Quality control tests and analysis of spirits and vinegar.

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Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 1
A Seminar as a part of curricular requirement
for I year M.Pharm I Semester
Presented by
Ms. T.Jayasree (20L81S0709)
Pharmaceutical analysis
Under the guidance/Mentorship of
Dr.K.Vinod Kumar., M.Pharm.,Ph.D
Professor of pharmaceutical analysis.
Head of department- pharmaceutical analysis.
Quality control tests &Analysis
of Spirits and Vinegar

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• Introduction of spirits
• Quality control of spirits
• Analysis of Spirits
• Introduction of Vinegar
• Quality control of vinegar
• Analysis of vinegar
Contents

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• A spirit is an alcohol beverages containing ethanol. The ethanol is
produced by fermenting grains,fruit,vegetables.
• Distilled spirits are all alcoholic beverages.
• The production of distilled spirits is based upon fermentation and
Distillation.
• The principle of alcoholic distillation is based upon the different
boiling points of alcohol (78.5 °C or 173.3° F) and water (100 °C or
212° F).
Spirits: Introduction

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• For a liquid to be deemed a spirit is must be atleast 20% alcohol by
volume(ABV)and contain no sugar. By adding sugar,flavours and
other additives creates a spirit called Liqueurs.
• Common spirits are Tequella,Rum,Vodka,whiskey and Gin. Within
these common types spirits are a multitude of styles,brands,flavours.

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• There are literally 100’s of different types and styles of spirits from each and every
country.
• Bourbon whiskey,Tennessee whiskey,Canadian whiskey,Irish whiskey,Rye
whiskey,Blended Scotch whisky,Single malt Scotch whisky
• Rum
• Vodka
• Gin
• Tequila
• Brandy
• Cognac
• Armagnac
• Grappa
Types and styles of Spirits

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• Spirits are not prone to microbial contamination due to high alcohol
content, yet contamination can still occur in distilleries resulting in
product spoilage or diminished ethanol efficiency.
• Routine testing at different points in production is key; from raw
materials, to production and proofing water through to ambient air in
the bottling area.
• You are Committed to creating high-quality spirits with consistent
look,smell,feel and flavour from one bottle to the next.
Quality Control

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• We are committed to providing you the products you need to ensure
your spirits,taste,aroma and quality.
• Alcohol Determination :
• Alcohol is present as a major component in most of gelanicals.
• There are 2 methods for its determination
• Distillation method
• Chromatographic method.

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• Special treatments:
• Volatile acids and bases : render the preparation containing volatile bases
slightly acidic with sulphuric acid and acid with bases like NaOH.
• Glycerin : preparation should be diluted in such a way that the residue
after distillation should not be less than 50% water.
• Iodine : Treat solutions with powdered zinc or decolorize with sodium
thiosulphate and add few drops of NaOH.

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Distillation
• Some precaution are taken.
• Distillate should be clear, if cloudy, add talc or Caco3 and filter, adjust
temperature.
• Loss of alcohol should be minimized.
• Size of the flask should be 3-4 time larger than volume of sample used.
• Frothing should be avoided by adding H3PO4,H2SO4,tannic acid.
• Bumping can be avoided by adding small pieces of broken glass, glass
beads or porous chips.

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Method: For liquids presumed to contain less than 30%v/v alcohol.
• Take 25ml sample, add equal volume of water and distil.
• Collect distillate 2 ml less than the original volume (23ml).
• Add water to make it 25 ml.
• Adjust the temp and find specific gravity or refractive index.
• From Alocholmetric table find the percentage of alcohol.

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 For liquids presumed to contain more than 30% v/v alcohol.
• Take 25 ml sample add 50 ml water and distil.
• Collect distillate 2 ml less than 50ml(48ml).
• Add water to make it 50ml.
• Adjust temp and find specific gravity or refractive index.
• From Alocholmetric table find the percentage of alcohol.
• The proportion of alcohol is 1/2 of liquid so multiply it with 2 to get
exact percentage of alcohol in sample.

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• Moisture Determination:
• To ensure the consistency and quality of your spirits, you need to
have confidence in the quality of your raw materials.
• To do this, you must prevent fungal contamination in your raw
materials by checking their moisture content before you start
fermentation and distillation.

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• Also, at the end of production, to recycle waste and get the most out of your by-
products, you can sell your spent grain as livestock feed.
• Here, testing its moisture content is again critical to avoiding fungal
contamination.
• we have to test Moisture determination of incoming raw materials and Moisture
analysis on spent grains.

