Microsoft Word C044876e doc Reference number ISO 15592 3 2008(E) © ISO 2008 INTERNATIONAL STANDARD ISO 15592 3 Second edition 2008 12 15 Fine cut tobacco and smoking articles made from it — Methods of[.]
General
This section of ISO 15592 identifies two primary classes of wrappers, designated as A and B It establishes a standard wrapper for each class to be utilized in determining the Non-Food Direct Product Material (NFDPM) of fine-cut tobacco samples, as outlined in Clause B.2.
Manufacture of standard tubes from wrappers
The laboratory device for producing smoking articles requires wrappers to be supplied as tubes, which may need to be formed before use, although they are commercially available It is essential to utilize cylindrical formers with diameters of 5.0 mm and 7.0 mm as needed.
Standard wrappers from both classes will be prefabricated into 70 mm long tubes with an internal diameter of 5.2 mm, using a wrapper that does not exceed 20.0 mm in width.
Further standard wrappers from both classes will be prefabricated into 70 mm long tubes with an internal diameter of 7.2 mm The width of the wrapper used for these tubes shall not exceed 26.0 mm.
Determination of standard tube mass
Weigh 10 tubes made in accordance with 7.2.2 and 7.2.3 and conditioned in accordance with ISO 15592-2
Determine the average mass of the tube This mass is required to determine the target average mass of the finished fine-cut smoking article
8 Making of the fine-cut laboratory smoking articles
General
Four types of FCSAs (see 3.12) shall be made from each laboratory sample (see 3.10) of fine-cut tobacco
If the tobacco blend to be tested contains tobacco of high filling value, the masses of the tobacco shall be adjusted appropriately
At the time of developing this section of ISO 15592, there was no universally accepted definition for the filling value or firmness of smoking articles Nevertheless, various devices for measuring these parameters are commercially available and widely utilized within the tobacco industry.
To control the firmness of smoking articles made from tobacco, differences in filling value can be accounted for For instance, if a specific mass of tobacco typically occupies volume A, but a sample occupies A + B, the mass should be adjusted by multiplying it by the factor A/(A + B) Any adjustments made to the mass of tobacco must be noted in the test report.
The laboratory fine-cut tobacco sample shall be conditioned in accordance with ISO 15592-2.
Specification of the FCSAs to be made
The four types of laboratory FCSAs shall be made as follows a) Article 1:
400 mg of conditioned fine-cut tobacco shall be enclosed in a wrapper conforming to standard wrapper A
(see Clause B.2) and made into a tube specified in 7.2.2
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`,,```,,,,````-`-`,,`,,`,`,,` - © ISO 2008 – All rights reserved 7 b) Article 2:
400 mg of conditioned fine-cut tobacco shall be enclosed in a wrapper conforming to standard wrapper B (see Clause B.2) and made into a tube specified in 7.2.2 c) Article 3:
750 mg of conditioned fine-cut tobacco shall be enclosed in a wrapper conforming to standard wrapper A (see Clause B.2) and made into a tube specified in 7.2.3 d) Article 4:
750 mg of conditioned fine-cut tobacco shall be enclosed in a wrapper conforming to standard wrapper B (see Clause B.2) and made into a tube specified in 7.2.3.
Preparation and selection of the FCSAs for test
To ensure compliance with the smoking plan, utilize the making device (5.3) to produce an adequate quantity of smoking articles, accounting for potential rejections due to damage or quality issues It is essential to identify the end of the FCSA connected to the making device for proper insertion into the article holder (refer to 9.3.3).
To ensure consistency in the physical properties of FCSAs, careful selection of samples for smoking is essential This selection process is based on mass, where each FCSA is weighed individually post-manufacture Any FCSA that deviates from the target mass of the tobacco plus wrapper by more than 20 mg will be discarded The manufacturing process can involve weighing a single portion of tobacco, creating the article, and then verifying its weight, or weighing multiple tobacco portions quickly, producing the articles, and selecting them based on their weight.
8.3.3 The mean mass of the 22 FCSAs after reconditioning shall be within ± 10 mg of the target mass of the tobacco plus wrapper mass (see 9.5)
8.3.4 If a selection by mass is necessary, the selection shall not be considered as a method of reducing the number of articles to be smoked.
