Making Alcohol Measurements in a Winery - Distillery

Co-founders of Black Dirt Distillery and Warwick Valley Winery, Jason Grizzanti and Jeremy Kidde, have been in the business of making alcohol based beverages for over 25 years. Starting as fruit cultivators, the two men fell in love with the idea of making hard cider form Apples, and opened their farm winery in 1994.

Since then, the two men have spent years perfecting their products, and have created even more product lines since. With the opening of their newest production facility, Black Dirt Distillery, in 2012, the co-founders have expanded the production of their spirit products to include bourbon whiskey, rye whiskey, and Apple Jack Brandy.

Warwick Valley Winery & Distillery is located in the foothills of the New York State’s Hudson Valley. With over 120 acres of manicured grounds, gardens, and various building it is a wonderful place to spend a day. The Winery and Distillery produce a wide range of products including award-winning and New York’s original hard cider, Doc’s Cider.

The Black Dirt Distillery was the first micro-distillery to open in New York State since prohibition and is where the Double Gold award winning Black Dirt Bourbon was created. In addition the Winery produces a critically acclaimed wine collection, and they make a mean sangria as well as excellent cocktails. Locally sourced food is available and they offer a gourmet farm-to-table style cuisine.

Warwick Valley Winery and Distillery has recently purchased a Rudolph AlcoTest-RI, and with the help of Darvin Martin from Rudolph Research Analytical, we would like to show you the many ways the AlcoTest-RI can be used in your winery and distillery. It is truly an all-purpose, time saving, instrument for a multi-product production environment such as a winery-distillery.

- Rudolph Research Analytical makes it faster than ever to test the % ABV value of alcoholic products with consistent accuracy, using the new AlcoTest-RI.

- The AlcoTest-RI, which includes the TTB approved DDM 2911 Plus density meter, is a great way to measure the specific gravity of “distiller’s beer” right before and right after fermentation to calculate % ABV of the finished beer. The results can be stored right on the instrument so you can monitor your batches over time.

This is a great way to monitor and maximize the %ABV yield from your mash. Varying the mash bill, fermentation time, the yeast, and temperature will have an effect of the %ABV yield of the finished distiller’s Beer.

- When making cuts from the still and when barreling, the highly accurate Density Meter component of AlcoTest-RI can be used to measure “Percent ABV” to make cuts and dilutions precisely and consistently, every time.

The DDM2911 PLUS also has on-board software for calculating dilutions as per the TTB gauging manual. This feature is called AlcoCalcTM

- The TTB requires that obscured products like an Apple Pie Moonshine be distilled in a lab still to remove just the water and alcohol so that the %ABV can be measured in a TTB approved density meter or with a hydrometer. When blending down an obscured spirit this might necessitate several, hour long distillations.

- One of the great advantages of the AlcoTest-RI is it can deliver accurate but “Unofficial” Percent ABV readings of obscured products. In less than 2 minutes you can have a Percent ABV measurement, then continue diluting and blending – this save hours of work on each batch and countless hours each month. Only the final measurement for label value would have to be done with the lab still and it is possible to eliminate many of those distillations as well.

- When using the AlcoTest-RI in production mode the % ABV measurements are quite accurate without distillation even on obscured samples like wines and ciders. The refractometer sees the obscuration in the sample and is able to compensate for this when testing the density / Percent ABV. Since tax is paid by volume at a flat on these lower %ABV products your main concern is being below the Percent ABV limit. The AlcoTest-RI will be more that accurate enough for measuring these products.

- If you are a winery, distillery, or a combination of both, the AlcoTest-RI is the perfect instrument for your application providing any and all alcohol related testing in one system. It is really the ideal testing solution for all of the many testing activities that might be used in the making of high proof spirits, wine and cider.

The TTB requires that obscured products like an Apple Pie Moonshine be distilled in a lab still to remove just the water and alcohol so that the Percent ABV can be measured in a TTB approved density meter or with a hydrometer. When blending down an obscured spirit this might necessitate several, hour long distillations.

We enjoyed spending the day with Jason and wish the team well with their new instrumentation.

Makers of Craft Spirits Beverages seek to produce high quality, consistent tasting products that fully comply with TTB regulations. Using good laboratory techniques and adding some addition quality control checks can help you produce a better finished product.

Refractometers perfect for the food, beverage, and chemical industry.

