Device for qualifying products containing volatile substances

• US 6,743,397 B1
• Filed: 08/21/2000
• Issued: 06/01/2004
• Est. Priority Date: 01/29/1998
• Status: Expired due to Term

• Current Assignee: Thierry Zesiger
• Original Assignee: Thierry Zesiger
• Inventors: Zesiger, Thierry
• Primary Examiner(s): Warden, Jill
• Assistant Examiner(s): Gordon, Brian R
• Application Number:
  US09/600,781
• Time in Patent Office: 1,380 Days
• Field of Search: 422/63, 422/67, 422/68.1, 422/100, 422/80, 422/83, 700/266, 700/273, 700/274, 436/180, 436/174, 436/147
• US Class Current: 422/67
• CPC Class Codes: G01N 2001/2229 Headspace sampling, i.e. vapour over liquid
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 30/18 using a septum or microsyringe
• CPC Class Codes: G01N 30/24 Automatic injection systems
• CPC Class Codes: G01N 35/1079 with means for piercing stoppers or septums
• CPC Class Codes: H01J 49/0031 Step by step routines describing the use of the apparatus H01J49/0081 takes precedence
• CPC Class Codes: H01J 49/0413 for automated handling
• CPC Class Codes: H01J 49/049 with means for applying heat to desorb the sample; Evaporation
• CPC Class Codes: Y10T 436/25 including sample preparation
• CPC Class Codes: Y10T 436/2575 Volumetric liquid transfer

Abstract

The invention concerns a device for qualifying products containing volatile substances forming an analyte. The devices includes a measuring apparatus (2) provided with an enclosure (21a) and an electronic analyzing circuit (21b) for defining said analyte characteristics, a pumping system (30) for producing a vacuum inside said enclosure, a sampling chamber (16) wherein the analyte is introduced and a capillary (22) for connecting said chamber (16) to said enclosure (21a). The invention also has a chamber (16) that includes: a first inlet (18) for introducing the analyte and provided with a sealed plug (27, 60, 62); a second inlet (17) connected to a blow-down gas (11) and provided with a valve (23); and an outlet (19) for evacuating the gas contained in the chamber (16) and likewise provided with a valve (29), and it further has a transfer device (35, 32) for introducing the analyte into the chamber and a programmer (15) controlling the analyzing circuit (21b), the transfer device (35, 32) and the valves (23, 29), and arranged such that the purge of the chamber (16), the enclosure (21a) and the capillary (22) can be carried out automatically.

Claims

1. Device to qualify products containing volatile substances forming together an analyte, comprising a measuring apparatus (2) with a measuring enclosure (21a) and an analysis electronic circuit (21b) to define the characteristics of said analyte, a pumping system (30) to make a vacuum inside said enclosure (21a), a sampling chamber (16) into which said analyte is introduced and a capillary (22) to connect said chamber (16) to said enclosure (21a), said chamber (16) comprising:

a first inlet (18) to introduce said analyte and fitted with a gastight cap (27;

60, 62),

a second inlet (17) connected to a source of purge gas (11) and fitted with a valve (23), and,

an outlet (19) allowing the exhaust of the gas contained in said chamber (16) and also fitted with a valve (29),

the device comprising furthermore a transfer system (35, 32, 63, 64) to introduce the analyte into the sampling chamber, and a command programmer (15) for the analysis circuit (21b), for the transfer system (35, 32, 63, 64) and those valves (23, 29), allowing to achieve sequentially the purge of the chamber, of the capillary and of the enclosure, then the introduction of the analyte into the enclosure, and, finally, its analysis, the device being characterized by the fact that the programmer (15) is set up in such a way that;

in a first phase (51, 52), the valves of the second inlet (23) and the outlet (29) are open to let the purge gas go through, as long as a significant number of analyte particles previously analyzed may remain in the chamber (16), the enclosure (21a) or the capillary (22),

in a second phase (53), the inlet valve (23) is closed, preventing the penetration of the purge gas,

in a third phase (54), the transfer system (35, 32, 63, 64) is activated, to introduce the analyte to measure into the chamber (16),

in a fourth phase (55), the outlet valve (29) is closed,

in a fifth phase (56), at least, the analysis apparatus (2) defines the characteristics of the analyte passing from said chamber (16) into the enclosure (21a), and

in a sixth phase (57), the operation starts again at the first phase, as long as there are still other products to qualify.

