WINE ANALYSIS COPYRIGHT F. GADEK 04/18/2003
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SOME CHEMICAL WINE ANALYSESSOME CHEMICAL WINE ANALYSES
FRANK J. GADEK, Ph.D., FAIC
ENOLOGY EDUCATION SERVICES
WINE ANALYSIS COPYRIGHT F. GADEK 04/18/2003
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TOPIC –TOPIC –
“ “ SOME CHEMICAL SOME CHEMICAL WINE ANALYSES “WINE ANALYSES “
SCIENCE, TECHNOLOGY & SOCIETY SCIENCE, TECHNOLOGY & SOCIETY { { “STS” “STS” }}
BYBY
FRANK J. GADEK, PH.D.FRANK J. GADEK, PH.D.
WINE ANALYSIS COPYRIGHT F. GADEK 04/18/2003
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WORK IN PROGRESS!!!
THOUSANDS OF SLIDES AND DOZENS OF PRESENTATIONS ARE
IN THE PROCESS OF BEING UPGRADED, REVISED, UPDATED,
IMPROVED, ETC. AS TIME AND RESOURCES PERMIT
08/08/99/© FRANK J. GADEK, PH.D., FAIC
WINE ANALYSIS COPYRIGHT F. GADEK 04/18/2003
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SO FAR AT LEAST 5000 COLORED SLIDES REDONE, UPDATED &
REVISED IN AT LEAST 40 SLIDE TRAYS
WITH AT LEAST THAT AMOUNT TO GO
PLUS NEW MATERIAL AND TOPICS BEING CONTINUOUSLY ADDED
08/08/99/© FRANK J. GADEK, PH.D., FAIC
WINE ANALYSIS COPYRIGHT F. GADEK 04/18/2003
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NOW CONVERSION OF SLIDE PRESENTATIONS TO MICROSOFT
POWERPOINT COMPUTER PRESENTATIONS
CAN READILY USE MICROSOFT WORD SLIDE TEXT FILES
BUT PICTURE SLIDES NEED TO BE DUPLICATED WITH A SPECIAL
SCANNER WHICH IS A RELATIVELY SLOW PROCESS
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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DISCLAIMER / WAIVER - GENERAL
1] PRESENTATIONS, INFORMATION, ACTIONS, AND PARTICIPATION ARE OFFERED IN GOOD FAITH AND ARE BELIEVED TO BE ACCURATE AND APPROPRIATE AT THE TIME GIVEN
2] NO LIABILITY AND / OR RESPONSIBILITY, INCLUDING
ANY ASSOCIATED EXPENSES, IN ANY WAY AND IN ANY FORM WHATSOEVER, CAN BE REQUIRED, ACCEPTED, IMPLIED AND / OR ASSUMED WITH RESPECT TO THE USE OR NON-USE OF THIS INFORMATION
3] THE DECISION TO USE AND HOW TO USE, OR NOT
USE, THIS INFORMATION AND ANY AND ALL RESULTING CONSEQUENCES, ARE TOTALLY AND ONLY UP TO THE INDIVIDUAL MAKING AND / OR RESPONSIBLE FOR THESE DECISIONS
4] LEGAL, PROFESSIONAL AND OTHER ADVICE /
INFORMATION SHOULD BE SOUGHT AS APPROPRIATE AND / OR AS NECESSARY
5] INFORMATION PROVIDED IS ONLY A STARTING POINT
AND DOES NOT REPRESENT THE MINIMUM THAT MAY BE REQUIRED
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DISCLAIMER / WAIVER – GENERAL - CONTINUED 6] NO WARRANTY, CERTIFICATION, GUARANTEE,
PROMISE AND / OR REPRESENTATION IS MADE AS TO THE ACCURACY AND / OR SUFFICIENCY OF THE INFORMATION
7] ADDITIONAL INFORMATION AND / OR MEASURES MAY
BE REQUIRED 8] PERTINENT LOCAL, STATE, FEDERAL AND OTHER
LAWS SHOULD BE CONSULTED AS NECESSARY AND / OR AS APPROPRIATE BEFORE INITIATING ANY ACTIONS AND / OR DECISIONS WITH RESPECT TO THIS INFORMATION.
