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|H||||IIIHHHHHIIII USOO5227135A United States Patent (19) 11 Patent Number: 5,227,135 Godec Et Al |H||||IIIHHHHHIIII USOO5227135A United States Patent (19) 11 Patent Number: 5,227,135 Godec et al. 45 Date of Patent: Jul. 13, 1993 (54) APPARATUS FOR SIMULTANEOUS Primary Examiner-James C. Housel MEASUREMENT OF SULFUR AND Assistant Examiner-Lyle A. Alexander NON-SULFUR CONTAINING COMPOUNDS Attorney, Agent, or Firm-Beaton & Swanson 75 Inventors: Richard Godec, Erie; Neil Johansen, 57 ABSTRACT Boulder; Donald H. Stedman, The present invention describes the process and appara Englewood, all of Colo. tus for the simultaneous measurement of sulfur-contain 73) Assignee: Sievers Research, Inc., Boulder, ing compounds and organic compounds with or with Colo. out sulfur in their structures. A detector cell is de scribed that allows simultaneous measurement of com (21) Appl. No.: 759,105 pounds that can be ionized in a flame and thereby cause (22 Filed: Sep. 6, 1991 the electrical conductivity of the flame to increase, and the selective measurement of sulfur-containing com Related U.S. Application Data pounds which simultaneously form sulfur monoxide. Sulfur monoxide, upon mixing with ozone, emits light 63 Continuation of Ser. No. 444,636, Dec. 1, 1989, aban from 240 to 450 nm. The intensity of the light can be doned, which is a continuation-in-part of Ser. No. measured and related to the concentration of sulfur in 275,980, Nov. 25, 1988. the sample, while changes in electrical conductivity of 51 Int. Cl. ............................................. G01N 25/22 the flame measured by imposing a voltage across the 52 U.S. Cl. ...................................... 422/98; 436/123; cell quantifies the organic compounds irrespective of 436/156; 436/159; 422/52 whether or not they contain sulfur. Ratios of the signals 58) Field of Search .................... 422/98, 52; 436/123, of light intensity and electrical conductivity are differ 436/156, 159 ent for each compound and, when the detector is cou 56 References Cited pled with a chromatographic separation column and process, this ratio facilitates the identification of un U.S. PATENT DOCUMENTS known constituents in a mixture. 4,018,562 4/1977 Parks et al. ......................... 436/14 4,717,675 1/1988 Sievers et al. ....................... 436/159 7 Claims, 6 Drawing Sheets 33 4. U.S. Patent July 13, 1993 Sheet 1 of 6 5,227,135 3 39 38 ra-ao42 3O Ea 56 ess 54 62 - N - A-C) N NS Y36 6O O "E-19 e O 5O 2 48 U.S. Patent July 13, 1993 Sheet 2 of 6 5,227,135 F==-à-IL)?\!ZZZZZÁZIEZZZZZZZZZZZZ LIZZAZ F. G. 2 U.S. Patent July 13, 1993 Sheet 3 of 6 5,227,135 FIG.3B U.S. Patent July 13, 1993 Sheet 4 of 6 5,227,135 9 g U.S. Patent July 13, 1993 Sheet 5 of 6 5,227,135 o O s U.S. Patent July 13, 1993 Sheet 6 of 6 5,227,135 FIG.6A O 5 O 5 2O TIME F.G. 6B 5,227,135 1. 2 mation, a calibration curve is constructed by comparing APPARATUS FOR SMULTANEOUS the detector response (e.g. peak area) to the amount of MEASUREMENT OF SULFUR AND NON-SULFUR injected compound. For both "universal' and "selec CONTAINING COMPOUNDS tive' detectors, retention time as well as response of a given chemical compound relative to a "standard' com CROSS-REFERENCE TO RELATED pound provide information regarding the identity of the APPLICATION chemical. This is a continuation of copending application Ser. Once response factors for a wide range of chemical No. 07/444,636 filed on Dec. 1, 1989 now abandoned, compounds are known, it is possible to determine the which is a continuation-in-part of co-pending applica 0 concentrations of different compounds based solely on tion Ser. No. 07/275,980 filed Nov. 25, 1988, for Pro their retention times and detection response without the cess and Apparatus for the Detection of Sulfur. need for constructing calibration curves for each indi vidual component. For example, relative response fac FIELD OF THE INVENTION tors using a flame ionization detector are available for a This invention relates to a process and apparatus for 15 large number of hydrocarbons and other chemical con simultaneously detecting and quantifying trace amounts pounds found in petroleum and petrochemical samples, of sulfur and non-sulfur containing compounds. thus greatly simplifying quantifications of these com plex samples. Comparison of the relative response fac BACKGROUND OF THE INVENTION tors for compounds on two or more different detectors Various processes have been devised for the measure 20 provides even more information regarding the identity ment of the chemical components of a complex mixture of a particular chemical compound, since fundamen separated by gas, liquid or supercritical fluid carriers, tally different measurement techniques are employed. and for the measurement of the composition of gas, An important class of selective detectors are devices liquid and supercritical fluid streams or the gases for the selective measurement of sulfur-containing com evolved upon heating a solid