Microwave ashing apparatuses and components

• US 5,318,754 A
• Filed: 01/15/1993
• Issued: 06/07/1994
• Est. Priority Date: 04/21/1983
• Status: Expired due to Term

• Current Assignee: CEM Global LLC
• Original Assignee: CEM Global LLC
• Inventors: Collins, Michael J., Hargett, Wyatt P.
• Primary Examiner(s): Housel, James C.
• Assistant Examiner(s): Snay, Jeffrey R.
• Application Number:
  US08/005,252
• Time in Patent Office: 508 Days
• Field of Search: 73/864.91, 220/4.21, 220/200, 219/10.55 R, 219/10.55 A, 219/10.55 D, 219/10.55 E, 219/10.55 F, 219/10.55 M, 422/78, 422/82.12, 422/102, 422/104, 422/109, 422/198, 422/288, 422/300, 422/307, 436/155, 436/160
• US Class Current: 422/109
• CPC Class Codes: B01J 19/126 Microwaves
• CPC Class Codes: B01J 2219/1218 Multiple reactors
• CPC Class Codes: B01L 7/00 Heating or cooling apparatus autoclaves B01J3/04; Heat insulating devices
• CPC Class Codes: C03B 37/15 with heat application, e.g. for making optical fibres fusion-splicing of light guides G02B6/255; treatment of light guides to shape optical elements G02B6/2835, G02B6/2856
• CPC Class Codes: C03B 5/08 Glass-melting pots
• CPC Class Codes: F27D 1/0009 Comprising ceramic fibre elements
• CPC Class Codes: F27D 2099/0028 Microwave heating
• CPC Class Codes: F27D 5/0068 Containers
• CPC Class Codes: F27M 2003/11 Incineration
• CPC Class Codes: G01N 1/44 Sample treatment involving radiation, e.g. heat
• CPC Class Codes: G01N 31/12 using combustion G01N25/20 takes precedence
• CPC Class Codes: G01N 33/04 Dairy products
• CPC Class Codes: H05B 6/64 Heating using microwaves containers, packaging elements or packages specially adapted to be heated by microwaves B65D81/3446
• CPC Class Codes: H05B 6/6455 the sensors being infrared detectors
• CPC Class Codes: H05B 6/66 Circuits

Abstract

An apparatus for use in analyzing materials for ash content includes a walled chamber which retains microwave radiation therein, a source of microwave radiation, such as a magnetron, for radiating onto contents of such chamber, and an ashing furnace in the chamber which includes a heat resistant wall of low thermal conductivity, which is transmissive of microwave radiation, and a microwave absorptive material which is capable of being heated by microwave radiation to an ashing temperature. The furnace includes a passageway through it for the entry into the furnace cavity of a gas, such as air, and for venting gas, such as combustion products, from the furnace cavity, and preferably also includes a removable trapezoidally shaped door in a front wall thereof, which, when the chamber door is open, is readily removable from the furnace by hand, without burning the operator'"'"'s fingers, despite the high internal temperature in the furnace cavity. Air flows through the chamber and around the furnace, helping to cool the exterior, of the furnace walls. It is preferred that the operation of the furnace and the ashing temperature be controlled by a combination of a temperature sensor, preferably a thermocouple, and a control mechanism, which turns the magnetron on and off as the temperature in the furnace cavity falls below or rises above a desired set temperature, respectively.

Claims

1. An apparatus for ashing ashable materials which comprises:

a walled microwave retaining chamber;

a source of microwave radiation for radiating onto contents of said chamber, which contents include said ashable material;

an ashing furnace within said chamber having a furnace wall of heat resistance material about an internal furnace cavity, with an opening in said furnace wall for insertion and removal of said ashable material, a door of heat resistant material for closing and opening said opening in said furnace wall, a microwave absorptive material which has a surface thereof exposed to said furnace cavity, which microwave absorptive material is capable of being heated to an ashing temperature by microwave radiation, and a passageway through said furnace for passing gas into the furnace cavity and for venting gas from said cavity, which passageway includes an upper portion through which gas is removed from an upper portion of the furnace cavity, with the furnace wall and furnace door being of heat resistant material of low thermal conductivity which is essentially transparent to microwave radiation;

a temperature sensor;

for sensing the temperature in the ashing furnace, which sensor is located in said upper portion of said passageway through the furnace and is of a size that allows passage of gas past it from the furnace cavity to the chamber through a clearance in the passageway; and

controlling means, responsive to the temperature sensor, for controlling the source of microwave radiation and thereby controlling the temperature in the ashing furnace.

2. An apparatus according to claim 1 wherein the passageway through the furnace for passing gas into the furnace cavity and for venting gas from said cavity includes an opening between the furnace door and the furnace door opening, through which gas can enter the furnace.

3. An apparatus for ashing ashable materials which comprises:

a walled microwave retaining chamber;

a source of microwave radiation for radiating onto contents of said chamber;

an ashing furnace within said chamber having a furnace wall of heat resistant material about an internal furnace cavity, with an opening in said furnace wall for insertion and removal of an ashable sample, a door of heat resistant material for closing and opening said opening in said furnace wall, a microwave absorptive material which has a surface thereof exposed to said furnace cavity, which material is capable of being heated to an ashing temperature by microwave radiation, and a passageway through said furnace for passing gas into the furnace cavity and for venting gas from aid cavity, with the furnace wall and furnace door being of heat resistant material of low thermal conductivity which is essentially transparent to microwave radiation;

a temperature sensor, for sensing the temperature in the ashing furnace, which sensor is located in said passageway through the furnace and which is of a size to allow passage of gas from the furnace cavity to the chamber through a clearance in the passageway;

controlling means, responsive to the temperature sensor, for controlling the source of microwave radiation other thereby regulating the temperature in the asking furnace; and

inlet and outlet openings in the microwave retaining chamber wall for passage of gas into and out of said chamber, around said furnace.

