CA1063865A - Dearomatization of coffee oil - Google Patents
Dearomatization of coffee oilInfo
- Publication number
- CA1063865A CA1063865A CA243,087A CA243087A CA1063865A CA 1063865 A CA1063865 A CA 1063865A CA 243087 A CA243087 A CA 243087A CA 1063865 A CA1063865 A CA 1063865A
- Authority
- CA
- Canada
- Prior art keywords
- sleeve
- chamber
- coffee
- aroma
- constituents
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F5/00—Coffee; Coffee substitutes; Preparations thereof
- A23F5/46—Coffee flavour; Coffee oil; Flavouring of coffee or coffee extract
- A23F5/48—Isolation or recuperation of coffee flavour or coffee oil
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F5/00—Coffee; Coffee substitutes; Preparations thereof
- A23F5/46—Coffee flavour; Coffee oil; Flavouring of coffee or coffee extract
- A23F5/48—Isolation or recuperation of coffee flavour or coffee oil
- A23F5/50—Isolation or recuperation of coffee flavour or coffee oil from coffee extract
- A23F5/505—Isolation or recuperation of coffee flavour or coffee oil from coffee extract by distillation, e.g. stripping the extract; Recovering volatile gases, e.g. during concentration
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Tea And Coffee (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Seasonings (AREA)
- Fats And Perfumes (AREA)
Abstract
ABSTRACT
This invention relates to an improved process for the separation and isolation of coffee aroma constituents from roasted coffee, combining the aroma constituents with an edible substance and subsequently incorporating the aromatized substance in a food product.
The process involves improving the condensation of vapors generated from the distillation of coffee oil by conden-sing the distilled aroma constituents onto a sleeve cooled by and snugly surrounding a container filled with coolant. The sleeve is removed and the aroma constituents condensed thereon are then preferably combined with an edible substance by manipu-lating the condensed constituents quickly and efficiently thus minimizing aroma loss and degradation caused by undesirable prolonged contact with air.
This invention relates to an improved process for the separation and isolation of coffee aroma constituents from roasted coffee, combining the aroma constituents with an edible substance and subsequently incorporating the aromatized substance in a food product.
The process involves improving the condensation of vapors generated from the distillation of coffee oil by conden-sing the distilled aroma constituents onto a sleeve cooled by and snugly surrounding a container filled with coolant. The sleeve is removed and the aroma constituents condensed thereon are then preferably combined with an edible substance by manipu-lating the condensed constituents quickly and efficiently thus minimizing aroma loss and degradation caused by undesirable prolonged contact with air.
Description
~063865 This invention is predicated on processing improvements in the separation, recovery and concentration of roasted coffee aroma constituents and the subsequent incorporation of the aroma constituents into food products and generally entails an improve-ment over the process disclosed by Feldman et al. in Canadian Patent Number 603,954. Through the use of the improvements described herein the Feldman et al. process can be more effi-ciently practiced.
Some problems that hampered extensive commercial use of the Feldman et al. process were that (1) the condensate could not be removed from the condenser without undesirable prolonged contact with air resulting in the loss and degradation of valuable aroma constituents, (2) the condenser had to be emptied of the cryogenic coolant and warmed every time the condensate had to be removed thus putting a condenser out of action for a prolonged period of time, wasting valuable coolant material, and due to the condenser's large mass it remained cold for extended periods of time thus hampering attempts to remove the condensate, and (3) the physical state of the condensate in the condenser could not ; 20 be effectively controlled thus making handling difficult as effi-cient operation makes desirable the formation of solid condensate ; on the collection surface.
In view of the above-mentioned difficulties encountered with the Feldman et al. process and in order to effect an efficient commercial process for the aromatization of food products, particularly instant coffee, this invention is predicated on processing improvements in the separation, recovery and concen-tration of roasted coffee aroma constituents and the subsequent incorporation of the concentrated aroma constituents in a food product, particularly instant coffee.
The invention entails subjecting coffee oil in a dis- -tillation chamber to distillation at sub-atmospheric pressures .. , .-; .. . .. . . .
.
. .
' ' ', , ~
.. . . .. .
~63~36S
and mild temperatures to separate aroma constituents therefrom and condensing said aromatic constituents in a condensing chamber on the outer surface of a heat-conductive sleeve removably and snugly surrounding a heat-conductive container filled with a coolant, then removing the sleeve with the condensed constituents thereon. --The condensed aromatic constituents in the condensing chamber are preferably collected as a solid by maintaining a sufficient pressure in the condensing chamber through the intro-duction of an inert gas.
The sleeve with the condensed aromatic constituentsthereon is then preferably immersed into an edible substance con-tained in a folding chamber in order to combine the condensed aromatic constituents with the edible substance.
- In order that the invention may be more clearly under-stood, reference will be made to the accompanying drawings in which Figure 1 is a cross sectional view of the condenser of this invention, and Figure 2 is a diagramatic sketch of apparatus suitable for carrying out the invention.
- 20 Other features and advantages of the invention wil7 be apparent from the following description taken in connection with the accompanying drawings.
Coffee aroma constituents are separated by distilling coffee oil at sub-atmospheric pressures and under mild tempera~
;, tures and then condensing the separated aroma constituents. The coffee aroma constituents are separated from the oil in such a manner that various desirable aroma constituent fractions can be isolated and subsequently incorporated in a final product in the proportions desired. Low boiling aroma constituents having a fragrance like that of roasted coffee grinder gas and lacking body form the bulk of the initial distilate. Medium boiling aroma constituents and some higher boiling aroma constituents . . .
~ - 2 -.. . . ..
~0~3~365 having a burnt or smo~y roasted character are also separated from the oil. As a result, the various aroma fractions can be propor-tioned by controlling the temperature, pressure and period of distillation to provide the desired levels of low, medium, and high boiling aroma constituents to obtain a desired coffee aroma.
Generally, the coffee oil is obtained by expressing roasted coffee at a temperature below 150C, and preferably at about 130C. This is a sufficiently elevated temperature com-patible with satisfactory yields of coffee oil and aroma therein.
