Abstract:
A dual power-supply system is used to produce a sharp rise-time characteristic and a high steady-state temperature in a platinum ribbon pyrolysis probe. First, a small &#34;boost&#34; power supply generates a very short, high power pulse that is applied to the probe. Then, at its peak, the first power supply is effectively disabled and a second power supply is brought into play to maintain the power (and the temperature) in the probe at a high steady-state value approximating the peak value of the boost pulse.

Description:
BACKGROUND OF THE INVENTION 
     A. Field of the Invention 
     This invention relates to pyrolysis instruments (pyrolyzers) and, more particularly, to improved pyrolysis instrument systems for attaining much higher pyrolysis temperatures within a much shorter time than are achieved by conventional ones. 
     B. Prior Art 
     Previously, pyrolyzers were known such as Model 121 &#34;Pyroprobe&#34; manufactured by Chemical Data Systems, Inc. of Oxford, Pa. These pyrolyzers, while useful for many purposes had certain limitations. One of them was an inability to produce within a very short time a desired very high temperature. For certain research projects, such as the pyrolysis study of products of combustion released by smoldering as opposed to flame type fires, the rate of increase in the temperature to which the substance being studied is subjected may reveal what pyrolysis products are released during successive time intervals. With conventional pyrolyzers if a very sharp rise time characteristic for the temperature on the probe was achieved, there was a noticeable dip in the temperature curve of the probe just after it first achieved a maximum temperature. Investigation revealed that the lowering of the temperature in that region of the curve, especially when very high temperatures were to be attained, was due to the construction of the probe used with the pyrolysis instrument. In the case of platinum ribbon used as the heat-generating element of the probe, it was found that its welding connections acted as a heat sink and were in large part responsible. This dip prevented the making of accurate and reproducible studies under high temperature conditions which were to be subsequently analyzed by apparatus such as gas chromatographs, for example. 
     It is therefore among the objects of the present invention to provide pyrolysis apparatus which: 
     1. Can more rapidly attain a desired steady-state temperature. 
     2. Having attained a higher temperature, can maintain it without significant &#34;dips&#34; just after the probe initially attains its predetermined maximum temperature. 
     3. Provide more diversified programmed pyrolyses including much slower increases in temperature as well as much faster ones than are conventionally available. 
     4. Provide a more accurate indication of the average temperature on a pyrolysis probe. 
     5. Provide greater diversity and flexibility in generating and choosing operating modes of the pyrolysis probe. 
     SUMMARY OF THE INVENTION 
     A pyrolysis probe energizing system is powered initially by a high voltage pulse of very short duration from a first power supply to achieve a very steep temperature rise-time characteristic. Then the first supply is effectively disabled and a second power supply is switched in to maintain the previously generated high steady state temperature. 
    
    
     BRIEF DESCRIPTION OF THE DRAWINGS 
     FIG. 1 is a drawing depicting the temperature-time characteristics of conventional pyrolysis apparatus and an idealized curve of a desired pryolyzer temperature-time characteristic; 
     FIG. 2 shows curves illustrating the general theory and operation of one feature of the present invention; 
     FIG. 3 is a block diagram of the dual power supply feature of the present invention; 
     FIG. 4 is a schematic circuit diagram corresponding to the blocks of FIG. 3; 
     FIG. 5 is a block diagram of the main components of the CPU shown in FIG. 3; 
     FIG. 6 is a block diagram of the probe driver shown in FIG. 3; and 
     FIG. 7 is a schematic electrical diagram of a probe driver corresponding to the block diagram in FIG. 6. 
    
    
     DETAILED DESCRIPTION OF THE INVENTION 
     FIGS. 1 and 2 
     FIG. 1 shows a generalized solid-line curve A indicating the temperature produced by a conventional pyrolysis probe using, for example, a platinum coil. It is seen that a number of milliseconds elapse from the time t o  that current is first applied to the probe to the time t 1  at which it reaches its maximum, steady-state or &#34;hold&#34; temperature T SS . As explained above, the time interval required to attain T SS  may be considerably longer than desired. The broken-line curve B is idealized and shows a much more rapid leading edge characteristic. 
