MXPA97008216A - Liquid smoke which has been removed from the alquitrany manufacturing method - Google Patents

Abstract

The present invention relates to a method for making a tar-depleted liquid smoke composition, characterized by the step of contacting for a sufficient period of time, a starting material composed of liquid smoke containing phenols including a component of tar, with an adequate amount of activated carbon that has enough active sites to produce a fully water-miscible, tar-depleted liquid smoke composition, which contains phenols with a reduced tar component

Description

LIQUID SMOKE TO WHICH THE TAR HAS BEEN REMOVED AND MANUFACTURING METHOD FIELD OF THE INVENTION The present invention relates, in general, to a liquid smoke composition. These liquid smoke compositions are used to color and flavor edible food products. More particularly, the present invention relates to a liquid smoke composition that has been refined to remove selected tar components therefrom.

BACKGROUND OF THE INVENTION Foods have been subjected to smoking processes since humans began using fire to prepare food. The smoked food has provided them with flavor, color and preservation.

Initially, conservation was the main reason for smoking food, but as technology advances, flavor and color have become the main reasons for smoking food. As the societies became more industrialized, the change from household or individual smoking to processing in specialized plants led to the need for better control of smoking procedures. In addition, the increase in P1540 / 97MX productivity led to the desire for more consistent smoke application techniques. As a result, liquid smoke compositions (also known as liquid smoke solutions and referred to colloquially as liquid fumes) were developed as a replacement for smoking of the food by direct contact with smoke, and such compositions have become standard practice in the industry. Liquid smoke when applied to the surface of meats and other protein food products, such as various types of sausages, German sausages, bologna sausages, meat rolls, hams and the like, gives the item a characteristic smoke flavor and produces a color smoked dark. The achievement of a product with a flavor similar to a homemade smoked by the application of an aqueous solution of smoke to a food product requires the control and compensation of many variables, such as food composition, temperature, humidity, processing time, time of contact, amount of liquid smoke and concentration of liquid smoke. It is well known to those skilled in the art that liquid smoke compositions contain a broad set of chemical compounds; More than 400 of these compounds have been identified. However, it is well known to those skilled in the art that the P1540 / 97MX Liquid smoke compositions are characterized by their content of certain classes of compounds, specifically, acids (titratable acid percent), phenols, and carbonyls. The acids are preservatives and, of course, pH control agents, as a result of which commercial liquid smoke compositions typically have a pH below about 2.5, and more typically below about 2.3, and a percent titratable acidity by volume from about 3. up to about 18%. Phenols give flavor, and also aroma, to liquid smoke compositions, and commercial compositions typically have a phenol content of from about 3 to about 45, and more typically, from about 14 to about 30 mg / ml. The carbonyls impart the brown color to liquid smoke compositions. Phenols and carbonyls can be measured as described in the aforementioned Nicholson US Patent No. 4,431,032. The color-forming potential of the liquid smoke compositions can be measured by the well known method of the brown color index described in Underwood US Patent No. 4,994,297, mentioned below, or by the P1540 / 97MX well-known method of staining index, which comprises the reaction of liquid smoke with glycine, as described below. It is pointed out that acids and carbonyls are secondary in the flavor contribution of liquid smoke compositions. More specifically, liquid smoke was developed more than 65 years ago and is the aqueous condensate of natural wood smoke, as described in US Patent No. 1,753,358 issued in 1930 to Wright. Also of interest, along with the older manufacturing processes for liquid smoke is US Pat. No. 2,400,466 issued in 1946 to Reiter et al. Improved liquid smoke compositions and techniques for the manufacture thereof are disclosed in US Patent No. 3,106,473 to Hollenbeck, US Patent No. 3,837,741 to Meicer et al., US Patent No. 4,298,435 to Ledford, US Patent No. 4,154,866 to Dainius. and collaborators, and US Patent No. 4,994,297 to Underwood. While the advent of liquid smoke compositions has significantly improved meat processing, attempts have been made over the past 20 years or so to deal with the problem P1540 / 97MX of liquid smoke tar. In the storage of a liquid smoke product, the tar will settle to the bottom of the liquid smoke vessel, forming a viscous, sticky, water-insoluble precipitate. Additionally, although water is present in liquid smoke, it is not totally soluble in water, which exacerbates the problem of tar. More specifically, for the commercial application of the liquid smoke to a food product, the liquid smoke is typically diluted with water in an amount that results in 2 to 5 times the original volume of the liquid smoke. However, the tar precipitate will also occur in the dilution of the liquid smoke with water and, thus, can be easily removed in the pipeline of a system used for the application of liquid smoke to the food product. In relation to the foregoing, it is pointed out that US Patent No. 4,112,133 to Rao discloses a liquid smoke composition and the related process to maintain the tar component of the liquid smoke in suspension, so that the tar does not form undesirable solids during the storage. More particularly, the patent to Rao is directed mixing liquid smoke with a fatty compound, such as polyoxyethylene sorbitan monooleate, polyoxyethylene monostearate, sorbitan monopalmitate or sorbitan Polyoxyethylene for P1540 / 97MX emulsify the tar. Removal of tar instead of keeping it in emulsion is achieved by an extraction process with solvents used in the liquid smoke to create a desirable supernatant liquid smoke, tar-depleted, and an undesirable fraction containing tar, followed by separation by gravity of the two fractions as described in U.S. Patent Nos. 4,431,032, 4,431,033 and 4,496,595, all of Nicholson and in US Patent No. 4,592,910 of Chiu. Solvents such as dichloromethane or chloroform are used. It related to the above is the process of removing tar described in U.S. Patent No. 4,504,507 to Nicholson, wherein the pH of liquid smoke is raised above 4 to create a desirable supernatant liquid smoke, tar-depleted, and an undesirable fraction containing tar, followed by gravity separation of the two fractions. Nicholson's four patents also describe the treatment of a surface of a food wrapper, for example a fibrous, cellulosic wrap used for sausages, with the tar-laden liquid smoke. Additionally, U.S. Patent No. 5,288,532 to Juhl et al. Describes an envelope of P1540 / 97MX food consisting of plastic, polymer film, as pred in a mixture of ethylene-vinyl acetate and polyethylene oxide, and during extrusion of the plastic film liquid smoke is mixed with the polymer beads. The liquid smoke is then transferred or moved from the film to the food product packed with the film. Finally, of interest in relation to the removal of unwanted components of liquid smoke, we have the process described in US Patent No. 4,959,232 of Underwood, which is directed to the passage of liquid smoke through a column of beads of polymeric resin , both ionic and nonionic (the suitable resins are copolymers of alkyl acrylates and polyvinylidene crosslinking), or alternatively, mixing the liquid smoke with the resin beads in a batch process, to remove the flavor components of the same , so that more of the resulting liquid smoke can be employed to impart more brown coloration to the treated food product. The descriptions of all the patents mentioned above are incorporated herein by reference. Despite the procedures discussed above to handle the removal or conservation of P1540 / 97MX certain components suspended from liquid smoke (such as the removal of tar by solvent extraction of liquid smoke or the preservation of tar in suspension when adding a fatty compound of sorbitan to liquid smoke), there are still problems with these procedures. For example, the solvent extraction process of the Nicholson patents and the resin treatment process of the Underwood patent both have a deficit since these processes leave residual solvents that are added directly, by Nicholson, or are used, by Underwood, to condition the resin. The preservation of suspended tar according to the Rao patent process requires the addition of sorbitan fatty compounds that dilute the liquid smoke, resulting in not only increased treatment requirements, but also the impediment of the color formation reaction. , whereby the hume can be removed by washing, leaving the food product, if not properly fixed during application to the food product. With this process, the tar is still in the liquid smoke, so that the tar, as well as the fatty compound of sorbitan added, is being ingested by the consumer of the smoke-treated food product. In addition, the sorbitan fatty compounds have not been approved for P15Í0 / 97MX application to food products in some countries, which limits the distribution of these food products treated with smoke. Thus, it is desirable to find an improved liquid smoke composition that is depleted in tar and a method for manufacturing it, the composition and the method avoid the aforementioned problems.