The pressures exerted on the coffee to provide a high yield of coffee oil and quality aromas cannot be stated precisely or directly. However, coffee oil is expelled in an acceptable condi-tion using apparatus estimated at exerting 5,000 to 20,000 p.s.i.
(approximately 350 to 1400 kg/sq cm) on the coffee. The pressures for adequate oil yield and aroma quality can be determined in terms of the temperatures of the expeller cake or meal and the ; expressed oil. The expeller cake (expressed roasted coffee or coffee meal) should have a temperature below 150C and preferably, a temperature of at least about 75C. The expressed oil should have a temperature ranging from about 25C to 120C when measured .
immediately after expression. Adherence to such expeller cake and oil temperatures assures that the necessary pressures have been applied to the coffee to recover oil therefrom without undesirable modification of the aroma constituents therein.
The distillation of the aroma constituents from the expressed coffee oil is preferably carried out within a tempera~
ture range of 15C to 100C with the preferred aroma constituents being distilled at a temperature below about 60C. The oil is maintained under a reduced pressure in the distillation chamber of generally less than 50 mm and preferably less than 10 mm.
The most preferred distillation conditions involves subjecting coffee oil at ambient temperatures (i.e., 20C to 35C), to a pressure ranging from 10 mm to about 60 microns.
' .:
~63865 The oil is preferably introduced into the distillation chamber by a method that maximizes the liquid/gas interfacial area. This allows a maximum of aroma constituents to be distilled in a minimum of time. This method is preferably carried out by atomization o~ the oil into fine droplets. This can be accom-plished by using an impingement type atomizing nozzle that operates by having the oil stream impinge, at high velocity, upon a pin held directly at the exit of the nozzle orifice. Alternatively the oil can be pxovided in a thin film for distillation; prefer-ably in a rapidly moving film having a thickness ranging from 10 to 100 microns. The process of desorbtion can also be employed to increase the efficiency and degree of separation of the aroma constituents from the oil. Desorbtion involves sweeping the coffee oil with an inert gas such as, for example, nitrogen, carbon dioxide, helium, etc. in the distillation chamber and thereby collecting the more fugitive aromatic constituents.
Referring to Figure 1 of the drawing the aroma consti-tuents are then carried off as a gas stream and are condensed onto the outer surface of a heat conductive sleeve 1 removably and snugly surrounaing a heat-conductive container 2 which has a coolant 3 therein. The heat-conductive sleeve is enclosed by a condensing chamber 4 which has ports 5 and 6 to allow the passage of the aromatic constituents within the space 7 between condensing ~-`
chamber 4 and the sleeve 1. The condensing chamber 4 also has a removable cover 8 which seals an opening through which the sleeve is removed from the container.
The sleeve is preferably a thin gauge metal and can be kept in place snugly surrounding the container by a number of - means. This can include the sleeve being screwed, latched, hooked, etc. in place, or being held in place by friction between the container and the sleeve or by the force of gravity. The container is preferably of metal and is in contact with the sleeve so as to maximize heat conduction between the container and the ~ ' ~3D638~5 sleeve. The container is also preferably cylindrical however this is not meant to exclude other desired shapes such as a truncated cone or a rectangular box, with the shape of the sleeve corres-ponding to the shape of the container.
The coolant within the heat-conductive container can have a temperature ranging from about 0C to about -26~C depend-ing upon what aroma constituents one wants to collect. It is possible though to condense all the aroma constituents with a coolant on the order of -196C such as liquid nitrogen. Alter-natively one may want to set up a fractional condensation system ~ utilizing several stages instead of one by using several of the ; above condensers in series each operating at a different coolant temperature. For example, a first stage can be cooled to a temperature on the order of 0C to -15C using a brine solution, while a second stage can be cooled to a temperature on the order of -80C using solid carbon dioxide as a coolant, while a third stage can be cooled on the order of -196C using liquid nitrogen.
As the gas stream of volatile aroma constituents enters the condensing chamber 4 through an inlet port 5 it comes into contact with the cooled surface of the sleeve 1 and the aroma constituents which condense form a frost thereon. The constituents of the gas stream which are not condensed exit out of the condensing chamber through an outlet port 6. After suf-ficient frost has been collected on the sleeve the condensing : :.
chamber preferably is isolated, vented tpreferably with an inert gas) the cover 8 opened and the sleeve removed, preferably by use of handle 9 on the sleeve. Preferably the apparatus can be so arranged that while one condensing chamber is being isolated another is activated thus providing for a continuously operating condenser system. This can be done by connecting two condensing chambers in parallel, with the required valving, between the distillation chamber and the vacuum source (as shown in Figure 2).
Through use of this sleeve no significant amount of 1~i3865 frosk condenses on the container ancl therefore it is not necessary to remove the coolant from the container to recover the frost.
Previously, due to the large mass of the container which collected the frost on its surface, after the coolant was removed the con-tainer retained the cold longer and when it was contacted with oil to incorporate the frost into the oil, the oil would freeze onto the container's outer surface and would have to be scraped off.
As well as being time consuming, this led to the use of a compli-cated mechanical scraper and unwanted exposure of the coffee aroma constituents to air. Now, due to the sleeve's low mass and high heat transfer coefficient the frost can be easily and quickly recovered when contacted with oil since there is little if any freezing of the oil on the sleeve's surface, and exposure of the condensed aroma constituents to air can be minimized due to the ease with which the sleeve may be handled. The condenser can also be quickly reactivated after inserting a clean sleeve onto the container.
The condensed aroma constituents on the sleeve can be collected by venting the condensing chamber preferably with an inert gas, then removing the cover of the condensing chamber and taking out the sleeve with the aroma constituents condensed thereon in the form of frost and contacting the constituents with an edible non-volatile fluid substance, e.g., an oil. The edible substance serves as an aroma carrier enabling the aroma consti-tuents to be conveniently added to a food product such as instant coffee. The coffee aroma is preferably folded into the edible -substance at a sufficiently high level to enable the concentrated -aroma and aroma carrier to be incorporated into the food product without imparting a "wet" appearance or causing poor flowability.
The preferred aroma carrier is coffee oil (expressed, solvent extracted or otherwise obtained) which, due to the presence of - natural emulsifiers therein, enables large quantities of aroma . .
