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Distillation – Obscured Alcohol Products
Distillation – Obscured Alcohol Products. – Let us take you through a quick overview of the process for preparing a sample of an obscured alcohol product such as a flavored Vodka for final measurement of % vol/vol for label value. The goal is to separate any alcohol and water from any other solids so the sample can be measured in a TTB Approved Density Meter such as the Rudolph DDM 2911 PLUS.
Understanding and measuring finished Alcohol products that are obscured by flavorings, sugars, or barrel aging.
Rudolph Research Recommends following the same methods utilized by the US TTB and using the Rudolph TTB approved DDM 2911 PLUS Density Meter.
Alcohol products containing flavorings, sugars, infusions, or barrel aged more than 2 years are referred to as “Obscured Alcohol Products”.
To measure the alcohol % by vol/vol of the finished product, it is necessary to remove anything that is not alcohol and water so the sample can be measured in a Density Meter according to TTB recommendations.
To remove the “Obscuration” and end up with just alcohol and water, a process known as distillation is utilized.
Distillation – Obscured Alcohol Products – Procedures
Distillation – Obscured Alcohol Products. To begin the distillation process to remove anything that is not alcohol or water. First measure out exactly 100 ml of sample. Place your sample flask in a water bath at room temperature. The bath should be large enough not to be effected by a flask or two of warmer sample. Turn on the water bath and set temperature to 20.0 ⁰C, give the unit twenty (20) minutes to stabilize.
Thoroughly clean and dry all glassware prior to use.
Overfill the flask initially by filling to a level above the line.
Once the sample has come to temperature you may use a pipette to remove excess sample
Building your distillation apparatus for alcohol separation
Parts and Glassware you will need:
- Stillhead – 3 Way Distilling Adaptor
- Vacuum Adaptor-Bent 105 degrees
- Distilling Flask
- Receiving Flask
- Heat Source (Flame or electric)
Step 1: Sample is placed in a flask that is fit with a distillation head.
Step 2: Attached to the Distillation head is a Condenser – a glass tube with a jacket around it which cold water is flushed through.
Step 3: Attached to the condenser is a Vacuum Adapter
Step 4: Receiver to collect distillate:
The liquid in the distillation flask is heated until it reaches the boiling point of water and alcohol. Thereby vaporizing just the water and alcohol.
The hot vapors above the boiling liquid rise through the distillation head and enter the condenser.
When the vapor enters the condenser, the vapor is cooled and condenses back to a liquid called a distillate or condensate.
The pure distillate flows through the condenser and is collected in the receiver.
When the distillation is nearly finished you will have collected all the alcohol and some of the water from the original sample. Stop the distillation just after
the distillate passes the neck of the collection flask and well before it reaches the etched mark on the flask.
Let the sample sit in the water bath for 20 minutes to bring it back to temperature. As the liquid warms it will expand.
Use a pipette of distilled water to fill the flask until the bottom of the meniscus is lined up with the top of the line on the neck of the flask
You have now added water to the collected sample to replace what was the volume of the obscuration in the original sample.
The obscuration has thus been removed during distillation and you have just the original amount of alcohol with water.
Having brought the sample back to its original volume of 100 ml it is now possible to measure the % vol/vol of alcohol in this prepared sample.
With the obscuring factors left behind and having just Alcohol and Water adjusted back to the original volume,
your sample is now ready to be injected into the TTB approved Rudolph 2911 PLUS Density Meter.