SUMMARY AND OBJECTS OF THE INVENTION Accordingly, the present invention provides a method for making a tar-depleted liquid smoke composition comprising the step of contacting a liquid smoke composition of starting material having a phenol content, the The phenol content includes a tar component, with an activated carbon having enough active sites to produce a tar-depleted liquid smoke composition, which has a content of phenols with a reduced tar component, so that the spent liquid smoke in the tar is completely miscible in water. Additionally, the present invention provides a tar-depleted liquid smoke composition, comprising a tar-depleted liquid smoke composition, completely miscible with water; the composition of P1540 / 97MX tar depleted liquid smoke is derived from a liquid smoke composition of phenol-containing starting material, the phenols include a tar component, wherein the phenols of the tar-depleted liquid smoke composition have a reduced component of tar resulting from contacting the liquid smoke composition of starting material with an activated carbon having sufficient sites to produce the reduction. Preferably, the liquid smoke composition of starting material has a phenol content of about 3 to about 45, and more preferably, about 14 to about 30 mg / ml. Typically, the phenol content of the resultant tar depleted liquid smoke composition will be reduced by about 10 wt. To about 90 wt.%, Compared to the phenol content of the starting material of the liquid smoke composition. However, in an alternative embodiment, the spent liquid smoke can be concentrated in tar, for example by vacuum evaporation, and the concentrate will have a higher phenol content than that of the starting material of the liquid smoke composition, but still It will be completely miscible in water.

