Selective, high speed detection of vapors with analysis of multiple GC-separated portions

• US 5,268,302 A
• Filed: 03/22/1993
• Issued: 12/07/1993
• Est. Priority Date: 05/29/1990
• Status: Expired due to Fees

• Current Assignee: Thermedics, Inc. (Thermo Fisher Scientific Incorporated)
• Original Assignee: Thermedics, Inc. (Thermo Fisher Scientific Incorporated)
• Inventors: Rounbehler, David P., Lieb, David P.
• Primary Examiner(s): Housel, James C.
• Assistant Examiner(s): Soderquist, Arlen
• Application Number:
  US08/035,541
• Time in Patent Office: 260 Days
• Field of Search: 73/23.2, 73/23.41, 73/23.42, 422/88, 422/89, 422/91, 436/106, 436/107, 436/111, 436/157, 436/158, 436/161, 436/174, 436/178, 436/96, 436/98, 436/816, 436/901
• US Class Current: 436/96
• CPC Class Codes: G01N 2030/121 cooling; cold traps
• CPC Class Codes: G01N 2030/128 Thermal desorption analysis
• CPC Class Codes: G01N 2030/3046 temperature control of column inlet
• CPC Class Codes: G01N 2030/8405 using pyrolysis
• CPC Class Codes: G01N 21/76 Chemiluminescence; Bioluminescence
• CPC Class Codes: G01N 30/12 by evaporation
• CPC Class Codes: G01N 30/16 Injection G01N30/24 takes precedence
• CPC Class Codes: G01N 30/461 with serial coupling of separation columns
• CPC Class Codes: G01N 30/84 Preparation of the fraction to be distributed
• CPC Class Codes: G01N 31/12 using combustion G01N25/20 takes precedence
• CPC Class Codes: Y10S 436/816 Alkaloids, amphetamines, and barbiturates
• CPC Class Codes: Y10S 436/901 Drugs of abuse, e.g. narcotics, amphetamine
• CPC Class Codes: Y10T 436/145555 Hetero-N
• CPC Class Codes: Y10T 436/147777 Plural nitrogen in the same ring [e.g., barbituates, creatinine, etc.]
• CPC Class Codes: Y10T 436/170769 N-Nitroso containing [e.g., nitrosamine, etc.]
• CPC Class Codes: Y10T 436/173845 Amine and quaternary ammonium
• CPC Class Codes: Y10T 436/255 including use of a solid sorbent, semipermeable membrane, or liquid extraction

Abstract

A method and apparatus for selective, high speed detection of vapors of specific gas-chromatographically-separable compounds. In the disclosed method separate analyses are performed on two portions of a gas sample formed by flash-heating trapped vapors to successively higher temperatures while flowing hydrogen carrier gas over coatings in/on which the vapors are held. Within a total time interval of about twenty seconds 1) two sample portions are formed, 2) each portion is rapidly separated in two series-connected, high speed, temperature-programmed gas chromatographs, and 3) specific compounds are identified by detection of NO gas formed during an oxidative pyrolysis of each separated portion. One application of the described method and apparatus is the rapid, selective, and sensitive detection of nitrogen-containing compounds such as the drugs methamphetamine, cocaine, and heroin.

Claims

1. A method of rapidly and selectively detecting first and second specific compounds in a gas sample, said compounds being separable by gas chromatography and said first compound having a volatility substantially higher than the volatility of said second compound, comprising:

trapping vapors of said specific compounds in a vapor concentrator;

and while flowing a carrier gas through the vapor concentrator, forming and analyzing a first portion of a gas sample containing said first specific compound during a first interval of time and thereafter forming and analyzing a second portion of a gas sample containing said second specific compound during a second interval of time;

said forming and analyzing of the first portion comprising the steps of (a) flash-heating the vapor concentrator to a first temperature effective to remove volatile materials including said first specific compound from said vapor concentrator with said flow of carrier gas without removing said second specific compound, (b) gas chromatographically (GC)-separating said first portion in a gas chromatograph connected to said vapor concentrator, and (c) detecting said first specific compound in said GC-separated first portion;

said forming and analyzing of the second portion comprising the steps of (a) flash-heating the vapor concentrator to a second temperature higher than said first temperature to form said second portion, (b) gas chromatographically (GC)-separating said second portion, and (c) detecting said second specific compound in said GC-separated second portion.