2. Device according to claim 1, characterized by the fact that the measuring apparatus (2) comprises a mass spectrometer (21) connected to said chamber (16) with said capillary (22).

3. Device according to claim 2, characterized by the fact that the spectrometer (21) is chosen to be able to characterize ions whose molar mass is lower or equal to 300.

4. Device according to claim 1, characterized by the fact that the transfer system is realized with a syringe (35) fitted with a needle (37) and that the gastight cap is realized with a septum (27).

5. Device according to claim 1, characterized by the fact that the transfer system comprises an adsorbing material (63) on which said analyte is adsorbed.

6. Device according to claim 5, characterized by the fact that said gastight cap is realized with removable lid (60) fitted with a tightness seam (62) and a device (66) to open and close said lid (60), to allow the introduction and extraction of said adsorbing material (63).

7. Device according to claim 6, characterized by the fact that said adsorbing material (63) is active carbon.

8. Device according to claim 1, characterized by the fact that said analysis device (21) is switched on when the purge gas penetrates into said chamber (16) and that the programmer (15) is set up in such a way that the inlet valve (23) is closed when the analysis circuit (21b) informs said programmer (15) of the disposing of the analyte previously analyzed in the gas penetrating the enclosure (21a).

9. Device according to claim 1, characterized by the fact that the outlet valve (29) is realized with a valve that lets the gas go out the chamber (16) when the pressure in it is higher than the one present beyond said valve (29).

10. Device according to claim 1, characterized by the fact that it comprises furthermore a vacuum pump (24) connected to said chamber (16) and that the programmer (15) is set up in such a way that, after the inlet valve (23) has been closed and before the transfer system is activated, said pump (24) empties the chamber (16) of the purge gas.

11. Device to qualify products containing volatile substances forming together an analyte, comprising a measuring apparatus (2) with a measuring enclosure (21a) and an analysis electronic circuit (21b) to define the characteristics of said analyte, a pumping system (30) to make a vacuum inside said enclosure (21a), a sampling chamber (16) into which said analyte is introduced and a capillary (22) to connect said chamber (16) to said enclosure (21a), said chamber (16) comprising:

a first inlet (18) to introduce said analyte and fitted with a gastight cap (27;

60, 62),

a second inlet (17) connected to a source of purge gas (11) and fitted with a valve (23), and,

an outlet (19) allowing the exhaust of the gas contained in said chamber (16) and also fitted with a valve (29),

the device comprising furthermore a transfer system (35, 32, 63, 64) to introduce the analyte into the sampling chamber, and a command programmer (15) for the analysis circuit (21b), for the transfer system (35, 32, 63, 64) and those valves (23, 29), allowing to achieve sequentially the purge of the chamber, the capillary and the enclosure, then the introduction of the analyte into the enclosure, and, finally, its analysis, the device being characterized by the fact that the transfer system comprises an adsorbing material (63) on which the analyte is adsorbed.

12. Device according to claim 11, characterized by the fact that the programmer (15) is set up in such a way that:

in a first phase (51, 52), the valves of the second inlet (23) and the outlet (29) are open to let the purge gas go through, as long as a significant number of analyte particles previously analyzed may remain in the chamber (16), the enclosure (21a) or the capillary (22),

in a second phase (53), the inlet (23) and outlet (29) valves are closed quite simultaneously, preventing particularly the penetration of purge gas,

in a third phase (54), the transfer system (35, 32, 63, 64) is activated, to introduce the analyte to measure into the chamber (16),

in a fourth phase, at least, the analysis apparatus (2) defines characteristics of the analyte passing from said chamber (16) into said enclosure (21a), and

in a fifth phase (57), the operation starts again at the first phase, as long as there are still other products to qualify.