~ - 6 -. . : . .; ~
10~865 frost to be combined with or incorporated into the oil. The aroma is preferably added to the coffee oil to obtain a 2- to 10-fold coffee aroma level ~aroma from 1 to 9 parts coffee oil combined with 1 part coffee oil), the level also depending upon how much aroma is to be added later to the food product such as instant coffee. Preferably at least a 5-fold level of aromatized oil is added to obtain a desired aroma level in a product such as instant coffee without adversely affecting its appearance and flowability.
This folding ~concentrating) step is preferably accom~
; plished by immersing the sleeve with the condensed aroma consti-tuents thereon into an appropriate amount of coffee oil contained -in a folding chamber (a chamber capable of being sealed to be fluid and air tight), sealing the chamber from the air, flushing the chamber with an inert gas and then allowing the aroma consti-tuents to combine with the coffee oil. The appropriate amount of ; expressed coffee oil is determined by the final concentration of aroma desired (i.e., 2- to 10-fold). So that the sleeve can be immersed in the coffee oil it may be desirable, depending upon the appropriate amount of coffee oil, that the folding chamber have a dead space which the sleeve will fit around so as to allow a minimum volume of oil to be in contact with a substantial portion of the condensed aroma constituents on the sleeve's outer surface. This can be carried out by having a vessel in the folding chamber which the sleeve fits around. This vessel occu-pies sufficient space in the folding chamber so that the appro-priate amount of coffee oil in the folding chamber will contact a substantial portion of the condensed aroma constituents on the outer surface of the sleeve.
After sufficient time has elapsed for the aroma consti-tuents to combine with the oil the aromatized oil is transferred from the folding chamber, the seal broken, the sleeve removed and the chamber resealed and recharged with fresh oil and flushed . .
~ 7 . . .. . ................... ; : .:: .................. : .
,, .. , ,, , ,:: : ' :' : ' ~063865 with an inert gas in readiness for another sleeve. By thus having one folding chamber ready per sleeve, the exposure of the aroma constituents to air is minimized to the transfer time of the sleeve from the condensing chamber to the folding chamber.
Also the use of this folding chamber provides a simple method for combining the aroma constituents with oil while minimizing con-- tact of the oil and aroma constituents with air.
After the aroma constituents have been combined with the oil the aromatized oil is then preferably blended in another chamber with other aromatized oils in desired proportions thus ~ obtaining a homogenous aromatized oil and minimizing batch to ; batch variations.
Generally the most preferable aroma constituents from the viewpoint of quality are those recovered as a frost. Further, in order to be able to remove the condensed aroma constituents from the condensing chamber it is also preferred that the aroma con-stituents be in the solid state, i.e , recovered as a frost. The sleeve permits the collection of the condensed aroma constituents as a frost, so that when one removes the sleeve one also removes all the aroma constituents frosted onto its outer surface. By appropriate adjustment of the temperatures and pressure the liquification of the recovered aroma constituents can be avoided.
The coolant temperature can be reduced or the condenser pressure increased. With respect to coffee aroma constituents if the pressure is raised to above approximately 60 microns, (preferably 140 microns,) and the coolant temperature kept at -196C the condensate is then collected as a frost.
This is preferably accomplished by introducing an inert gas (e.g., nitrogen, carbon dioxide, etc.) at a flow rate effec-tive to control the pressure within the space between the sleeve and the condensing chamber at a level sufficient to keep the condensed aromatic constituents solid. Preferably the inert gas -, .~ . .~
~63865 is introduced in the distillation chamber, so as the pressure of the inert gas is controlling the physical state of the condensate in the condensing chamber as a solid, the inert gas is also aiding in the separation of the volatile aromas from the coffee oil in the distillation chamber by the process of desorbtion.
- The process of the instant invention can also be ; employed in-the separation of aroma constituents from other types ;~
of coffee oils such as solvent-extracted coffee oil.
In order that the present invention may be more clearly -understood reference will now be made to the following exampleand to Figure 2.
EXAMPLE
; The distillation and condensing chambers were totally enclosed and flushed with carbon dioxide, then depressurized to ;
approximately 20 microns, while the eirst feed tank was charged with 140 pounds of expressed coffee oil.
The expressed coffee oil was obtained by subjecting ` roasted whole coffee beans to pressures of at least 5,000 p.s.i.
in an expeller and wherein said expressed coffee oil recovered from the expre~sing operation had a temperature ranging from 25C
to 120C and the coffee meal residue had a temperature ranging from 75C to 150C, the environment of the expressing operation being cooled to a temperature below about 150C.
The oil was then pumped into the distillation chamber 11 at ambient temperature from the first feed tank 12 at pressures up to approximately 1000 p.s.i.g. through an impingement type atomizing nozzle 13 which operated by having a liquid stream at a high velocity strike a pin held at the exit of the nozzle orifice resulting in a wide angle, hollow cone, fine spray under the vacuum environment of the distillation chamber 11. Meanwhile nitrogen 14 was bled into the distillation chamber in order to maintain a pressure of 140 to 160 microns. This was done ~o _ 9 _ -. ' ' ' ', ',, ~ . " . ~
. .
' ~63~16S
maintain the condensed aroma constituents in the condenser in the solid state and to aid in separation of the aroma constituents from the expressed coffee oil through the process of desorbtion.
The 140-pound oil charge was sprayed into the distillation chamber 11 over a period of approximately 60 minutes. As the partially spent oil collected in the bottom of the distillation chamber, it was transferred by pumping to a second feed tank 19 wherein it was heated to a temperature of approximately 66C.
Isolating a second condensing chamber 20, as the gas stream passed through a first condensing chamber 15 the aroma constituents were condensed onto a thin gauge aluminum sleeve 16 cooled by and snugly surrounding a stainless steel container 17 filled with liquid nitrogen 18.
After the first charge had passed through the distil-lation chamber 11 once, this first condensing chamber 15 was isolated and a second condensing chamber 20 connected in parallel with the first was put into operation by appropriate valve 21 adjustment. The first condensing chamber 15 was then vented to atmospheric pressure using nitrogen gas and opened by unfastening the hinged cover 22 of the condensing chamber 15. The sleeve 16 was removed manually and immediately placed into a folding chamber 23 with 17.5 pounds of fresh expressed coffee oil therein.