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• Water Testing
• Although routinely perform microbiological and chemical water monitoring,
contamination can occur in your distillery during the production process, so regular,
weekly testing of water supplies and piping, tubing/gaskets is recommended.
• Water is also added at the proofing stage of your spirit production to reduce the
percentage alcohol or “proof” to a safe, drinkable level.
• The water quality you use for this application must be of a purity standard appropriate
for drinking water, or there is a risk of "floc haze" appearing in the spirits during
bottling due to chemical contaminants precipitating out or a microbial biofilm
developing.

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• Spoilage Testing:
• Despite the anti‐microbial properties of spirits and having a Hazard
Analysis and Critical Control Point system (HACCP) system in place,
microbial contamination can occur before distillation and in your proofing
water.
• This can lead to the formation of floc or haze in your spirits, which can
affect your shelf life stability and customer’s confidence in your brand.
• The products and solutions for fast,effective,and efficient detection and
capture of potential spoilage-producing microorganisms to maintain the
quality of your spirits on the shelf.

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• Analytical QC:
• If your spirits age in wooden barrels, they acquire tannins, sugars, complex biochemical
compounds and color, as well as undergo significant chemical reactions.
• The profile of your spirits are modified in ways that are complex and analytical sample
testing can be used to detect or follow changes as your spirits age.
• Based on blending, process, aging and additives, you can characterize distinct
fingerprints both within the same type of spirit and detect differences in your brand.
• Eventually, it is possible to generate a product fingerprint library that you can use to
help maintain product quality and detect adulteration of your spirits to ensure it meets
your customer’s high standards.

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• These tests can detect the following:
• Sugar content, nitrogen compounds, salts and minerals, and other
compounds that may be present
• Alcohol content
• Measurement of pH value
• Compounds such as international bitterness units (IBUs),
polyphenols , free amino nitrogen, sulfur dioxide

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• Ash content before distillation (in rum only)
• Color measurements
• Overall "proof" or alcohol concentration after distillation using a
hygrometer
• Alcohol content using a pycnometer or dry matter determination of
residue on ignition.

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• To run any analytical or sensory tests, you need the right tools for
sample preparation, such as pipettes, laboratory balances, syringe
filters, filter papers and water purification systems.
• The quality of your results is dependent on the quality of your
sample, and we provide the right products and solutions to make
your sample preparation for analytical testing quick, accurate and
efficient.

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• Check Weighing
• Accurately determining if your bottles are over or unfilled with spirits, is a critical step in
ensuring product quality and maintaining your brand’s reputation with customers.
• Our balances provide a reliable method of checking the weight of filled bottles of spirits.
• Their height supports easy handling of glass bottles and using the Check Weighing program
with defined limits and weighing visual aids means that with minimal training your staff can
control the weight of filled bottles or nominal gross weights more accurately and cost-
effectively than you would using balance technology built into your production line.

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 Gas chromatography
• Gas chromatography (GC) is an analytical technique for volatile and semi-volatile
compounds.
• Many ethanol analyses have done with GC since impurities in ethanol are basically
volatile as well as ethanol itself .
• A sample is vaporized at an injection port by heat. The sample vapor is sent to
column packed with adsorbent or absorbent.
• Inside column, each component in sample is separated depending on its physical
and chemical property. The end of column the concentration of each compounds
are measured by a detector. There are many kinds of coatings for column.
Analysis of Spirits:

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• A coating should be chosen depending on the target compounds. Also, there are
many kinds of detectors.
• Each detector has advantages and disadvantages. Thus, a detector should also be
chosen carefully to detect target compounds.
• Gas chromatography-mass spectrometry (GC-MS) is an integrated system of two
analytical equipments.
• Gas chromatography separates analytes and mass spectrometry identifies them.
GC-MS accelerates ethanol analysis with its simultaneous separation and
identification capavities.

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• A typical GC chromatogram of alcoholic beverage is shown in the figure:
Typical GC chromatography of alcoholic beverages (rum)(Garruti et.al.,2006)

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Infrared spectroscopy
• Infrared spectroscopy (IR) is an analytical technique utilizing infrared adsorption.
• Infrared with different wavelengths are passed though a liquid sample.
• Infrared is adsorbed by a compound, and the absorbability of infrared varies among
different compounds and different infrared wavelengths.
• Samples are identified by comparing absorbability of infrared,.IR does not have as high
resolution as GC or HPLC.
• However, the equipment is relatively cheap and analysis is simple and quick.
• Thus, it utilizes more for quality assurance (Lachenmeier, 2007) and classification purposes
(Pontes et al., 2006).

