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Protocol - Physical Properties of Tobacco Products - Smokeless Tobacco

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Description

This is a Federal Register Notice laboratory measurement protocol providing instructions for measuring the total moisture content within smokeless tobacco products (i.e., dry snuff, moist [wet] snuff, moist [wet] snuff portion packs, plug, twist, loose leaf, dry snuff portions packs, snus, snus portion packs, and pellet or compressed).

Specific Instructions

N/A

Availability

Available

Protocol

Sample Preparation

There are ten different categories of commercial smokeless tobacco products:

1) Dry snuff;

2) Moist (wet) snuff;

3) Moist (wet) snuff portion packs;

4) Plug;

5) Twist;

6) Loose leaf;

7) Dry snuff portion packs;

8) Snus;

9) Snus portion packs; and

10) Pellet or Compressed.

Because of their physical characteristics, some of the ten product categories must be ground (whole or in part) before nicotine, total moisture, and pH analyses can be conducted. The objective of grinding the samples is to obtain a homogeneous sample with particles measuring approximately 4 mm. Grinding to achieve this particle size should take no more than 3 minutes. To ensure proper grinding and an adequate amount of the ground sample for analysis, the minimum sample size of all commercial products to be ground should not be less than 100 grams.

To ensure precision of analyses for nicotine, total moisture, and pH, the samples that require grinding should be ground using a Robot Coupe Model RSI 2V Scientific Batch Processor or its equivalent. This is a variable speed (0 to 3,000 RPM) processor. The variable speed motor is required to ensure proper grinding of the tobacco tissues (and in the case of pH determination, the portion pack). Elevated temperatures can result in moisture loss and an underestimated value for moisture content. Hence, care must be taken during grinding to avoid elevated temperatures. The bowl should be cleaned after each grinding to obtain accurate results. Freeze- or cryo-grinding is also an acceptable grinding method.

1) Dry snuff: Dry snuff samples do not need to be ground since the product is a powder. The sample must be thoroughly mixed before weighing for nicotine, total moisture, and pH analysis.

2) Moist (wet) snuff: Moist (wet) snuff samples do not need to be ground. The sample must be thoroughly mixed before weighing for nicotine, total moisture, and pH analysis.

3) Moist (wet) snuff portion packs: The tobacco contents of the moist (wet) snuff portion packs do not need to be ground for nicotine, total moisture, or pH analysis.

4) Plug tobacco: Break or cut apart plugs and add in portions to grinder at 2,000 RPM. Reduce RPM or stop grinding if sample bowl becomes warm. Pulse the Robot Coupe, when needed, to complete grinding. Grind samples until approximately 4 mm in size. The total grinding time should be no more than 3 minutes.

5) Twist tobacco: Separate twists, add to grinder, and grind at 2,000 RPM. Reduce RPM or stop grinding if sample bowl becomes warm. Continue grinding until sample particles are approximately 4 mm in size. The total time for grinding should be no more than 3 minutes.

6) Loose leaf: Grind in the same manner as described in 4 and 5 to obtain product with particle size of approximately 4 mm.

7) Dry snuff portion packs: The tobacco contents of the dry snuff portion packs do not need to be ground for nicotine, total moisture, or pH analysis.

8) Snus: Snus samples do not need to be ground since the product is a powder. The sample must be thoroughly mixed before weighing for nicotine, total moisture, and pH analysis.

9) Snus portion packs: The tobacco contents of the snus portion packs do not need to be ground for nicotine, total moisture, or pH analysis.

10) Pellet or compressed: Break apart compressed tobacco pellets and add in portions to grinder at 2,000 RPM. Reduce RPM or stop grinding if sample bowl becomes warm. Pulse the Robot Coupe, when needed, to complete grinding. Grind samples until approximately 4 mm in size. The total grinding time should be no more than 3 minutes.