The folding chamber was closed and then flushed with carbon dioxide to remove any air.
A clean sleeve was inserted onto the container 17 in the first condensing chamber 15, the chamber was then closed by refastening the hinged cover 22 and depressurized. The first condensing chamber 15 was then ready to be put back into opera-tion as soon as the second condensing chamber 20 was isolated.
The preheated partially stripped oil from the second feed tank 19 was then passed through the distillation chamber 11 in a manner identical to the oil from the first feed tank 12, ~063865 except that on collection in the bottom of the distillation chamber the totally spent (stripped) oil was transferred to a collection tank rather than a feed tank. From the collection -~
tank this dearomatized oil was either routed to be used as fuel or used in some other desired fashion.
At the end of the second stripping pass, the second ~ condensing chamber 20 was vented to atmospheric pressure using ; nitrogen gas. The sleeve 24 was then removed and immediately placed into a second folding chamber 25 with 17.5 pounds of freshly expressed coffee oil therein. The folding chamber 25 was closed and flushed with carbon dioxide to remove any air.
The contents of the first folding chamber 23, which had been allowed to sit for approximately 60 minutes, was then trans- ~
ferred to a 35-pound capacity oil pot 26 by applying pressure ~ -using carbon dioxide gas to the folding chamber's headspace. The first folding chamber 23 was then opened and the sleeve 17 removed and cleaned. The folding chamber was then closed and `charged with 17.5 pounds of fresh oil in readiness for another aroma laden sleeve.
After an additional 60 minutes, the remaining 17.5 pounds of aroma laden oil from the second folding chamber 25 was transferred to the identical 35-pound pot 26, wherein it was blended with the oil from the first folding chamber 23 to produce a homogeneous 35-pound batch of 5-fold oil. As before, the sleeve 24 was removed and cleaned, and a new 17.5-pound charge of fresh coffee oil was placed in the second folding chamber 25.
- Using a new charge of 140 pounds of fresh coffee oil, the cycle was then repeated to manufacture another batch of 5-fold oil.
The 5-fold oil was then plated on an instant coffee at a level of less than one percent by weight resultiny in a product - which has an unusually long storage life during which the original balance, strength and fragrance of the aromas are substantially retained without development of undesirable stale notes.
-- 11 -- ~
Some problems that hampered extensive commercial use of the Feldman et al. process were that (1) the condensate could not be removed from the condenser without undesirable prolonged contact with air resulting in the loss and degradation of valuable aroma constituents, (2) the condenser had to be emptied of the cryogenic coolant and warmed every time the condensate had to be removed thus putting a condenser out of action for a prolonged period of time, wasting valuable coolant material, and due to the condenser's large mass it remained cold for extended periods of time thus hampering attempts to remove the condensate, and (3) the physical state of the condensate in the condenser could not ; 20 be effectively controlled thus making handling difficult as effi-cient operation makes desirable the formation of solid condensate ; on the collection surface.
In view of the above-mentioned difficulties encountered with the Feldman et al. process and in order to effect an efficient commercial process for the aromatization of food products, particularly instant coffee, this invention is predicated on processing improvements in the separation, recovery and concen-tration of roasted coffee aroma constituents and the subsequent incorporation of the concentrated aroma constituents in a food product, particularly instant coffee.
The invention entails subjecting coffee oil in a dis- -tillation chamber to distillation at sub-atmospheric pressures .. , .-; .. . .. . . .
.
. .
' ' ', , ~
.. . . .. .
~63~36S
and mild temperatures to separate aroma constituents therefrom and condensing said aromatic constituents in a condensing chamber on the outer surface of a heat-conductive sleeve removably and snugly surrounding a heat-conductive container filled with a coolant, then removing the sleeve with the condensed constituents thereon. --The condensed aromatic constituents in the condensing chamber are preferably collected as a solid by maintaining a sufficient pressure in the condensing chamber through the intro-duction of an inert gas.
The sleeve with the condensed aromatic constituentsthereon is then preferably immersed into an edible substance con-tained in a folding chamber in order to combine the condensed aromatic constituents with the edible substance.
- In order that the invention may be more clearly under-stood, reference will be made to the accompanying drawings in which Figure 1 is a cross sectional view of the condenser of this invention, and Figure 2 is a diagramatic sketch of apparatus suitable for carrying out the invention.
- 20 Other features and advantages of the invention wil7 be apparent from the following description taken in connection with the accompanying drawings.
Coffee aroma constituents are separated by distilling coffee oil at sub-atmospheric pressures and under mild tempera~
;, tures and then condensing the separated aroma constituents. The coffee aroma constituents are separated from the oil in such a manner that various desirable aroma constituent fractions can be isolated and subsequently incorporated in a final product in the proportions desired. Low boiling aroma constituents having a fragrance like that of roasted coffee grinder gas and lacking body form the bulk of the initial distilate. Medium boiling aroma constituents and some higher boiling aroma constituents . . .
~ - 2 -.. . . ..
~0~3~365 having a burnt or smo~y roasted character are also separated from the oil. As a result, the various aroma fractions can be propor-tioned by controlling the temperature, pressure and period of distillation to provide the desired levels of low, medium, and high boiling aroma constituents to obtain a desired coffee aroma.
Generally, the coffee oil is obtained by expressing roasted coffee at a temperature below 150C, and preferably at about 130C. This is a sufficiently elevated temperature com-patible with satisfactory yields of coffee oil and aroma therein.
The pressures exerted on the coffee to provide a high yield of coffee oil and quality aromas cannot be stated precisely or directly. However, coffee oil is expelled in an acceptable condi-tion using apparatus estimated at exerting 5,000 to 20,000 p.s.i.
(approximately 350 to 1400 kg/sq cm) on the coffee. The pressures for adequate oil yield and aroma quality can be determined in terms of the temperatures of the expeller cake or meal and the ; expressed oil. The expeller cake (expressed roasted coffee or coffee meal) should have a temperature below 150C and preferably, a temperature of at least about 75C. The expressed oil should have a temperature ranging from about 25C to 120C when measured .
immediately after expression. Adherence to such expeller cake and oil temperatures assures that the necessary pressures have been applied to the coffee to recover oil therefrom without undesirable modification of the aroma constituents therein.
