It’s that time of year again: bottling time! The past year’s vintage is slowly starting to take up too much room in the cellar and now is the time for decision making in terms of preparing for the pending vintage. Finalizing a good bottling schedule before harvest starts is an essential good winemaking practice, but bottling comes with its own set of challenges.
It is not uncommon for winemakers to express feelings of “not being able to sleep at night” when wines get bottled, as they are worried about possible re-fermentation issues. As wine naturally changes through its maturity, it is easy to feel insecure about bottling wines, especially those wines that may have had challenges associated with it throughout production.
However, there are several analytical tests that winemakers can add to their record books every year to ensure they are bottling a sound product. The following briefly describes a series of analytical tests that provide information to the winemaker about stability and potential risks associated with the product when it goes in bottle.
Bottling comes with its own set of challenges and risks, but several analytical tests can help put a winemaker’s mind to ease regarding bottle stability. Photo by: Denise M. Gardner
Basic Wine Analysis Pre-Bottling:
This first list is the bare minimum data that should be measured and recorded for each wine getting bottled, regardless of the wine’s variety or style. Keeping accurate records of these chemistries is also helpful in case something goes wrong while the bottle is in storage or after it is purchased by a customer.
pH is essential to know as it gives an indication for the wine’s stability in relation to many chemical factors including sulfur dioxide, color, and tannin. For example, high pH (>3.70) wines provide an indication that more free sulfur dioxide is needed to obtain a 0.85 ppm molecular free sulfur dioxide content. At the 0.85 ppm molecular level, growth of any residual yeast and bacteria in the wine should be adequately inhibited.
High pH wines tend to have issues with color stability. At this point, color stability can be addressed by blending or with use of color concentrates (e.g.,Mega Purple). Keep in mind that if the wine is blended with another wine, all chemical analyses, including pH, should be completed on the blend (as opposed to average individual parts) prior to bottling.
Free and Total Sulfur Dioxide Concentration
In the United States, total sulfur dioxide is regulated and must fall under 350 mg/L for all table wines (CFR: https://www.ecfr.gov/cgi-bin/text-idx?SID=eddaa2648775eb9b2423247641bf5758&mc=true&node=pt27.1.24&rgn=div5#sp27.1.24.a).
However, the free sulfur dioxide concentration provides an indication to the winemaker regarding antioxidant strength and perceived antimicrobial protection. To inhibit growth of yeast and bacteria during bottle storage, a 0.85 ppm molecular free sulfur dioxide concentration must be obtained. The free sulfur dioxide concentration required to meet the molecular level is dependent on pH. Therefore, free sulfur dioxide additions should be altered and based on a wine’s pH for optimal antimicrobial protection.
Analytically, it can be daunting to measure free sulfur dioxide as the wet chemistry set up looks intimidating. However, many small commercial wineries have benefited from the integration of a modified aeration-oxidation (AO) system, and with a little practice, have been relatively successful at monitoring free sulfur dioxide concentrations. A few wineries have worked to validate use of Vinmetrica’s analyzer (https://vinmetrica.com/), and found results comparable to those obtained by use of the AO system.
Residual (or Added) Sugar
Any remaining sugar in the bottle, whether through an arrested fermentation or direct addition, can pose a risk for re-fermentation post-bottling. This is especially true if the winery lacks good cleaning and sanitation practices. Nonetheless, it is a good idea to assess the sugar content pre-bottling to record a baseline value of the sugar concentration going into bottle. If bottles were to start re-fermenting, a sugar concentration could be analyzed and used to compare against the baseline value in order to assess the potential of yeast re-fermentation.
For wineries with minimal residual sugar concentrations, a glucose-fructose analysis (often abbreviated glu-fru) is often used to help determine accurate sugar content. For wines with added sugar an inverted glucose-fructose analysis may be required.
If you are concerned about potential risk for Brettanomyces (Brett) bloom post-bottling, it is usually encouraged to reduce the sugar content in the finished wine below 1% (<10 g/L sugar) in the bottle.