9] NEW INFORMATION MAY BECOME AVAILABLE AT
ANY TIME AND SHOULD BE OBTAINED AND EVALUATED AS NECESSARY AND / OR AS APPROPRIATE
10] ADDITIONS TO THIS DISCLAIMER / WAIVER MAY BE
MADE AS NECESSARY AND / OR AT ANY TIME 11] WRITTEN COPY OF THE ABOVE CAN BE OBTAINED
UPON REQUEST FRANK GADEK, PH.D., FAIC ENOLOGY EDUCATION SERVICES 4744 EAST MILL HILL ROAD EAST GREENVILLE, PA 18041-2633 PHONE / FAX: 215-679-8289
WINE ANALYSIS COPYRIGHT F. GADEK 04/18/2003
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MUST AND WINE ARE
EXTREMELY COMPLEX “BIOCHEMICAL SOUPS!
[BEELMAN, PW, 1-2/1984, 38-42]
09/01/99 FRANK J. GADEK, PH.D., FAIC
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WINEMAKING
IS BOTH
A SCIENCE [PREDICTABLE]
AND
AN ART [NOT PREDICTABLE]
08/08/99/© FRANK J. GADEK, PH.D., FAIC
WINE ANALYSIS COPYRIGHT F. GADEK 04/18/2003
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“LIKE TRYING TO HIT A MOVING TARGET IN THE DARK”
09/01/99 FRANK J. GADEK, PH.D., FAIC
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“SUPERIOR” VITICULTURE AND ENOLOGY
BOTH REQUIRED FOR
CONSISTENCY AND IMPROVING
QUALITY
IN ORDER TO INCREASE PROFITS
08/08/99/© FRANK J. GADEK, PH.D., FAIC
WINE ANALYSIS COPYRIGHT F. GADEK 04/18/2003
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WINEMAKING
USES VARIABLE AGRICULTURAL PRODUCT / PROCESS
NEED CONTROLS TO GET
CONSISTENCY
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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“TODAY, THE CHEMICAL ANALYSIS OF WINE IS ONE OF THE MOST
POWERFUL TOOLS IN THE PRODUCTION OF WINES, DURING THEIR AGING AND FINISHING, AS WELL AS IN THEIR RESEARCH.”
[AMERINE & OUGH IN THEIR W & M
ANALYSIS TEXT] 08/08/99/© FRANK J. GADEK, PH.D., FAIC
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PHILIP WAGNER
AT 11TH PA WINE CONFERENCE
“TO SOLVE BAD WINE PROBLEMS -
1] LOCAL WINE ANALYSIS LABS
2] INSTRUCTION - SHORT COURSES”
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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“THERE IS A NEED FOR MODEST LABORATORIES, PUBLIC OR
PRIVATE, THAT CAN PROVIDE ROUTINE WINE PRODUCTION
ANALYSES AND RECOMMENDATIONS, SUCH AS
EXIST THROUGHOUT WINEGROWING EUROPE AND IN
CALIFORNIA” [WAGNER IN PTITUS,COMSTOCK,210]
09/01/99 FRANK J. GADEK, PH.D., FAIC
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“TODAY, THE CHEMICAL ANALYSIS OF WINE IS ONE OF THE MOST POWERFUL TOOLS IN THE PRODUCTION OF WINES, DURING THEIR AGING AND FINISHING, AS WELL AS IN THEIR
RESEARCH.” [A&O,MFAOMAW,WILEY,PV-VI,1980]
09/01/99 FRANK J. GADEK, PH.D., FAIC
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“IN ADDITION, THE MODERN ENOLOGIST MUST BE CONCERNED ABOUT LEGAL LIMITS ON THE AMOUNTS OF NATURAL AND ADDED
COMPONENTS. MOREOVER, QUALITY CONTROL DEMANDS CONSTANT ANALYSES, TO ENSURE THAT ACCEPTABLE STANDARDS ARE MAINTAINED FOR THE EVER-INCREASING
NUMBER OF COMPONENTS.”
[A&O,MFAOMAW,WILEY,PV-VI,1980] 09/01/99 FRANK J. GADEK, PH.D., FAIC
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MANAGING WINE PROBLEMS BY DEVELOPING OPTIONS REQUIRES
SOPHISITICATED INTERPRETATION OF KEY PROCESSING, CHEMICAL
AND MICROBIOLOGICAL INFORMATION
“OUTSIDE EXPERTISE MAYBE
REQUIRED”
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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“COSTS OF WINE CHEMICAL ANALYSES FOR A SMALL WINERY,” FRANK & LOIS GADEK, WINE EAST, 9(1), 14 - 20 (1981).