Special precautions
The tobacco for FCSAs, as outlined in section 8.2, is conditioned at (22 ± 2) °C and (75 ± 3) % RH according to ISO 15592-2 However, the preparation of FCSAs typically occurs under different temperature and humidity conditions, which can alter the tobacco's moisture content To mitigate this issue, it is essential to maintain the tobacco as close as possible to the specified conditions until it is used This can be achieved through two methods.
Only the necessary amount of tobacco should be extracted from the conditioning chamber to produce a limited number of articles, ensuring that the tobacco remains in optimal condition throughout the manufacturing process.
2) conditioned tobacco shall be placed in separate sealed containers such that the tobacco in one container is likely to remain in condition during the making process
The number of articles that can be produced while maintaining the quality of tobacco varies based on the operator's experience and the specific conditions in which the articles are created.
For optimal results, it is advised to limit the smoking session to one hour Before smoking, it is essential to assess the condition of the tobacco, ensuring it meets the weight requirements outlined in section 9.5.
In addition, it is necessary to ensure that the FCSAs do not change in weight whilst in the smoking room
A smoke run with a linear smoking machine can last up to 2 hours, during which the weight of the FCSAs may fluctuate if stored in unsealed containers To maintain quality, it is essential to keep only the necessary items in sealed containers until they are ready for loading into the smoking machine Typically, a rotary machine requires twenty items plus two spares, while a linear machine usually needs five items, with two spares stored separately.
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9 Determination of total particulate matter
Symbols
The following symbols are used in 9.2 and 9.6:
N is the number of FCSAs of a given group to be smoked, resulting from sampling at one point in time or from a sub-period sample;
C is a multiplying factor, represented by value W1, which accounts for losses incurred from damage or selection processes occurring between the initial sampling and the smoking phase The variable n denotes the number of replicate determinations of total particulate matter, while q indicates the number of FCSAs smoked into the same trap.
Q is the total number of FCSAs (laboratory smoking articles, see 3.12).
Preparation of the fine-cut smoking articles for smoking
If N FCSAs of a given group are to be smoked, C × N FCSAs shall be prepared from Q FCSAs for conditioning and butt and insertion depth marking
The multiplier \( C \) is typically set at a minimum of 1.3 to ensure additional FCSAs are available in the event of damage and to accommodate any optional tests that may be needed (refer to section 9.5) If a selection process is required, the value of \( C \) may need to be increased, potentially reaching 2.0, depending on the specifics of the selection criteria.
For accurate results, a sample size of 100 to 200 is typically necessary This requirement may increase significantly if the sample exhibits high variability Conversely, the sample size can be decreased when N pertains to a sub-period sample.
N shall never be less than forty when twenty FCSAs are smoked per trap, or less than twenty when five FCSAs are smoked per trap
At least forty FCSAs are required to be smoked when twenty FCSAs are smoked per trap, thus providing replicate analyses and data replication
The N FCSAs designated for smoking will undergo testing in n = N/q determinations when q FCSAs are smoked into a single trap It is essential that these n determinations represent different test portions of the sample whenever possible.
Selection of each test portion will depend upon the form of the test sample
9.2.2 Selection of test portions from a bulk of Q FCSAs
For each group of smoking articles, the test sample is in the form of a single bulk, consisting of Q FCSAs
Select at random C × N FCSAs so that every FCSA has an equal probability of being selected
To ensure accurate testing of laboratory smoking articles, it is essential to reserve a duplicate set of n test portions when the sample size is sufficiently large (greater than 2 C × N) This approach allows for the parallel selection of both the test portion and its duplicate, enhancing the reliability of the results.
Marking the insertion depth and butt length
The standard insertion depth for FCSAs made as in 8.3.1 shall be 13 mm ± 0,5 mm
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The standard butt length for FCSAs made as in 8.3.1 shall be 27 mm
9.3.3 Marking the insertion depth and butt length
The end of the tube connected to the making device should be positioned in the holder To assist with the insertion depth and butt length, mark it on the lap for easy reference.
Before conditioning, it is essential to mark the insertion depth and butt length on the FCSAs It is advisable to use a fine, soft-tipped marker to draw two thin lines The first line should indicate the insertion depth, accurate to within 0.5 mm from the butt end of the FCSAs, reflecting the standard depth of insertion The second line should denote the standard butt length, also accurate to 0.5 mm from the butt end, specific to the respective FCSA group.