Total Moisture Determination Procedure

1) Accurately weigh 5.00 grams of the sample (ground to pass ≤ 4 mm screen) 20 into a weighed moisture dish and place uncovered dish in oven.21 The number of products sampled should reflect an acceptable level of precision.16 The test material is to be representative of the product that is sold to the public and therefore should consist of sealed, packaged samples of finished product that is ready for commercial distribution. Samples are to be analyzed in duplicate.

2) Do not exceed 1 sample/10 sq in (650 sq cm) shelf space, and use only 1 shelf. Dry 3 hr at 99 ± 1.0°C. Remove from oven, cover, and cool in desiccator to room temperature (about 30 min). Reweigh and calculate percent moisture.

3) Report the final moisture determination as a percentage (%), to an accuracy level of one decimal place for each brand name (e.g., Skoal Bandits Wintergreen, Skoal Long Cut Cherry, Skoal Long Cut Wintergreen, etc.). All data should include the mean value with a 95% confidence interval, the range of values, the number of samples tested, the number of lots per brand name, and the estimated precision of the mean. Information will be reported for each manufacturer and variety (including brand families and brand variations) and brand name (e.g., Skoal Bandits Wintergreen, Skoal Long Cut Cherry, Skoal Long Cut Wintergreen, etc.).

Footnotes:

20The method is a modification of AOAC Method 966.02 (1990) in that the ground tobacco passes through a 4 mm screen rather than a 1 mm screen.

21When drying samples, do not dry different products (e.g., moist [wet] snuff, dry snuff, loose leaf) in the oven at the same time since this will produce errors in the moisture determinations.

16The testing facility is referred to ISO Procedure 8243 for a discussion of sample size and the effect of variability on the precision of the mean of the sample (ISO 8243, 1991).

Assay Criteria for Quality Assurance:

All quality control parameters must be determined within the laboratory in which they are to be used. At least 10 within-laboratory runs must be performed to establish temporary confidence intervals for the quality control parameters. Permanent limits should be established after 20 runs and should be reestablished after each additional 20 runs.

Good Laboratory Practice Guidelines:

The comments and notes listed below can be described as Good Laboratory Practice guidelines; they are described in detail in this protocol to ensure minimal interlaboratory variability in the determination of nicotine, total moisture, and pH in smokeless tobacco.

1This protocol assumes that the testing facility will implement and maintain a stringent Quality Assurance/Quality Control program to include, but not be limited to, regular interlaboratory comparisons, determination of the quality and purity of purchased products, and proper storage and handling of all reagents and samples.

2When a specific product or instrument is listed, it is the product or instrument that was used in the development of this method. Equivalent products or instruments may also be used. Use of trade names is for identification only and does not constitute endorsement by the Public Health Service or the U.S. Department of Health and Human Services.

Sampling Guidelines

For total Moisture determination in multiple samples, sample each smokeless tobacco brand name according to the provided testing frequency schedule.19

19 The testing frequency for each smokeless tobacco brand name (e.g., Skoal Bandits Wintergreen, Skoal Long Cut Cherry, Skoal Long Cut Wintergreen, etc.) is based on the manufacturing duration (refer to table below). Each smokeless tobacco brand name will be sampled and tested for nicotine, total moisture, and pH no fewer than twice and no more than four times during a calendar year.

Manufacturing duration in weeks

Test frequency*

up to and including 4 ................

2

up to and including 28 ..............

3

up to and including 52 ..............

4

* Use a statistical program to determine random sampling dates based on the total manufacturing duration during a calendar year. Sampling dates should fall on actual manufacturing days for the product when test material that is representative of the product that is sold to the public (consisting of sealed, packaged samples) is available. If a statistically determined sampling date falls on a day that does not meet this criterion, sample the product on the next date that does meet the criteria.

