Spectrophotometer

• US 3,935,463 A
• Filed: 12/05/1974
• Issued: 01/27/1976
• Est. Priority Date: 12/05/1974
• Status: Expired due to Term

• Current Assignee: LDC Analytical Incorporated
• Original Assignee: Milton Roy Company
• Inventors: Jacobsen, John Kenneth
• Primary Examiner(s): Lawrence, James W.
• Assistant Examiner(s): Grigsby, T. N.
• Application Number:
  US05/529,838
• Time in Patent Office: 418 Days
• Field of Search: 250/365, 250/364, 250/238, 250/373, 356/207, 356/51, 350/61
• US Class Current: 250/373
• CPC Class Codes: G01N 2021/152 Scraping; Brushing; Moving band
• CPC Class Codes: G01N 21/314 with comparison of measurements at specific and non-specific wavelengths dual wavelength spectrometry G01J3/427

Abstract

An improved spectrophotometer of the non-dispersive absorption type useful for detecting the presence of SO₂ in a gaseous sample, despite the simultaneous presence of NO₂. Ultraviolet light from a commercially-available source impinges upon a fixed phosphor screen which fluoresces to produce ultraviolet radiation at a first wavelength, at which both SO₂ and NO₂ absorb radiation; and at a second wavelength at which absorption by SO₂ is minimal but NO₂ absorption is approximately the same as at the first wavelength. The radiation is directed through a sample chamber having windows which are transversely slidable to effect cleaning without destroying the integrity of the chamber seal, then introduced into an envelope enclosing filters and a pair of photosensors. One photosensor receives light at the second wavelength and produces a signal which reflects the attenuation by NO₂ at that wavelength. The other sensor has disposed in front thereof a filter for blocking the second wavelength, and passing the first; and a phosphor for converting the passed (first) wavelength radiation into radiation at the second wavelength, which is then detected to produce a measure of the combined effect of NO₂ and SO₂. A comparison circuit then detects the differential between the first and second photosensors to determine the concentration of SO₂. Means are provided to maintain the lamp, sample chamber and envelope at predetermined temperatures. A source of mercury vapor within the envelope saturates the interior of the envelope with the vapor for selectively attenuating undesired radiation at the 254 wavelength.

Claims

1. Non-dispersive spectrometric apparatus for detecting the presence of a first gaseous material despite the presence of a second gaseous material, said first gaseous material absorbing electromagnetic radiation at a relatively high rate at a first wavelength, said second gaseous material absorbing electromagnetic radiation at both said first wavelength and at a second wavelength, comprising:

a source of electromagnetic radiation;

first and second photosensor means, said photosensor means being responsive to one of said first or said second wavelengths;

a chamber for receiving a sample to be tested for the presence of the first gaseous material, said chamber being disposed between said radiation source and said photosensor means;

first phosphor means disposed between said radiation source and said chamber for receiving radiation from said source and emitting in response thereto radiation at said first and said second wavelengths;

filter means disposed between said first photosensor means and said chamber for substantially attenuating radiation at that wavelength to which said photosensors are responsive, and passing the other of said wavelengths;

second phosphor means disposed between said first photosensor means and said filter means and responsive to said other of said wavelengths to produce radiation of the wavelength to which said photosensors are responsive; and

means coupled to said first and said second photosensor means for comparing the relative responses thereof to impingent radiation.

2. The invention defined in claim 1, wherein said first and said second wavelengths are in the ultraviolet range of the spectrum.

3. The invention defined in claim 2, further including second filter means disposed between said second phosphor means and said first and said second photosensor means, said second filter means being adapted to selectively pass radiation at the wavelength at which said photosensors are responsive.

4. The invention defined in claim 3, wherein said first gaseous material is SO₂ and said second gaseous material is NO₂.

5. The invention defined in claim 4, wherein said photosensor means are disposed within a sealed envelope, further including a source of mercury vapor disposed within said envelope;

and

heating means for maintaining the temperature within said envelope at a level sufficient so that adequate mercury vapor is present to attenuate radiation occuring at a wavelength of 254nm.

6. The invention defined in claim 5, further including heating means for maintaining said source of electromagnetic radiation and said chamber at predetermined temperatures.

7. The invention defined in claim 2, wherein said chamber is provided with window means at either end thereof, each of said window means comprising a frame and a pane which is substantially transparent to ultraviolet light, at least one of said panes being elongate, and further comprising resilient gasket means between said frame and said pane to seal said chamber and to allow said elongate pane to be displaced transversely with respect to said chamber, said gasket means serving to wipe accumulated impurities from the portion of the window so translated.