When marking, it is crucial to handle the FCSAs carefully to prevent any damage If any FCSAs are accidentally torn, punctured, or identified as defective during the marking process, they must be discarded and replaced with spare FCSAs from the test portion.
When using a smoking machine that allows for pre-setting butt lengths in accordance with section 9.3.2, it is unnecessary to mark the butt lengths on the FCSAs themselves.
Conditioning and testing conditions
Condition all the article test portions in the conditioning atmosphere specified in ISO 15592-2 [temperature
(22 ± 2) °C and relative humidity (75 ± 3) %] for a minimum of 72 h and a maximum of 10 d
For optimal preservation, laboratory samples and smoking articles should be stored in their original packaging or in airtight containers if they need to be kept for more than 10 days Ensure the containers are just large enough to hold the samples securely.
The testing atmosphere in the laboratory where the smoking is to be carried out shall be in accordance with ISO 15592-2 [temperature (22 ± 2) °C and relative humidity (60 ± 5) %]
Transfer the article test portions to the smoking location in airtight containers just large enough to contain the portions (see 8.4).
Preliminary tests before smoking
The average mass of the FCSAs from each test portion must be verified through weighing, ensuring that each average mass does not exceed the combined mass of the wrapper and specified tobacco mass by more than 10 mg.
IMPORTANT — It is important that the instructions given in 8.4 be observed, otherwise the average mass is likely to exceed this specification
The test report must include the following data: a) the total length of the FCSA wrapper measured to the nearest 0.5 mm; b) the nominal diameter, noting that due to the soft and irregular shape of FCSAs, pressure-based or pneumatic diameter tests should be avoided; instead, the diameter should be measured using slit wrapper tubes with a millimeter scale; c) the draw resistance of an FCSA must be determined according to ISO 6565, ensuring the holder specified in section 5.2 is free of leakage, which can be verified using the leakage tester provided with the smoking machine; d) the average mass of the conditioned FCSAs selected for smoking, expressed in milligrams per FCSA; e) the water content of the tobacco in the conditioned FCSA, reported as a mass fraction and determined in accordance with ISO 6488.
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Smoking and collection of particulate matter
Choose a smoking plan; examples of plans are given for information in Annex A of ISO 4387:2000
The plan shall show the number of FCSAs to be smoked into each trap, q, and the number in the test sample for conditioning sample (C × N)
9.6.2 Preparation of smoke traps and FCSA holders
For all operations, the operator shall prevent contamination from the fingers by wearing gloves (5.11) of a suitable material
Insert filter discs conditioned in the test atmosphere as specified in ISO 15592-2 for a minimum of 12 hours into their holders, ensuring the rough side faces the incoming smoke After assembly, verify that the discs are properly fitted and secure the sealing devices (end caps) Weigh the assembled smoke traps to the nearest 0.1 mg To account for potential water absorption by the smoke traps and solvent, determine a sample blank value by treating additional smoke traps (at least 2 per 100 FCSAs) in the same manner as the smoke collection process.
9.6.3 Setting up the smoking machine
A smoking machine complying with ISO 3308 shall be used except for the holder (5.2)
If necessary, replace any protective filters on the machine Switch on the machine and allow it to warm up on automatic cycling for at least 20 min
With the machine warmed up, check that the puff duration and puff frequency on each channel are in accordance with the standard conditions
A timer (5.5) shall be used to measure the period of time which elapses between the triggering operations which begin and end a puffing action of the smoking machine
Measure the period of time which elapses between the triggering operations which begin successive puffing actions of the smoking machine, thus determining the puff frequency
The displacement of a bubble in a soap bubble flow meter directly measures puff volume and checks for system leaks It should be connected to a standard pressure drop device of 1 kPa ± 5% to the FCSA holder of the smoking machine channel being tested Prior to conducting a series of measurements, the instrument must be wetted twice with a detergent solution and allowed to drain Measurements should continue until the results are repeatable.
The bubble flow meter shall contain a mass fraction of 15 % aqueous solution of a surface active agent
NOTE Teepol L ® 1) has been found to be satisfactory
Teepol L, a product offered by Shell, is mentioned for user convenience in ISO 15592, but this does not imply ISO's endorsement of the product Users may opt for equivalent products that demonstrate comparable results.