11The testing facility must ensure that samples are obtained through the use of a survey design protocol for sampling ‘‘at one point in time’’ at the factory or warehouse. The survey design protocol must address short-, medium-, and long-term smokeless tobacco product variability (e.g., variability over time and from container to container of the tobacco product) in a manner equivalent to that described for cigarette sampling in Annex C of ISO Protocol 8243. Information accompanying results for each sample should include, but not be limited to:

For each product-manufacturer and variety (including brand families and brand variations) and brand name (e.g., Skoal Bandits, Skoal Long Cut Cherry, Skoal Long Cut Wintergreen, etc.):

− Product ‘‘category,’’ e.g., loose leaf, plug, twist, dry snuff, moist (wet) snuff, etc.

− Lot number.

− Lot size.

− Number of randomly sampled, sealed, packaged (so as to be representative of the product that is sold to the public) smokeless tobacco products selected (sampling fraction) for nicotine, moisture, and pH determination.

− Documentation of method used for random sample selection.

− "Age" of product when received by testing facility and storage conditions prior to analysis.

For smokeless tobacco brand names with episodic production during a calendar year, the total number of sampling dates is determined by the sum of the individual test frequencies, not to exceed four. For the purpose of the Protocol, episodic production is defined as manufacturing intervals separated by periods of 30 or more days when the smokeless tobacco brand name is not manufactured.

Example 1: Within a single calendar year a smokeless tobacco brand name is manufactured from January 1 to March 31 and from September 1 to December 15. The testing frequency for the first manufacturing interval is 3 and for the second manufacturing interval is 3. The Protocol allows that each smokeless tobacco brand name be tested for nicotine, total moisture, and pH no more than four times during a calendar year. Therefore, 4 random sampling dates, as described in the footnote to the above table, are determined for the smokeless tobacco brand name. The values for nicotine, moisture, and pH determinations, and unionized (free) nicotine calculations and the mean of the 4 data points for that smokeless tobacco brand name are reported.

Example 2: Within a single calendar year a smokeless tobacco brand name is manufactured from April 5 to May 3 and from September 1 to December 15. The testing frequency for the first manufacturing interval is 2 and for the second manufacturing interval is 3. The values for nicotine, moisture, and pH determinations, andunionized(free)nicotinecalculationsand the mean of the 4 data points for that smokeless tobacco brand name are reported.

Example 3: Within a single calendar year a smokeless tobacco brand name is manufactured from January 1 to January 15 and from September 1 to September 22. The testing frequency for the first manufacturing interval is 2 and for the second manufacturing interval is 2. Four random sampling dates are selected to fall within the 6 weeks of manufacturing for the smokeless tobacco brand name. The values for nicotine, moisture, and pH determinations, and unionized (free) nicotine calculations and the mean of the 4 data points for that smokeless tobacco brand name are reported.

Personnel and Training Required

Laboratory Personnel must be trained in Good Laboratory Practice guidelines to ensure proper quality assurance and quality control procedures.

Equipment Needs

Analytical balance. Forced-air oven, Fisher Isotemp®, regulated to 99° ± 1.0°C. Suggested dimensions: 18 x 18 x 20 inches. Robot coupe model RSI 2V Scientific Batch Processor or an equivalent processor with a variable speed (0 to 3,000 RPM).

Requirements
Requirement CategoryRequired
Major equipment Yes
Specialized training Yes
Specialized requirements for biospecimen collection No
Average time of greater than 15 minutes in an unaffected individual No
Mode of Administration

Laboratory measurement

Lifestage

Participants

N/A

Selection Rationale

The Federal Register Notice protocol clearly outlines the procedure for the measurement of moisture content in a variety of smokeless tobacco products.

Language

English

Standards
StandardNameIDSource
caDSR Form PhenX PX730502 - Physical Properties Of Tobacco Products Smokeless Tobacco 6238937 caDSR Form
Derived Variables

N/A

Process and Review

Not applicable.

