1. Proving the Proof USBEVX CONFERENCE 2016 YVETTE GLENN, PHD CHEMIST, BEVERAGE ALCOHOL LABORATORY SCIENTIFIC SERVICES DIVISION February 16 – 18, 2016| Washington, DC Alcohol and Tobacco Tax and Trade Bureau

2. TTB’s Mission Collect the taxes on alcohol, tobacco, firearms and ammunitions Analyze products to determine class and type for proper tax Protect the public by ensuring the integrity of alcohol products Analyze products for truthful and accurate label claims Analyze products for limited and prohibited ingredients, adulterants, contaminants, and additives in alcohol products Analyze products to support TTB investigations for illegal trade practices to prevent unfair and unlawful market activity ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 2

3. TTB’s Scientific Services Division Provides comprehensive technical support to all TTB program offices in line with the bureau’s mission to collect taxes and protect consumers. Carries out its mission through operation of 4 labs: Beverage Alcohol Laboratory Nonbeverage Products Laboratory Tobacco Laboratory Beltsville, Maryland Compliance Laboratory Walnut Creek, California ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 3

4. Quality of Data ISO 17025 Accredited Laboratories Validated Test Methods Must be accurate, precise, and specific for its intended purpose. Test results are precise, accurate, and reproducible. Formally Validated Test Methods: Use official methods of the Association of Official Analytical Chemists (AOAC) TTB Test Methods: Developed and validated in-housed. Available to Regulated Industry TTB methods listed on our website ( www.ttb.gov ) www.ttb.gov ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 4

5. Points of Importance Proofing Spirits Regulations Methodologies Techniques Determining Obscuration Avoiding problems from dissolved solids such as sugar Title 26 US Code & 27CFR30.11 Proof is the ethyl alcohol content of a liquid at 60 degrees Fahrenheit stated as twice the percent of ethyl alcohol by volume. ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 5

6. Definitions Apparent proof is the measured proof of the neat spirit, typically by hydrometer or density meter. True proof is the measured proof after distillation, or can be determined by correcting the apparent proof with the obscuration: True Proof = Apparent Proof + Obscuration Solids such as sugars in a spirit obscure the proof measurement. The amount of solids in the spirit can be determined by evaporation and used to calculate the obscuration. ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 6

7. Regulatory Limits: Distilled Spirits 27 CFR 5.37(b) Tolerances ◦0.5 proof drop for high solids (>600 mg/100 mL) ◦0.5 proof drop for 50 mL and 100 mL container sizes ◦0.3 proof drop for low solids (≤600 mg/100 mL) ◦Over proof = Noncompliance (CFR = Code of Federal Regulations) http://www.ecfr.gov ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 7

8. Regulations for Determining Proof ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 8 Product Examples: ≤400 mg/100 mL solids: Vodka >400 and ≤600 mg/100 mL solids: Rum >600 mg/100 mL solids: Cordial

9. Proofing Methodologies Apparent Proof ◦Neat samples with solids ≤ 400 mg/100 mL True Proof by Distillation ◦Any sample, regardless of proof or solids content True Proof by Obscuration ◦Spirits with 80  to 100  ◦Solids ≤ 600 mg/100 mL ◦Apparent Proof + Obscuration (determined by solids by evaporation) ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 9

10. Proofing Technique: Hydrometer Used to determine Apparent Proof on low solid products ◦(≤ 600 mg/100 mL) and True Proof after distillation. Available in different proof ranges so be sure sample to be measured is within the appropriate range for the hydrometer. Must be calibrated and must meet the minimum requirements as stated in 27 CFR 30.22. ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 10

11. Hydrometer Set-up Thermometer Glass Container Hydrometer Bottom of Meniscus Sample Bottle Sample Read at Eye Level Apply thermometer and hydrometer correction factors (obtained from third-party vendor). ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 11