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Fit the smoking trap and FCSA holders onto the machine, ensuring the latex sleeve on each FCSA holder operates correctly by applying the vacuum source to confirm it opens completely Attach a suitably sized plastic insert for the FCSAs to the tube connected to the soap bubble flow meter Prepare the flow meter by wetting the inside of the tube with a detergent solution above the top graduation mark Connect the indicator to the FCSA holder in channel 1 to determine the puff volume, adjusting it to (35 ± 0.3) ml if necessary, and repeat this process for all remaining channels.
Continue repeating the measurements until the desired precision is achieved If more than three replicates are needed, ensure to replace the filter disc before smoking, reweigh the smoke trap, and verify the puff volume with the new filter disc installed.
Measure the temperature and relative humidity of the air surrounding the smoking machine and note the atmospheric pressure
Insert the conditioned FCSAs into the holders at the standard depth to prevent wrapper deformation and minimize leaks Discard any FCSAs with visible defects or damage incurred during insertion, and replace them with spare, conditioned FCSAs.
To ensure optimal performance, position the FCSAs so that the angle between their longitudinal axis and the horizontal plane is minimized, aligning the FCSA axis with the channel axis Adjust each FCSA's position so that the puff termination device activates when the burning coal reaches the butt mark When using a 100% cotton thread (48 ± 4 tex) to terminate smoking at the butt mark, ensure that the cotton just touches the FCSA without altering its positioning.
At the start of the smoking process, reset the puff counters and ignite each FCSA using a non-flame method If re-lighting is needed, utilize a hand-held electrical lighter Once the butt mark is reached, remove the burning coal and record the final puff counter readings After completing the smoking, allow the FCSA butt to remain in place for at least 30 seconds to facilitate the deposition of any residual smoke in the trap.
Avoid disturbance of the smoking by artificial removal of ash Allow the ash to fall naturally into the ashtray
If necessary, a new FCSA will be added, and the smoking process will continue until the specified number of FCSAs, as outlined in the smoking plan, has been collected in the smoke trap Following this, the assessment of total particulate matter will commence as detailed in section 9.7.
Removal of smoke traps and FCSA holders
To ensure safety, wear gloves (5.11) while removing the smoke traps from the smoking machine If needed, detach the FCSA holder from the smoke trap and seal both the front and back apertures with the sealing devices (5.10).
To prevent contaminants from the FCSA holder from reaching the filter disc, it is advised to remove the holder while keeping the smoke trap oriented with its FCSA-facing side downwards.
After smoking, weigh the smoke traps to the nearest 0.1 mg and inspect the back of each filter disc for any brown stains that may indicate overloading or damage Discard any discs that show such stains or signs of damage.
Glass fibre filter discs with a diameter of 44 mm can retain up to 150 mg of total particulate matter (TPM), while 92 mm diameter discs can hold 600 mg of TPM If the TPM mass is exceeded during smoking, the results become invalid, necessitating a repeat smoking test with a reduced number of FCSAs and an adjusted calculation for the decreased quantity smoked.
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Calculation of total particulate matter
The TPM content, m TPM , for each channel, expressed in milligrams per FCSA, is given by Equation (1):
The mass of the smoke trap before smoking, denoted as \( m_0 \) in milligrams, is subtracted from the mass after smoking, represented as \( m_1 \) in milligrams, to determine the amount of smoke collected This difference is related to the number of FCSAs smoked into the trap, denoted as \( q \).
Treatment of total particulate matter for the determination of water and nicotine
To properly handle the smoke trap, first remove the sealing devices while wearing gloves (5.11) Next, open the trap and use forceps to extract the filter disc Carefully fold the disc twice, ensuring that the total particulate matter is folded inwards, and only handle the edges with forceps and gloved fingers Finally, place the folded disc into a suitable dry flask, with a maximum capacity of 150 ml.
For 44 mm discs, use a maximum of 250 ml for 92 mm discs Clean the inner surface of the filter holder front with two separate quarters of an unused conditioned filter disc and place them into the flask Add solvent (propan-2-ol with internal standards for nicotine and water determinations) to the flask, using 20 ml for 44 mm discs or 50 ml for 92 mm discs Refer to ISO 10315 and ISO 10362-1 for guidelines.