Protocol Name from Source

Federal Register Notice, Laboratory measurement, 74 Fed. Reg. 4, Jan. 7, 2009

Source

Notice regarding revisions to the laboratory protocol to measure the quantity of nicotine contained in smokeless tobacco products manufactured, imported, or packaged in the United States, 74 Fed. Reg. 4. (Jan. 7, 2009).

General References

Richter, P., Hodge, K., Stanfill, S., Zhang, L., & Watson, C. (2008). Surveillance of moist snuff: Total nicotine, moisture, pH, un-ionized nicotine, and tobacco-specific nitrosamines. Nicotine and Tobacco Research, 10, 1645-1652.

Richter, P., & Spierto, F. W. (2003). Surveillance of smokeless tobacco nicotine, pH, moisture, and unprotonated nicotine content. Nicotine and Tobacco Research, 5, 885-889.

Protocol ID

730502

Variables
Export Variables
Variable Name Variable IDVariable DescriptiondbGaP Mapping
PX730502_Moisture_Content_ DrySunff_Portion_Packs
PX730502070000 Dry Snuff portion packs Moisture N/A
PX730502_Moisture_Content_ Loose_Leaf_Tobacco
PX730502060000 Loose leaf Tobacco Moisture N/A
PX730502_Moisture_Content_ MoistWet_Snuff_PortionPacks
PX730502030000 Moist (wet) snuff portion packs Moisture N/A
PX730502_Moisture_Content_ PelletorCompressed_Tobacco
PX730502100000 Pellet or Compressed Tobacco Moisture N/A
PX730502_Moisture_Content_ Plug_Tobacco
PX730502040000 Plug Tobacco Moisture N/A
PX730502_Moisture_Content_ Snus_Tobacco
PX730502080000 Snus Tobacco Moisture N/A
PX730502_Moisture_Content_ Snus_Tobacco_PortionPacks
PX730502090000 Snus portion packs Tobacco Moisture N/A
PX730502_Moisture_Content_ Twist_Tobacco
PX730502050000 Twist Tobacco Moisture N/A
PX730502_Moisture_Content_Dry_Snuff
PX730502010000 Dry Snuff Moisture N/A
PX730502_Moisture_Content_MoistWet_Snuff
PX730502020000 Moist (wet) snuff Moisture N/A
PX730502_Nicotine_Content_ DrySunff_Portion_Packs
PX730502170000 Dry Snuff portion packs nicotine content N/A
PX730502_Nicotine_Content_ Loose_Leaf_Tobacco
PX730502160000 Loose leaf Tobacco nicotine content N/A
PX730502_Nicotine_Content_ MoistWet_Snuff_PortionPacks
PX730502130000 Moist (wet) snuff portion packs nicotine content N/A
PX730502_Nicotine_Content_ PelletorCompressed_Tobacco
PX730502200000 Pellet or Compressed Tobacco nicotine content N/A
PX730502_Nicotine_Content_ Plug_Tobacco
PX730502140000 Plug Tobacco nicotine content N/A
PX730502_Nicotine_Content_ Snus_Tobacco
PX730502180000 Snus Tobacco nicotine content N/A
PX730502_Nicotine_Content_ Snus_Tobacco_PortionPacks
PX730502190000 Snus portion packs Tobacco nicotine content N/A
PX730502_Nicotine_Content_ Twist_Tobacco
PX730502150000 Twist Tobacco nicotine content N/A
PX730502_Nicotine_Content_Dry_Snuff
PX730502110000 Dry Snuff nicotine content N/A
PX730502_Nicotine_Content_MoistWet_Snuff
PX730502120000 Moist (wet) snuff nicotine content N/A
PX730502_PH_ DrySunff_Portion_Packs
PX730502270000 Dry Snuff portion packs pH N/A
PX730502_PH_ Loose_Leaf_Tobacco
PX730502260000 Loose leaf Tobacco pH N/A
PX730502_PH_ MoistWet_Snuff_PortionPacks
PX730502230000 Moist (wet) snuff portion packs pH N/A
PX730502_PH_ PelletorCompressed_Tobacco
PX730502300000 Pellet or Compressed Tobacco pH N/A
PX730502_PH_ Plug_Tobacco
PX730502240000 Plug Tobacco pH N/A
PX730502_PH_ Snus_Tobacco
PX730502280000 Snus Tobacco pH N/A
PX730502_PH_ Snus_Tobacco_PortionPacks
PX730502290000 Snus portion packs Tobacco pH N/A
PX730502_PH_ Twist_Tobacco
PX730502250000 Twist Tobacco pH N/A
PX730502_PH_Dry_Snuff
PX730502210000 Dry Snuff pH N/A
PX730502_PH_MoistWet_Snuff
PX730502220000 Moist (wet) snuff pH N/A
PX730502_UnionizedFree_Nicotine_ DrySunff_Portion_Packs
PX730502370000 Dry Snuff portion packs unionized (free) nicotine N/A
PX730502_UnionizedFree_Nicotine_ Loose_Leaf_Tobacco
PX730502360000 Loose leaf Tobacco unionized (free) nicotine N/A
PX730502_UnionizedFree_Nicotine_ MoistWet_Snuff_PortionPacks
PX730502330000 Moist (wet) snuff portion packs unionized more
(free) nicotine show less
N/A
PX730502_UnionizedFree_Nicotine_ PelletorCompressed_Tobacco
PX730502400000 Pellet or Compressed Tobacco unionized more
(free) nicotine show less
N/A
PX730502_UnionizedFree_Nicotine_ Plug_Tobacco
PX730502340000 Plug Tobacco unionized (free) nicotine N/A
PX730502_UnionizedFree_Nicotine_ Snus_Tobacco
PX730502380000 Snus Tobacco unionized (free) nicotine N/A
PX730502_UnionizedFree_Nicotine_ Snus_Tobacco_PortionPacks
PX730502390000 Snus portion packs Tobacco unionized (free) more
nicotine show less
N/A
PX730502_UnionizedFree_Nicotine_ Twist_Tobacco
PX730502350000 Twist Tobacco unionized (free) nicotine N/A
PX730502_UnionizedFree_Nicotine_Dry_Snuff
PX730502310000 Dry Snuff unionized (free) nicotine N/A
PX730502_UnionizedFree_Nicotine_MoistWet_Snuff
PX730502320000 Moist (wet) snuff unionized (free) nicotine N/A
Tobacco Regulatory Research: Agent
Measure Name