P1540 / 97MX The present invention also contemplates a food wrap treated with a tar depleted liquid smoke composition. The treatment may consist of spraying or spraying the tar-laden liquid smoke onto a surface of the envelope, or in the case that the shell is made of plastic, polymeric, extruded film, the tar-laden liquid smoke can be sprayed onto a surface of the film or it can be incorporated into the extruder with the beads of the polymeric resin and mixed with this way in the resulting plastic film. The present invention also contemplates a protein food product, such as various types of sausages, German sausages, bologna sausages, meat rolls, hams and the like, treated with the new tar depleted liquid smoke composition. Accordingly, it is an object of the present invention to provide a liquid smoke composition and the related method of manufacture, wherein the composition is tar-depleted and, therefore, will not form a tar precipitate upon dilution with water. Therefore, it is an advantage of the present invention that the liquid smoke composition is completely miscible in water since when liquid smoke is applied to food products or food wrappings P1540 / 97MX food, is typically diluted with water and forms tar precipitates that become tacky to the pipe system of the application apparatus, this problematic situation will not occur with the tar depleted liquid smoke composition of the present invention. Some of the objects and advantages of the invention have been pointed out above, other objects, as well as other advantages, will become apparent as the description proceeds, when taken in conjunction with the Laboratory Examples and the detailed description that follows.

DETAILED DESCRIPTION OF THE INVENTION The present invention is directed to a tar depleted liquid smoke composition made by contacting the liquid smoke with activated carbon having sufficient active sites to reduce the tar component of the liquid smoke. While not intended to be limited by any particular theory, it is believed that the tar component is part of the phenol component of the liquid smoke, as explained below.

