Smoking device incorporating a breakable capsule, breakable capsule and process for manufacturing said capsule

The present invention relates to a smoking device comprising a frangible capsule, and more particularly a filter smoking device comprising such a capsule in its filter element.

In the present invention, the term "capsule" means a substance delivery system, said substance being hereinafter referred to as "cores that are encapsulated". The term "breakable capsule" refers to the capsule as defined above, in which the casing may be broken by pressure to release the core, and more specifically the casing may be broken under pressure exerted by the fingers of the smoker when the smoker wants to release the capsule core.

Several smoking devices containing a breakable capsule are known in the prior art (see for example WO 03/009711 A). Document US2004 / 0261807 describes a cigarette comprising a tobacco rod and a filter element connected to the tobacco rod, said filter having a cavity in which a capsule is placed. Said capsule contains an outer gelatin shell and an internal liquid composition containing fragrances. The purpose of US2004 / 0261807 is to allow a smoker to break a capsule while smoking a cigarette, allowing the capsule core to be released.

The gelatin capsule is a good storage capsule, but it is sensitive to moisture and may soften during smoking. This softening causes the gelatin sheath to lose its fragility, i.e. its ability to break under the pressure exerted by the fingers of the smoker when the smoker wants to release the capsule core. The prior art gelatin capsule typically has a very large deformation when placed in humid smoking conditions, which prevents the smoker from breaking it by the pressure of his / her fingers.

The breaking capacity is measured by the crushing force exerted to break the capsule and the capsule deformation when pressure is applied.

In the case of the present invention, the crushing forces in the dry state will not exceed 2.5 kp, and the crushing force greater than 2.5 kp appears to be too high to obtain the expected results.

Hence, there is a need to construct new capsules that have a crush strength of at most 2.5 kp and are able to retain their fragility even when exposed to moisture introduced into the filter during smoking.

The applicant has now found that the incorporation of selected hydrocolloids into the outer capsule shell and / or coating the outer shell with a moisture barrier layer results in the capsule retaining its ability to crack in the smoking device even after being exposed to moisture introduced by the smoker into said device for smoking.

The invention therefore relates to a smoking device comprising:

- receivers containing or capable of receiving smoking products, preferably tobacco,

- a filter element that is connected to the receiver, said filter containing at least one breakable capsule, and said capsule - has a crush strength of 0.5 to 2.5 kp,

- maintains the crush strength Cf from 0.5 to 2.5 kp and after subjecting it to a burning test, A has a deformation less than two-thirds of its diameter before breaking (a specialist in the field knows that 1 kp equals 9.8 N).

The receiver may be a cigarette rod in which the burning product is tobacco.

The initial crush strength of the capsules is measured before smoking by continuously applying a load vertically to one particle until rupture using a LLOYD-CHATILLON Digital Force Gauge measuring instrument, model DFIS 50, which has a capacity of 25 kg, resolution of 0.02 kg and accuracy + / - 0.15%. The force measuring device is attached to the stand, and the capsule is placed in the center of the plate, which moves upwards with a hand-threaded screw device. The pressure is then applied manually and the measuring instrument records the maximum force applied at each moment of capsule rupture (measured in kg or pounds). Breakage of the capsule results in the release of the core.

The A smoking test is carried out on a HEINR BORGWALDT RM 4 / cs smoking machine. The cigarette containing the breakable capsule is placed on the smoking machine in a standard starting position. The adjustable parameters are set as follows:

blast volume:

ml (as defined in the internationally standard method for the smoking machine) blowing period: 60 seconds blowing duration: 2 seconds sweeping time 1.8 seconds when blowing 1 second sweeping time after exhaustion

The test ends when the cigarette is completely smoked or after 7 or 8 puffs. The final crush strength Cf is measured after the smoking test A has been completed, following the same measurement procedure used to measure Ci.

The deformation of the capsule is also measured after smoking test A, just before breaking the capsule.

The deformation corresponds to the ratio between the diameter of the capsule and the width of the capsule when it is compressed to the breaking point.

According to one embodiment of the invention, the smoking device comprises a capsule which has a crush strength Ci from 0.6 to 2 kp, preferably from 0.8 to 1.2 kp, and maintains a crush strength Cf in the range from 0.6 to 2 kp, preferably in the range of 0.8 to 1.2 kp when subjected to a smoking test A.

