Laboratories for Small Brewers Kevin Mutch Peripatetic Brewer 11 - - PowerPoint PPT Presentation

Laboratories for Small Brewers

Kevin Mutch Peripatetic Brewer 11 April 19

Topics

Product consistency Sample Plan Product Specification Product testing

In-process Post-process

Equipment Required

Methodologies

Product Consistency

Consumers need consistent product Establish, measure for comparison, set of process and product specifications Take corrective action if process or product ‘out of specification’

Measuring instrument tolerance Raw materials Sampling errors Specification and tolerances i.e. Range

Sampling Schedule

Specifying where, how and frequency of sampling

Product Sample Plan

Sample Plan

Key measurements taken without exception, across whole process

– too late if quality issues come from customers

Record and present graphically

– look at trends, compare MoM/YoY

Example of Sample Plan

Stage Frequency Notes Stage Frequency Notes Raw & Packaging Materials Each delivery Frequency depends on supplier performance & reliability Fermented beer & beer ready for filtration Each vessel Monitor quality/prepare for corrective action Brewhouse

• perations

Each gyle Corrective action taken quickly Beer ready for packaging Each vessel Confirm compliance & suitability for package & consumption Unfermented wort Each gyle Corrective action taken quickly Packaged beer Each batch Monitor packaging performance Yeast Each batch for pitching Only select good yeast Plant Specified vessels per week Monitor cleaning performance Fermentation Each vessel Twice a day Process control Cleaning materials Specified samples per week Ensure plant is cleaned effectively

Product and Process Specifications

Parameter Relevance ABV Product strength & value to customer Degree of consumer intoxication Original & Present Gravities Product strength & value to customer Indicates flavour strength pH Mash & wort pH affects enzyme performance Wort & beer pH affects hop utilisation & bitterness Wort & beer pH affects microbial growth Beer pH affect flavour Variable pH affects flavour Beer Colour Immediately perceived by consumer Beer Bitterness Strong flavour effect

Product and Process Specifications

Parameter Relevance Trace flavour compounds - Diacetyl, DMS, Acetaldehyde, Esters Fermentation by-products give beer its flavour Balance ensures ‘trueness to type’ Excess will cause flavour problems Dissolved oxygen Promotes good yeast growth ergo good fermentation Oxidation in beer – stale, wet cardboard Unstable – hazes in packaged beer Dissolved carbon dioxide Sparkling characteristic of beer – head High levels – fob, dispense issues Dissolved nitrogen Foam stability, cling, flavour inhibition Beer Flavour - Trueness to type Why product is consumed Consumer expectation

Product and Process Specifications

Parameter Relevance Clarity - Haze, Potential haze Consumers expectation – attractive if ‘bright’ Cloudy beer – poor quality, contamination, infection? Head stability - Foam, Cling Consumer expectation – foamy head, cling to glass sides Sterility Microbial contamination – most destructive defect Wild yeasts, moulds, bacteria grow readily in beer Effects flavour, aroma, clarity – undrinkable? Small contaminations – growth rate – major issue

Wort Production and Brewhouse Operations

Parameter Determining factors Wort specific gravity Amount of malt and water used Extraction process efficiency Wort colour Amount of coloured material used Degree of wort boiling Wort pH Mash & wort pH Brewing water quality Liquor treatment Malt quality Adjunct type and usage rates Wort fermentability Wort attenuation limit Enzymic activity affected by mash conditions – time, temperature & pH Fermentability of raw materials & adjuncts Wort sterility Wort chiller, wort mains, FVs

Pitching Yeast Analysis

Parameter Determining factors Microbial contamination Contamination from the plant Previous generation infection Yeast viability (% dead cells) Age of the yeast Condition of the yeast Yeast vitality Health pf previous generation

Fermentation Operations

Parameter Determining factors ABV Final gravity (FG) Fermentation degree/efficiency OG Beer pH Wort pH Fermentation degree/efficiency Beer colour Wort colour Bitterness Brewhouse hop addition & utilisation Yeast counts

• cells in suspension

Strain/flocculation characteristics Cropping operation Beer flavour Brewhouse and fermentation operations Raw material quality and usage rates Contamination Beer sterility Wort sterility Yeast purity

Maturation/Conditioning Operations

As previous slide plus

Parameter Determining factors Diacetyl Maturation time and temperature Dissolved oxygen Transfer procedure Air content of vessel prior to fill Dissolved carbon dioxide Degree of fermentation Vessel back pressure at fill Beer sterility Fermented beer Transfer mains Maturation vessel

Bright Beer Production and Filtration Operations

As previous slide plus

Parameter Determining factors ABV FG Filtration/liquor flush operations Bitterness Mature beer bitterness Bitterness loss on filtration Dissolved oxygen Filtration performance Dissolved carbon dioxide Mature beer content Content trimming during filtration Clarity Maturation time & temperature Filtration performance Stabilisation

Packaging

As previous slide plus

Parameter Determining factor Air in headspace Packaging performance Fill level Packaging performance Label quality Packaging performance, labeller Label stock quality Crown quality Packaging performance, crowner Crown stock quality Can print quality Can stock quality Can seam quality Packaging performance, seamer

Out of Specification Actions

1 Current problem 2 Prevention of reoccurrence

• who, what, when, where, why & how

Real? Results correct? Extent of issue, other beers affected? When, where did it happen? What else happening at the time? Possible causes? Likely causes? What can be done about it?