The tar-depleted liquid smoke composition of the invention still remains with the smoke coloring and the smoke flavoring capacity. As you can see from the Examples of P1540 / 97MX Subsequent Laboratory, the inventive method results in a reduction of the phenols in the resulting liquid smoke, as compared to the liquid smoke of starting material. When the resulting product was then diluted with water, the tar did not precipitate. Rather, the diluted liquid smoke remained clear at a dilution with water of up to 5 times the original volume of the resulting product, and in this way the resulting product was completely miscible with water. In an alternative embodiment, when the resulting product was concentrated by vacuum evaporation, to remove some of the water therefrom, the concentrate had a higher phenol content than that of the liquid starting material smoke. However, the concentrate in the dilution with water of up to 5 times, still remained clear. (See sample No. 4 of Example 4 below). In addition, with certain activated carbons having insufficient active sites, although the content of phenols was lower in the resulting product than in the liquid smoke of starting material, the resulting product still contained tar (see Example 5 below). Thus, for those activated carbons with sufficient active sites, it appears that the inventive method reduces the phenols by reducing the tar component therefrom. In the selected Lab Examples that P1540 / 97MX are described below, in order to produce a tar-laden liquid smoke, the tar-containing liquid smoke thus treated by the method of the present invention was Code 10, which is commercially available from Hickory Specialties, Inc., from Brentwood, Tennessee. In one of the subsequent Laboratory Examples, the liquid smoke starting material used was SUPERSMOKE, also commercially available from Hickory Specialties, Inc., and manufactured by a well-known vacuum evaporation process that concentrates Code 10 by removing from it Some water. As a result, the SUPERSMOKE has a typical acidity of approximately 16%, while the Code 10 has a typical acidity of approximately 11 o. Other commercially available liquid smoke compositions can also be employed with the method of the present invention to produce a tar-laden liquid smoke. Each of the activated carbon products useful in the present invention for treating the liquid smoke starting material, such as Code 10, has sufficient active sites in the carbon particles to produce a tar-depleted liquid smoke composition having a content of phenols with a reduced component of tar, so that the liquid smoke exhausted in tar is completely miscible in P1540 / 97MX water. Compared to the liquid smoke starting material, the tar-depleted liquid smoke typically has a phenol content reduced by at least about 10% by weight, and the reduction can be up to about 90% by weight, but more typically is up to about 85% by weight. Preferably, the reduction is at least about 15% by weight, and more preferably at least about 30% by weight. In conjunction with this, it is reiterated that the tar-depleted liquid smoke can be concentrated by the vacuum concentration process (the process outlined above for manufacturing SUPERSMOKE from Code 10 and well known to those skilled in the art) and, for therefore, the concentrate will be depleted in tar but will have a higher phenol content than that of the starting material of the liquid smoke. The activated carbon products having sufficient active sites and employed in the present invention were purchased from Calgon Carbon Corporation of Pittsburgh, Pennsylvania, and are described in their sales booklet entitled "Activated Carbon Products for Liquid and Vapor Phase Applications" ("Activated Carbon Products for Liquid and Vapor Phase Applications"). "Products of Activated Carbon for Liquid Phase and Vapor Applications ") (November 1993). Preferred activated carbon that has enough active sites for use in the present P1540 / 97MX invention is sold by Calgon under the trade name ADP, and is sprayed with a mesh size of North American standard of 80 x 325. Less preferred is activated carbon which has sufficient active sites and is sold by Calgon under the trade name APA, which is granular and has a North American standard mesh size of 12 x 40. Also useful, it is an activated carbon that has enough active sites and is sold by Calgon under the trade name PWA, which is pulverized, but is much less preferred because either much more must be used or the contact time with commercially available liquid smoke must be much greater. Calgon does not indicate in its sales brochure what the North American mesh size of the PWA is, but has made public the fact that the PWA is not as highly activated as any of APA or ADP. Any carbon having enough active sites or mixtures of those carbons can be employed in the present invention. Therefore, an activated carbon having sufficient active sites can be selected from the group consisting of ADP, APA, PWA, and combinations thereof. In conjunction with this, it is noted that certain activated carbons do not have sufficient active sites and do not work in the present invention. An activated carbon of this type with insufficient active sites is P1540 / 97MX sold under the tradename TOG by Calgon and is further described in Example 5 below. As described in its technical information brochure entitled "Activated Carbon Principles" (May 1993), Calgon manufactures activated carbon by treating materials such as mineral coal, wood, peat, coconut husks and coke. oil with a process of heat and steam, which results in graphite platelets. As explained in your brochure, part of the material is selectively oxidized with a gaseous, acidic, water vapor and carbon dioxide mixture to develop a certain pore structure, that is, create active sites. More particularly, the amount of activation is related to the resulting volume of activated carbon pores, which affects the Van der Waals forces that bind activated carbon to the products to be absorbed. With the present invention, the contact of the liquid smoke with the activated carbon, in order to produce the spent liquid moisture in tar, must be under ambient conditions of temperature and pressure. In addition, the contact time should be approximately at least 15 minutes, and may be up to approximately 12 hours or more, depending on the particular type, amount and volume of pores of the activated carbon employed. More preferably, the contact time should be approximately 0.5 hours until P1540 / 97MX about 9 hours, and most preferably from about 1.5 hours to about 5 hours. Batch processes may be employed, where the particles of activated carbon are placed in the liquid smoke in a stirred vessel, followed by filtration to separate the particles of the resulting liquid smoke exhausted in tar. In addition to filtration, the method for separating the particles may include decanting by gravity, liquid treatment in a cyclone, and decanting by centrifuge. However, in a commercial establishment in a factory, a column process would be more economically viable. In a column process, a cylindrical vessel is packed with a bed of activated carbon particles, and then the liquid smoke flowing down through the column is passed, and the effluent of the spent liquid smoke is collected in tar compliant leaves the bottom of the column. The activated carbon particles useful in the present invention absorb phenols (which include the tar-producing components thereof) from the liquid smoke of starting material, and the bound phenols can be displaced from the spent particles of activated carbon under appropriate. The removal of the adsorbed compounds, for example by countercurrent washing of spent carbon particles P1540 / 97MX activated, is well known to those skilled in the art, and will allow the carbon to be reused and recycled. As noted above, the food wraps can be treated with the liquid smoke composition depleted in tar. In the case that the envelope is of the fibrous type, the treatment may be by spraying the tar-laden liquid smoke onto a surface of the envelope. Typical fibrous casings are cellulosic in nature. In the event that the shell is made of plastic, polymeric, extruded film, the spent tar-laden liquid smoke can be sprayed or sprayed onto the surface of the film. Alternatively, the tar-depleted liquid smoke can be incorporated in the extruder apparatus with beads or beads of polymeric resin and is thus mixed in the resulting plastic film. Typical polymeric plastic films include, without limitation, the polymer films selected from the group consisting of: ethylene-vinyl acetate, ethylene-acrylic acid, ethylene-methacrylic acid, linear low density polyethylene, linear polyethylene low density, very low density (sometimes referred to as ultra low density polyethylene), and combinations thereof. Additionally, a product can be treated P1540 / 97MX protein food with the liquid smoke composition depleted in tar, such as by spraying on the surface thereof. Examples of various types of protein foods include, without limitation, the following: sausages, German sausages, bologna sausages, meat rolls, hams and combinations thereof.