According to another embodiment of the invention, the deformation of the breakable capsule in the smoking device at the break point before and after being subjected to the smoking test A is less than 2 mm, preferably less than 1 mm.

According to a preferred embodiment of the invention, the capsule is such that when it breaks, it creaks or makes an audible 'cracking'.

The capsule shell thickness is preferably 10-500 microns, preferably 30-150 microns, even more preferably 50-80 microns, the outer diameter of the capsule is 2 to 8 mm, preferably 3 to 5 mm, more preferably 3.4 to 4.8 mm and even more preferably 3.5 to 4.5 mm, and the ratio of capsule diameter to shell thickness is in the range of 10 to 100, preferably 50 to 70.

The shell comprises at least one hydrocolloid selected from gellan gum, agar, alginates, carrageenans, pectins, acacia, ghatti gum, pullulan gum, mannan gum or modified starch, alone or in a mixture thereof or in combination with gelatin. The amount of said hydrocolloid (s) present in the casing is

1.5 to 95% by weight, preferably 4% to 75% by weight, even more preferably 20% to 50% by weight based on the total dry weight of the casing. In a preferred embodiment, the hydrocolloid selected is gellan.

In a preferred embodiment of the invention, when used in combination with at least one other gelling agent, the weight ratio between gellan gum and other gelling agent (s) is from 80/20 to 20/80, preferably from 75/25 to 25/75 and even more preferably from 60/40 to 50/50.

According to another embodiment of the invention, the casing contains less than 80% gelatin, preferably less than 75% gelatin, and even more preferably less than 70% by weight gelatin, based on the total dry weight of the casing.

In an alternative embodiment of the invention, the capsule contains a moisture barrier coating. In this embodiment, the capsule shell is coated with at least one moisture barrier layer comprising at least one moisture barrier agent, dispersed in an organic solvent or in an aqueous solution or suspension. In this embodiment, the sheath may be made of any hydrocolloid, including gelatin, which may in this case be the only gelling agent for the sheath. However, it is preferred, even in the presence of a hydrophobic coating, that the casing also contain a certain amount of gellan or agar or carrageenan or alginates or acacia or pectin or pullulan or mannan gum sufficient to give it some moisture resistance. In this case, the casing may contain 1.5 to 95%, preferably 4% to 75% by weight, and even more preferably 20% to 50% by weight, based on the total dry weight of the casing, of at least one hydrocolloid selected from the group consisting of gellan , agar, carrageenan and pullulan gum. According to another embodiment of the invention, the coating of the coated capsule contains gellan or acacia or pectin or agar or alginates or carrageenan or ghatti or pullulan or mannan or a mixture thereof but does not contain gelatin.

barrier connection

According to a certain solution, the weight of the shell is 8-50%, preferably 8-20%, more preferably 8-15% by weight based on the total weight of the capsule.

The at least one moisture barrier agent is preferably at least one hydrophobic agent selected from those suitable for confectionery or pharmaceutical products, preferably selected from the group consisting of waxes, in particular carnauba wax, candelilla wax or beeswax, carbowax, shellac (in alcoholic or aqueous solution), ethyl cellulose, hydroxypropyl methyl cellulose, hydroxypropyl cellulose, latex composition, polyvinyl alcohol or even more preferably, at least one anti-moisture agent is ethyl cellulose or a mixture of ethyl cellulose and shellac.

According to another embodiment of the invention, the hydrophobic moisture barrier can be a combination of hydroxypropyl methylcellulose, plasticizer, microcrystalline cellulose and dye, or any other commercially available combination known under the name Seppifilm from SEPPIC or Opadry from COLORCON.

According to another embodiment of the invention, the hydrophobic moisture barrier is a film-forming gelling agent, preferably gellan gum alone.

The casing may contain a plasticizer, which may be maltitol, triacetin or polyethylene glycol or other polyalcohol with plasticizing properties and possibly one monoacid, diacid and triacid, preferably citric acid, fumaric acid, malic acid, etc. The amount of plasticizer is from 1% to 30 % by weight, preferably from 2 to 15% by weight, even more preferably from 3 to 10% by weight based on the total dry weight of the casing.

The casing may preferably contain a coloring agent, hereinafter at least one being glycerin, sorbitol, which facilitates the location of the capsule in the filter during the filter making process. The colorant is preferably selected from dyes and pigments.