Immediately stopper the flask and gently shake it on an electric shaker for a minimum of 20 minutes, taking care to prevent the disintegration of the disc Adjust the shaking duration to guarantee complete extraction of nicotine and water from the particulate matter.
Follow the same procedure with each of the blank smoke traps used for the determination of water
9.9.2 Water determination and calculation of DPM
Carry out the water determination of the solution in each flask in accordance with ISO 10362-1
The DPM content, m DPM , for each trap, expressed in milligrams per FCSA, is given by Equation (2):
DPM TPM W m = m −m (2) where m TPM is the TPM content, in milligrams per FCSA; m W is the water content in the TPM, in milligrams per FCSA
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9.9.3 Nicotine determination and calculation of NFDPM
Carry out the nicotine determination of the solution in each flask in accordance with ISO 10315
The NFDPM content, m NFDPM , for each trap, expressed in milligrams per FCSA, is given by Equation (3):
NFDPM DPM N m = m −m (3) where m DPM is the DPM content, in milligrams per FCSA; m N is the nicotine content in the TPM, in milligrams per FCSA
General
The test report must detail the methodology and results, including any operating conditions not specified in ISO 15592 or considered optional, as well as any factors that may have affected the outcomes It should provide all necessary information for the complete identification of the sample, and if relevant, include the information outlined in sections 10.2 to 10.5.
Characteristic data about the fine-cut tobacco
When identifying commercial fine-cut tobacco, it is essential to include the manufacturer's name and country of manufacture, the brand and sub-brand names, the pouch number of the sampled product, any marks on the tax stamp, and the printed smoke yields, if available.
Sampling
The article should include essential details such as the type of sampling procedure, the date of sampling, the location of purchase or sampling, the kind of sampling point, the specific sampling point (for instance, the address of the retail outlet or machine number), and the number of FCSAs present in the laboratory sample.
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Description of test
The report must include specific details such as a reference to ISO 15592-3:2008, the date of the test, the type of smoking machine and smoke trap used, the total number of FCSAs smoked within the group, the number of FCSAs smoked into each smoke trap, the butt length, and the temperature and relative humidity in the smoking room during the test Additionally, it should note the atmospheric pressure in kilopascals if it falls outside the specified limits.
Test results
The presentation of laboratory data is influenced by its intended use and the precision level of the laboratory Confidence limits must be calculated and reported based on the raw laboratory data prior to any rounding.
For each variety of fine-cut tobacco articles, specific data must be provided, including: a) the average length of FCSA wrappers in millimeters (to the nearest 0.1 mm); b) the butt length smoked in millimeters; c) the average diameter of FCSAs in millimeters (to the nearest 0.1 mm); d) the average draw resistance of conditioned FCSAs in pascals (to the nearest 10 Pa); e) the average mass of conditioned fine-cut smoking articles per FCSA in milligrams; f) the average mass of the wrapper per FCSA in milligrams; g) the water content of the tobacco in conditioned FCSAs as a mass fraction in percent (referencing ISO 6488); h) the average number of puffs per FCSA for each channel (to the nearest 0.1 puff); i) the TPM content per FCSA for each channel in milligrams (to the nearest 0.1 mg) and the average per FCSA (to the nearest 1 mg); j) the DPM content per FCSA for each channel in milligrams (to the nearest 0.1 mg) and the average per FCSA (to the nearest 1 mg); k) the nicotine content per FCSA for each channel in milligrams (to the nearest 0.01 mg) and the average per FCSA (to the nearest 0.1 mg); l) the NFDPM content per FCSA for each channel in milligrams (to the nearest 0.1 mg) and the average per FCSA (to the nearest 1 mg); m) any issues related to re-lighting or other smoking problems with FCSAs.
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Expression of test results
The findings on NFDPM and nicotine from the four articles mentioned in section 8.2 will be presented in a matrix format, illustrating the impact of fine-cut tobacco mass and wrapper specifications, as exemplified in Table 1.
Table 1 — Example of the data matrix
NFDPM Nicotine NFDPM Nicotine Tobacco mass Diameter mg/FCSA mg/FCSA mg/FCSA mg/FCSA
An international collaborative study on the precision of the method was conducted in 2001 It involved
20 laboratories, 2 wrappers and 3 blends of tobacco A monitor test piece was also analysed
The article discusses three distinct tobacco blends: a finely cut fire-cured tobacco blend primarily sold in the Netherlands; a coarser blend of equal parts fire- and flue-cured tobaccos, mainly available in Europe; and a blend of flue-cured tobacco with a small amount of air-cured tobacco, which is more coarsely cut and primarily sold in Scandinavian countries.