LABORATORY EXAMPLES In the subsequent Laboratory Examples, the methods used to determine phenols and carbonyls are well known to those skilled in the art and are set forth in columns 11 and 12 in Nicholson US Patent No. 4,431,032, mentioned above . Also, in the subsequent Laboratory Examples, the methods used to determine the staining index and percent acidity are well known to those skilled in the art and are set forth as follows: TINY INDEX Reagent of 2.5% Glycine in Acetic Acid at 95 o. A slurry of 2.50 grams of glycine (Eastman # 445) is formed with 5.0 ml of distilled water in a 150 ml beaker. Approximately 70 ml of glacial acetic acid are added and P1540 / 97MX heats in a steam bath, stirring occasionally to dissolve the glycine. Transfer to a 100 ml volumetric flask, cool to room temperature, and fill volume with glacial acetic acid used to rinse the original beaker. The solution is filtered before use if some of the glycine crystallizes. The solution is stable for at least 3 weeks, and probably indefinitely. Liquid Smoke Solution at 5%. 2.50 ml of liquid smoke is diluted to a final volume of 50.0 ml with glacial acetic acid. Reaction: 1. Using two 25 ml graduated test tubes, add 1.0 ml of the liquid smoke solution to 5 or 10.0 ml of the glycine reagent and add 1.0 ml of the 5% liquid smoke solution to 10 ml of glacial acetic acid (white). 2. Each tube is covered tightly with a square of protective film, and mixed by vortex effect and placed in a water bath at 85 ° C for 30 minutes. 3. Transfer to a cold water bath and partially dilute with distilled water to accelerate cooling. When is it P1540 / 97MX room temperature, finish the dilution to the 25 ml mark and mix by inversion. 4. Set a spectrophotometer to 0 using distilled water. The absorbance of each solution is read in a 0.5-inch cell using a spectrophotometer at 440 millimicrons. 5. The net absorbance is calculated by subtracting from the reading of the test sample the blank reading (consisting of 1.0 ml of 5% liquid smoke solution, 10.0 ml of glacial acetic acid and distilled water up to a volume of 25 ml ). 6. Calculate the staining index: SI = Net Absorbance x 100.

PERCENTAGE OF ACETIC ACID 250 ml of distilled water is poured into a clean, 400 ml beaker. 6 ml of liquid smoke are introduced. A pH meter is standardized with buffer solution pH 7. The pH meter should be at 7.00. If not, use the control knob and place it there. The glass electrode is thoroughly rinsed with distilled water from the pan. Place the beaker of the water-smoke mixture on the platform P1540 / 97MX test and lower the pH electrodes. The mixture is stirred, adding a sodium hydroxide solution with a normality of 1.0 normal. There the sodium hydroxide is added until the pH meter measures 7.0. The amount of milliliters of sodium hydroxide added to the water-smoke mixture is the percentage of acetic acid. For example, 1 ml of sodium hydroxide entering the smoke-water mixture will have a point of acetic acid until the pH meter reaches a value of 7.0. In other words, if 9.4 ml of 1.0 N sodium hydroxide solution is introduced, the acetic acid reading will be 9.4% acetic acid by volume. The calculations are as follows: % acetic acid = [(ml of NaOH) x (Normality of NaOH) x (equivalent weight of acetic acid)] divided by ml of liquid smoke. . of acetic acid = [(11.3 ml of NaOH) x (Normality of 1.0) x (approximately 60)] divided by 6.0 ml of liquid smoke, and thus or of acetic acid = 11.3 EXAMPLE 1 (COLUMN) A 55-gallon metal drum, shaped P1540 / 97MX cylindrical, approximately 22.5 inches (approximately 57 cm) in diameter and approximately 34 3/8 inches (approximately 87 cm) in height was equipped with a drain hole in the bottom and a feed tube in the top. Approximately 160 pounds [approximately 352 kg, which was a column height of approximately 28 inches (approximately 71 cm)] of APA, an acid washed, granular Calgon granular, was placed in the drum. Liquid smoke having a titratable acidity of 11.0% (approximately 30 gallons of Code 10 of Hickory Specialties, Inc.) was fed into the drum, and allowed to stand overnight (approximately 12 hours), and the effluent depleted in tar, The resultant drained hole from the bottom of the drum was designated in Table 1 below as the first sample. On the next day, a continuous feed by gravity of Code 10 was started via the feed tube at the top and drained via the bottom hole. The flow rate through the drum was 30 gallons per hour, which was a contact time of about 2 hours. Samples of liquid smoke from the effluents were collected sequentially in 55-gallon drums, and designated in Table 1 below as the 2nd, 3rd, 4th, 5th and 6th and 7th samples. The samples were analyzed with the following results P1540 / 97MX reported in Table 1 below, TABLE 1 Index Carbo- Dilu - Weight Acidity of nilos Phenols in Speci- Sample (%) pH ttiinncciióónn (g / 100 g) (mg / ml) Water Feeding 11.0 2., 11 90.0 22.9 18.7 Cloudy 1.077 Code 10 8.7 1., 97 58.6 11., 2 2.7 Clara 1., 050 2a 11.5 2., 01 91.6 20, .3 6.3 Clara 1. .079 3a 11.2 2., 05 98.0 19, .6 10.0 Clara 1., 080 4a 10.9 2., 05 98.1 20, .6 16.6 Clara 1., 082 5a 10.8 2., 05 93.5 20,, 3 15.3 Clara 1., 082 6a 10.8 2., 06 87.8 20, .3 19.0 Light 1, .082 cloudy weather 7a 10.9 2.0E 91.3 20, .3 17.1 Cloudy 1, .082 For dilution in water, water was added to create a 2x volume for all samples. The Code 10 food sample exhibited cloudiness (ie, tar precipitate) of the dilution, which was expected since Code 10 is a commercially available liquid smoke containing tar. For the samples from 2a to 5a, the water at a volume of 2x did not result in the tar precipitate and in this way more water was added to create a volume of 5x. Even the samples remained clear, P1540 / 97MX which illustrates that these samples exhausted in tar were completely miscible in water. Additionally, the data clearly show a reduction in total phenolic compounds that is parallel to miscibility in water, for each of the samples up to the 5th. Accordingly, a mixture of the samples up to 5a must be effective as a tar-depleted liquid smoke having essentially the same staining properties as the starting material. Also, each of the samples from the first to the 5th could be used individually to treat a food product, depending on the desired flavor and desired brown color. Subsequently, for samples 6a and 7a, the activated carbon particles were apparently worn and had to be washed countercurrent to remove the adsorbed compounds since the ° of phenols was approximately the same as that of the Code 10 start feed and only a 2x dilution of water resulted in haze.