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• A typical IR spectra of alcoholic beverage is shown in the figure:
Typical FTIR spectra of different commercial alcoholic beverages
(Gallignani et.al 2005)

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Olfactometry
• Olfactometry is a sensory analysis usually coupled with GC. For a typical GC-
Olfactometry (GC-O) system, a GC column is connected to a separator where
analytes are separated to two ways.
• Olfactometry and a detector such as FID, PID, and MS. Olfactometry is a simple
system which is just an open-end column, and a panelist sniffs analytes coming
from the column.
• The panelist records the odor character and intensity of the analyte which
correspond with a peak in chromatogram.
• Olfactometry provides flavors data rather than stoichiometric chemical data.
• It is utilized for alcoholic beverage analysis to develop its flavor.

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• Vinegar is a product resulting from the conversion of alcohol to
acetic acid by acetic acid bacteria , Acetobacter spp.
• The name is derived from French(Vin=wine; Aigre-sour )
• When alcoholic fermentation occurs and later during acidifications
many other compounds are produced.
• Depending mostly on the nature of the material fermented and
some of these find their way into vinegar.
Vinegar: Introduction

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• Reactions also occurs between these fermentation products.
• Ethyl acetate , for example, is formed from the reaction between
acetic acid and ethanol.
• It is these other compounds which give the various vinegars their
organoleptic properties.
• Vinegar is regulated by the Food and Drug administration (FDA) and
to be legal must have a minimum of 5% acidity.

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• Food condiment, sprinkled on certain foods such as fish.
• For pickling and preserving meats and vegetables; it can reduce the pH
of food below that which even spore formers may not survive
• Manufacture of sauces, salads dressings, mayonnaise ,tomato
productions, cheese dressings, mustard and soft drinks.
• Wide variety of illness such as plague ,ringworms,burns,lameness.
• Used as cosmetic acid and cleansing agent.
Uses of Vinegar:

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• The composition and specifications of various types of vinegars are defined
by regulations set up the governments of different countries.
• In the United States, for example, vinegar should not contain less than
0.4%(w/v) acetic acid and not more than 0.5% ethanol (v/v).
• The various major vinegars are defined briefly:
(i) Cider vinegar, apple vinegar: Vinegar produced from fermented apple juice
and non-grape fruits.
Types of Vinegar:

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(ii) Wine vinegar, grape vinegar :Fermented grape juice.
(iii) Malt vinegar: Produced from a fermented infusion of barley malt
with or without adjuncts.
(iv) Sugar,glucose,dried fruits.
(v) Spirit vinegar: Vinegar made from distilled alcohol.
(vi) Some specialty vinegars: formulated or flavored to provide a
special or unusual taste when added to foods .

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• The quality control of vinegar regards to strength or pH of the
vinegar. This therefore, refers to the ethanoic or acetic acid content
in the vinegar.
• There are two ways of describing the strength of vinegar:
1. Its acidity ,which is measured as a pH value.
2. Its concentration, which is the amount of acidity in a given volume
of liquid and which is measured in percent.
Quality control of Vinegar

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• To measure the pH of vinegar ,simply use a pH strip
• The resulting color will tell you how strong the vinegar is.
• Distilled white vinegar usually measures around pH 2.4,with a
strength of at least 5%.
• The vinegar should be pure of any additional flavors,sugars,or
bacteria.
Measuring the pH value of vinegar

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• To determine the amount of acetic acid in the vinegar liquid, you
need special equipment.
• You can use acid test kits at a beer- and wine making supply shop
these are designed to test the acidity of wine, and generally will not
measure an acidity of more than 1%.
• To be described as “vinegar", a liquid must have at least 4% volume
of acetic acid.
Measuring the strength of Vinegar

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• Vinegar is a sour liquid consisting mainly of acetic acid and water.
Acetic acid (CH3COOH or HC2H3O2) is the source of the acidity in
vinegar. Acetic acid is an organic acid (Carboxylic acid) and is classified
as weak acid
• The percent acidity in a sample of vinegar is calculated by
%acidity = (grams of acetic acid/grams of vinegar) x 100
Vinegar analysis

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• In this experiment a commercial vinegar sample will be analyzed for its
percent acidity by an analytical procedure called Titration.
• Titration is an analytical method for determining the concentration of an
acid or base by adding quantities of either the acid or the base of known
concentration(standard solution) to a measured volume of the test
solution until complete neutralization occurs.
• In this experiment the gradual addition of a basic solution (NaOH) of
known concentration will be gradually added to a known volume of the
vinegar solution.