     In an effort to attain a very short rise time to the steady state temperature condition, much higher temperatures have been generated in the main element of the pyrolysis probe. For this purpose, some probes were used having an active heating element made of platinum ribbon. The ribbon has a very low thermal inertia as compared with a platinum coil used in conventional models which are considerably slower in attaining the desired temperature. The use of such ribbons and appropriate energizing circuits has enabled the production of much steeper leading edges of the temperature-time characteristic curve as shown at curve C in FIG. 2. However, as seen in the hyphenated portion D, just after the temperature T SS  is first attained at time t x , even though the probe continued thereafter to be energized with a constant voltage. a dip would appear in the curve C. At a time t 1  the amplitude of the curve C would regain its former maximum value. In accordance with the present invention, it is desirable to offset the dip by producing a corrective or compensatory signal voltage E (dotted line) in the interval t 0  -t 1 . Since the dip is caused by the characteristics of the probe itself, the corrective voltage E restores the temperature produced in the probe in the interval t x  -t 1  to the value as shown by the solid line section F of curve C. 
     The platinum ribbon is very expensive and very temperature-vulnerable. If it is heated too quickly or for too long a time, it could be destroyed. If it is subjected to a sudden initial surge of power say, 100 watts, from a power supply, it might easily be damaged. Moreover, if that amount of current were continuously applied to it after a gradual build-up, it also risks being burned up. Therefore, one way to solve the problem would be to provide means for dissipating that excessive power. This would entail a large and expensive power supply system. 
     In accordance with the present invention, the desired temperature characteristic of the probe from t 0  to t 1  is produced by first using a &#34;boost&#34; pulse type of power supply for a very short predetermined time interval derived as a function of the ultimate steady state temperature to be attained. Then, at t 1 , the boost power supply is effectively turned off and from that point on, the energization of the probe is supplied by a second or main power supply. The latter&#39;s output is closely regulated by a special driving circuit including timers and acting in response to a central processing unit and to the sensed true average temperature signal derived from the probe itself. 
     FIG. 3--General Overview of System 
     FIG. 3 shows the overall system in a block diagram. It comprises a central processing unit 18 (FIG. 5) which includes the usual arithmetic, memory and associated circuits. The CPU is coupled to a probe driver circuit 16. AC is inductively applied in boost power supply 20 to a transformer 24 to whose output a bridge 26 is connected. A large capacitor 28 is connected to the output of the bridge which is coupled to a transistor switch 29. The switch is enabled to pass to the probe 25 the voltage built up in the capacitor 28 when the &#34;boost trigger&#34; signal from CPU 18 is applied to it via amplifier 27. Boost power supply 20 provides the initial high power pulse to the probe 25 during the first interval t x  -t 1  (FIG. 2). 
     The second or main power supply 22 also includes a transformer 34 to whose input AC is applied inductively. The output of the transformer is coupled to a rectifying bridge 36 and the output of the latter is coupled to a large capacitor 38 and to an amplifier 39. The latter&#39;s output is also connected to an isolation diode 23 intermediate the amplifier 39 and probe 25. The diode prevents the &#34;boost&#34; power pulse from boost power supply 20 from affecting the main power supply 22. 
     The two power supplies are so arranged that the probe will effectively produce a single solid line curve C (FIG. 2) comprised of the initial high power boost pulse during the period t 0  -t 1  and, then without interruption, the steady state portion of curve C beginning at t 1  and ending at t 3  (FIG. 2). 
     FIG. 4--Power Supplies Schematic 
     As stated above, there are two power supplies, the boost power supply 20 for the initial supply of the high power pulse to the pyrolysis probe 25 and the main power supply 22. Both supplies are operating at the time, computed by the CPU, that the boost power supply 20 is triggered by the boost trigger signal from the CPU. The trigger signal is applied to Zener diode CR2, through resistor R4 to an amplifying circuit comprising transistors Q3, Q2, and Q1. The amplified boost trigger signal from Q1 is applied to the base of switching transistor 29 whose emitter receives the DC from capacitor 28. 