The distillation of the aroma constituents from the expressed coffee oil is preferably carried out within a tempera~
ture range of 15C to 100C with the preferred aroma constituents being distilled at a temperature below about 60C. The oil is maintained under a reduced pressure in the distillation chamber of generally less than 50 mm and preferably less than 10 mm.
The most preferred distillation conditions involves subjecting coffee oil at ambient temperatures (i.e., 20C to 35C), to a pressure ranging from 10 mm to about 60 microns.
' .:
~63865 The oil is preferably introduced into the distillation chamber by a method that maximizes the liquid/gas interfacial area. This allows a maximum of aroma constituents to be distilled in a minimum of time. This method is preferably carried out by atomization o~ the oil into fine droplets. This can be accom-plished by using an impingement type atomizing nozzle that operates by having the oil stream impinge, at high velocity, upon a pin held directly at the exit of the nozzle orifice. Alternatively the oil can be pxovided in a thin film for distillation; prefer-ably in a rapidly moving film having a thickness ranging from 10 to 100 microns. The process of desorbtion can also be employed to increase the efficiency and degree of separation of the aroma constituents from the oil. Desorbtion involves sweeping the coffee oil with an inert gas such as, for example, nitrogen, carbon dioxide, helium, etc. in the distillation chamber and thereby collecting the more fugitive aromatic constituents.
Referring to Figure 1 of the drawing the aroma consti-tuents are then carried off as a gas stream and are condensed onto the outer surface of a heat conductive sleeve 1 removably and snugly surrounaing a heat-conductive container 2 which has a coolant 3 therein. The heat-conductive sleeve is enclosed by a condensing chamber 4 which has ports 5 and 6 to allow the passage of the aromatic constituents within the space 7 between condensing ~-`
chamber 4 and the sleeve 1. The condensing chamber 4 also has a removable cover 8 which seals an opening through which the sleeve is removed from the container.
The sleeve is preferably a thin gauge metal and can be kept in place snugly surrounding the container by a number of - means. This can include the sleeve being screwed, latched, hooked, etc. in place, or being held in place by friction between the container and the sleeve or by the force of gravity. The container is preferably of metal and is in contact with the sleeve so as to maximize heat conduction between the container and the ~ ' ~3D638~5 sleeve. The container is also preferably cylindrical however this is not meant to exclude other desired shapes such as a truncated cone or a rectangular box, with the shape of the sleeve corres-ponding to the shape of the container.
The coolant within the heat-conductive container can have a temperature ranging from about 0C to about -26~C depend-ing upon what aroma constituents one wants to collect. It is possible though to condense all the aroma constituents with a coolant on the order of -196C such as liquid nitrogen. Alter-natively one may want to set up a fractional condensation system ~ utilizing several stages instead of one by using several of the ; above condensers in series each operating at a different coolant temperature. For example, a first stage can be cooled to a temperature on the order of 0C to -15C using a brine solution, while a second stage can be cooled to a temperature on the order of -80C using solid carbon dioxide as a coolant, while a third stage can be cooled on the order of -196C using liquid nitrogen.
As the gas stream of volatile aroma constituents enters the condensing chamber 4 through an inlet port 5 it comes into contact with the cooled surface of the sleeve 1 and the aroma constituents which condense form a frost thereon. The constituents of the gas stream which are not condensed exit out of the condensing chamber through an outlet port 6. After suf-ficient frost has been collected on the sleeve the condensing : :.
chamber preferably is isolated, vented tpreferably with an inert gas) the cover 8 opened and the sleeve removed, preferably by use of handle 9 on the sleeve. Preferably the apparatus can be so arranged that while one condensing chamber is being isolated another is activated thus providing for a continuously operating condenser system. This can be done by connecting two condensing chambers in parallel, with the required valving, between the distillation chamber and the vacuum source (as shown in Figure 2).
Through use of this sleeve no significant amount of 1~i3865 frosk condenses on the container ancl therefore it is not necessary to remove the coolant from the container to recover the frost.
Previously, due to the large mass of the container which collected the frost on its surface, after the coolant was removed the con-tainer retained the cold longer and when it was contacted with oil to incorporate the frost into the oil, the oil would freeze onto the container's outer surface and would have to be scraped off.
As well as being time consuming, this led to the use of a compli-cated mechanical scraper and unwanted exposure of the coffee aroma constituents to air. Now, due to the sleeve's low mass and high heat transfer coefficient the frost can be easily and quickly recovered when contacted with oil since there is little if any freezing of the oil on the sleeve's surface, and exposure of the condensed aroma constituents to air can be minimized due to the ease with which the sleeve may be handled. The condenser can also be quickly reactivated after inserting a clean sleeve onto the container.
The condensed aroma constituents on the sleeve can be collected by venting the condensing chamber preferably with an inert gas, then removing the cover of the condensing chamber and taking out the sleeve with the aroma constituents condensed thereon in the form of frost and contacting the constituents with an edible non-volatile fluid substance, e.g., an oil. The edible substance serves as an aroma carrier enabling the aroma consti-tuents to be conveniently added to a food product such as instant coffee. The coffee aroma is preferably folded into the edible -substance at a sufficiently high level to enable the concentrated -aroma and aroma carrier to be incorporated into the food product without imparting a "wet" appearance or causing poor flowability.
The preferred aroma carrier is coffee oil (expressed, solvent extracted or otherwise obtained) which, due to the presence of - natural emulsifiers therein, enables large quantities of aroma . .
~ - 6 -. . : . .; ~
10~865 frost to be combined with or incorporated into the oil. The aroma is preferably added to the coffee oil to obtain a 2- to 10-fold coffee aroma level ~aroma from 1 to 9 parts coffee oil combined with 1 part coffee oil), the level also depending upon how much aroma is to be added later to the food product such as instant coffee. Preferably at least a 5-fold level of aromatized oil is added to obtain a desired aroma level in a product such as instant coffee without adversely affecting its appearance and flowability.
