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Protocol - Physical Properties of Tobacco Products - Smokeless Tobacco

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Protocol Name from Source:

This section will be completed when reviewed by an Expert Review Panel.

Availability:

Publicly available

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).

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
Average time of greater than 15 minutes in an unaffected individualNo
Major equipmentYes
Specialized requirements for biospecimen collectionNo
Specialized trainingYes

Mode of Administration

Self-administered

Life Stage:

Not applicable

Specific Instructions:

N/A

Research Domain Information

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.

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
Common Data Elements (CDE)Smokeless Tobacco Property Assessment Text4883624CDE Browser

Process and Review

This section will be completed when reviewed by an Expert Review Panel.

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 NameVariable IDVariable DescriptionVersiondbGaP Mapping
PX730502_Moisture_Content_Dry_SnuffPX730502010000Dry Snuff Moisture4N/A
PX730502_Moisture_Content_MoistWet_SnuffPX730502020000Moist (wet) snuff Moisture4N/A
PX730502_Moisture_Content_ MoistWet_Snuff_PortionPacksPX730502030000Moist (wet) snuff portion packs Moisture4N/A
PX730502_Moisture_Content_ Plug_TobaccoPX730502040000Plug Tobacco Moisture4N/A
PX730502_Moisture_Content_ Twist_TobaccoPX730502050000Twist Tobacco Moisture4N/A
PX730502_Moisture_Content_ Loose_Leaf_TobaccoPX730502060000Loose leaf Tobacco Moisture4N/A
PX730502_Moisture_Content_ DrySunff_Portion_PacksPX730502070000Dry Snuff portion packs Moisture4N/A
PX730502_Moisture_Content_ Snus_TobaccoPX730502080000Snus Tobacco Moisture4N/A
PX730502_Moisture_Content_ Snus_Tobacco_PortionPacksPX730502090000Snus portion packs Tobacco Moisture4N/A
PX730502_Moisture_Content_ PelletorCompressed_TobaccoPX730502100000Pellet or Compressed Tobacco Moisture4N/A
PX730502_Nicotine_Content_Dry_SnuffPX730502110000Dry Snuff nicotine content4N/A
PX730502_Nicotine_Content_MoistWet_SnuffPX730502120000Moist (wet) snuff nicotine content4N/A
PX730502_Nicotine_Content_ MoistWet_Snuff_PortionPacksPX730502130000Moist (wet) snuff portion packs nicotine content4N/A
PX730502_Nicotine_Content_ Plug_TobaccoPX730502140000Plug Tobacco nicotine content4N/A
PX730502_Nicotine_Content_ Twist_TobaccoPX730502150000Twist Tobacco nicotine content4N/A
PX730502_Nicotine_Content_ Loose_Leaf_TobaccoPX730502160000Loose leaf Tobacco nicotine content4N/A
PX730502_Nicotine_Content_ DrySunff_Portion_PacksPX730502170000Dry Snuff portion packs nicotine content4N/A
PX730502_Nicotine_Content_ Snus_TobaccoPX730502180000Snus Tobacco nicotine content4N/A
PX730502_Nicotine_Content_ Snus_Tobacco_PortionPacksPX730502190000Snus portion packs Tobacco nicotine content4N/A
PX730502_Nicotine_Content_ PelletorCompressed_TobaccoPX730502200000Pellet or Compressed Tobacco nicotine content4N/A
PX730502_PH_Dry_SnuffPX730502210000Dry Snuff pH4N/A
PX730502_PH_MoistWet_SnuffPX730502220000Moist (wet) snuff pH4N/A
PX730502_PH_ MoistWet_Snuff_PortionPacksPX730502230000Moist (wet) snuff portion packs pH4N/A
PX730502_PH_ Plug_TobaccoPX730502240000Plug Tobacco pH4N/A
PX730502_PH_ Twist_TobaccoPX730502250000Twist Tobacco pH4N/A
PX730502_PH_ Loose_Leaf_TobaccoPX730502260000Loose leaf Tobacco pH4N/A
PX730502_PH_ DrySunff_Portion_PacksPX730502270000Dry Snuff portion packs pH4N/A
PX730502_PH_ Snus_TobaccoPX730502280000Snus Tobacco pH4N/A
PX730502_PH_ Snus_Tobacco_PortionPacksPX730502290000Snus portion packs Tobacco pH4N/A
PX730502_PH_ PelletorCompressed_TobaccoPX730502300000Pellet or Compressed Tobacco pH4N/A
PX730502_UnionizedFree_Nicotine_Dry_SnuffPX730502310000Dry Snuff unionized (free) nicotine4N/A
PX730502_UnionizedFree_Nicotine_MoistWet_SnuffPX730502320000Moist (wet) snuff unionized (free) nicotine4N/A
PX730502_UnionizedFree_Nicotine_ MoistWet_Snuff_PortionPacksPX730502330000Moist (wet) snuff portion packs unionized (free) nicotine4N/A
PX730502_UnionizedFree_Nicotine_ Plug_TobaccoPX730502340000Plug Tobacco unionized (free) nicotine4N/A
PX730502_UnionizedFree_Nicotine_ Twist_TobaccoPX730502350000Twist Tobacco unionized (free) nicotine4N/A
PX730502_UnionizedFree_Nicotine_ Loose_Leaf_TobaccoPX730502360000Loose leaf Tobacco unionized (free) nicotine4N/A
PX730502_UnionizedFree_Nicotine_ DrySunff_Portion_PacksPX730502370000Dry Snuff portion packs unionized (free) nicotine4N/A
PX730502_UnionizedFree_Nicotine_ Snus_TobaccoPX730502380000Snus Tobacco unionized (free) nicotine4N/A
PX730502_UnionizedFree_Nicotine_ Snus_Tobacco_PortionPacksPX730502390000Snus portion packs Tobacco unionized (free) nicotine4N/A
PX730502_UnionizedFree_Nicotine_ PelletorCompressed_TobaccoPX730502400000Pellet or Compressed Tobacco unionized (free) nicotine4N/A