Analytical process in which materials to be analyzed are directly and indirectly heated and dried by microwave radiation

• US 4,681,996 A
• Filed: 12/19/1985
• Issued: 07/21/1987
• Est. Priority Date: 12/16/1982
• Status: Expired due to Fees

• Current Assignee: CEM Global LLC
• Original Assignee: CEM Global LLC
• Inventors: Collins, Michael J., Hargett, Wyatt P. Jr.
• Primary Examiner(s): Leung, Philip H.
• Application Number:
  US06/811,540
• Time in Patent Office: 579 Days
• Field of Search: 219/10.55 F, 219/10.55 E, 219/10.55 B, 219/10.55 M, 219/10.55 R, 99/DIG. 14, 99/451, 34/1, 374/14
• US Class Current: 219/759
• CPC Class Codes: G01N 22/04 Investigating moisture content
• CPC Class Codes: G01N 5/045 for determining moisture content
• CPC Class Codes: H05B 2206/046 Microwave drying of wood, ink, food, ceramic, sintering of ceramic, clothes, hair
• CPC Class Codes: H05B 6/80 Apparatus for specific applications stoves or ranges F24C7/02

Abstract

An apparatus for controllably heating material, such as a material to be analyzed for volatiles or non-volatiles contents, directly and indirectly by microwave radiation, includes a chamber, in which the material to be heated is placed, a source of microwave radiation, for radiating onto materials in the chamber and for controllably heating such a material, and a support for such material, which support includes a matrix of a material which transmits microwave radiation, and also includes particulate material therein which absorbs microwave radiation. The absorptive material is one that has a Curie temperature, above which it is transmissive of microwave radiation, so as thereby to prevent excessive heating of the support and the supported material which is to be heated. The matrix material is stable and form-retaining at the Curie temperature of the dispersed material. Preferably the support matrix will be of a silicone rubber or of a polyfluoroalkylene polymer, such as polytetrafluoroethylene, and the dispersed material will be a ferrite, garnet or a mixture thereof. The apparatus may include a turntable for one or more supports, an automatic electronic balance, computerized controls and readout means. Also within the invention are the described support, and processes for heating and drying, in a preferred embodiment of which processes a particulate diluent or dispersant for the sample being treated is employed to prevent overheating of the sample.

Claims

1. A process for/analyzing a thermally sensitive material for its content of volatilizable components without degrading the material, which comprises supporting the material to be analyzed, which includes lossy and non-lossy volatilizable component(s), by means of a support which comprises 40 to 95% of a matrix material which is transmissive of microwave radiation, 5% to 60% of a microwave absorptive material dispersed in such matrix material, which microwave absorptive material has a Curie temperature in the range of 85°

to 650°

C., above which it becomes microwave transmissive, so as thereby to prevent excessive heating of the support and the material to be analyzed, which matrix material is stable and form retaining at the Curie temparature of the dispersed material, and directing microwave radiation onto the material to be analyzed and onto the support for such material so as directly to heat the material when it contains lossy volatilizable component(s) and indirectly to heat such material by heating the support when the material to be analyzed no longer contains any lossy component(s), which support heats the material to a temperature no higher than the Curie temperature of the dispersed microwave absorptive material in the matrix of the support, at which temperature the material being analyzed is not degraded, and applying sufficient microwave radiation to bring the microwave absorptive material of the support to its Curie temperature.

2. A process according to claim 1 wherein the support comprises a body of matrix material which is transmissive of microwave radiation, with a coating thereon of a microwave absorptive material dispersed in such matrix material.

3. A process according to claim 2 wherein the material to be controllably heated and analyzed is a material containing moisture which is removable by microwave heating and which is removed by such heating during the process, which material contains additional moisture which resists removal by microwave heating and is removable by indirect microwave heating, whereby heat is transmitted to it from the microwave heated support through the intermediate fiberglass mat, and which additional moisture is removed by such indirect heating during the process.

4. A process according to claim 3 wherein the material to be controllably heated and analyzed is in particulate form, of particle sizes substantially all of which are in the range of Nos. 10 to 325 sieves, U.S. Sieve Series, and is dispersed in a particulate inert and thermally stable material, the particles of which are substantially all in the range of Nos. 10 to 325 sieve, U.S. Sieve Series, with the proportion of material to be controllably heated and analyzed to the dispersant being within the range of 1:

0.2 to 1;

5.

5. A process according to claim 2 wherein the matrix material is polytetrafluoroethylene, the Curie temperature of the microwave absorptive material is in the range of 105°

to 500°

C., the microwave absorptive material is in finely divided particulate form, the percentages of matrix material and microwave absorptive material in the coating are from about 40 to 95% and 5 to 60%, respectively, and the support is in the form of an evaporating dish, the body portion of which is of a thickness in the range of 0.5 to 3 mm. and the coating of which is of a thickness in the range of 0.5 to 3 mm.

6. A process according to claim 1 wherein the support is in the form of a supporting body in which the matrix material is a continuous phase and the microwave absorptive material is in finely divided particulate form, substantially evenly dispersed throughout the matrix material, and the microwave absorptive material is selected from the group consisting of ferrites, garnets and mixtures thereof.

7. A process according to claim 6 wherein the thermally sensitive material to be controllably heated and analyzed contains a lossy dielectric, which makes it microwave absorptive, at least a major proportion of which lossy dielectric is removed by direct microwave heating of the material, and the material is supported directly by an intermediate fiberglass mat which rests on the support.

8. A process according to claim 1 wherein the material to be controllably heated and analyzed is in particulate form, of particle sizes substantially in the range of Nos. 10 to 325 sieves, U.S. Sieve Series, and is dispersed in a particulate, inert and thermally stable material, the particles of which are substantially in the range of Nos. 10 to 325 sieves, with the proportion of material to be analyzed to the dispersant being within the range of 1:

0.2 to 1;

5, by weight.

9. A process according to claim 8 wherein the material being analyzed is milk powder, the volatilizable component of which is water, the dispersant for the milk powder is selected from the group consisting of salt, sand and quartz, and the proportion of milk powder to dispersant for it is in the range of 1:

0.5 to 1;

3.

10. A process according to claim 9 wherein the milk powder contains about equal proportions of protein and lactose, and 2 to 5% of water, the dispersant for the milk powder is salt, the microwave absorptive material is selected from the group consisting of ferrites, garnets and mixtures thereof, the matrix material is selected from the group consisting of silicone rubbers and polyfluoroalkylene polymers, and the sample of milk powder being analyzed is on an intermediate fiberglass mat which rests on and is in contact with the support.