2. A method as in claim 1 wherein said GC-separating steps include directing each of said portions of the gas sample into a first gas chromatograph and directing the effluent of said first gas chromatograph into a second gas chromatograph

3. A method as in claim 2 wherein said GC-separating steps include heating each of said gas chromatographs in accordance with predetermined heating schedules.

4. A method as in claim 3 wherein each of said heating schedules includes a substantially linear increase of temperature during said second interval of time to accelerate removal of separated vapors from each of said gas chromatographs substantially without decomposition of vapors of said specific compounds contained in said second portion of the gas sample.

5. A method as in claim 4 wherein each of said heating schedules includes, prior to GC-separating said second portion, heating each of said gas chromatographs to preset temperatures.

6. A method as in claim 2 wherein the sum of said first and second intervals of time is less than about thirty seconds.

7. A method as in claim 6 wherein the sum of said first and second intervals of time is less than about twenty seconds.

8. A method as in claim 1 wherein said detection steps (c) for said first portion and said second portion each comprises heating said respective portion under conditions sufficient to produce a specific gas from said vapors of said specific compounds and thereafter detecting the specific gas produced during said heating step.

9. A method as in claim 8 wherein said specific compounds are organic nitrogen-containing compounds and said specific gas is nitric oxide.

10. A method as in claim 9 wherein said detecting steps include generating detection signals from which the presence and identity of said specific compounds may be automatically determined.

11. A method as in claim 10 wherein said first specific compound is methamphetamine and said second compound is cocaine or heroin, and said heating steps include passing said first and second portions in a flow of carrier gas through a pyrolyzer to which oxygen is also supplied.

12. A method as in claim 10 wherein said specific compounds include methamphetamine, cocaine, and heroin, said flash-heating step to form said first portion of the gas sample is operable to remove vapors of methamphetamine from said vapor concentrator, and said flash-heating step to form said second portion of the gas sample is operable to remove vapors of cocaine and heroin from said vapor concentrator.

13. A method as in claim 1 wherein said GS-separating steps include directing each of said portions of the gas sample into a gas chromatograph and heating said gas chromatograph according to a predetermined heating schedule, said heating schedule including the steps of:

(i) between the steps of GC-separating said first portion and flash-heating the vapor concentrator to said second temperature, heating said gas chromatograph to a third temperature, (ii) then maintaining said gas chromatograph at substantially said third temperature for a predetermined period of time, and (iii) then increasing the temperature of said gas chromatograph above said third temperature in a substantially linear, fashion.

14. A method of rapidly and selectively detecting one or more of the compounds methamphetamine, cocaine, and heroin comprising:

(a) directing air containing vapors of one or more of said compounds into a vapor concentrator so as to trap said vapors in said vapor concentrator;

(b) while flowing a carrier gas through the vapor concentrator and through a gas chromatograph connected to said vapor concentrator, flash-heating said vapor concentrator to a first temperature effective to remove vapors of methamphetamine, if present, from said vapor concentrator substantially without removing vapors of cocaine or heroin from said vapor concentrator;

(c) gas chromatographically (GC)-separating said vapors of methamphetamine, if present, from other materials removed from said vapor concentrator as a result of said flash-heating step;

(d) analyzing the effluent of said gas chromatograph to detect methamphetamine, if present, in said effluent;

(e) flash-heating said vapor concentrator to a second temperature to remove vapors of cocaine and heroin, if present, from said vapor concentrator;

(f) GC-separating said vapors of cocaine and heroin, if present, from each other and from other materials removed from said vapor concentrator in said second flash-heating step; and

(g) analyzing the effluent of said gas chromatograph to detect cocaine and heroin, if present, in said effluent.

15. A method as in claim 14 including, between steps (d) and (e), heating said gas chromatograph to a predetermined temperature.

16. A method as in claim 14 wherein steps (b) through (g) are performed in a total interval of time less than 30 seconds.