EXAMPLE 2 (LOT) The impact of the carbon particle size on the efficiency in the generation of tar-laden liquid smoke was evaluated using powder forms and P1540 / 97MX granules of the same activated carbon. APA coal from Calgon is a granular form of highly activated carbon, while carbon ADP is a powder form of the same material. To two equal aliquots (100 ml) of liquid smoke of Code 10 (titratable acidity of 10.7%) were added each of the activated carbons in various amounts. The samples were mixed with a magnetic stirrer during the time intervals indicated in Table 2 below, and at that time small portions (1 ml) were taken and filtered through Whatman filter paper # 1 to remove the carbon. Each filtered sample of liquid smoke was mixed with 2 to 5 times its volume of water to judge the miscibility. The lack or absence of tar or formation of precipitate during 2 hours (the sample remained clear) was established as the final point in the determination that the sample was completely miscible in water, and those are reported in Table 2 below. The following Table 2 shows the similarity in the minimum levels of carbon needed to achieve a depleted liquid smoke in tar with a total miscibility in water, and highlights the greater amount of carbon required to achieve miscibility, in shorter contact times for the granular carbon compared to powdered coal.

P1540 / 97MX The differential in the amounts of carbon for shorter periods of time is proportional to the adsorption speed of the tar-forming components to the internal active sites in the carbon matrix.

TABLE 2 COMPARISON OF GRANULAR CHARCOAL AGAINST DUST CHARCOAL Type of Charcoal Contact Time Amount (grams) Magnetic Agitation (hours) APA 15 0.75 12.5 1.25 10 1.7 8 3 5.25 4.25 4 8 ADP 8 1.5 5 5.25 4 8.5 As you can see, the AD? powder has more active sites on its surface than granular APA, since 8 grams of powdered ADP produced tar-laden liquid smoke with 1.5 hours of contact time, while to produce tar-laden liquid smoke in approximately the same amount of time, 10 grams (1.25 hours) to 12.5 grams (1.75 hours) of granular APA were required.

P1540 / 97MX EXAMPLE 3 (OTE) The impact of the amount of carbon activation on the production of fully miscible water smoke was evaluated using the ADPC and PWA coals in Calgon powder. These two carbons were derived from the same source materials, but Calgon reports that they differ in the amount of activation with the ADP that has a higher activation level. The procedure of Example 2 was repeated and different levels of carbon were mixed with aliquots of 100 ml of Code 10 liquid smoke (titratable acidity of 10.7%). It was found that the more activated a given carbon, the greater the removal efficiency of the tar-forming materials. The results are reported in the following Table 3 that shows the significant impact of the activation level on coal efficiency. TABLE 30 CARBON POWER COMPARISON Type of Charcoal Carbon Contact Time Amount (grams) Magnetic Agitation (hours) ADP 8 1.5 5 5.25 4 8.5 PWA 15 0.25 12.5 1.0 8 8.5 P1540 / 97MX As you can see, 8 grams of the most activated powder ADP produced tar-laden liquid smoke with only 1.5 hours of contact time, while the same 8-gram amount of the less activated powder PWA took 8.3 hours to produce the liquid smoke exhausted in tar.

EXAMPLE 4 (COLUMN) The following Table 4a represents the products used to produce depleted liquid fumes in tar of different concentrations, using the column procedure of Example 1 with activated Calgon APA coal, except that the column was continuous when bonded together. drums The flow rate was 2 gallons / minute through a total of approximately 810 pounds of carbon for all 6 drums (ie 135 pounds / drum). To determine the miscibility in water, the effluent was diluted with water at 5x the previous volume.

TABLE 4a EXISTING COMMERCE PRODUCTS (1) Code 10 (basic liquid smoke) (2) SUPERSMOKE (smoke concentrate).