The sheath composition may also contain fillers. By filler is meant any suitable material that can increase the percentage of dry material in the external liquid phase, and thus after co-extrusion in the obtained casing. Increasing the amount of dry material in the casing results in solidifying the casing and making it physically more resistant. The filler is preferably selected from the group consisting of starch derivatives such as dextrin, maltodextrin, cyclodextrin (alpha, beta or gamma) or cellulose derivatives such as hydroxypropyl methyl cellulose (HPMC), hydroxypropyl cellulose (HPC), methyl cellulose (MC), carboxymethyl cellulose (CMC), polyvinyl alcohol, polyols and mixtures thereof. The preferred filler is dextrin. The amount of filler in the casing is at most 98.5%, preferably from 25 to 95%, even more preferably from 40 to 80%, and even more preferably from 50 to 60% by weight based on the total weight of the dry casing.

The core of the casing contained in a smoking device according to the invention may comprise a mixture of materials or products that are lipophilic or partially soluble in ethanol, or a mixture of particles prepared as oil / water / oil emulsions.

According to a preferred embodiment of the invention, the core of the breakable capsule according to the invention represents 50 to 92% by weight of said capsule, preferably 80 to 92%, and even more preferably 85 to 92%.

The capsule core may contain one or more lipophilic solvents conventionally used in the food, pharmaceutical or cosmetics industry. In a preferred embodiment, these lipophilic solvents may be triglycerides, in particular medium chain triglycerides, in particular triglycerides of caprylic and capric acid, or mixtures of triglycerides such as vegetable oil, olive oil, sunflower oil, corn oil, peanut oil, oil from vine seeds, wheat germ oil, mineral oils and silicone oils. The amount of lipophilic solvent in the capsule core according to the invention is in the order of 0.01 to 90%, preferably 25 to 75% by weight, based on the total weight of the capsule.

The core may also contain molecules of one or more aromas conventionally used in the preparation of flavor or aromatic compositions, preferably aromatic, terpene and / or sesquiterpene hydrocarbons, in particular essential oils, alcohols, aldehydes, phenols, carboxylic acids and their various forms, aromatic acetals and ethers, nitrogen heterocycles, ketones, sulfides, disulfides and mercaptans, which may be aromatic or non-aromatic. The core may also contain one or more molecules or extracts for use in cosmetics.

The core may also contain one or more fillers used in aromatic emulsions. Mention should be made of damara, ester gum wood resins, sucrose acetate isobutyrate (SAIB) or brominated vegetable oils. The function of these loading agents is to adjust the density of the liquid core.

The core or sheath may also contain one or more sweeteners, which may be provided in the form of a solution or suspension in ethanol. Examples of suitable sweeteners may include, but are not limited to, aspartame, saccharin, NHDC, sucralose, acesulfame, neotame, etc.

The core may also contain one or more "sensory" flavors that give the mouth a refreshing or hot effect. Suitable refreshers may be, but are not limited to, menthyl succinate and its derivatives, and in particular Physcool® incorporated

A suitable means, but not only, ether that can be subjected to a device filter for permanent moisture.

According to the invention it is commercially available to the Applicant having a hot effect may be vanillyl ethyl.

Flavor solvent solubilization of the capsule core includes, but is not limited to, natural or synthetic flavors and / or flavors. Examples of suitable fragrances are fruit, confectionery, floral, sweet, woody fragrances. Examples of suitable flavors are vanilla, coffee, chocolate, cinnamon and mint.

According to one embodiment of the invention, the total weight of the capsule is 5-60 mg, preferably 10-50 mg, and even more preferably 20-40 mg.

The invention also relates to a breakable capsule suitable for smoking, which is essentially "substantially moisture stable" means that the outer shell or outer shell of the capsule has the ability to delay the breakdown of the capsule due to water introduced into the smoking device by the smoker.

The breakable capsule according to the invention consists of the core and shell described above, and said capsule has a crush strength of 0.5 to 2.5 kp and after being subjected to a smoking test A maintains a crush strength of 0.5 to 2 , 5 kp and deformation less than two thirds of its diameter.