Example Investigation

OOS - High colour

Investigation Action Correct results? Recheck analysis Issue extent? Check other beers When did it happen? Check previous results What else was happening? Check raw materials Possible/likely cause? New batch of raw materials What can be done? Current issue – blend gyles Future – amend recipe change supplier?

Product Specification Sheet

Example – Brewhouse specification

Parameter Addition Rate/Specification & Range Comments

• 1. Liquor Treatment:

Gypsum

(Kg/100Hl)

Sodium Chloride

(Kg/100Hl)

To achieve Product Ionic Specification: Cl=403ppm, SO4=246ppm, K=520ppm, Na=190ppm, Mg=55ppm, Ca=60ppm min NaCl & CaSO4 added to MV

• 2. Mash Grist: (As % Extract)

Plae Ale Malt Crystal Malt 88.3 1.9

• 3. Mash Additions:

B Glucanase l/tonne malt As required Optimised to suit malt performance

• 3. Hop Grist:

Variety 1 Dry Hops Variety 2 only Pellet hops to give target bitterness of 28 EBU in final pack Where added 1) Copper 2) Dry – 2 oz/brl

Example – Process Specifications

Parameter Addition Rate/ Specification & Range Comments Mashing: Mash Liquor: Liquor : Grist - Target 2.6 l/kg (Hl : Tonnes) Range Temperature Profile: Mashing Temperature °C 65 +/- 2 Variable and plant dependent Sacharification Stand °C Time of temp rise (mins) Sacharification Stand (mins) 60 mins Or until starch -ve Raise to Run-off °C 76 =/- 1 Sparge Liquor: Total Liquor : Grist: Target 4 l/kg Temperature (max) 76 Run Off: Weak wort cut off PG Last Runnings PG as ° 1004 Boiling: Pre-boil temp profile Temperature >95°C Evaporation Rate %: Target 8 Cu up pH= 5-5.3 Min 6 Cu cast pH= 4.9-5.2 Max 10 Typical FAN=120-140 at 1038 Boil Time (mins): Target 60 Apparent fermentability 84-90% Late Additions: Copper Fining As required Added prior to cast and re-boil

Example - Process Specifications

Parameter Addition Rate/ Specification & Range Comments Wort Cooling: Fill time 20 Whirlpool Stand Time: As required Target To achieve clarity Run-off profile/time (trub out proceed) Trub to drain Collection Temperature °C 16 Oxygenation ppm: Target 18 Variable on fermentation performance Range 15-22 Wort cooling additions Zinc sulphate Target 0.1 mg/l Z++ Collection gravity 1038.0 Collection time

• No. of Brews/FV

1/2 Fermented in conical

Example - Yeast Specification

Parameter Addition Rate/ Specification & Range Comments Pitching Details: Yeast Type: Ale

• Max. Generation No

15 Viability (% min) 85 Rate (million cells / ml): Target 9 x 106 Max Range 7-10 x 106 Acid Wash: Yes if required Acid Type Phosphoric pH Target 2.1 pH range 2.0 – 2.2 Contact Time Target (mins) Max 120

Example – Process Specification

Parameter Addition Rate/ Specification & Range Comments Fermentation: Profile Reference Number Temperature Profile: Collection Temperature °C 16 First Rise to °C 21 Second Rise to °C at VDK Stand - Temp Time Hold at 21 Cool to °C 6 - 8 C cask Cooling Rate °C/Hr FV Residence Targets : Time to half gravity Time to racking gravity Time to Cooling On Total Residence 3 Days 4 Days 7 Days RG target 8.5 Cycle Time target 4 days, range 3 - 5.0 days VDK Target, prior to cool as ppm N/A Time to yeast crop Rousing Regime Nil Auxiliary Finings added post - skim Fermenter Type conical

Example – Pre-packaging Specification

Parameter Addition Rate/ Specification & Range Comments Cask Run-Down: Run Down from FV to Racking Tank Yeast count 6C 1 x 106 / ml Cask Racking: Beer received into Draught Racking Tank for final checks. DO spec CO2 range Isinglass finings added to cask at rack Casks dry-hopped 0.5 ppm max. 0.9-1.1 volumes 3.25 pints/brl 2 oz/brl Typical rate