8. A non-dispersive spectrometer of the absorption type for detecting the presence of SO₂ in a sample regardless of the simultaneous presence of NO₂ comprising:

first and second photosensors responsive to ultraviolet light of a first wavelength;

a source of ultraviolet light;

a chamber disposed between said photosensors and said light source for receiving a sample to be analyzed for the presence of SO₂, said chamber having windows transparent to ultraviolet light disposed at the ends thereof;

a first phosphor element disposed between said light source and said chamber and responsive to said light source to emit ultraviolet light at said first and at a second wavelength;

the SO₂ exhibiting a relatively high degree of absorption at one of said first and second wavelengths and the NO₂ exhibiting predictably proportioned degree of absorption at both said first and said second wavelengths;

a filter disposed between said chamber and said first photosensor for attenuating light at said first wavelength and passing light at said second wavelength;

a second phosphor element disposed between said filter and said first photosensor and responsive to light at said second wavelength to produce light at said first wavelength; and

means coupled to said first and second photosensors for outputting a signal representative of the differential response thereof to impingent radiation.

9. The invention defined in claim 8, further including heating means for maintaining said source of ultraviolet light, said chamber, and said photosensors at predetermined temperatures.

10. The invention defined in claim 9, further including second filter means disposed between said phosphor means and said first and second photosensor means, said filter being adapted to selectively pass radiation at said first wavelength.

11. In a spectrophotometer including a chamber for receiving a gaseous sample to be analyzed, a source of radiation to be directed through said sample, and window means disposed in the walls of said chamber for allowing the passage of radiation therethrough, at least one of said window means comprising:

a frame extending generally transversely to the path of said radiation, said frame having an aperture therein to allow the passage of radiation;

a window comprising an elongate pane of radiation-transparent material;

said frame further comprising upper and lower guide means adapted to slidingly receive said pane whereby said pane may be displaced transversely with respect to said chamber so that an area of the pane in registry with said aperture may be succeeded by another area thereof; and

gasket means disposed between said frame and said pane for substantially sealing the interior of said chamber during displacement of said pane.

12. The invention defined in claim 11, wherein said frame is provided with a groove extending about said aperture for receiving a resilient element therein.

13. The invention defined in claim 12, wherein said gasket means comprise a first member disposed in said groove and a second, generally planar member disposed between said frame and said pane, said first gasket element serving to bias said second gasket element against said pane.

14. The invention defined in claim 13, wherein said second gasket element is formed of a fluorocarbon resin having a relatively low coefficient of friction.

15. The invention defined in claim 14, wherein said pane is formed of quartz.

16. A spectrophotometer for the analysis of a sample by identification of the electromagnetic absorption qualities thereof, said spectrophotometer comprising:

a lamp for providing ultraviolet radiation;

first heat responsive means in thermal communication with said lamp;

a first heating element associated with said lamp;

first control means coupled to said heat responsive means and said first heating element for maintaining said lamp at a predetermined temperature;

a chamber for receiving a sample to be analyzed, said chamber having window means disposed at the ends thereof to allow ultraviolet radiation to pass through said chamber and said sample;

second heat responsive means in thermal communication with said chamber;

a second control means coupled to said second heat responsive means in said second heating element for maintaining said chamber at a predetermined temperature;

a second heating element associated with said chamber;

photosensor means responsive to ultraviolet radiation received from said chamber;

an envelope surrounding said photosensor means;

a third heating element associated with said envelope; and

third control means coupled to said third heat responsive means and said third heating element for maintaining said envelope at a predetermined temperature.

17. The invention defined in claim 16, further comprising filter means disposed within said envelope for selectively transmitting ultraviolet radiation.

18. The invention defined in claim 17, further including a source of mercury vapor disposed within said envelope for providing sufficient mercury vapor to effect substantial attenuation of ultraviolet radiation having a wavelength at 254nm.

19. The invention defined in claim 18, wherein said lamp is of the metallic vapor type.

20. A spectrophotometer for determining the presence of a specified gaseous material in a sample comprising:

a source of electromagnetic radiation producing radiation at desired wavelengths for analyzing the sample, and radiation at at least one additional undesired wavelength;

photosensor means responsive to impingent radiation at a predetermined wavelength;

a sample chamber intermediate said radiation source and said photosensor means and having window means therein for allowing radiation to traverse a sample within said chamber;

an envelope enclosing said photosensor means; and

a source of metallic vapor disposed within said envelope for saturating the interior of said envelope with said vapor, whereby said vapor selectively absorbs the radiation at said undesired wavelength.

21. The invention defined in claim 20, wherein said metallic vapor is mercury.

22. The invention defined in claim 21, wherein said vapor source comprises a segment of metal, at least the surface of said segment being amalgamated with said mercury.

23. The invention defined in claim 22, further including heat responsive means in thermal communication with said envelope;

a heating element with said envelope; and

control means coupled to said heat responsive means and said heating element for maintaining said envelope at a predetermined temperature.

24. The invention defined in claim 23, further including filter means disposed in said envelope for selectively passing ultraviolet radiation at a predetermined wavelength.

25. The invention defined in claim 24, further including a phosphor element disposed within said envelope and responsive to impingent radiation at one wavelength for emitting radiation at another wavelength.