Bourbon, Brews & UFOs!

Identifying Unknown Materials in the Food & Beverage

Industry Using FTIR Microspectroscopy

ABSTRACT
Nothing beats a cold, refreshing beverage on a hot day. But that refreshing experience
can quickly fade when a small unknown material is spotted in your glass. Food, beverage and
spirit producers are constantly faced with the daunting task of ensuring the upmost quality of
their products for this very reason. Whether it’s an old recipe or a new creation, unknown
contaminants can occur and delay the delivery of product. To understand the root cause, quick
identification is needed over a wide range of materials. Although contaminants are very small
and barely visible to the unaided human eye, they plague producers and exasperate consumers
ever more frequently.

This webinar will provide an overview of the sampling and identification techniques used
to solve contamination issues in beverage and spirits. We will demonstrate how simplified FT-IR
microspectroscopy can provide rapid identification of unknown materials. We will further
examine the most suitable approaches to microanalysis for a range of contamination issues
related to the production and bottling of various beverages and spirits. Although the main topic
relates to the spirits industry, the technique can be applied to the food and beverage industry as a
whole.

Topics Covered:
 Learn how to prepare samples for microanalysis using FTIR microspectroscopy

 Understand the information FTIR analysis can provide and how to relate that back to the
process

 Useful insights to common contaminants in the distilling and brewing process

Speakers:

Dr. David Schiering Founder & Principal, Czitek

Dr. Gary Spedding, Brewing, Distilling Analytical Services

Agenda

- Contaminants in the food and beverage industry

- Brewery and distillery industries challenges
- Technical solutions
- FTIR microspectroscopy introduction
- SurveyIR microanalysis accessory
- Contaminants in Brews and Spirits
FOOD AND BEVERAGE INDUSTRY

- Food and beverage industry is controlled by consumers

- Despite of manufacturers’ best efforts, contamination of products still occur
- Contaminants cause adverse effects (production downtime, customer impact)
- Social media platforms help spread vital information but can also spread bad news very
quickly ( e.g. E.coli in Romaine letture, plastics in salts)

How problematic can they be?

- Contamination shuts down process line 6 times per year

- Outside analytical service can take even longer

Common Food contaminants

- Salmonella, E. Coli, Norovirus
- Pesticides
- Plastics
- Bugs
- Fibers & hairs
- Packaging materials
What about beverages?
- Commonly stored in transparent containers (The human detect particles 50-100
micrometers dimension. Leaving contaminants in plain sight)
- Visible contaminants are actually small pieces of raw materials and are naturally in the
beverages (Tea, unfiltered Beer & wine)
- The brewing and distilled spirits industry is plagued with visible contaminants in the
form of hazes and UFO’s (unidentified floating objects)
- Large, well established spirit and beer producers have sorted out many of the haze issues.

- Spirits are more difficult to address with than beer

- Old distilleries have passed down knowledge and have perfected their recipe over the
years

- New distilleries face many challenges (new production processes, new spirit creation
etc.)
How Do Producers address these issues?
- Visible observation and advanced imaging technology
- Quality test using specific instrumentation
o Visible Microscopy
 o IR spectroscopy
- Near IR (process control, raw material qualification, mixing, e.g
Carbohydrate concentration in grains)
- Mid IR (Reaction monitoring, trans fat, protein, sugar and concentrations,
e.g. Dairy and Wine analyzers)
- Filter Photometers (dedicated to process analyzers, e.g. ethyl alcohol in
beverages)
o Gas chromatography ( Pesticides and Toxic industrial Chemicals)
o X-ray ( Metals)

WHAT IS IR SPECTROSCOPY (Same with definition sa Webinar 4)

Additional notes
 Water has IR spectrum exhibiting bending and stretching vibrations of OH bonds
 Extensive spectral libraries can be used to identify unknown samples.

INSTRUMENT PRESENTED (SurveyIRTM Advantage)

- A simplified IR Microspectroscopy
- Interfaces to virtually all commercial FTIR spectrometers
- Has ease of use features and has user friendly software
1. Sample compartment mounted
2. Single USB connection
 3. Quick clip on diamond attenuated total reflection (ATR) element
4. Large depth and field of view
5. Transmission/ Refelction/ ATR modes
- No liquid nitrogen required
- Portable
- Affordable microspectroscopy solution

 ATR – a contact technique where measures material by contacting it with diamond

crystal
THE HAZE PROBLEM
 - Hazs are result of light scattering by colloidal or larger particles suspended in a
solution
- Hazes are unappealing and signal an issue with beverage to consumers
MATERIAL THAT CONTRIBUTES TO HAZES

 Pink to red stain – indicates polyphenol protein problem

 Tool used = light microscopy
  Needle like crystals ( like on spirits) indicate problems
 Oxalate crystals on beers are commonly calcium oxalates ( beer stone build
ups)

LIMITATIONS
Traditional Limitations
o Small amount of particulate ( Small , 3-10 mg/L)
o Unambiguous identification of the nature of material ( time consuming
and difficult, “If oxalate crystals aren’t seen nor staining reveal protein or
carbohydrate then what?”)
FTIR Microspectroscopy Solution
o A single particle can be used for identification and reused for other
sampling technologies (just like SurveyIR)
o Libraries are good as you make them
Data Analysis
CONCLUSION:
- Increasing number of new spirits/brews and new approaches to their creation are
leading to a plethora and new haze & UFO’s
- Current methods of addressing haze/ UFO issues can be time consuming and tedious
 - Careful brewing and distillation processes can resolve some haze issues
- New FTIR microspectroscopy tools can expose important details on UFO and haze
issues
- The SurveyIR microanalysis accessory can provide the necessary details without
burden typically associated with FTIR microspectroscopy
Q&A
 What if the sample cannot be identified by data base search?
- Data bases can be bought commercially. The best results that can be
obtained with library searching method by mixing commercial data bases
and home-grown data bases….. These libraries can be user-generated or
user edited and the best result is when you developed your own library
based on the material that you encounter in a daily basis either process or
manufacturing of product.
 What IR collection mode should be used in the analysis?
- It depends on the sample. Not all samples are amenable to ATR
analysis such as small samples especially that are below 100 microns.
 Do you have to use 200 proof ethanol or water as reference or
background so it does not interfere with search match data base?
- Yes, if you are doing solution spectroscopy. But in the context of
microspectroscopy, those dried films had water present. They were dried but water were
bound to carbohydrates, polysaccharides (which contains OH groups and hydrogen
bonds.). In that case, you will not collect the background through solvent matrix.
 How can you identify mixture samples?
- There are two ways. First spectral library search method incorporated with automated
mixture software. The mixture is resolved using known materials in the library.
Second method is manual, you will still infrared data base use when you do spectral
search of the unknown, the component with high concentration in mixture, which was
high on the match list .It is important to overlay the unknown spectrum with library
spectra and make sure that you have overlap, correlation, correspondent of the
signature of the unknown. And with the use of the software, you can subtract out the
component at highest con and remove it on from spectral signature and search the
residual and identify the second component and continue the process.