According to the invention, the technical features of the breakable capsule in the smoking device described above are as such features of the breakable capsule of the invention.

a preferred embodiment of the capsule according to a seamless capsule obtained by the method described in the introduction

Under extrusion co-extrusion. The co-extrusion method is the synchronous extrusion of two liquids: an external hydrophilic liquid phase and an internal lipophilic liquid phase. The co-extrusion process involves three main stages: compound drop formation, shell solidification, and capsule accumulation. The drop of compound is a ball of liquid filling phase inside the shell phase. The liquid filling phase is here referred to as the "core". The casing phase is here referred to as "casing". Capsules of the invention can be made by any suitable co-extrusion process.

preferably produced by means of the device and EP 513603, by reference.

an embodiment of the invention after the co-extrusion step is a solidification step by keeping the capsules cold in order to ensure proper gelation of the casing, for example by contacting them with a cold bath.

The cold dip is preferably cold oil. By cold in the sense of this invention is meant a temperature from 1 to 15^aboutC, preferably from 2 to 10^aboutC, and even more preferably from 4 to 6^aboutC.

The capsules can then be centrifuged to remove excess oil, optionally washed with an organic solvent (such as acetone, ethyl acetate, ethanol, petroleum ether, etc.) also to remove excess oil, and dried.

with one embodiment of the invention, after the concurrent stage and optionally the stage

The capsules the disclosure method is here. According to some solidification, the capsules are centrifuged.

Optionally, the capsules are coextruded, centrifuged and immersed in a solution containing the curing agent in accordance with another embodiment of the invention.

The curing agent can also be either ethanol or an emulsion with any other anhydrous organic solvent, such as ethyl acetate or isopropanol, maintained at a temperature of 0 to 25^aboutC, especially from 10 to 20^aboutC.

The curing agent may alternatively or also be a calcium ion bath, e.g. calcium chloride, dicalcium phosphate or calcium sulfate or an acid bath containing calcium ions with a pH less than 5, preferably 3 to 4. Examples of acids may be adipic acid, acid fumaric, gluconic acid or gluconodelta-lactone. The calcium ion or acid bath is preferably at a temperature from 0 to 25^aboutC, especially from 10 to 20^aboutC.

The effect of the dipping step is the washing out of the oil remaining on the periphery of the capsule and the gradual strengthening of the casing, namely as a result of dehydration and osmotic balance.

According to one embodiment of the invention, after immersion, the capsules are dried in a stream of air at controlled temperature and humidity. The relative humidity of the drying air is from 20% to 60%, preferably from 30 to 50%, and the temperature of the drying air is from 15 to 60^aboutC, preferably from 35 to 45^aboutC.

According to one embodiment of the invention, the capsules can be obtained by the following method: co-extrusion of the outer and hydrophilic liquid phase on the one hand and the inner and lipophilic liquid phase and core components on the other hand, optionally optionally dipping the calcium ion baths thus obtained, or acid and then optionally drying.

According to another embodiment, the method according to the invention further comprises a coating step during which the outer barrier layer is applied to the capsules before said coating step is carried out by spinning the capsules in moisture.

preferably by immersing the capsules in a coating solution or by spraying the coating solution onto the capsules. Said coating step is preferably carried out after the drying step.

Capsules made by the process of the invention are essentially or perfectly spherical and very uniform in size.

The invention is further illustrated by means of the following examples, which should not be considered as limiting the scope of the invention, and they will be read with reference to the figures.

Figure 1 is a graph comparing the crush strength of a capsule that only has hydrocolloid gelatin, referred to herein as "gelatin capsule", and capsules of the invention.

Figure 2 is a graph comparing the crush strength of a capsule that only has hydrocolloid gelatin, referred to herein as "gelatin capsule", and capsules of the invention after smoking.

Examples

Example 1

Two types of capsules of the same size are prepared by coextrusion as disclosed in patent document EP 513603. The composition of the capsules of the present invention, designated 1004 / H11 (containing less than 80% gelatin and containing gellan gum) is given below in Table 1, and the composition of the prior art capsules containing 80% gelatin, designated 1004 / C30, is given below in Table 2.