The Rudolph Research bench top J47 and J57 refractometers offer High Accuracy and Wide Range models as well as temperature corrected and temperature controlled models.

Understanding Temperature Controlled Vs Temperature Corrected Refractometers.

Rudolph makes two refractometers, the J47 and the J57. Both look similar, both have similar specifications. The J57 is 30% more expensive —why?
Let’s look at this in a brief experiment.

What we have here is 2 nearly identical looking refractometers. The J47 and the J57

These two instruments have very similar specifications and they look almost identical. The only way to quickly tell them apart is the J57 has cooling fins and the J47 does not. What's the difference in actual operation though?

The J47 is temperature of corrected while the J57 is fully temperature controlled.

These instruments have both been on for a while and you what you'll notice is this sitting in a room at ambient temperature the instrument will read approximately 22-23 degrees Celsius. The J57 being temperature controlled will hold steadily at exactly 20 C.

Why does that matter in a real-world situation? If you're working in a factory environment where most of your samples are primarily sugar and water, temperature correction will work well.

As an example we will measure something simple like sweet ice tea. You will see it will read about the same on both instruments. However, let's imagine now that our factory is ISO-certified. In a situation like this all instruments would need to be regularly calibrated back to a traceable standard.

What I have here is a calibration standard traceable to NIST which is made for Rudolph by a company named Cargill. While different countries will each have different authorities to answer to, using a traceable standard will always be a component of remaining in compliance. In addition the calibration standard will not be sugar and water based as these are not stable over time.

In this case the standard we will use should measure very close to 9.94 BRIX (Pronounced like bricks). Thus, If the refractometer measures this correctly it proves the refractometer is properly calibrated and within specifications.

If we place the calibration standard on both refractometers they should in theory measure the exact same results. What we find is the temperature controlled refractometer measures the calibration standard almost perfectly. The temperature corrected refractometer however cannot measure the calibration standard since temperature correction will not work on a sample (or standard) that is not primarily sugar and water.

We have just seen exactly why even a refractometer that measures primarily sugar and water based samples will still need to be Temperature Controlled. The issue becomes traceability.

[Refractometers come in many shapes, sizes, accuracies, and with different features. Selecting the right refractometer for your application is often critical! Many applications require samples to be measured at specific temperatures, 20c for example. To determine the BRIX of a sample at 20c two methods can be employed to determine what the BRIX would be at 20C when the sample is not. Method one is to use tables to take the actual reading and mathematically correct back to what the temperature would be at 20C. The second method is to accurately hold the sample temperature at 20C and then make the measurement.]

Temperature correction is acceptable and accurate for certain samples – those samples that are primarily sugar and water will measure well with temperature correction only, even when the sample temperature is far from the desired measurement temperature.

Samples including calibration standards that are not sugar and water based must be measured using accurate temperature control.

Production facilities that require the refractometer be calibrated to a NIST traceable standard must be Temperature Controlled – Why, NIST Traceable standards are not Sugar and water based.

For more advice about selecting the correct refractometer for your application please contact us at Rudolph Research Analytical.

www.rudolphreserach.com
info@rudolphresearch.com
973-584-1558

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:

Condenser
Stillhead - 3 Way Distilling Adaptor
Vacuum Adaptor-Bent 105 degrees
Thermometer
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.

http://rudolphresearch.com

Refractometers perfect for the food, beverage, and chemical industry. The Rudolph Research bench top J47 and J57 refractometers.

Automatic Measurement of highly viscous samples

Making Density Meter measurements with the R837 Automation system with highly viscous samples. Even very thick substances can be loaded and measured with the very capable R837 Automation System.

Introducing the AUTOFLEX R837 from Rudolph Research Analytical

Laboratory Automation Redefined

The Autoflex R837
Superior Material Construction – Unmatched Durability

Rugged stainless steel needle with sufficient torque to pierce any septum

PTFE, TEFLON and PEEK liquid flow path material

Modular design to reduce footprint
Safety guard to protect hands


Eliminate sample cross contamination with complete needle cleaning – A RUDOLPH EXCLUSIVE FEATURE

Automation systems should have no net effect on your sample measurements.

The Rudolph R837 is the only brand that cleans both the INSIDE and OUTSIDE of the needle to eliminate cross contamination.

The R837 rinses the entire system with your choice of 3 solvents and also includes low solvent detection.

Flexible Rack Configurations are Available


The R837 is the only brand that allows for the use of custom racks and bottles so that the customer does not have to decant the sample into manufacturer supplied bottles or tubes.