matrix. Representative of 25 pounds. When present as impurities at low concentra such processes are detection by changes in physical tions, sulfur-containing compounds are detrimental to a properties of the streams, including changes in the re wide range of chemical processes. In consumer prod fractive index and thermal conductivity. Another de ucts, trace levels of sulfur-containing compounds can tection scheme is based on the measurement of electri impart objectionable taste and odor to products. In cal currents induced by the formation of ionic species 30 during combustion of a stream (flame ionization). Irra petrochemical applications, trace sulfur contaminants diation of a stream using electromagnetic radiation and can rapidly poison costly catalysts. For these reasons, radioactive sources or changes in the absorption of numerous processes and apparatus have been developed electromagnetic radiation by components of a stream for the measurement of low concentrations of sulfur are also employed. 35 containing compounds in sample streams. In general, these processes allow detectors that can Representative of such processes is that disclosed in be classified as either "general' or "universal' detec West German Patent No. 1,133,918 to H. Dragerwerk tors. These detectors produce a response for all of the and B. Drager for the flame photometric detector chemical constituents contained in a carrier strean (ex (FPD). Sulfur-containing compounds are oxidized in a cept for the eluent or carrier itself). Selective detectors, hydrogen/air flame to form diatomic sulfur S2 in an on the other hand, respond to specific chemical constit electronically excited state. Emission of light from this uents based on one or more elements within each com species can be measured using a photomultiplier tube or pound detected and/or unique physical or chemical similar light detection device equipped with an optical properties of the components. Selective detection is filter to eliminate the light emitted from other species in often required when the chemical components of inter 45 the flame. Through the use of different optical filters, est are present at low concentrations, together with the FPD can also be used for the measurement of phos much higher concentrations of other chemicals in the phorus-containing compounds based on the emission of steam. light from electronically excited phosphorus dioxide Detection systems can be further classified as being (PO2) formed in the hydrogen/air flame. Compounds non-destructive detectors, in which the chemical com 50 that do not contain sulfur or phosphorus cannot be position of the stream is not altered by the measurement measured using the FPD. However, compounds that do process, or destructive detectors, in which the sample is not contain sulfur or phosphorous can result in a de destroyed or chemically altered as a result of the mea crease or "quenching” of the detector response for surement process. Generally, to use a destructive detec sulfur-and phosphorus-containing compounds. S. O. tor, such as a flame ionization detector, in combination 55 Farwell and C. J. Barinaga, Sulfur-Selective Detection with a selective detector, it is necessary to split the with the FPD. Current Enigmas, Practical Usage, and sample stream prior to measurement of the chemical Future Directions, 24 Journal of Chromatographic Sci constituents by the respective detectors. Difficulties in ence, 483 (1986). controlling the amount of the sample stream which The reactive sulfur and phosphorus species generated flows into the different detectors using stream splitting 60 in the FPD flame are short-lived and therefore require has severely limited the utility of this technique. that the light measurement device be located in close In chromatographic analysis, the identity of a chemi proximity to the flame. This basic design requirement cal compound is determined based on the "retention has precluded the simultaneous operation of the FPD time' of the compound in a chromatographic system. with other "universal' detection systems, such as the The amount of the compound is determined based on 65 flame ionization detector. Of course, there is no such the detector response. Typically, several analyses are thing as a truly universal detector. For example, the performed using standard solutions of the test com flame ionization detector responds sensitively to nearly pound at different concentrations. Based on this infor all organic compounds (excluding formaldehyde and 5,227,135 3 4. formic acid) but not to inorganic compounds (e.g., O2, Kinetics of Elementary Reactions Involving the Oxides of N2, Ar, CO2, CO, SO2, H2S, COS, etc.). Sulphur III. The Chemiluminescent Reaction Between Another example of selective detection of sulfur-con Sulphur Monoxide and Ozone, C. J. Halstead, B. A. taining compounds is that disclosed in U.S. Pat. Nos. Thrush, 295 Proceedings of the Royal Society, London, 4,678,756 and 4,352,779 of R.
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