09/01/99 FRANK J. GADEK, PH.D., FAIC
WINE ANALYSIS COPYRIGHT F. GADEK 04/18/2003
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WINE ANALYSES OPTIONSWINE ANALYSES OPTIONS
§ DO AT WINERY
§ COMMERCIAL LABS
§ COMBINATION
¥ONLY ABOUT 10 TO 20 ¢ / BOTTLE
¥ INEXPENSIVE INSURANCE!
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MY EMPHASIS
PRACTICAL
WINEMAKING
WINE ANALYSES & INTERPRETATION
09/01/99 FRANK J. GADEK, PH.D., FAIC
WINE ANALYSIS COPYRIGHT F. GADEK 04/18/2003
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FOCUS
INFORMATION ON 10,000 TO 20,000 GALLON
SMALL WINERIES
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SMALL FARM WINERIES
4 RANGE FROM SOPHISTICATED TO PRIMITIVE
4 MOST ESSENTIALLY 1 MAN OR FAMILY OPERATIONS
4 UNINHIBITED BY TRADITION, HIGHLY EXPERIMENTAL IN ATTITUDE TOWARD GRAPES & WINE TYPES
4 MARKETS PRIMARILY LOCAL [WAGNER IN PTITUS,COMSTOCK,205]
09/01/99 FRANK J. GADEK, PH.D., FAIC
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LLOOWW TTEECCHH / HIGH TECH
“PROPER USE” OF TECHNOLOGY
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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EMPHASIZE “PRACTICAL” LAB METHODS THAT SMALL WINERIES
CAN REASONABLY DO WITH RESPECT TO PERSONNEL,
EQUIPMENT, CHEMICALS, TECHNIQUES, TRAINING AND
RESULTS REQUIRED FOR A SMALL WINERY
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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BASIC COMPONENTS OF THE “MUST”
¤ MAIN INGREDIENT
¤ WATER
¤ SUGAR
¤ ACIDS
¤ YEAST
¤ YEAST NUTRIENT
¤ MISCELLANEOUS – COLOR, TANNIN, FLAVOR, BODY, AROMA, BOUQUET, ETC.
03/15/2003 FRANK J. GADEK, PH.D., FAIC
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COMPOSITION OF TABLE WINE
WATER: 85 – 95% ALCOHOL: 8 – 14% OTHER: <1 - 2% ACIDS: 0.4 – 1.0% MISC.: <0.2 – 1.0% - CONTRIBUTE TO COLOR, FLAVOR, BOUQUET, ETC. – VERY CRITICAL TO QUALITY OF WINE
- MANY IN PPM, PPB, PPT, ETC. RANGE
03/15/2003 FRANK J. GADEK, PH.D., FAIC
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KNOWN WINE CONSTITUENTS 1820 – 6 – ACID, ALCOHOL,
TARTAR, BOUQUET, EXTRACTIVE, COLORING PRINCIPLE
1956 – 150 1961 – 200 1970’S – 300 TODAY – MANY THOUSANDS AND
CONTINUING TO INCREASE DRAMATICALLY!
[MADE POSSIBLE BY SOPHISTICATED MODERN INSTRUMENTATION AND
COMPUTERS]
03/15/2003 FRANK J. GADEK, PH.D., FAIC
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SOME GENERAL GUIDELINES
TO AT LEAST GET YOU INTO THE
“BALLPARK”
OF MAKING ACCEPTABLE
TABLE WINE!!!
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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NOTE:NOTE: SOME WINE ANALYTICAL VALUES ARE NOW REPORTED -
AS GRAMS / LITER [G / L] [E.G., TOTAL TITRATABLE ACIDITY VOLATILE ACIDITY, ETC.