The monitor test piece, as outlined in ISO 16055, is a filter-tipped cigarette produced under stringent manufacturing conditions This test piece is utilized to ensure the stability of analytical processes when operated with a smoking machine.
In normal and correct operation, the difference between two single results obtained from matched blend samples by the same operator using the same apparatus will exceed the repeatability limit, r, no more than once in 20 cases within the shortest feasible time interval.
In the normal and correct operation of the method, single results from matched blend samples reported by two laboratories are expected to differ by more than the reproducibility limit, R, in no more than 5% of cases.
Data analysis provided estimates for NFDPM and nicotine, as detailed in Tables 2 and 3 To calculate the values of r and R, the mean yield from smoking was used as the defining test result.
20 fine-cut smoking articles or 20 monitor test pieces in a single run
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Table 2 — Estimates given by data analysis for NFDPM Blend Tobacco mass mg
Value NFDPM mg/FCSA made with wrapper A
NFDPM mg/FCSA made with wrapper B Mean 9,4 12,1 r 1,41 1,61
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Table 3 — Estimates given by data analysis for nicotine Blend Tobacco mass mg
Value Nicotine mg/FCSA made with wrapper A
Nicotine mg/FCSA made with wrapper B Mean 1,00 1,25 r 0,136 0,173
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Summary of report of the CORESTA task force on roll-your-own
This report provides details of the technical studies carried out by the task force established by CORESTA, to meet the following defined objectives (see reference [1]):
⎯ to document how roll-your own (RYO) smokers in different countries make their cigarettes;
⎯ to establish the effects of materials and cigarette design on particulate matter and nicotine yields of RYO cigarettes;
⎯ to make recommendations to the Smoke Study Group on the relevance to the consumer of proposed standard procedures;
⎯ to consider the establishment of a recommended method to give meaningful comparisons among fine-cut tobaccos or fine-cut smoking articles (FCSAs)
The term "fine-cut smoking article" was established early by the task force to differentiate it from the manufactured product known as "cigarette."
The project successfully achieves the first three objectives and lays the groundwork for a standardized method aligned with the fourth objective Below are the key findings and conclusions derived from the work.
Consumer practices for smoking articles vary significantly across different markets and even among individuals There are notable differences in mass, diameter, shape, and wrapper types The decisions consumers make play a vital role in influencing smoke yields.
Current national procedures for measuring non-filtered dry particulate matter (NFDPM) and nicotine yields from fine-cut smoking articles (FCSAs) are insufficient, failing to adequately inform consumers about the impact of their choices in fine-cut tobacco products.
Consumers need to be informed about how their choices impact smoke yields A straightforward method to achieve this is through a 2 by 2 matrix that illustrates the effects of tobacco quantity and the type of wrapper used Additionally, a classification system for wrappers is proposed and endorsed.
Devices have been developed to create satisfactory articles from fine-cut tobaccos and wrapper materials, accommodating two different diameters for varying tobacco masses These devices have been successfully evaluated, producing articles that demonstrate sufficient consistency for a standard method However, the ends of these articles lack the firmness and cylindrical shape of manufactured cigarettes, which is a significant factor contributing to the high variability observed in smoking test results.
Laboratory-made smoking articles exhibit significant variability in smoke yields, even when produced under controlled conditions, necessitating careful attention to the smoking procedures used In contrast, consumer-made articles demonstrate even greater variability, highlighting the need for extra caution during the smoking process.
Most participating laboratories reported practical difficulties, experiencing significant variability when smoking FCSAs with the Labyrinth Seal holder as per ISO 3308 A newly developed alternative holder effectively minimizes this variability, particularly when utilized with a deeper insertion depth to accommodate the irregular and under-filled ends of the article.
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Even with the improvements established by the work set out in this report, variability is inevitably greater for data from laboratory-produced FCSAs than that from manufactured cigarettes
This report does not specify the necessary level of variability for establishing satisfactory standards for FCSAs intended for regulatory use CORESTA believes that input from regulatory laboratories is essential and is prepared to share its documented experimental data with ISO to facilitate the completion of the method under its guidance.