Pyrometric temperature measurements in flameless atomic absorption spectroscopy

• US 4,283,934 A
• Filed: 11/07/1979
• Issued: 08/18/1981
• Est. Priority Date: 01/29/1979
• Status: Expired due to Term

• Current Assignee: Bodenseewerk Perkin-Elmer GmbH (Revvity, Inc.)
• Original Assignee: Bodenseewerk Perkin-Elmer
• Inventors: Siess, Gerhard
• Primary Examiner(s): Gill, James J.
• Application Number:
  US06/092,247
• Time in Patent Office: 650 Days
• Field of Search: 73/1 F, 73/355 EM, 356/43, 356/45
• US Class Current: 374/2
• CPC Class Codes: G01J 3/42 Absorption spectrometry; Double beam spectrometry; Flicker spectrometry; Reflection spectrometry beam switching arrangements G01J3/08
• CPC Class Codes: G01J 3/443 Emission spectrometry
• CPC Class Codes: G01J 5/0003 for sensing the radiant heat transfer of samples, e.g. emittance meter
• CPC Class Codes: G01J 5/041 Mountings in enclosures or in a particular environment
• CPC Class Codes: G01J 5/042 High-temperature environment G01J5/0007, G01J5/0044, G01J5/0088 and G01J5/004 take precedence
• CPC Class Codes: G01J 5/046 Materials; Selection of thermal materials
• CPC Class Codes: G01J 5/08 Optical arrangements
• CPC Class Codes: G01J 5/0801 Means for wavelength selection or discrimination
• CPC Class Codes: G01J 5/0802 Optical filters
• CPC Class Codes: G01J 5/0804 Shutters
• CPC Class Codes: G01J 5/0805 Means for chopping radiation
• CPC Class Codes: G01J 5/0806 Focusing or collimating elements, e.g. lenses or concave mirrors
• CPC Class Codes: G01J 5/53 Reference sources, e.g. standard lamps; Black bodies
• CPC Class Codes: G01J 5/602 using selective, monochromatic or bandpass filtering

Abstract

A method and circuitry for maintaining the precise temperature of atomic absorption spectroscopy graphite specimen tubes over wide temperature ranges independently of the tube emission factor. The infrared radiation of a heated tube is measured by a detector, the signal from which is amplified in a variable gain amplifier, then compared with an externally generated "temperature select" signal, and the error signal therefrom controls a circuit that in turn controls the heating power to the graphite tube. A second measurement of the heated tube is made by a detector sensitive only to short wavelength radiation, e.g., visible, which is substantially unaffected by emission factors, and the signal therefrom adjusts the gain of the variable gain amplifier to thereby correct the infrared generated signal for variation in tube emission factors.

Claims

1. Circuitry for automatically adjusting the calibration of a first pyrometric radiation detector for extended temperature range measurements of a heated atomic absorption spectroscope graphite tube independently of the radiation emission factor of said tube, said first radiation detector being positioned to receive radiation from said tube and generating an output signal indicative of the temperature thereof, said circuit including:

a variable gain amplifier coupled to said radiation detector and responsive to the signal generated therefrom;

a second radiation detector positioned to sense the radiation emitted by said graphite tube, said second detector being accurate within a limited wavelength range and generating a second output signal that is independent of the emission factor of said graphite tube; and

circuitry means responsive to said second output signal for adjusting the gain of said variable gain amplifier whereby the output signal of said amplifier represents the temperature sensed by said first radiation detector corrected for emission factor;

the improvement comprising;

said second radiation detector being sensitive to a limited radiation wavelength range, the center of which is a shortwave with respect to a radiation emitted by said graphite tube, said second detector including said first radiation detector and a short wavelength transmitting filter interposable in the radiation beam from said graphite tube.

2. The circuitry claimed in claim 1 wherein said second radiation detector is positioned to receive the radiation from said graphite tube through a filter that transmits only said limited shortwave length range.

3. The circuitry claimed in claim 1 wherein said second detector is sensitive to a limited wavelength range, the center of which is visible light.

4. The circuitry claimed in claim 3 wherein said second detector is a silicon diode.

5. The circuitry according to claims 1, 2, 3 or 4 further including heating control circuitry for the accurate control of temperature of said graphite tube in accordance with an externally generated temperature control input signal, said control circuitry including:

a differential circuit coupled to the temperature control input terminal and to the output of said variable gain amplifier, said differential circuit producing an output error signal proportional to the difference between said control input signal and said variable gain output signal; and

tube control circuitry coupled to the output of said differential circuitry, the output of said tube control circuitry coupled to said graphite tube, said tube control circuitry varying the heating power to said graphite tube in accordance with said error signal.