IN THE PAST, MANY WINE ANALYTICAL VALUES WERE REPORTED AS PERCENT [%, GRAMS / 100 ML, G / 100 ML]
IMPORTANT WHEN COMPARING PAST AND NEW LITERATURE VALUES
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DESIRED MUST ANALYSIS FOR DRY TABLE WINES
DEGREE BRIX pH % TTA WHITE 19.5-23.0% 3.0-3.3 0.7-0.8% RED 20.5-23.5% 3.2-3.4 0.65-0.75% [BOULTON, PPW, P#54]
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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DESIRED “WINE” ANALYSIS FOR DRY TABLE WINES
%TTA pH %VA %RRS EtOH 0.6-0.9 < 3.6 <0.030 0.1-0.2 10-14
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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NOTE – STARTING IN 2003
ALCOHOL AND TOBACCO TAX AND TRADE [ATTTB OR TTB]
NOW IS RESPONSIBLE FOR WINERIES INSTEAD OF
BUREAU OF ALCOHOL, TOBACCO AND FIREARMS [BATF OR ATF]
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SOME TABLE WINE COMPONENTS REGULATED BY “BATF”
ETHANOL - MAX. 14% EXTRACT - G / 100 ML WHITE - MIN. 1.6 RED - MIN. 1.8 TOTAL SULFUR DIOXIDE - 350 PPM [MG / L]
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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VOLATILE ACIDITY {VINEGAR}
[EXCLUSIVE OF SO2, G AcOH / 100 ML OR %] WHITE - 0.120 RED - 0.140 [CALIF. AND OTHER COUNTRIES HAVE OTHER LIMITS]
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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SIX CRITICAL CHEMICAL ANALYSES [TESTS]
JUICE SUGAR - % TSS - MAKES ALCOHOL, LEGAL, TASTE, PRESERVATION ACID - % TTA - PROPER FERMENTATION, TASTE, PRESERVATION pH - PROPER FERMENTATION, TASTE, PRESERVATION
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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WINE SUGAR - % RRS - >0.2 - THEN PRESERVATION NEEDED ACID - % TTA - TASTE, PRESERVATION pH - TASTE, PRESERVATION
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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BESIDES “6 ESSENTIAL TESTS” ON MUST / WINE
FREE SULFUR DIOXIDE - “TITRETS™” ALCOHOL - BATF REQUIRES ACCESS TO DETERMINATION [ALSO HOW TO USE EQUIPMENT?] - EBULLIOMETER OR DISTILLATION / HYDROMETRY MLF CHROMATOGRAPHY - ALSO FOR TA / MA RATIO & DEACIDIFICATION?
09/01/99 FRANK J. GADEK, PH.D., FAIC
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MINIMUM BATF REQUIREMENTS
ARE THE CAPABILITY TO MEASURE ETHANOL AND FILL LEVEL
[ZFGN,WAAP,1995,#5]
09/01/99 FRANK J. GADEK, PH.D., FAIC
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ONLY A FEW DIFFERENT BASIC LAB PROCEDURES / TECHNIQUES CAN
BE USED FOR MANY OF THE CRITICAL CHEMICAL ANALYSES
FOR MUST / WINE 08/08/99/© FRANK J. GADEK, PH.D., FAIC
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VERY SIMPLE * HYDROMETRY / REFRACTOMETRY / TEMPERATURE MEASUREMENT / CHART CORRECTIONS * pH - CALIBRATION / ELECTRODE CARE / TEMPERATURE CORRECTIONS * TEST PAPERS / KITS - pH, SO2, ACIDITY [E.G., CLINITEST, TITRETS, QUANTOFIX, ETC.]
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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MORE COMPLEX * TITRATION - ACID / BASE OXIDATION / REDUCTION * DISTILLATION - REGULAR STEAM * PAPER CHROMATOGRAPHY
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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SOME COMMON CHEMICAL ANALYSIS [TEST] PROCEDURES
* TOTAL SOLUBLE SOLIDS [%TSS] - HYDROMETER, REFRACTOMETER * TOTAL TITRATABLE ACIDITY [%TTA] - TITRATION, KITS, TEST PAPERS * pH - METER, TEST PAPERS * ALCOHOL [ETHANOL, EtOH] - EBULLIOMETER, DISTILLATION / HYDROMETER
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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* SULFUR DIOXIDE - FREE & TOTAL
TITRATION - - RIPPER, - DISTILLATION [AIR OR N2] - THEN - AERATION / OXIDATION, - MONIER- WILLIAMS SPECIAL TEST PAPERS “TITRETS™” KITS - [AMPULES, RIPPER]