12. Proofing Technique: Densitometers ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 12

13. Densitometers – Alternative to the Hydrometer Advantages Quality ◦High accuracy ◦High precision Speed ◦Can be automated with an autosampler ◦High sample throughput ◦Calculations automated with a computer Other ◦Requires much less sample ◦Results can be saved and uploaded Disadvantages Costs ◦More expensive to buy ◦Require expenses to repair ◦Downtime if out of service Additional Training for Analyst: ◦Calibration ◦Maintenance ◦Operation ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 13

14. Proofing Technique: Distillation Distillation is a separation process performed by boiling a sample and condensing the vapors. The distillate is the resulting liquid and is free of dissolved solids that obscure proof measurements. ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 14

15. Proofing Technique: Distillation Fill 100-mL volumetric flask with slightly more than 100 mL sample and equilibrate in a water bath for 30 minutes. Transfer 100 mL of the sample into the distillation flask. Collect slightly less than 100 mL of the distillate into a receiving flask which is kept in an ice bath. Equilibrate in water bath for 30 minutes and add DI water to reach 100 mL volume. ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 15

16. Temperature Equilibration for Distillation Temperature equilibration of sample Performed before and after distillation. Allows for consistent volume readings. ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 16

17. True Proof by Distillation Can be determined after distillation using a hydrometer or densitometer. Can be used for any sample regardless of its solids content or proof. Samples with >60% ABV are distilled 1:2 (i.e., using 50 mL sample + 50 mL water). Samples with > 600 mg/100 mL solids must be distilled. Scale up if more than 100 mL distillate is needed. ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 17

18. Proofing Technique: True Proof by Obscuration Applicable for spirits with ◦Proof in the range of 80 to 100 ◦Solids content  400 mg to ≤600 mg/100 mL Apparent proof determined from neat sample ◦using a hydrometer or a densitometer Obscuration determined from solids by ◦evaporation True Proof by Obscuration = Apparent Proof + Obscuration ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 18

19. Proof Technique: Obscuration by Evaporation Transfer 25 mL sample to previously weighed dry empty aluminum dish. Evaporate sample to dryness on steam table. Place sample in oven at 100  C for 30 minutes. Cool sample in desiccator then weigh to get final weight. Subtract initial pan weight from the final weight to get residue weight. ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 19

20. Solids by Evaporation 27 CFR 30.32(b) Example: (2.5768 g – 2.4392 g) = 0.1376 g (Weight of Residue) 0.1376 g X 4 = 0.5500 g/100 mL (Amount of Solids) g to mg: 0.5500 g/100 mL X 1000 = 550 mg/100 mL Initial Weight of Pan Final Weight of Evaporated Sample in Pan = Weight of Residue - Weight of Residue X 4 = Solids in mg/ 100 mL ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 20

21. Proof Obscuration By Evaporation 27 CFR 30.32(b) 0.5500 g/100 mL X 4 = 2.2° 27 CFR 30.32(a): -Only valid for proof range of 80° to 100° Solids Obscuration X 4 = ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 21

22. True Proof by Obscuration Example: 77.7° + 2.2° = 79.9  Apparent Proof Obscuration True Proof by Obscuration += ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 22

23. Determining Alcohol Content for Beer and Wine Proofing not needed for beer (27 CFR 7.71(b)) or wine (27 CFR 4.36(b)). Alcohol content for beer and wine can be determined using techniques such as: ◦Distillation followed by Densitometer ◦Gas Chromatography with Thermal Conductivity Detection (GC- TCD) ◦Gas Chromatography with Flame Ionization Detection (GC-FID) ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 23

24. TTB Online Proofing Videos ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 24 http://www.ttb.gov/spirits/proofing.shtml

25. Acknowledgements Cathy Halverson, BAL Chief Neil Pennington, BAL Chemist Marsha Galicia-Monroe, CL Chemist Armen Mirzoian, PhD, BAL Chemist Abdul Mabud, PhD, SSD Director ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 25

26. Speaker Contact Information Yvette Glenn, PhD Chemist Beverage Alcohol Laboratory Email: Agnes.Glenn@ttb.govAgnes.Glenn@ttb.gov ALCOHOL AND TOBACCO TAX AND TRADE BUREAU 26