Measuring and testing – Gas analysis – Gas chromatography
Reexamination Certificate
2003-02-12
2004-03-23
Larkin, Daniel S. (Department: 2856)
Measuring and testing
Gas analysis
Gas chromatography
Reexamination Certificate
active
06708550
ABSTRACT:
FIELD OF THE INVENTION
The present invention relates to obtaining odors from odor emitting objects. More particularly, the present invention relates to an apparatus and process for acquiring odor(s) emitted from odor emitting objects.
BACKGROUND OF THE INVENTION
The emission of odor(s) from objects has given rise to attempts to copy or to acquire odors of interest. For example, aromas from botanical sources, such as living flowers, leaves or other parts of living trees or plants, are sought after in the perfumery arts.
A technique for capturing and analyzing the scent of flowers is described in Perfumes Art Science and Technology edited by P. M. Muller and D. Lamparsky and summarized by R Kaiser in The Scent of Orchids. The method disclosed involves placing a living flower, which is part of a living plant or tree, into an enclosed glass vessel. The glass vessel must be of suitable size and shape to permit the flower to be enclosed without damaging the plant or flower. Specially designed glassware is often required to accommodate particular types of flowers.
When such vessels are employed, the aroma chemicals surrounding a flower. i.e., the headspace, fill the vessel with a vapor phase. The headspace volatiles are drawn through an adsorption trap by means of a pump, over a period of thirty minutes to two hours. Adsorbents commonly employed in the trap are activated charcoal or special polymeric materials, such as TENAX® (2,6-diphenylene polymer) or Porapak Q® (ethylvinylbenzene-divinylbenzene copolymer). The trapped aroma chemicals are eluted from the trap with a solvent, and injected into a gas chromatograph and analyzed by mass spectrometry (GC/MS).
Mookherjee, et al., U.S. Pat. No. 5,369,978, which is incorporated herein by reference, discloses improvements in the above noted method, although essentially the same principles apply.
In addition, a technique using solid phase micro extraction (SPME) has been described by Mookherjee, et al., Perfumer and Flavorist 23, pp. 1-11 (1998). This technique requires placing a single SPME needle, which is a 2-3 mm solid glass fiber coated with a high boiling point liquid adsorbent, in close proximity to a flower for thirty minutes to sixty minutes. The aroma molecules are adsorbed onto the needle-like glass fiber and are then analyzed by GC/MS.
Great difficulty, however, has been encountered in attempting to collect scents from certain aroma sources using conventional aroma collecting devices. Special glassware for enclosure of flowers can be inconvenient to use, particularly when the flowers are not readily accessible. Also, they can be awkward to carry to and from remote locations. The rain forest, for example, has a cornucopia of fragrant scent-emitters. However, flowers are often at the end of high slender branches in the forest canopy and are difficult to reach.
Additionally, it is very difficult to attach the conventional collecting devices to the outer branches of trees. Often they do not support the weight of either a person or the equipment employed to collect a sample, particularly in view the length of time required, which can thwart efforts to obtain aromas from some sources.
With respect to the SPME technique, SPME needles are very delicate. The single needle employed to obtain the scent may break at any time in dense canopy. In fact, more often than not, such needles may break during capture in such an environment. Additionally, the time required to adsorb the aroma chemicals using the SPME needles can exceed thirty minutes, making it impractical for remote collections.
SUMMARY OF THE INVENTION
The present invention addresses these problems by providing an apparatus for obtaining odor(s) emitted from an odor emitting source. The apparatus of the present invention includes an adsorption unit having at least two openings, which may be one or more capillary tubes. The interior surfaces of the tubes comprise an adsorbent material for adsorbing odor chemicals. A suction device for drawing odor chemicals into the adsorption unit, is positioned for and connected to the tube assembly and a connector connects the tube assembly and the drawing device.
The invention also provides a process for obtaining or capturing odor chemicals. The process includes placing an adsorption unit, which comprises on its interior surface an adsorbent material for trapping aroma chemicals, in proximity to an aroma-emitter, and drawing aroma chemicals into an opening of the adsorption unit with a gas drawing means which is operably connected to the adsorption unit.
Further, the invention allows for the thermal desorption of adsorbed sample, cryogenic focusing, and resolution and identification odor components by GC/MS.
It is an object of the present invention to provide an apparatus for obtaining aroma chemicals from, in particular, difficult to reach aroma emitters.
It also is an object of the present invention to provide an apparatus which is readily portable and is durable for obtaining aroma chemicals from, in particular, a dense canopy.
It also is an object of the present invention to provide a process for obtaining aroma chemicals from, in particular, difficult to reach aroma emitters.
It is a further object of the invention to provide a process for obtaining aroma molecules which facilitates a short capture time.
DETAILED DESCRIPTION OF THE INVENTION
The apparatus for obtaining odors includes an adsorption unit, a suction device for drawing the odor chemicals into the adsorption unit, and a connector for connecting the adsorption unit and the suction device.
The adsorption unit has an opening for receiving odor chemicals and an opening displaced away from the first for drawing the odor chemicals through. The adsorption unit can be a tube or preferably, a plurality of tubes. A plurality of capillary tubes are the most preferred type of adsorption unit. As used herein, the term odor includes, but is not limited to aromas, as for example, fragrant scents.
The type and dimensions of the tubes of the adsorption unit may vary. For example, a single tube having a plurality of crossing wall portions contained within the tube are considered to be an equivalent alternative to the plurality of capillary tubes. Similarly, tubes having concentric tubes of decreasing diameter contained within a tube also are considered to be equivalent, because of the favorable surface area exposed to odor chemicals. Generally, the inside diameter of the capillary tube ranges from about 0.07 mm to about 1.0 mm, and more preferably from about 0.75 mm to about 0.9 mm.
The interior surface(s) of the adsorption unit are coated with an adsorbent material for adsorbing odor chemicals from the air to the stationary material. It is also contemplated that the adsorption unit integrally have interior surface(s) of an adsorbing material. As used herein, an adsorption unit which comprises an adsorbent material on its surface(s) encompasses both of these situations.
The adsorbent employed can vary depending on the odor chemicals sought to be obtained. Generally adsorbent materials, e.g., charcoal, may be used. Preferably, highly adsorbent materials of differing polarity are used to ensure that all aroma chemicals are obtained. The adsorbent material can be selected from the group consisting of a polar adsorbent, a non-polar adsorbent, an intermediate polarity adsorbent, and any combination thereof. A portion of the capillary tubes may be internally coated with a polar adsorbent, another portion with a non-polar adsorbent, and another portion with an intermediate polarity or neutral adsorbent. Examples of adsorbent materials that are useful in the practice of the invention are Carbowax 20-M as a polar phase adsorbent, methyl silicone as a non-polar adsorbent, and phenyl methyl silicone and polyacrylate as intermediate polarity adsorbents. These materials are coated on the inside of the capillary tube to a thickness of from about 0.1 .mu.m to about 1.25 .mu.m, preferably from about 0.1 to about 0.7 .mu.m, and most preferably from about 0.15 .mu.m to about 0.7 .mu.m.
In addition, while preferr
McGee Thomas
Purzycki Kenneth Leo
Givaudan Roure ( International ) SA
Larkin Daniel S.
Norris & McLaughlin & Marcus
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