Malic Acid Concentration
While using paper chromatography to monitor malolactic fermentation (MLF) is useful, it does not give an accurate reflection of residual malic acid concentration. In fact, some winemakers find that a paper chromatogram may show a MLF has been “completed,” but would prefer to have lower residual malic acid concentrations remaining in the wine.
During my time at an analytical company, 0.3 g/L of malic acid and below was considered “dry.” This is typically a safe level of residual malic acid to avoid post-bottling MLF.
Volatile acidity (VA) is federally regulated, and levels are indicated in the Code of Federal Regulations (CFR: https://www.ecfr.gov/cgi-bin/text-idx?SID=eddaa2648775eb9b2423247641bf5758&mc=true&node=pt27.1.24&rgn=div5#sp27.1.24.a). For most states, with California as an exception, the maximum allowable VA for red wines is 1.40 g/L acetic acid (0.14 g/100 mL acetic acid) and for white wines is 1.20 g/L acetic acid (0.12 g/100 mL acetic acid).
Monitoring VA through production is a good indicator of acetic acid bacteria spoilage. At minimum, wineries should record VA
- immediately post-primary fermentation,
- periodically through storage (e.g., every 2-3 months) and
Whiling monitoring VA, sharp increases in VA should alarm the winemaker of some sort of contamination. Typically, these increases are caused by acetic acid bacteria, which can only grow with available oxygen.
As a general rule of thumb, knowing the final alcohol concentration is a good idea. Alcohol content helps determine a tax class for the wine and is required for the label.
Titratable Acidity (TA)
All wines are acidic in nature as they fall under the pH 7.00. However, titratable acidity (TA) acts as an indicator for the sour sensory perception associated with a given wine. For example, two wines, Wines 1 and 2, with a pH of 3.40 may have different TAs. If Wine 1 has a TA of 8.03 g/L tartaric acid while Wine 2 has a TA of 6.89 g/L tartaric acid, Wine 1 would likely taste more acidic (assuming all other variables are the same).
Titrations are an easy analytical testing method to learn and understand when testing wine’s chemistry. Photo by: Denise M. Gardner
Cold stability tests are often recommended to ensure the wine is cold stable, and will, therefore, not pose a threat of precipitating tartrate crystals during its time in bottle. Not all wines require a cold stability process (e.g., seeding and chilling). Cold stability testing can be done prior to a cold stabilization step in order to avoid extraneous processing operations, saving time and money.
For more information on cold stability processes and testing, please visit Penn State Extension’s website: http://extension.psu.edu/food/enology/analytical-services/cold-stabilization-options-for-wineries
These crystals on this cork illustrate what can happen when a wine is not properly cold stabilized. While the tartrate crystals pose no harm to consumers, they may find the crystals unappealing or questionable. Photo by: Denise M. Gardner
Additionally, haze formation is a potential risk post-bottling. While hazes do not typically offer any safety threat to wine consumers, they often look unappealing. Protein hazes tend to make the wine look cloudy. Some varieties are more prone to protein hazes then others, and running a protein stability trial could minimize the risk for a protein haze in-bottle.
It is important to remember that due to the fact protein stability is influenced by pH, cold stability production steps should take place before analyzing the wine for protein stability and before going through any necessary production steps to make the wine protein stable. This is due to the fact that cold stability processes ultimately alter the wine’s pH, and the chemical properties of proteins are influenced by the pH.
Analysis for Those that May Consider Bottling Unfiltered:
Yeast and Bacteria Cultures (Brett, Yeast, Lactic Acid Bacteria, Acetic Acid Bacteria)
Having a microscope in the winery can be a great reference point in terms of scanning for potential microbiological problems. However, if the winery does not have a microscope, but knows that some microbiological issues or risks may exist in a wine, having a lab set test the wine on culture plates is a good indicator for potential growth risks during the wine’s storage.