Weight of each capsule: 20.56 mg, including shell weight: 3.68 mg (17.89%) Core weight: 16.88 (82.11%)

Table 1 - 1004 / H11 capsules

<td>Outer liquid phase, dry material: 15.5%</td><td>% / total weight</td><td>% / dry material</td>

<td>Gellan gum, Kelco F.</td><td> 1,800%</td><td> 11,62%</td>

<td>260A gelatin</td><td> 4,000%</td><td> 25,82%</td>

<td>sorbitol</td><td> 1,000%</td><td> 6,46%</td>

<td>Glycerine</td><td> 0,500%</td><td> 3,23%</td>

<td>Dextrin Cristal Tex</td><td> 8,000%</td><td> 51,65%</td>

<td>Sodium bicarbonate</td><td> 0,180%</td><td> 1,16%</td>

<td>Brilliant blue FD &amp; C # L</td><td> 0,010%</td><td> 0,06%</td>

<td>Process water</td><td> 84,510%</td><td></td>

<td></td><td> 100,000%</td><td> 100%</td>

<td>Inner liquid phase</td><td></td><td></td>

<td>Ethanol</td><td> 6,0000%</td><td></td>

<td>Mygliol</td><td> 65,5000%</td><td></td>

<td>Menthol</td><td> 28,5000%</td><td></td>

<td>altogether</td><td> 100,0000%</td><td></td>

Table 2 - 1004 / C30 capsules

<td>Outer liquid phase, dry material: 24.5%</td><td>% / total weight</td><td>% / dry material</td>

<td>260A gelatin</td><td> 19,800</td><td> 80,82</td>

<td>sorbitol</td><td> 2,7000</td><td> 11,02</td>

<td>Caramel dye</td><td> 2,000</td><td> 8,16</td>

<td>Process water</td><td> 75,500</td><td></td>

<td></td><td> 100,000%</td><td> 100%</td>

<td>Inner liquid phase</td><td></td><td></td>

<td>Ethanol</td><td> 5,0000</td><td></td>

<td>Mygliol 812S</td><td> 87,0000</td><td></td>

<td>Green mint flavor # 831661, supplied by MANE</td><td> 8,0000</td><td></td>

<td>altogether</td><td> 100,0000%</td><td></td>

<td colspan="3">The 1004 / C30 capsules and the 1004 / H11 capsules have a diameter of respectively 3489 +/- 40 and 3394 +/- 35 μιη</td>

The crush strength of the capsules is measured as follows using a LLOYD-CHATILLON Digital Force Gauge, model DFIS 50

Capacity = 25 Kgf (501b)

Resolution = 0.02 KgF (0.051b)

Accuracy = +/- 0.15%

Sampling rate = 1000 times per second

Methodology:

The y force measuring device attaches to the stand. The capsule is placed in the center of the plate, which moves upwards with a hand screw device. Then the pressure is manually applied and once the capsule wall breaks, the measuring instrument records the maximum force applied before breaking (measured in kg or pounds). A sample of 10 to 20 capsules is measured.

The result is as follows:

<td>capsules</td><td>Crushing Strength (Kp)</td><td>Deviation standard</td>

<td>1004 / C30</td><td> 4, 60</td><td> 1, 11</td>

<td>1004 / H11</td><td> 1,70</td><td> 0,26</td>

<td colspan="3">The results are also shown in Fig. 1</td>

Example 2

The capsules are prepared according to Example 1. The core content is about 89% and the shell content about 11%, which corresponds to a dry shell thickness of about 50 microns. The capsules are then dried to yield

3.5 mm spherical capsules with a crush strength of 1 kp. The average weight of a capsule is about 20 mg.

Capsules according to the prior art containing gelatin (ref. 1004 / C1), including 72% gelatin in the form of a sol hydrocolloid, and the capsule described in Example 1 above are introduced into the cavity filter of a cigarette. The crush strength value Ci is measured for both capsules according to the method described herein.

The resulting cigarettes are then smoked on a smoking test machine (smoking test A) according to the international standard procedure.

Capsule-containing filters are collected and capsules removed from the filter to measure the crush strength Cf after the smoking process.

In the case of gelatin capsules, the capsules melted in the filter during the smoking process and the crush strength values ​​could not be measured. The capsules deform and cannot break when pressed on. Conversely, when you push the filter, the gellan-containing capsule always breaks.

Weight of each capsule: 20.57 mg, including sheath weight: 2.37 mg (11.51%) Core weight: 18.20 mg (88.49%)

Instrumentation:

HEINR BORGWALDT RM 4 / cs Smoking Test Machine Cigarettes containing breakable capsules are placed on the smoking test machine as a standard position for other types of analysis. The adjustable parameters are set as follows: blast volume:

blowing period:

blowing time: sweeping time when blowing sweeping time ml (as specified in the internationally standard method for the smoking machine) seconds seconds

1.8 seconds a second after running out

Crush resistance is measured by the procedure described above in Example 1.