This folding ~concentrating) step is preferably accom~
; plished by immersing the sleeve with the condensed aroma consti-tuents thereon into an appropriate amount of coffee oil contained -in a folding chamber (a chamber capable of being sealed to be fluid and air tight), sealing the chamber from the air, flushing the chamber with an inert gas and then allowing the aroma consti-tuents to combine with the coffee oil. The appropriate amount of ; expressed coffee oil is determined by the final concentration of aroma desired (i.e., 2- to 10-fold). So that the sleeve can be immersed in the coffee oil it may be desirable, depending upon the appropriate amount of coffee oil, that the folding chamber have a dead space which the sleeve will fit around so as to allow a minimum volume of oil to be in contact with a substantial portion of the condensed aroma constituents on the sleeve's outer surface. This can be carried out by having a vessel in the folding chamber which the sleeve fits around. This vessel occu-pies sufficient space in the folding chamber so that the appro-priate amount of coffee oil in the folding chamber will contact a substantial portion of the condensed aroma constituents on the outer surface of the sleeve.
After sufficient time has elapsed for the aroma consti-tuents to combine with the oil the aromatized oil is transferred from the folding chamber, the seal broken, the sleeve removed and the chamber resealed and recharged with fresh oil and flushed . .
~ 7 . . .. . ................... ; : .:: .................. : .
,, .. , ,, , ,:: : ' :' : ' ~063865 with an inert gas in readiness for another sleeve. By thus having one folding chamber ready per sleeve, the exposure of the aroma constituents to air is minimized to the transfer time of the sleeve from the condensing chamber to the folding chamber.
Also the use of this folding chamber provides a simple method for combining the aroma constituents with oil while minimizing con-- tact of the oil and aroma constituents with air.
After the aroma constituents have been combined with the oil the aromatized oil is then preferably blended in another chamber with other aromatized oils in desired proportions thus ~ obtaining a homogenous aromatized oil and minimizing batch to ; batch variations.
Generally the most preferable aroma constituents from the viewpoint of quality are those recovered as a frost. Further, in order to be able to remove the condensed aroma constituents from the condensing chamber it is also preferred that the aroma con-stituents be in the solid state, i.e , recovered as a frost. The sleeve permits the collection of the condensed aroma constituents as a frost, so that when one removes the sleeve one also removes all the aroma constituents frosted onto its outer surface. By appropriate adjustment of the temperatures and pressure the liquification of the recovered aroma constituents can be avoided.
The coolant temperature can be reduced or the condenser pressure increased. With respect to coffee aroma constituents if the pressure is raised to above approximately 60 microns, (preferably 140 microns,) and the coolant temperature kept at -196C the condensate is then collected as a frost.
This is preferably accomplished by introducing an inert gas (e.g., nitrogen, carbon dioxide, etc.) at a flow rate effec-tive to control the pressure within the space between the sleeve and the condensing chamber at a level sufficient to keep the condensed aromatic constituents solid. Preferably the inert gas -, .~ . .~
~63865 is introduced in the distillation chamber, so as the pressure of the inert gas is controlling the physical state of the condensate in the condensing chamber as a solid, the inert gas is also aiding in the separation of the volatile aromas from the coffee oil in the distillation chamber by the process of desorbtion.
- The process of the instant invention can also be ; employed in-the separation of aroma constituents from other types ;~
of coffee oils such as solvent-extracted coffee oil.
In order that the present invention may be more clearly -understood reference will now be made to the following exampleand to Figure 2.
EXAMPLE
; The distillation and condensing chambers were totally enclosed and flushed with carbon dioxide, then depressurized to ;
approximately 20 microns, while the eirst feed tank was charged with 140 pounds of expressed coffee oil.
The expressed coffee oil was obtained by subjecting ` roasted whole coffee beans to pressures of at least 5,000 p.s.i.
in an expeller and wherein said expressed coffee oil recovered from the expre~sing operation had a temperature ranging from 25C
to 120C and the coffee meal residue had a temperature ranging from 75C to 150C, the environment of the expressing operation being cooled to a temperature below about 150C.
The oil was then pumped into the distillation chamber 11 at ambient temperature from the first feed tank 12 at pressures up to approximately 1000 p.s.i.g. through an impingement type atomizing nozzle 13 which operated by having a liquid stream at a high velocity strike a pin held at the exit of the nozzle orifice resulting in a wide angle, hollow cone, fine spray under the vacuum environment of the distillation chamber 11. Meanwhile nitrogen 14 was bled into the distillation chamber in order to maintain a pressure of 140 to 160 microns. This was done ~o _ 9 _ -. ' ' ' ', ',, ~ . " . ~
. .
' ~63~16S
maintain the condensed aroma constituents in the condenser in the solid state and to aid in separation of the aroma constituents from the expressed coffee oil through the process of desorbtion.
The 140-pound oil charge was sprayed into the distillation chamber 11 over a period of approximately 60 minutes. As the partially spent oil collected in the bottom of the distillation chamber, it was transferred by pumping to a second feed tank 19 wherein it was heated to a temperature of approximately 66C.
Isolating a second condensing chamber 20, as the gas stream passed through a first condensing chamber 15 the aroma constituents were condensed onto a thin gauge aluminum sleeve 16 cooled by and snugly surrounding a stainless steel container 17 filled with liquid nitrogen 18.
After the first charge had passed through the distil-lation chamber 11 once, this first condensing chamber 15 was isolated and a second condensing chamber 20 connected in parallel with the first was put into operation by appropriate valve 21 adjustment. The first condensing chamber 15 was then vented to atmospheric pressure using nitrogen gas and opened by unfastening the hinged cover 22 of the condensing chamber 15. The sleeve 16 was removed manually and immediately placed into a folding chamber 23 with 17.5 pounds of fresh expressed coffee oil therein.
The folding chamber was closed and then flushed with carbon dioxide to remove any air.
A clean sleeve was inserted onto the container 17 in the first condensing chamber 15, the chamber was then closed by refastening the hinged cover 22 and depressurized. The first condensing chamber 15 was then ready to be put back into opera-tion as soon as the second condensing chamber 20 was isolated.