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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* VOLATILE ACIDITY {VINEGAR} CASH DISTILLATION / TITRATION * TOTAL PHENOLS [TANNINS] TITRATION [PERMANGANATE] SPECTROMETRY
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ORGANOLEPTIC
[SENSORY, TASTING]
EXAMINATION
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SENSES TOUCH - BODY, TEMPERATURE TASTE - ACID, SUGAR, SALT, BITTER SMELL - AROMA, BOUQUET SIGHT - CLARITY, COLOR HEARING - CARBONATION, POURING
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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PARTS PER MILLION [PPM]
MILLIGRAMS / LITER = PARTS PER MILLION MG / L = PPM
0.001 GRAMS / 1000 MILLILITERS 1 / 1,000,000
A VERY SMALL AMOUNT! * 1 CAR IN TRAFFIC JAM FROM CLEVELAND TO SAN FRANCISCO [2650 MILES] * 1 PANCAKE IN STACK 4 MILES HIGH * 1 SOUP CAN IN ROW 40 MILES LONG
09/01/99 FRANK J. GADEK, PH.D., FAIC
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PARTS PER BILLION [PPB] * 1 HAMBURGER IN CHAIN CIRCLING EARTH
2.5 TIMES * 1 STRIDE ON TRIP TO MOON & BACK * 1 SILVER DOLLAR IN STACK 1500 MILES HIGH
PARTS PER TRILLION [PPT] * 1 POSTAGE STAMP IN AREA SIZE OF DALLAS, TX * 1 SIX INCH “LEAP” ON 93 MILLION MILE TRIP TO SUN * 1 SECOND OF TIME IN PAST 32,000 YEARS
09/01/99 FRANK J. GADEK, PH.D., FAIC
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COMPARE PPM, PPB, PPT
IF PPT = 1 SECOND / 32,000 YEARS PPB = 1 SECOND / 32 YEARS PPM = 1 SECOND / .03 YEAR OR ABOUT 11 DAYS
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“MY TASTES ARE SIMPLE; I AM EASILY SATISFIED
WITH THE BEST.”
BY WINSTON CHURCHILL
[TWO&WOWC,JCHUMES,P94,1994] 09/01/99 FRANK J. GADEK, PH.D., FAIC
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MATHEMATICS BEFUDDLED CHURCHILL
“WE ARRIVE IN AN ‘ALICE-IN-WONDERLAND’ WORLD, AT THE PORTALS OF WHICH STOOD
‘A QUADRATIC EQUATION’ FOLLOWED BY THE DIM CHAMBERS INHABITED BY THE
DIFFERENTIAL CALCULUS AND THEN A STRANGE CORRIDOR OF SINES, COSINES,
AND TANGENTS IN A HIGHLY SQUARE-ROOTED CONDITION.”
[CSOTC,JHUMES,157,1980]
09/01/99 FRANK J. GADEK, PH.D., FAIC
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SENSORY AND LAB ANALYSES SENSORY ANALYSES - BETTER FOR SUBTLE, COMPLEX ATTRIBUTES - BUT CAN HAVE GREAT VARIABILITY IN JUDGES - LAB ANALYSES NEED GC - MS LAB ANALYSES - CHEMICAL ANALYSES - CAN CONFIRM “GROSS CHARACTERISTICS” OF SENSORY ANALYSES - CAN HAVE MUCH LESS VARIABILITY THAN SENSORY ANALYSES 09/01/99 FRANK J. GADEK, PH.D., FAIC
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MICROBIOLOGICAL ANALYSES - CAN
CONFIRM, ESPECIALLY “ODOR” ISSUES, THAT CAN BE PRODUCED BY MICROORGANISMS THAT ARE INDICATED BY SENSORY AND CHEMICAL ANALYSES [E.G., VOLATILE ACIDITY, MLF - DIACETYL, ETC.]
09/01/99 FRANK J. GADEK, PH.D., FAIC
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NOTENOTE:
A CHEMICAL ISSUE IN A WINE CAN BE
MEASURED AND CORRECTED
A MICROBIOLOGICAL ISSUE NEEDS TO HAVE THE
OFFENDING MICROORGANISM COMPLETELY
REMOVED, SINCE THEY REPRODUCE!
[CHEMICALS DO NOT REPRODUCE]
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EQUIPMENT / MATERIALS NEEDED FOR 6 CRITICAL CHEMICAL
ANALYSES [TESTS] JUICE SUGAR - HYDROMETER OR REFRACTOMETER + THERMOMETER ACID - TITRATION EQUIPMENT / MATERIALS, OR KIT OR TEST PAPERS pH - METER OR TEST PAPERS 08/08/99/© FRANK J. GADEK, PH.D., FAIC
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WINE SUGAR - CLINITEST™ KIT OR TITRATION ACID & pH - SAME AS FOR JUICE
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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NOTE:NOTE:
THERE ARE A LOT OF DIFFERENT KITS, TEST PAPERS
DEVICES, ETC. THAT CAN ALSO BE USED TO GIVE AT
LEAST “BTN” [“BETTER THAN NOTHING”] INFORMATION
HOWEVER, FOR BEST RELIABILITY / CREDIBILITY, ETC.