If the wine is going to be bottled using a sterile filtration step, keep in mind that wines are not bottled sterile. Assuming the absolute filtration method is working properly, the wine has potential to become re-contaminated with yeasts and bacteria from the point of which it exits the filter. In fact, it is not uncommon for wines to pick up yeast or bacteria contamination during the bottling process.
Managing free sulfur dioxide concentrations can help inhibit any potential growth from contamination microorganisms if the proper antimicrobial levels (0.85 ppm molecular) are obtained at that wine’s pH and retained during the bottle’s storage.
4-EP and 4-EG Concentrations for Reds
For wines that may have had a Brettanomyces (Brett) bloom, knowing the concentrations of 4-EP and 4-EG in the wine going into bottle is a good result to keep on file. If a Brett bloom occurs later in the bottle, it is likely (although, not guaranteed) that the volatile concentration of 4-EP and/or 4-EG may increase and confirm the problem.
Furthermore, evaluating a wine for 4-EP and 4-EG concentrations can also help isolate a possibility of Brett existence, especially if their concentrations are below threshold. However, it should be noted that both compounds can also exist in wines that are stored in wood, even without a Brettcontamination.
Double Check: PCR for Reds
Brett can be a tricky yeast to isolate and identify. It is usually recommended to run multiple analytical tests related to Brett in order to confirm its existence or removal from a wine. While culture plating identifies living populations of microorganisms, PCR cannot typically differentiate between live and dead cells as it is measuring the presence of DNA. A microorganism’s DNA can get into a wine after yeast death and through autolysis. Therefore, a positive PCR result for Brettanomyces is hard to confirm if the result includes live cells, dead cells, or a combination of both.
Culture plating can help confirm the presence of active, live cells, but the success rate of growing Brettanomyces in culture plates is variable.
Nonetheless, scanning wines by PCR for Brett can help winemakers isolate a general presence and risk of Brett in their wines.
Wine samples prepare for analytical evaluation. Photo by: Denise M. Gardner
Still Worried About Your Wine Post-Bottling?
Bottle sterility testing is helpful, especially when a winemaker wants to ensure wines have been bottled cleanly. For this type of testing, it is best to sample a few bottles
- at the beginning of a bottling run,
- immediately before any breaks,
- immediately after any breaks, and
- at the end of a bottling run.
Bottles can, again, be evaluated under a microscope and evaluated for the presence of microorganisms. Bottles can also be sent to a lab for culture plating. The growth of yeasts or bacteria from culture plates at this stage indicates a failure of the sterile filtration system or contamination of the wine post-filtration. Clean wines, obviously, should help put a winemaker’s mind at ease as it matures in bottle.
Ensuring a wine’s stability post-bottling is a challenge. However, with proper cleaning and sanitation methods coupled with the right analytical records, winemakers can reduce their worry. For information on any of these topics, please visit:
- An Overview of Winery Sanitation by Patricia Howe: https://www.umpqua.edu/images/areas-of-study/career-technical/viticulture-enology/downloads/conferences/technical-symposia/2011-march-wine-flaws/2011-ts-howe-winery-sanitation.pdf
- Making Cleaning and Sanitation Practical for the Small Commercial Winery by Denise M. Gardner: http://bit.ly/PracticalWinerySanitation
- Minimizing Spoilage of Wines in Barrel by Denise M. Gardner: http://bit.ly/WineBarrelSanitation
- Bottling Line Cleaning Protocol by Scott Labs: http://www.scottlab.com/uploads/documents/technical-documents/1191/Bottling%20Line%20Cleaning%20Protocol.pdf
- Preparing Wines for Bottling by Enartis Vinquiry: http://www.enartis.com/upload/images/03_2016/160311011309.pdf
- Starting a Lab in a Small Commercial Winery: http://extension.psu.edu/food/enology/analytical-services/setting-up-your-winerys-lab
- Wine Analytical Labs: How Your Winery Can Use Them: http://extension.psu.edu/food/enology/analytical-services/wine-analytical-labs-how-your-winery-can-use-them