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K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721
• The point at which the neutralization is complete is referred to as the endpoint and is
observed by the color change in the added indicator , phenolphthalein.
• The analysis of vinegar will be accomplished out by titrating a 5.00mL of sample of
vinegar with a solution of NaOH of known molarity .
CH3COOH(aq ) + NaOH(aq )CH3COONa (aq ) + H2O(I)
• Because the reaction stoichemetry is one mole of acetic acid reacting with one mole
of sodium hydroxide ,the number of moles of acetic acid in the portion of the vinegar
sample titrated can be found from equation.
moles of acetic acid = (MNaOH) (VNaOH)
37

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• MNaOH is the molarity of the sodium hydroxide solution in moles/L and
VNaOH is the volume of sodium hydroxide solution in liters
• The grams of acetic acid in the vinegar sample can be calculated by
multiplying the moles of acetic acid by the molecular weight of acetic acid
(MW).
grams of acetic acid = (moles of acetic acid )(MW)
• By assuming the density of the vinegar sample to be 1.00g/mL,the grams
of vinegar by the density.
grams of vinegar = (volume of vinegar)( density of vinegar)

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• The percent by mass of acetic acid in the vinegar sample can be found from
equation .
%acetic acid = (grams of acetic acid/grams of vinegar)x 100
Procedure:
• Clean a burette by rinsing it with tap water and discarding the water.Next,rinse the
burette with two 5mL portions of NaOH standard solution, discarding the NaOH
after each rinse.
• Fill the burette with NaOH standard solution to slightly above the zero mark and
setup the burette as demonstrated by the lab instructor.

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• Drain enough NaOH solution from the burette so as to remove all the air bubbles from
the tip of the burette and read the level.
• Record this reading as the intial volume to ±0.01mL on the data sheet for NaOH.
• Repeat steps 2-4 for the vinegar burette.
• Drain approximately 5mL of the vinegar from the burette into a clear 250mL
Erlenmeyer flask. Record the final volume to 0.01mL on the data sheet for vinegar.
• To the vinegar sample, add about 20mL of distilled water and four drops of
phenolphthalein indicator solution.

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• Carefully place the flask containing the vinegar and indicator under the
burette .slowly add NaOH from the burette to the flask ,while swirling the
flask, until the solution in the flask is a faint permanent pink.
• At the end point ,the solution will be red and you must discard your results.
• Record the final volume to ± 0.01mL on the data sheet of NaOH.
• Perform a second titration by refilling the NaOH and repeating steps 6-8.
• Carry out the calculations.

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1. Biernacka P, Wardencki W. Volatile composition of raw spirits of different
botanical origin. Journal of the Institute of Brewing. 2012 Dec;118(4):393-
400.
2. American Society of Brewing Chemists. Technical Committee, Kneen E.
Methods of Analysis of the American Society of Brewing Chemists. The
Society; 1976.
3. Nascimento RF, Marques JC, Neto BS, De Keukeleire D, Franco DW.
Qualitative and quantitative high-performance liquid chromatographic
analysis of aldehydes in Brazilian sugar cane spirits and other distilled
alcoholic beverages. Journal of Chromatography A. 1997 Oct 3;782(1):13-23.
References:

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4.Caligiani A, Acquotti D, Palla G, Bocchi V. Identification and quantification of the
main organic components of vinegars by high resolution 1H NMR spectroscopy.
Analytica Chimica Acta. 2007 Feb 28;585(1):110-9.
5.Sáiz-Abajo MJ, González-Sáiz JM, Pizarro C. Prediction of organic acids and other
quality parameters of wine vinegar by near-infrared spectroscopy. A feasibility study.
Food Chemistry. 2006 Jan 1;99(3):615-21.
6.Kahn JH, Nickol GB, Conner HA. Analysis of vinegar by gas-liquid chromatography.
Journal of Agricultural and Food Chemistry. 1966 May;14(5):460-5.

Quality control tests and analysis of spirits and vinegar.

Quality control tests and analysis of spirits and vinegar.

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Quality control tests and analysis of spirits and vinegar.