P1540 / 97MX PRODUCTS OF THE INVENTION (3) Depleted in tar (resulting from the carbon treatment of Code 10) (4) Concentrate depleted in tar (made from the use of the same vacuum evaporation process in No. 3, as it is used commercially to make SUPERSMOKE from Code 10). (5) Depleted in tar (resulting from the SUPERSMOKE coal treatment) The composition of each of these products is defined in the following Table 4b with the products identified by the number in parentheses.

TABLE 4b Product Test Parameter (1) (2) (3) (4) (5) Titratable acidity (° Ó) 10.9 10.2 11.1 10.95 17.9 staining index 102.3 201.8 88.7 217.2 232.6 Specific gravity 1.080 1.168 1.074 1.172 1.176 Carbonyl (g / 100 Mi; 22.1 39.5 20.4 36.9 36.3 Phenols (mg / ml) 17.6 28.4 9.1 23.6 16.8 Solubility in Water No No Yes Yes Yes It is easily apparent that they can be derived P1540 / 97MX several products through alternative routes.

Specifically, the effectiveness of activated carbons in the production of fully miscible water products in water is not impacted by the concentration of Code 10 depleted in tar (product No. 3) to create the concentrate of SUPERSMOKE depleted in tar (product No. 4), as compared by elaborating SUPERSMOKE exhausted in tar (product No. 5) directly by the commercial SUPERSMOKE carbon treatment (product No. 2). In this way, the product No. 4 has a higher phenol content than that of the starting material, specifically the product No. 1, but the product No. 4 is still completely miscible in water, since it is depleted in tar.

EXAMPLE 5 (COMPARISON) The impact of an activated carbon with insufficient active sites to produce a tar-depleted liquid smoke was evaluated using Calgon's TOG activated carbon. The batch process of Example 2 was repeated and different levels of grams of carbon (reported as g of C) were mixed, with aliquots of 100 ml of liquid smoke (titratable acidity of 11.) For 3 hours, followed by filtration for Remove the carbon particles. Each sample of liquid smoke, treated P1540 / 97MX with charcoal, resulting mixed with 2 times its volume of water to judge the miscibility. All the samples diluted in water were tar-containing since the tar precipitate always formed within 2 hours and the samples were cloudy. It was found that although at a level > 2.5 g of activated carbon, the carbon reduced the content of phenols of each sample of liquid smoke treated with carbon, the active sites were insufficient to remove the tar-forming materials from the phenols. Furthermore, in conjunction with the content of phenols in the liquid smoke samples treated with carbon, it is noted that at a level from 0.05 g to 1.0 g of carbon, the carbon reduced the content of phenols of each sample of liquid smoke treated with carbon only with a minimum amount (ie, <; of 1 Ó), or actually increased the phenol content of each sample of liquid smoke treated with carbon. Also, for those samples treated at a level of > 2.5 g of activated carbon, where the carbon reduced the content of phenols, there was also a positive correlation of the pH of the sample increase, which, as can be seen from the review in Table 1, did not occur from the treatment with carbon APA of Calgon. The results are reported in the following Table 5 that shows the significant impact of the lack of P1540 / 97MX sufficient activation sites in the capacity of the coal for the removal of the tar component of the phenols.

TABLE 5 CarboDilu¬ index Sample g Acidity of niles Phenols in Alquitrái de C (%) pH staining (g / 100 g) (mg / ml) Water Seated Alimen11.0 2.01 88.4 15.8 14.05 Cloudy Code Code Si (none) 0.05 11.2 2.02 85.3 14.5 16.13 Cloudy Yes Cloudy 0.1 11.15 2.02 85.5 15.7 13.94 Cloudy Yes 0.2 11.0 2.04 84.0 14.4 16.20 Cloudy If Cloudy 0.5 11.2 2.05 80.6 15.8 13.24 Cloudy Yes 1.0 11.0 2.07 80.0 15.1 16.51 Cloudy If Cloudy 2.5 11.0 2.19 81.3 15.7 11.73 Yes 5.0 10.75 2.30 83.7 14.8 10.69 Yes 10.0 10.8 2.47 83.7 13.90 9.23 Yes Example 6 (Treatment of Food Products) Protein foodstuffs were treated with the depleted liquid fumes in tar of Example 1 (samples 1 to 5), of Example 2 (all samples of Table 2), of Example 3, (all the samples of Table 3) and of Example 4 (samples 3, 4 and 5) and with these liquid fumes diluted with water up to 5x. The food products treated in this way by the application of the liquid smoke exhausted in tar to the surface thereof are sausages, P1540 / 97MX German sausages, meat rolls, hams, and bologna sausages. Excellent staining and taste was obtained.