     The DC is derived from a secondary winding 24 coupled to a primary winding (not shown) energized with AC. This power supply is not regulated. The line AC voltage is measured by the CPU and that quantity is factored into an equation by the CPU which sends the boost trigger signal in response thereto. The AC induced in winding 24 is rectified in bridge 26 and stored in a very high capacitor 28 which may have a value of, for example, 67,000 mf. With this large capacitor, even if there is a small initial AC applied to it, a voltage of approximately 20 volts DC can be produced. It is this voltage which is essentially switched into the circuit via switching transistor 29 when the latter has been rendered conductive by the amplified boost trigger signal originating in the probe driver 16 when commanded by the CPU 18. The DC signal is applied to the probe represented by the resistance 25. While it is so applied, the blocking diode 23 prevents the high power from affecting adversely the components of the main power supply 22. 
     The duration of the boost pulse might be, typically, 5.0 milliseconds, depending upon the ultimate temperature to be generated in the probe. Calculation of the duration of the initial pulse is accomplished in CPU 18 and when the boost trigger signal is applied to the switching transistor 29, about 40 volts may be produced across the probe. 
     The main power supply 22 includes a secondary winding 34 for producing an AC voltage which is then rectified in bridge 36 and applied to another very large capacitor 38 which may have the same or similar value as capacitor 28. The voltage builds up across the capacitor 38 and is applied to an amplifying circuit comprising Q5, Q4, and Q8. The isolating diode 23 is not needed to protect the main power supply 22 once the pulse from boost supply 20 has terminated since the latter power supply then goes off. However, once the boost pulse is ended, the amplified output appearing at the emitter of transistor Q8, which is a power transistor, passes through diode 23 and energizes the probe 25. 
     Not shown in the block diagram of FIG. 3 is a circuit just below coil 34, bridge 36, capacitor 38 and resistance R5 in FIG. 4. That includes a winding 35 into which AC is induced from a transformer primary, a bridge 37, and a filter (R7, C2) that supplies DC through resistor R6 to the base of Q7 which is in series with the base of Q6, the latter two transistors operating to determine whether or not AC power is present. If someone were to unplug the unit, or should there be a power failure, Q6 and Q7 operate to prevent the ramp signal, shown in FIG. 4 being applied to amplifier 33, from passing through amplifier 31 since the output signal of transistor Q6 will not appear at the positive input of circuit 31. This prevents possible burnout of the expensive platinum sensing element of probe 25. 
     In certain applications, it is desired that the temperature of the probe be raised or lowered in response to a ramp signal fed to main power supply by CPU 18. This signal is derived in accordance with a predetermined program for producing programmed temperatures at the probe. The ramp signal comes from the probe driver (from an output of digital-analog converter Z13 of FIG. 6) as will be explained later. The ramp signal goes to a buffer amplifier 33 whose output is applied to another amplifier 31. The latter amplifier must be protected from the high voltage produced in the boost power supply and for the reason Zener diode CR1 is used at one of its inputs. It prevents an excessive voltage pulse from being applied to one of the inputs of circuit 31. Amplifier 31 responds only to signals at its inputs having a predetermined ratio whereupon its output signal energizes the probe after amplification in the amplifier circuit 39 comprising transistors Q5, Q4 and Q8. 