Example – In Package Product Specification

PARAMETER SPECIFICATION AQL RQL* OG PG FG FR % Alc v/v Colour, EBC Haze MU'S Bitterness, EBU Bitterness ppm iso by HPLC VDK ppm YEAST COUNT at rack CO2 (Vols)

• Keg
• Tank
• Bottle
• Can
• Cask

D.O. ppm T.I.P.O ppm HRV secs

• Rudin
• Nibem

Chloride Sulphate pH Total Carbohydrate g/100ml Calorific Value Kcals/100ml P.U's Nitrogen ppm 1037 1008.4 1007.4 1.0 max 3.7 14.5 28 28 0.07 max 1 million cells/ml 1.0 403 246 3.9 +/- 0.1 +/- 0.1 0.1 +/- 0.5 +/- 1 +/- 0.25 x 106 +/-0.2 +/-0.2 0.2 =/-0.75 +/- 2 +/- 0.5 x 106

Laboratory Analyses

What do you need for the analyses?

Minimum Required Laboratory Equipment - General

Item <25brl/wk >26brl/wk Temperature probes NOT GLASS THERMOMETERS Y Y Record/confirm process temps, long & small probes Refrigerator / cooler Y Y Sample storage, chemical storage Wrist &/or table shaker Y Beer Bitterness Centrifuge Y* Y Bitterness Units, Colour, *Yeast Solids % by Spin‐down Stir plate / hot plate Y Degassing, chemical preparation Titration burette Y Bitterness Water bath Y Y Sample attemperation Analytical balance Y Y Use in many methods for weighing all types of items. Production balance Y Y Check weigh full product containers

Minimum Required Laboratory Equipment – Physical & Chemical

Item <25brl/wk >26brl/wk Alcohol meter ? Alcohol determination CO2 meter Y* Y Dissolved CO2 - * if kegging/small pack Digital density meter ? Extract, specific gravities Distillation equipment ? Alcohol determination, bitterness Hydrometer Y Y Extract, specific gravities Oxygen meter Y* Y O2 content - * if kegging/small pack pH meter Y Y pH of source water, brewing liquor, wort, fermenting beer, fermented beer, packaged beer. CIP rinse waters UV-Visible spectrophotometer Y Beer bitterness & colour, diacetyl, FAN, total polyphenols, wort colour Haze meter Y Physical Stability

Minimum Required Laboratory Equipment – Microbiological & Sensory

Item <25brl/wk >26brl/wk Microscope Y Y Yeast cell count, viability, morphology, bacterial presence differential staining ATP luminometer Y Y Surface Hygiene Using ATP Bioluminescence Descriptive analysis Y Y Descriptive Analysis Training Y Y Selection and training of assessors, flavour terminology and reference standards

Temperature Probes

How many? Master probe Calibration check – how, when? 0oC - ice 100oC - kettle Record findings

pH meters

How many? Master meter? Calibration check – how, when? pH 4, 7, 10 Probe care! Record findings

Refractometer – area of use? Calibration check – how, when? Sample chamber care! Record findings Saccharometers - how many? HMRC acceptable ranges?

*Use a suitably calibrated saccharometer adjusted for the temperature of the representative sample Precision 10° or 20° range saccharometers (305mm long)

Gravity

Excise Notice 226: Beer Duty

ABV

Distillation method for alcohol determination Remove known volume (measured at 20°C) of beer, degas and clarify by filtration Remove the alcohol by distilling the sample and collect the distillate Make up the volume of the distillate with distilled water to that of the original sample measured at 20°C Measure the density of the sample Calculate the content of alcohol by reading the value from the official tables

Dissolved gasses

CO2 meters - areas of use? Calibration checks – how, when? Corning 965 & 50 μl pipette Sample volume check! Sample chamber care! Total in pack CO2 ‘Spike’ care DO2 Probe care!

Colour

Lovibond Colourimeter Calibration checks – how, when? Cuvette size and care? UV-Vis Spectrophotometer Calibration checks – how, when? Cuvette care? Chemical reagents required for samples

Balances

Calibrate – how , when Laboratory

• 0 - 2.0kg
• Small pack volumes

Plant

• 0 - 100kg
• Raw materials
• Large pack volumes

Microscope

Binocular microscope x40 & x100 objective lenses TV link to screen? Visual check Yeast counts Keep clean!

Heamocytometer

Methylene blue stain in yeast suspension

Usual to use centrifuge

Spin known weight slurry Pour off barm ale Weigh packed yeast The relationship between cell count and spun solids is given approximately as 10 million cells per ml = 2.5 - 3.0 g/litre spun wet yeast

Wet Yeast Pitching calculation

Microbial Contamination – Electron Micrographs

Biofilm Colonised SS surface

Microbial Presence Testing - CIP

ATP bioluminescence Swabs Records

Haze/Turbidity

Imhoff cones Hot & cold breaks Haze meter

Questions?