The preheated partially stripped oil from the second feed tank 19 was then passed through the distillation chamber 11 in a manner identical to the oil from the first feed tank 12, ~063865 except that on collection in the bottom of the distillation chamber the totally spent (stripped) oil was transferred to a collection tank rather than a feed tank. From the collection -~
tank this dearomatized oil was either routed to be used as fuel or used in some other desired fashion.
At the end of the second stripping pass, the second ~ condensing chamber 20 was vented to atmospheric pressure using ; nitrogen gas. The sleeve 24 was then removed and immediately placed into a second folding chamber 25 with 17.5 pounds of freshly expressed coffee oil therein. The folding chamber 25 was closed and flushed with carbon dioxide to remove any air.
The contents of the first folding chamber 23, which had been allowed to sit for approximately 60 minutes, was then trans- ~
ferred to a 35-pound capacity oil pot 26 by applying pressure ~ -using carbon dioxide gas to the folding chamber's headspace. The first folding chamber 23 was then opened and the sleeve 17 removed and cleaned. The folding chamber was then closed and `charged with 17.5 pounds of fresh oil in readiness for another aroma laden sleeve.
After an additional 60 minutes, the remaining 17.5 pounds of aroma laden oil from the second folding chamber 25 was transferred to the identical 35-pound pot 26, wherein it was blended with the oil from the first folding chamber 23 to produce a homogeneous 35-pound batch of 5-fold oil. As before, the sleeve 24 was removed and cleaned, and a new 17.5-pound charge of fresh coffee oil was placed in the second folding chamber 25.
- Using a new charge of 140 pounds of fresh coffee oil, the cycle was then repeated to manufacture another batch of 5-fold oil.
The 5-fold oil was then plated on an instant coffee at a level of less than one percent by weight resultiny in a product - which has an unusually long storage life during which the original balance, strength and fragrance of the aromas are substantially retained without development of undesirable stale notes.
-- 11 -- ~
Claims (17)
1. A process of obtaining coffee aroma constituents useful in the aromatization of a foodstuff which comprises:
(a) subjecting coffee oil in a distillation chamber to distillation at sub-atmospheric pressures and mild temperatures to obtain aroma constituents therefrom;
(b) condensing said aroma constituents onto the outer surface of a heat-conductive sleeve removably and snugly surrounding a heat-conductive container, said container having a coolant therein and said sleeve being enclosed by a condensing chamber, said condensing chamber having ports for the passage of said aroma constituents within the space between the sleeve and the condensing chamber, and said condensing chamber having a removable cover which seals an opening through which the sleeve is passed when removed from the container;
(c) removing said cover and taking out said sleeve with the condensed aroma constituents thereon; and (d) recovering said condensed aroma constituents.
(a) subjecting coffee oil in a distillation chamber to distillation at sub-atmospheric pressures and mild temperatures to obtain aroma constituents therefrom;
(b) condensing said aroma constituents onto the outer surface of a heat-conductive sleeve removably and snugly surrounding a heat-conductive container, said container having a coolant therein and said sleeve being enclosed by a condensing chamber, said condensing chamber having ports for the passage of said aroma constituents within the space between the sleeve and the condensing chamber, and said condensing chamber having a removable cover which seals an opening through which the sleeve is passed when removed from the container;
(c) removing said cover and taking out said sleeve with the condensed aroma constituents thereon; and (d) recovering said condensed aroma constituents.
2. The process of Claim 1 further comprising:
introducing an inert gas at a flow rate effective to maintain the pressure within the space between the sleeve and the condensing chamber at a level sufficient to keep the condensed aroma constituents solid.
introducing an inert gas at a flow rate effective to maintain the pressure within the space between the sleeve and the condensing chamber at a level sufficient to keep the condensed aroma constituents solid.
3. The process of Claim 1 further comprising:
introducing an inert gas into the distillation chamber at a flow rate effective to maintain the pressure within the space between the sleeve and the condensation chamber at a level sufficient to keep the condensed aroma constituents solid and to further aid the distillation in the distillation chamber by desorbtion of the aroma constituents from the coffee oil.
introducing an inert gas into the distillation chamber at a flow rate effective to maintain the pressure within the space between the sleeve and the condensation chamber at a level sufficient to keep the condensed aroma constituents solid and to further aid the distillation in the distillation chamber by desorbtion of the aroma constituents from the coffee oil.
4. The process of Claim 2 or 3 wherein the pressure within the space between the sleeve and the condensing chamber is at least about 60 microns, and said coolant has a temperature of about -196°C.
5. The process of Claim 1 wherein said condensed aroma constituents are recovered by:
(a) immersing said sleeve with said condensed aroma constituents thereon into an appropriate amount of an edible substance contained in a folding chamber;
(b) sealing said folding chamber from the outside air;
(c) flushing said folding chamber with an inert gas;
(d) allowing the sleeve to remain in the edible substance for a period of time effective to allow the condensed aroma constituents to combine with the edible substance.
(a) immersing said sleeve with said condensed aroma constituents thereon into an appropriate amount of an edible substance contained in a folding chamber;
(b) sealing said folding chamber from the outside air;
(c) flushing said folding chamber with an inert gas;
(d) allowing the sleeve to remain in the edible substance for a period of time effective to allow the condensed aroma constituents to combine with the edible substance.
6. The process of Claim 5 wherein said folding chamber has a vessel therein which the sleeve fits around when immersed in the edible substance, said vessel occupying sufficient space so that the appropriate amount of the edible substance is in contact with a substantial portion of the condensed aroma constituents on the outer surface of said sleeve.
7. The process of Claim 5 or 6 wherein said edible substance is coffee oil.
8. The process of Claim 7 wherein said aroma consti-tuents are combined with coffee oil at a 2- to 10-fold level.
9. The process of Claim 8 further comprising incor-porating said aromatized coffee oil in an instant coffee.
10. The process of Claim 1 wherein said coolant has a temperature ranging from about 0°C to about -269°C.
11. The process of Claim 1 wherein said coffee oil is subjected to a distillation temperature below 100°C and an absolute pressure less than 50 mm.
12. The process of Claim 11 wherein the distillation is conducted by atomizing the coffee oil into the distillation chamber.
13. The process of Claim 11 wherein the distillation is conducted by providing a rapidly moving film of the coffee oil in the distillation chamber.