     FIG. 5--CPU 18 
     As stated above, the CPU 18 instructs and controls the probe driver 16 which supplies the boost input signal to the boost power supply 20 and the ramp signal to the main power supply 22. The CPU includes a keyboard 50 and a monitor display 49 coupled to a keyboard display controller 48. The person at the keyboard controls the operation of the entire system. Commands are entered on the keyboard and displayed on display 49 and the signals are relayed from the keyboard via the keyboard display controller 48 to the various components of the CPU. While many connections are shown as single lines, it is to be understood that they represent, in most cases, a plurality of leads, the number of them being shown in parentheses in many cases. The commands entered onto the keyboard by the operator are executed by the CPU according to the program entered into the PROM 46. Processing of the command signals is done in the microprocessor 45 to which an AC timer 52 is connected. Cooperating with the microprocessor are a plurality of address latches 51 that are coupled to the PROM 46 and RAM 47, respectively. Batteries 53 are provided as a back up for the RAM 47 in case of power loss. A control bus conveys the READ, WRITE, RESET, clock, S1 (timing), and IO/M signals to the probe driver 16. The IO/M signal controls the directing of signals between the CPU and memory and between the CPU and the hardware devices. There is also a connection between the miroprocessor 45 and the address latches 51 for the ALE (address latch-enable) signal which actuates various ones of the address latches 57 as determined by the microprocessor 45. The display 49 may be, for example, 24 discrete LED&#39;s and 8 IEE alphanumeric LED&#39;s. The keyboard 50, for example, may be a keyboard manufactured by KB Denver Company of Denver, Colo. 
     FIGS. 6 and 7--Probe Driver 16 
     FIG. 6 is a block diagram of the probe driver 16 shown in shematic form in FIG. 7. The driver includes an input-output chip Z1. It serves to couple the CPU 18 to the external hardware. It also provides an analog voltage output signal corresponding to the value of the digital signal computed in CPU 18. This output signal, appearing at an output of digital-analog converter Z13, constitutes the ramp signal that is applied to main power supply 22. Additionally, it provides signals, in response to information received from the CPU 18, which instructs its counters whether they should count up or down so that the slope of the ramp signal may be determined accordingly. Z1 receives control, reset, write, read, address and data information from CPU 18 as do timers Z2 to which it is connected. Z1 also transmits a load signal to counters Z4, Z5 and Z6 for transferring the digital information at their inputs to outputs of Z4, Z5 and Z6 and to the inputs of the converter Z13. 
     A variable frequency pulse train of pin 10 of Z2 controls the rate at which the temperature of probe 25 is increased or decreased. This signal is applied to one input of a gate Z3A. So long as the probe is not of the desired temperature, Z3A passes the pulses on to gates Z3B and Z3C. The latter also receive on UP/DN signal from Z1 which determines which way the counters Z4, Z5, and Z6 should count, i.e., up to the desired temperature or down to it. 
     Eventually the CPU 18 must know when the correct set or predetermined temperature has been generated and thus cease supplying digital signals representing higher temperatures to be generated. Since the CPU is not fast enough to work at the speeds required to drive the probe, there are provided a number of latches Z7, Z8 and Z9 which cooperate with a number of comparators Z10, Z11 and Z12 to monitor the count in counters Z6, Z5 and Z4. Latches store the temperature-representative digital signals from CPU, and comparators Z10, Z11 and Z12 continuously compare the count in Z7, Z8 and Z9 with the count of the digital signal relayed via counters Z4, Z5 and Z6 to converter Z13. So long as the two counts are unequal, gate Z3A will allow the pulses from Z2 to pass and this continues until parity of the counts is attained. At that instant a parity signal is generated at pin 6 of Z12 which is applied to amplifier 77 whose output signal applied to gate Z3A cuts the latter off. The same parity signal is applied to gate 75 and thence to one input of gate 76. The other input of the latter is connected to Z1 which supplies it with the probe ramp interrupt enable signal. 
     Associated with converter Z13 is an operational amplifier 71 which calibrates Z13. The potentiometer 70 setting determines how many volts one bit is equal to. 
     A reset signal from CPU 18 is applied to an input to Z1 and also directly to counters Z4, Z5 and Z6 to clear them so there is no voltage on probe 25 when the system is actuated. 
     Z2 provides at one of its outputs the boost trigger signal just discussed in connection with the boost power supply. This trigger signal is applied via gate 72 to power supply 20. Z2 is also coupled via gate 73 and 74 to a programmed temperature timing circuit 58 which times the steps of the ramp signal that controls the heating of the probe 25. Timer 58 consists of three chips which are coupled to Z2 for receiving time interval instructions computed by the CPU 18 in response to operation of the keyboard 50. After the predetermined time interval has elapsed, the timer 58 informs Z1 that it has timed out and steady state operation begins. 