RESULTS, VALIDATION AND OTHER STUDIES ARE
NEEDED TO COMPARE THESE RESULTS WITH
APPROVED WINE ANALYSIS METHODS
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“BTN”
BETTER
THAN
NOTHING
09/01/99 FRANK J. GADEK, PH.D., FAIC
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REFLECTOQUANT
TITRETS
CLINITEST OR DEXTROCHECK
GALLARD-SCHLESSINGER QUANTOFIX AND EMSCIENCE TEST PAPERS
VARIETY OF SPECIALTY KITS, ETC.
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SOME MINIMAL LAB SAFETY EQUIPMENT / PROGRAMS
SAFETY GLASSES
EYE WASH
LAB APRON / COAT
ASSORTED GLOVES
FIRST AID KIT
FIRE EXTINGUISHER
LIST OF EMERGENCY PHONE NUMBERS
“A PLAN” - WRITTEN / TRAINING / PRACTICE 09/01/99 FRANK J. GADEK, PH.D., FAIC
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REFERENCE BOOKS
HAZARDOUS WASTE - PERMITS / NOTIFY PROPER AGENCIES / WRITTEN PLAN / TRAINING SPILL KITS
HAZARDOUS WASTE DISPOSAL COMPANY
SOMEONE IN CHARGE / RESPONSIBLE
PROGRAM TO MAINTAIN CURRENCY
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% TOTAL SOLUBLE SOLIDS [%TSS] * 90% ARE SUGARS * GLUCOSE & FRUCTOSE * HOWEVER LABRUSCA AND ITS HYBRIDS MAY CONTAIN UP TO 25% SUCROSE * BUT LITTLE SUCROSE REMAINS IN FINISHED WINE NORMALLY - SO CLINITEST KIT CAN STILL BE USED * MEASURED BY HYDROMETRY OR REFRACTOMETRY - TEMPERATURE CORRECTION MAY BE SIGNIFICANT
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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ESTIMATE ½ OF % SUGAR CONCENTRATION IS % ALCOHOL
NORMALLY OBTAINED FROM FERMENTATION
20% SUGAR = 10% ALCOHOL
[ACTUALLY, CONVERSION RATE IS
USUALLY 55%, BUT CAN VARY]
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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RANGE WHITE - 19.5 - 23.0%
[CAN GIVE 10.7 - 12.6% ALCOHOL AT 55% CONVERSION RATE]
RED - 20.5 - 23.5% [CAN GIVE 11.3 - 12.9 % ALCOHOL AT 55%
CONVERSION RATE]
[UNITS OF % OR DEGREE BRIX OR BALLING]
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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ARCHIMEDES 287 - 212 BC GREEK MATHEMATICIAN / INVENTOR LAW OF HYDROSTATICS - ARCHIMEDES PRINCIPLE - BODY IMMERSED IN FLUID LOSES WEIGHT EQUAL TO WEIGHT OF AMOUNT OF FLUID DISPLACED SAID TO HAVE BEEN MADE WHEN HE STEPPED INTO HIS BATH AND NOTICED DISPLACED WATER OVERFLOWING [ENCARTA97] 09/01/99 FRANK J. GADEK, PH.D., FAIC
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WAR MACHINES - CATAPULT AND MIRROR SYSTEM [TO IGNITE INVADERS’ BOATS BY FOCUSING SUN’S RAYS] PROVED VOLUME OF SPHERE IS 2/3 VOLUME OF CYLINDER THAT CIRCUMSCRIBES IT DEVOTED HIS ENTIRE LIFE TO RESEARCH AND EXPERIMENTATION DEFINED PRINCIPLE OF THE LEVER
INVENTED COMPOUND PULLEY [ENCARTA97]
09/01/99 FRANK J. GADEK, PH.D., FAIC
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INVENTED HYDRAULIC SCREW TO RAISE WATER TO HIGHER LEVEL KILLED BY ROMAN SOLDIER WHO WAS OFFENDED BY HIM SAYING “DO NOT DISTURB MY DIAGRAMS” [HE HAD DRAWN IN THE SAND] KNOWN FOR APPLYING SCIENCE TO EVERDAY LIFE [ENCARTA97]
09/01/99 FRANK J. GADEK, PH.D., FAIC
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TOTAL TITRATABLE ACIDITY [%TTA]
MEASURED BY TITRATION WITH 0.1 N NaOH [SODIUM HYDROXIDE]
AND EITHER
PHENOLPHTHALEIN INDICATOR [COLORLESS TO LIGHT PINK AT
ENDPOINT OF TITRATION] 08/08/99/© FRANK J. GADEK, PH.D., FAIC
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OR
pH METER - 8.2 AT ENDPOINT OF TITRATION
[NO RED WINE COLOR INTERFERENCE]
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TOTAL TITRATABLE ACIDITY = VOLATILE ACIDITY
+ NONVOLATILE ACIDITY [%TTA = % VA + %NVA]
VOLATILE ACIDITY = FATTY ACIDS, CAN BE DISTILLED, LIQUIDS E.G., FORMIC, ACETIC, PROPIONIC, BUTYRIC, ETC.
