Measuring probe which delimits the zone of thorough mixing by typically pulling 1-4 ml from the template through a piston stroke into the tube of the probe and simultaneously mixing it with reagent (typically 50-200 ul).
- reagent typically 50-200 ul.
- the shape of the mixing zone is designed in such a way that diffusion and mixing with the rest of the system are delayed so that a local temperature peak can be measured. If this process is repeated, a sequence of signals of decreasing intensity is obtained, which contain all information relating to a thermometric titration.
- Corrections for the temperature change in the template and for the course of the calorimetric system can be detected via thermal sensors and compensated for using the known methods of electronics or data processing.
- Fig. 3 Signal sequence in the thermometer titration.
- Fig. 1 gives an overview of the experimental arrangement, it being pointed out that the vessel with the template does not have to be covered by the apparatus.
- the piston (5) is moved by a rod on a rotating disc (2) driven by an electric motor (1).
- we used 60 ml of a solution with C (HCl) - 0.0083 mol / L as template ( 3) for the thermometric titration.
- Fig. 2 we have the actual measuring probe with a stroke - • volume for the mixing zone of approx. 4 ml.
- the piston (5) and the closure head (6) are made of Teflon, while the cylinder is made of one Glass tube exists.
- the internal thermistor (8) and the external thermal disturbance (9) are connected as two arms of a Wheatstone bridge and enable tapping of a signal which corresponds to the temperature difference between the reaction space and the original.
- the reagent is added through the reagent capillary (7) during the suction process.
- a cycle with stroke - reagent addition - compensation in the mixing room - emptying typically takes 20 s.
- the absolute temperature (11) is plotted, measured with a platinum resistance thermometer.
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
Description
Claims
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CH235391A CH682769A5 (de) | 1991-08-09 | 1991-08-09 | Vorrichtung zur Messung kalorimetrischer Daten, insbesondere der thermometrischen Titration. |
CH2353/91-2 | 1991-08-09 |
Publications (2)
Publication Number | Publication Date |
---|---|
WO1993003353A2 true WO1993003353A2 (de) | 1993-02-18 |
WO1993003353A3 WO1993003353A3 (de) | 1993-04-15 |
Family
ID=4231805
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/CH1992/000159 WO1993003353A2 (de) | 1991-08-09 | 1992-08-04 | Lösungskalorimetrie durch inkrementelle mischung |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP0552335A1 (de) |
CH (1) | CH682769A5 (de) |
WO (1) | WO1993003353A2 (de) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2712090A1 (fr) * | 1993-11-04 | 1995-05-12 | Bernard Lyon I Universite Clau | Procédé et dispositif de mesure de la solubilité d'au moins un soluté solide, liquide ou gazeux dans un solvant, par analyse thermique isopléthique. |
DE10042568A1 (de) * | 2000-08-25 | 2002-03-21 | Univ Dresden Tech | Durchflussmesszelle zur Konzentrationsmessung aus Temperaturveränderungen |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2514509A1 (fr) * | 1981-10-14 | 1983-04-15 | Energiagazdalkodasi Intezet | Procede pour la qualification rapide de matieres solides |
-
1991
- 1991-08-09 CH CH235391A patent/CH682769A5/de not_active IP Right Cessation
-
1992
- 1992-08-04 WO PCT/CH1992/000159 patent/WO1993003353A2/de not_active Application Discontinuation
- 1992-08-04 EP EP19920916298 patent/EP0552335A1/de not_active Withdrawn
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2514509A1 (fr) * | 1981-10-14 | 1983-04-15 | Energiagazdalkodasi Intezet | Procede pour la qualification rapide de matieres solides |
Non-Patent Citations (1)
Title |
---|
JOURNAL OF ANALYTICAL CHEMISTRY OF THE USSR Bd. 30, Nr. 5, Mai 1975, Seiten 946 - 950 R.P.PANTALER ET AL. 'kinetic thermometric method of determining microamounts of cobalt' * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
FR2712090A1 (fr) * | 1993-11-04 | 1995-05-12 | Bernard Lyon I Universite Clau | Procédé et dispositif de mesure de la solubilité d'au moins un soluté solide, liquide ou gazeux dans un solvant, par analyse thermique isopléthique. |
DE10042568A1 (de) * | 2000-08-25 | 2002-03-21 | Univ Dresden Tech | Durchflussmesszelle zur Konzentrationsmessung aus Temperaturveränderungen |
DE10042568C2 (de) * | 2000-08-25 | 2002-11-14 | Univ Dresden Tech | Durchflussmesszelle zur Konzentrationsmessung aus Temperaturveränderungen |
Also Published As
Publication number | Publication date |
---|---|
EP0552335A1 (de) | 1993-07-28 |
WO1993003353A3 (de) | 1993-04-15 |
CH682769A5 (de) | 1993-11-15 |
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