Example 7 (Treatment of Food Casings) Food casings were treated with the spent tar smoked liquids of Example 1 (samples 1 through 5), of Example 2 (all samples of Example 2), of Example 3 (all the samples of Table 3) and of Example 4 (samples 3, 4 and 5) and with these liquid fumes diluted with water up to 5x. The selected casings are fibrous, cellulosic casings and are treated by spraying the spent liquid smoke in tar on the surface thereof. The selected wrappers are plastic, polymeric, clogged films and are treated by spraying or spraying the spent tar-smoked liquid fumes onto the surfaces thereof. The selected casings are plastic, polymeric, extruded films and are treated by incorporating the spent liquid fumes in tar into the extruder apparatus with the beads or beads of polymeric resin and thus mixing the fumes in the resulting films. Plastic, polymeric films are P1540 / 97MX ethylene-vinyl acetate, ethylene-acrylic acid, ethylene-methacrylic acid, linear low density polyethylene, and linear low density polyethylene, very low density. The food products of Example 6 are packaged with the various wraps, and the packaged food products have excellent stain and taste. It will be understood that various details of the invention can be changed without departing from the scope thereof. Additionally, the foregoing description is for purposes of illustration only, and is not intended to limit the invention, which is defined by the claims.

P1540 / 97MX

Claims (20)

1. NOVELTY OF THE INVENTION Having described the present invention, it is considered as a novelty and, therefore, the content of the following CLAIMS is claimed as property: 1. A method for making a tar-depleted liquid smoke composition, comprising the step of contacting a liquid smoke composition of starting material having a content of phenols, the content of phenols includes a tar component, with an activated carbon having sufficient active sites to produce a liquid smoke composition exhausted in tar having a content of phenols with a reduced tar component, so that the liquid smoke exhausted in tar is completely miscible in water. The method according to claim 1, wherein the contact occurs for a time from about 15 minutes to about 12 hours. The method according to claim 1, wherein the liquid smoke composition of starting material has a phenol content of about 3 to about 45 mg / ml. 4. The method according to claim 1, wherein activated carbon having enough sites Active P1540 / 97MX is selected from the group consisting of ADP, ADP, PWA, and combinations thereof. The method according to claim 1, wherein the tar-depleted liquid smoke composition has a reduced phenol content from about at least 10% by weight to about 90% by weight. The method according to claim 1, further including the step of concentrating the spent liquid smoke composition in tar by subjecting the spent smoke-in-tar composition to vacuum evaporation, whereby the liquid smoke composition exhausted in Concentrated tar has a higher content of phenols than that of the liquid smoke composition of starting material. 7. A tar depleted liquid smoke composition, comprising a tar-depleted liquid smoke composition, completely miscible with water, the tar-depleted liquid smoke composition is derived from a liquid smoke composition of starting material that contains phenols, the phenols include a tar component, wherein the phenols of the tar-depleted liquid smoke composition have a reduced tar component resulting from contacting the liquid smoke composition of starting material with P1540 / 97MX an activated carbon that has enough sites to produce the reduction. The tar depleted liquid smoke composition according to claim 7, wherein the contact occurs for a time from about 15 minutes to about 12 hours. The tar depleted liquid smoke composition of claim 7, wherein the liquid smoke composition of starting material contains about 3 to about 45 mg / ml of phenols. The tar depleted liquid smoke composition according to claim 7, wherein the activated carbon having sufficient active sites is selected from the group consisting of ADP, ADP, PWA, and combinations thereof. The tar depleted liquid smoke composition according to claim 7, wherein the tar depleted liquid smoke composition has the phenols reduced from about 10 ° by weight to about 90% by weight. 12. The tar depleted liquid smoke composition according to claim 7, wherein after the contact, further includes concentrating the spent liquid humeral composition into tar by subjecting the composition of P1540 / 97HX liquid smoke exhausted in tar under vacuum evaporation, whereby the concentrated composition of liquid smoke exhausted in tar contains a higher amount of phenols than that contained in the liquid smoke composition of starting material. 13. A food casing treated with the tar depleted liquid smoke composition according to claim 7. 14. The food casing according to claim 13, wherein the wrapper is a fibrous wrapper treated by spraying the tar-laden liquid smoke onto a surface of the wrapper. 15. The food wrap according to claim 13, wherein the wrapper is a polymeric plastic film. 16. The food wrap according to claim 15, wherein the wrapper is a plastic, polymeric film, treated by spraying or spraying the tar-laden liquid smoke onto a surface of the polymeric plastic film. 17. The food wrap according to claim 15, wherein the wrapper is a polymeric plastic wrap, treated by mixing the tar-laden liquid smoke into the polymeric plastic film during the extrusion of the polymeric plastic film. P1540 / 97MX 18. The food wrap according to claim 15, wherein the film is of a polymer selected from the group consisting of ethylene-vinyl acetate, ethylene-acrylic acid, ethylene-methacrylic acid, linear low density polyethylene, linear polyethylene of very low density, and combinations thereof. 19. A protein food product treated with the tar depleted liquid smoke composition according to claim 7. 20. The protein food product according to claim 19, wherein the food product is selected from the group consisting of sausages, German sausages. , bologna sausages, meat rolls, hams and combinations thereof. P1340 / 97MX