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SOME “VOLATILE” ORGANIC ACIDS
FOUND IN WINE
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H - C - O - H || O FORMIC ACID [METHANOIC ACID]
CH3 - C - O - H || O ACETIC ACID [“VINEGAR”, ETHANOIC ACID]
CH3 CH2- C - O - H || O PROPANOIC ACID
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CH3 CH2CH2- C - O - H || O BUTANOIC ACID [“BUTYRIC ACID”]
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NONVOLATILE ACIDITY = CANNOT BE DISTILLED, SOLIDS E.G., MALIC, TARTARIC, CITRIC, SUCCINIC, ETC.
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TARTARIC ACID
* MAKES UP ½ OR MORE OF ACIDS IN MUST AND WINE * STONGEST ORGANIC ACID IN MUST / WINE * RANGE = 0.2 - 0.8%, DEPENDING ON VARIETY, SEASON, REGION, ETC. * MORE RESISTANT TO RESPIRATORY OXIDATION [57°C, 134°F AND BACTERIAL ATTACK
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* IMPORTANT IN PRECIPITATION OF POTASSIUM ACID TARTRATE [KHT, “CREAM OF TARTAR”] TO COLD STABILIZE WINE AND TO DEACIDIFY WINE * DETERMINATION: PRECIPITATION OF POTASSIUM ACID TARTRATE [“CREAM OF TARTAR”] BY ADDITION OF POTASSIUM CHLORIDE + TITRATION PAPER CHROMATOGRAPHY SPECTROMETRY
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MALIC ACID * OTHER MAIN ACID IN MUST AND WINE BESIDES TARTARIC ACID * IMPORTANT IN MALOLACTIC FERMENTATION [MLF] * RANGE: MUST - 0.1 - 0.6% WINE - 0 - 0.5% * RESPIRED FROM GRAPES AT 40.5°C, 104°F * CONCENTRATION DECREASES AS GRAPES MATURE
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* MORE SUSCEPTIBLE TO ATTACK BY MICROORGANISMS [MLF] THAN OTHER MAIN ACID IN MUST / WINE - TARTARIC ACID * DETERMINATION: PAPER CHROMATOGRAPHY ENZYMATIC / SPECTROMETRY
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RELATIONSHIPS AMONG SOME
ORGANIC ACIDS FOUND IN WINE
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FOR THOSE WHO
SPEAK & UNDERSTAND
ORGANIC CHEMISTRY
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CO2H CO2H CO2H CO2H l l l l H - C - H HO - C* - H HO - C* - H HO - C* - H
| | | | H – C - H H - C - H HO - C* - H H - C - H l l l l CO2H CO2H CO2H H SUCCINIC ACID MALIC ACID TARTARIC ACID LACTIC ACID CO2H CO2H l l H - C H - C | | | | C - H H - C l l CO2H CO2H FUMARIC ACID MALEIC ACID [TRANS] [CIS] {NOT FOUND IN WINE}09/01/99 FRANK J. GADEK, PH.D., FAIC
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CO2H CO2 K CO2 NH4
l l l H - C* - OH H - C* - OH H - C* - OH | | | HO - C*- H HO-C*- H HO - C* - H l l l CO2H CO2H CO2 Na TARTARIC ACID POTASSIUM SODIUM L, LEVO, + , d BITARTRATE AMMONIUM DEXTROROTATORY [“CREAM OF TARTRATE “NATURAL” TARTAR”] [PASTEUR’S WORK] [7THMERCK,8381012;FIESER,AOC,70] 08/08/99/© FRANK J. GADEK, PH.D., FAIC
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CH2 - CO2H
l
HO - C - CO2H |
CH2 - CO2H CITRIC ACID
[7THMERCK,266]09/01/99 FRANK J. GADEK, PH.D., FAIC
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DESIRED % TTA:
“MUST” = 0.9 - 1.0 CALIF - CAN BE LOWER 0.7-0.8 EAST - CAN BE HIGHER 1.1 - 1.3
WINE = 0.7 - 0.8
CALIF - CAN BE LOWER 0.6 - 0.7 EAST - CAN BE HIGHER 0.8 - 1.0
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EQUATION USED TO EXPRESS TOTAL TITRATABLE ACIDITY [%TTA]
IN UNITS OF TARTARIC ACID [TA]
NOTE: SOMETIMES OTHER UNITS ARE USED [E.G., SULFURIC, CITRIC ACID, ACETIC ACID, LACTIC ACID,
MALIC ACID, ETC.]