     The particular digital-analog converter Z13 used requires negative inputs to produce an output. Associated with converter Z13 is an operational amplifier 71 which is used to set a reference voltage across the potentiometer 70 that calibrates Z13. 
     Z2, as stated above, provides the boost trigger voltage through gate 72. It is also coupled via gates 73 and 74 to the programmed timer 58. 
     
         ______________________________________FIG. 4  Item         Description______________________________________  R1           10K  R2           1K  R3           20K  R4           10K  R5           10K  R6           10K  R7           10K  R8           1K  R9           10K  R10          10K  R11          10K  R12          10K  R13          1K  R14          310  R15          310  R16          47  Q1           2N5195  Q2           2N2907A  Q3           2N3416  Q4           MJE200  Q5           MPS2222  Q6           2N3416  Q7           2N3416  Q8           2N3055  C1           .01 mf  28           67K mf  38           67K mf  C2           .1 mf  C3           .01 mf  C5           1 mf  C6           1 mf  CR1          1N4742A  23           MDA9906  29           2N5745  31           LM1458  33           LM1458______________________________________ 
    
     
         ______________________________________FIG. 5Item          Description______________________________________45            808546            271647            5101 (NEC) or 6116 (Hitachi)48            827949            8-IEE alphanumeric LED&#39;s         and is also 24 discrete LED&#39;s50            KB Denver keyboard51            8212______________________________________ 
    
     
         ______________________________________FIG. 7______________________________________Z1                8255Z2                8253Z3                7400Z4                74LS193Z5                74LS193Z6                74LS193Z7                74LS75Z8                74LS75Z9                74LS75Z10               74LS75Z11               74LS75Z12               74LS75Z13               758055                740456                740457                740W58                8253, 8255, 8259A59                (2)74LS0060                10K61                404962                404963                404964                404965                404966                100K67                1K68                10K69                .01 mf70                5K71                0P-0772                74LS0073                74LS0074                74LS0075                74LS0076                74LS0077                7404______________________________________ 
    
     APPENDIX 
     The accompanying print out of the program sets forth the program steps for controlling the apparatus shown in FIG. 3. Many of the program steps are directed to functions which are not pertinent to the invention, such as the keyboard/display interface and the oven control interface. 
     Those program steps which relate to the pyroprobe control are pertinent to the present invention. The pyroprobe control receives data inputted through the keyboard and performs calculations based on the inputted parameters as well as current temperature, final temperature, oven type and probe type. The calculations are completed before control of the probe is initiated. The results of the calculations are used to set the timers Z2 and 58 and the comparators Z10 through Z12. The &#34;boost time&#34; required to operate the second power supply to obtain high heating rates without overshoot or temperature dip is also determined along with the other calculations. 
     The program steps following the title &#34;PYRO PROBE 1000&#34; are broadly directed to the pyroprobe control. The initial portion of program steps under the aforementioned title deal with initially setting up the control. 
     The MSEC subroutine (steps 3303 through 331C) obtains the value for the time (in milliseconds) the probe is to be fired. 
     The RAMP subroutine (steps 331D through 3336) obtains the controlled heating rate for operating the second power supply. 
     The Boost subroutine (steps 3337 through 3350) provides the turn on for the second power supply. 
     The CALCULAPT (calculate probe temperature subroutine beginning at step 400C) performs preliminary calculations and sets up the IC&#39;s employed to control the pyroprobe. 
     The FAST LEVEL INTERVAL routine (beginning at program step 42FA) determines the corrections necessary for removing the dip in the temperature curve. 
     The VERY FAST RAMP routines 1 through 8 (program steps 451E through 48F8) performs the dip correction by generating 8 segments which comprise a mirror image of the dip in the temperature curve. ##SPC1##