4. An apparatus according to claim 3 wherein the door for the furnace wall is removable from the furnace wall to enable chargings of the furnace with containers of ashable samples and removals of such containers after ashings, when the furnace is still hot, which door has handle or gripping means on an exterior portion thereof, and is of a material of low thermal conductivity so that the handle can be grasped by the fingers of an operator while the interior of the door is at or near ashing temperature, without burning the operator.

5. An apparatus according to claim 3 wherein the wall and door of the ashing furnace are of an open cell ceramic foam which is transparent to microwave radiation and is of low thermal conductivity, the microwave absorptive material is silicon carbide, and the furnace door and wall opening are so shaped that the door may be partially opened to permit controlled air flow into the furnace through the passageway resulting.

6. An apparatus according to claim 3 wherein the source of microwave radiation is a magnetron and the temperature in the furnace cavity is controllable by the temperature sensor and controlling means, which turn the magnetron on when the temperature in the furnace cavity is less than a set temperature and which turn it off when the temperature in the cavity is more than such set temperature.

7. An apparatus according to claim 3 wherein the ashing furnace wall is of separable upper and lower portions and is of open cell ceramic foam and, with the furnace door, which is of open cell ceramic foam, defines said furnace cavity having a top, a bottom and sides, with the sides and bottom being at least partially lined with silicon carbide.

8. An apparatus according to claim 3 wherein there is present in the furnace cavity at least one heat resistant container for holding an ashable analytic sample.

9. An apparatus for ashing ashable samples which comprises:

a walled microwave retaining chamber;

a source of microwave radiation for radiating onto contents of said chamber;

an ashing furnace within said chamber having a furnace wall about an internal furnace cavity, with an opening in said furnace wall for insertion therein and removal therefrom of an ashable sample, a door for closing and opening said opening in said furnace wall, a microwave absorptive material which has a surface thereof exposed to said furnace cavity, which absorptive material is capable of being heated to an ashing temperature by microwave radiation, a passageway through said furnace for passing gas into the furnace cavity and for venting gas from said cavity, said passageway comprising an opening in an upper portion of the heat resistant wall of the asking furnace for passage of gas from the furnace cavity to the chamber, with the furnace wall and furnace door being of heat resistant material of low thermal conductivity which is essentially transparent to microwave radiation;

a thermocouple;

a controlling means, responsive to said thermocouple, for controlling the source of microwave radiation and thereby regulating the temperature in the ashing furnace; and

electrically conducting means for connecting the controlling means and the thermocouple;

with the thermocouple being located in the opening in the upper portion of the wall of the ashing furnace and with said opening being larger than the thermocouple so as to allow passage of gas from the furnace cavity to the chamber through a clearance between said opening and said thermocouple; and

inlet and outlet openings in the microwave retaining chamber wall for passage of gas into and out of said chamber, around said furnace.

10. An apparatus according to claim 9 wherein the walled microwave retaining chamber has a doorway opening therein and a door to selectively close and open the doorway, with such door and doorway being aligned with the furnace opening and door so that ready access to the furnace cavity is obtainable through the chamber opening and furnace opening when both the chamber door and the furnace door are in open positions.

11. An apparatus according to claim 10 wherein the ashing furnace wall is made of a quartz or ceramic foam which is stable at furnace cavity temperatures up to 1,000°

C., the microwave absorptive material is silicon carbide, the source of microwave radiation is a magnetron, and the temperature in the furnace cavity is controllable within 10°

C. of a set ashing temperature, up to 1,000°

C., by the thermocouple and controlling means, which turn the magnetron on when the temperature in the cavity is less than the set temperature and which turn it off when the temperature in said cavity is more than the set temperature.

12. An apparatus according to claim 11 wherein the wall of the ashing furnace is made of an open celled fused quartz foam which is of a density in the range of 0.3 to 0.8 g./c. cm., the open celled fused quartz foam is stable at a furnace cavity temperature up to 1,650°

C., and the temperature in the furnace cavity is controllable to within 5°

C. of a set ashing temperature in the range of 600°

to 1,000°

C. by the thermocouple and controlling means.

13. An apparatus according to claim 12 wherein the ashing furnace wall that defines the furnace cavity and the furnace wall opening for the door is made of upper and lower unitary pieces of the open celled fused quartz foam and the furnace door is made of a separate piece of the same material.

14. An apparatus according to claim 13 wherein the ashing furnace wall defines said furnace cavity having top, bottom and side portions, with the sides and bottom being at least partially lined with silicon carbide, and the furnace door is substantially of trapezoidal shape in horizontal cross-section, and fits with said opening in the furnace wall, enabling removal of the door, partial opening, and closure thereof, as desired.

15. An apparatus according to claim 14 wherein the bottom portion of the ashing furnace includes grooves for insertion of silicon carbide strips or slabs therein, and the furnace door includes handle or gripping means to enable holding of said door with an operator'"'"'s fingers when it is being opened or closed.

16. An apparatus according to claim 15 wherein there is present in the furnace cavity at least one heat resistant container for holding analytical sample(s).

17. An apparatus according to claim 16 wherein at least one said container for the analytical sample(s) is a light weight walled container of essentially microwave transparent quartz microfibers which allow gas flow therethrough but prevent passage of ash therethrough.