Capsules 1004 / C1

<td>Inner phase dry material:</td><td colspan="3">liquid, 25.0%</td>

<td>Ingredients</td><td></td><td> %</td><td>% dry material u</td>

<td>Gelling agent</td><td>gelatine</td><td> 18,000%</td><td> 72,00%</td>

<td>plasticizer</td><td>sorbitol</td><td> 4,000%</td><td> 16,00%</td>

<td>extender</td><td>calcium carbonate</td><td> 1,000%</td><td> 4,00%</td>

<td>Dye</td><td>caramel</td><td> 2,000%</td><td> 8, 00%</td>

<td>Solvent</td><td>water</td><td> 75,000%</td><td></td>

<td>altogether</td><td></td><td> 100,000%</td><td> 100%</td>

<td colspan="4">Inner liquid phase</td>

<td>Name</td><td></td><td> %</td><td></td>

<td>Center solubilizing</td><td>ethanol</td><td> 5,0000%</td><td></td>

<td>Carrier</td><td>miglyol</td><td> 87,0000%</td><td></td>

<td>Aroma</td><td>mint flavor # 831661, supplied by MANE</td><td> 8,0000%</td><td></td>

<td></td><td>altogether</td><td> 100,0000%</td><td></td>

The results are as follows:

<td>capsules</td><td>Crush strength you</td><td>Crush strength Cf</td>

<td>1004 / C1</td><td>1.70 kp</td><td>cannot be measured (the capsules have melted)</td>

<td>1004 / H11</td><td>1.2 kp</td><td>1.2 kp</td>

Capsules of the prior art were no longer breakable after smoking.

Example 3

Capsules are prepared according to Example 1 using the following composition:

1004 / H6 capsules

<td colspan="7">Outer liquid phase Dry material: 16.5%</td>

<td colspan="2">Ingredients,%% / dry material</td><td colspan="2"></td><td colspan="2"> %</td><td>% / dry material</td>

<td colspan="2">Gelling agent 1</td><td colspan="2">gellan gum</td><td colspan="2"> 2,200%</td><td> 13,33%</td>

<td colspan="2">Gelling agent 2</td><td colspan="2">gelatine</td><td colspan="2"> 4,000%</td><td> 24,24%</td>

<td colspan="2">extender</td><td colspan="2">CT648 dextrin</td><td colspan="2"> 10,000%</td><td> 60,61%</td>

<td colspan="2">Acid or salt</td><td colspan="2">bicarbonate sodium</td><td colspan="2"> 0,200%</td><td> 1,21%</td>

<td colspan="2">Dye</td><td colspan="2">brillant blue FD &amp; C # 1</td><td colspan="2"> 0, 10%</td><td> 6, 61%</td>

<td colspan="2">Solvent</td><td colspan="2">osmosis water</td><td colspan="2"> 83,500%</td><td></td>

<td colspan="2">altogether</td><td colspan="2"></td><td colspan="2"> 100,000%</td><td></td>

<td colspan="7">Inner liquid phase</td>

<td>Ingredients</td><td colspan="2"></td><td colspan="2"> %</td><td colspan="2"></td>

<td>Center solubilizing</td><td colspan="2">ethanol</td><td colspan="2"> 5,0000%</td><td colspan="2"></td>

<td>Carrier</td><td colspan="2">Miglyol 812S</td><td colspan="2"> 90,0000%</td><td colspan="2"></td>

<td>Aroma</td><td colspan="2">mint flavor</td><td colspan="2"> 5,0000%</td><td colspan="2"></td>

<td></td><td colspan="2">altogether</td><td colspan="2"> 100,0000%</td><td colspan="2"></td>

Weight of each capsule: 20.96 mg, including shell weight: 3.72 mg (17.74%) Core weight: 17.24 mg (82.26%)

One capsule was introduced into the cigarette filter cavity. Crushing strength Ci was measured by the procedure described above in Example 1.

Ci = 0.80 +/- 0.20 Kp

The cigarette was then subjected to Test A, as described above in Example 2, for 8 puffs. After 8 puffs, the capsule burst with an audible 'pop'.