Send us your vial and we will manufacture a customized rack for your lab.

Racks can be created for your samples: Test Tubes, Boston Rounds, 1 oz, ½ oz, virtually any size bottle.

Heated and Unheated Racks in the same carousel

Flexible Automation Solution
Automate your Density, Specific Gravity, Optical Rotation, Specific Rotation,
Refractive Index, Color, and pH measurements

Push the start button and measure any or all of the following - Density, Specific Gravity, Refractive Index, BRIX, Optical Rotation , Specific Rotation, Color, and pH.

The R837 is the only brand that operates in a Windows 7 Embedded environment and can connect directly to the customer's LIMS or SAP system for data handshake, download, and transfer.

One or more Methods may be assigned to each carousel rack or individual sample locations.

Load the samples in the rack based on the measurement you want to make or change the Method for that rack for complete flexibility.


A Rudolph Research Exclusive Feature.

The R837 is the only method based autosampler solution in the marketplace that allows a different method for each rack section. Each method can have its own pump speed rinse time which can include up to 3 rinses and a custom drying time. Each method can also function in suction mode for light samples or in pressure mode for viscous thick samples.

A Method includes any combination of measurement types, sample bottle size, heating, and sample handling options including suction mode, pressure mode, and system cleaning options.

The R837 is the only automation system offering automatic barcode reading with test tube or bottle spin detector so the tube or bottle can be placed in any position in the rack.

Vials are automatically rotated for faster more accurate label reading

No need for special bar code placement or handling.

Samples may be mixed by agitation prior to sample load.
Samples are then loaded using suction or pressure mode.

SMART TECHNOLOGY automatically adjusts pumping speed to handle various viscosities.

The R837 has a sample reclaim feature that returns at least 95% of the sample to the vial.

Smart Sample Load Technology
SMART TECHNOLOGY automatically adjusts pump speed ranging from thin to high viscosity samples up to 36,000 mPa-s (cP)
The heated rack option handles heavy crudes and waxes.

Flexibility Unmatched with embedded Windows 7
User interface allows the operator to interrupt a measurement routine with an urgent sample. Use the auto-find feature to search and quickly find a specific sample.

Automated Data Collection
Use any format of barcodes
PDF 417
QR Code
2D Matrix
UPC CODE

AUTOFLEX R837

- Engineered for maximum sample handling flexibility

Rudolph Polarimeter Mobile Fill Station

The Rudolph Research Polarimeter Mobile Fill Station

Rudolph Research Polarimeter Sample Cells are designed to be easily filled and easily cleaned. Air bubbles should not be left in the sample cell as this will have an adverse effect on measurements.

When held at the correct angle and filling the cell from the bottom inlet port, the cell is easily filled with almost no possibility of leaving any air in the cell. Filling from the bottom up forces any air bubbles up and out ahead of the sample.

Your cell is now filled and air bubble free.

Rudolph recommends that Polarimeter Cells should never be filled in the instrument to avoid damage due to spillage of strong acids or bases.

To avoid damage to the instrument sample cells should be filled in the Rudolph Mobile Fill Station, over the sink, or under a fume hood.

For users who prefer not to hold the cell when working with caustic samples the Rudolph Mobile Fill Station should be used.

By design, the filling station will hold the cell at a suitable angle. Simply place the Polarimeter cell in the filling station and again fill the cell from the lower inlet.

As the cell becomes fully loaded and sample begins to appear at the upper inlet, cap off the upper, then lower inlets. Your cell is now fully loaded and air bubble free. The filling station includes a light that will go from darker to bright white when the cell is filled and air-bubble free.

The Rudolph Polarimeter Mobile Fill Station accessory is available for all Rudolph Autopol Polarimeters and is included free with Autopol V, Autopol VPLUS, and Autopol VI Polarimeter Models.

Digital Refractometer – J157 available in several models and option configurations.

The Rudolph J157 model of Refractometers offers high performance and a range of features to suit many demanding applications in laboratories and harsh industrial environments. Rudolph Research Analytical, working together with refractometer (Refraktometer) users from various countries and disciplines, has developed the J157 series of Digital Refractometers. The Rudolph J157 benchtop line combines the features, measurement range, and accuracy that meet the most demanding applications both in and out of the laboratory and shares many features with the Rudolph Research Refractometer Product Line.