14. The process of Claim 1 wherein said coffee oil is an expressed coffee oil obtained by subjecting roasted coffee to pressures of at least 5,000 p.s.i.
15. The process of Claim 14 wherein said expressed coffee oil recovered from the expressing operation has a tempera-ture ranging from 25°C to 120°C and the expressed roasted coffee has a temperature ranging from 75°C to 150°C.
16. A condenser which comprises:
a heat-conductive sleeve removably and snugly surrounding a heat-conductive container, the container having a coolant therein, and a condensing chamber enclosing said heat-conductive sleeve, said condensing chamber having ports for the passage of a gas stream within the space between the sleeve and the conden-sing chamber, and said condensing chamber having a removable cover which seals an opening through which the sleeve is passed when removed from the container.
a heat-conductive sleeve removably and snugly surrounding a heat-conductive container, the container having a coolant therein, and a condensing chamber enclosing said heat-conductive sleeve, said condensing chamber having ports for the passage of a gas stream within the space between the sleeve and the conden-sing chamber, and said condensing chamber having a removable cover which seals an opening through which the sleeve is passed when removed from the container.
17. The condenser of Claim 16 further comprising:
means for introducing an inert gas at a flow rate effective to maintain the pressure within the space between the sleeve and the condensing chamber at a level sufficient to keep any condensed constituents of the gas stream solid.
means for introducing an inert gas at a flow rate effective to maintain the pressure within the space between the sleeve and the condensing chamber at a level sufficient to keep any condensed constituents of the gas stream solid.
Priority Applications (8)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA243,087A CA1063865A (en) | 1976-01-07 | 1976-01-07 | Dearomatization of coffee oil |
AU20025/76A AU501005B2 (en) | 1976-01-07 | 1976-11-26 | Dearomatization of coffee |
SE7613568A SE432689B (en) | 1976-01-07 | 1976-12-02 | PROCEDURE FOR MANUFACTURING COFFEE COMPONENTS AND CONDENSOR FOR IMPLEMENTATION OF THE PROCEDURE |
DE19762655187 DE2655187A1 (en) | 1976-01-07 | 1976-12-06 | METHOD OF OBTAINING COFFEE FLAVOR INGREDIENTS AND COOLER FOR CARRYING OUT THE METHOD |
FR7636683A FR2337505A1 (en) | 1976-01-07 | 1976-12-06 | COFFEE EXTRACT DESAROMATIZATION PROCESS AND DEVICE |
GB5086076A GB1544925A (en) | 1976-01-07 | 1976-12-06 | Process for the dearomatization of coffee oil and a condenser for use in the process |
ES454782A ES454782A1 (en) | 1976-01-07 | 1977-01-04 | Process for the dearomatization of coffee oil and a condenser for use in the process |
JP71477A JPS5943140B2 (en) | 1976-01-07 | 1977-01-07 | Method for removing aroma components from coffee oil and apparatus therefor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CA243,087A CA1063865A (en) | 1976-01-07 | 1976-01-07 | Dearomatization of coffee oil |
Publications (1)
Publication Number | Publication Date |
---|---|
CA1063865A true CA1063865A (en) | 1979-10-09 |
Family
ID=4104916
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CA243,087A Expired CA1063865A (en) | 1976-01-07 | 1976-01-07 | Dearomatization of coffee oil |
Country Status (8)
Country | Link |
---|---|
JP (1) | JPS5943140B2 (en) |
AU (1) | AU501005B2 (en) |
CA (1) | CA1063865A (en) |
DE (1) | DE2655187A1 (en) |
ES (1) | ES454782A1 (en) |
FR (1) | FR2337505A1 (en) |
GB (1) | GB1544925A (en) |
SE (1) | SE432689B (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61158451A (en) * | 1984-12-29 | 1986-07-18 | Toshiba Electric Equip Corp | Ultraviolet-ray irradiating device |
JP3773524B1 (en) * | 2005-11-09 | 2006-05-10 | ケミ・コム・ジャパン株式会社 | Coffee extract production method and beverages and foods containing the same |
JP5196770B2 (en) * | 2006-11-24 | 2013-05-15 | サミット製油株式会社 | Coffee oil and method for producing the same |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CA603954A (en) * | 1960-08-23 | General Foods Corporation | Distillation of expressed coffee oil | |
US2947634A (en) * | 1956-07-20 | 1960-08-02 | Gen Foods Corp | Process for preparing soluble coffee |
US3704132A (en) * | 1971-03-19 | 1972-11-28 | Procter & Gamble | Purification of coffee oil as a stable coffee aroma carrier |
CA995511A (en) * | 1971-10-13 | 1976-08-24 | The Procter And Gamble Company | Aroma condensation process |
GB1499756A (en) * | 1974-05-20 | 1978-02-01 | Gen Foods Corp | Method of manufacturing coffee-aroma material |
-
1976
- 1976-01-07 CA CA243,087A patent/CA1063865A/en not_active Expired
- 1976-11-26 AU AU20025/76A patent/AU501005B2/en not_active Expired
- 1976-12-02 SE SE7613568A patent/SE432689B/en not_active IP Right Cessation
- 1976-12-06 DE DE19762655187 patent/DE2655187A1/en not_active Withdrawn
- 1976-12-06 GB GB5086076A patent/GB1544925A/en not_active Expired
- 1976-12-06 FR FR7636683A patent/FR2337505A1/en active Granted
-
1977
- 1977-01-04 ES ES454782A patent/ES454782A1/en not_active Expired
- 1977-01-07 JP JP71477A patent/JPS5943140B2/en not_active Expired
Also Published As
Publication number | Publication date |
---|---|
SE7613568L (en) | 1977-07-08 |
SE432689B (en) | 1984-04-16 |
ES454782A1 (en) | 1978-01-01 |
JPS5287248A (en) | 1977-07-20 |
FR2337505B1 (en) | 1982-07-09 |
DE2655187A1 (en) | 1977-07-21 |
AU501005B2 (en) | 1979-06-07 |
AU2002576A (en) | 1978-06-01 |
JPS5943140B2 (en) | 1984-10-19 |
GB1544925A (en) | 1979-04-25 |
FR2337505A1 (en) | 1977-08-05 |
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