Physical Properties of Tobacco Products

Release Date

June 24, 2015

Definition

This measure is a set of standard physical tests for cigarettes and filtered cigars capturing the following design descriptors: Length, Circumference, Tobacco weight, Filter type, Filter ventilation.

Purpose

The purpose of this measure is to evaluate and compare existing product modifications as well as new products and brands, which can help investigators understand the effect of design features on product chemistry.

Keywords

agent, Tobacco Regulatory Research, TRR, tobacco product design, filtered cigar, cigarette, cigarette length, cigarette circumference, filter ventilation, tobacco weight, filter composition, tobacco product feature, tobacco design descriptor, physical test of cigarettes, tobacco brand, automatic hopper loader, 1999 Massachusetts Benchmark Study, Brown & Williamson, Philip Morris, tobacco product modifications

Measure Protocols
Protocol ID Protocol Name
730501 Physical Properties of Tobacco Products - Cigarettes and Filtered Cigars
730502 Physical Properties of Tobacco Products - Smokeless Tobacco
Publications

Garcia-Cazarin, M.L., Mandal, R.J., Grana, R., Wanke, K.L., Meissner, H. (2020) Host-agent-vector-environment measures for electronic cigarette research used in NIH grants. Tobacco Control. 2020 January; 29(1). doi: 10.1136/tobaccocontrol-2017-054032