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% TTA AS TARTARIC ACID [TA] OR
GRAMS [G] TA / 100 MILLILITER [ML]
EQUALS
[V1]x[N]x[75]x[100] / [1000]x[V2] OR
[V1]x[N]x[7.50] / [V2]
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WHERE: % TTA = [V1]x[N]x[7.50] / [V2]
V1 = VOLUME OF BASE USED [NaOH, OR SODIUM HYDROXIDE] N = STRENGTH OF BASE, NORMALITY, USUALLY 0.1 N V2 = AMOUNT OF MUST OR WINE USED, USUALLY 5 OR 10 ML 08/08/99/© FRANK J. GADEK, PH.D., FAIC
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MW OF TARTARIC ACID = 150
SINCE IT IS A DIACID, DIVIDE BY 2
SO 150 / 2 = “THE 75 FACTOR”
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MOLECULAR FORMULA = C4H6O6
L, D AND MESO ISOMERS
L [BUT DEXTROROTATORY, “d” OR “+”] IS THE “NATURAL” ISOMER
[SINCE L & D ARE RELATED TO L & D GLYCERALDEHYDE, NOT OPTICAL ROTATION] 08/08/99/© FRANK J. GADEK, PH.D., FAIC
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PRACTICAL SIMPLIFICATION:
IF ALWAYS USE:
0.1 N NaOH AND 10 ML OF WINE, %TTA = [V1] x [0.08]
0.1 N NaOH AND 5 ML OF WINE
% TTA = [V1] x [0.15]
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AN EXAMPLE: IF USE 10 ML OF WINE AND IT IS TITRATED TO THE ENDPOINT WITH 12.50 ML OF 0.1N NaOH: %TTA AS TA = [V1]x[N]x[7.5] / [V2] = [12.50]x[0.1]x[7.5] / [10] = 0.94 G OF TARTARIC ACID / 100 ML OF WINE [OR 9.4 G OF TARTARIC ACID / LITER OF WINE]
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USE 0.1N NaOH SINCE: * YOU CAN BUY IT FAIRLY INEXPENSIVELY ALREADY PREPARED AT THIS CONCENTRATION * IT IS FAIRLY STABLE * THE “MATH” WORKS OUT BETTER!
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pH = “P”OTENTIAL OF “H”YDROGEN CHEMICALLY = FREE HYDROGEN CATION, PROTON, H MATHMATICALLY = NEGATIVE LOGARITHM OF MOLAR CONCENTRATION OF H pH = - LOG [H] MEASURED BY pH METER AND ELECTRODE
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H - O - H H + O - H IONIZE WATER CATION ANION NEUTRAL PROTON HYDROXIDE FREE ACID FREE BASE IONIZE = FORM IONS, CHARGED SPECIES
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FREE AND NOT FREE ACID:
H-A IONIZE H+ + A-
→ ACID PROTON ANION
NEUTRAL POSITIVE NEGATIVE ION ION
NOT FREE FREE NOT AN ACID ACID
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CONCEPT OF pH MEASURES FREE ACID CONCENTRATION OF AN ACID BUT DOES NOT MEASURE THE NOT FREE ACID CONCENTRATION TITRATION MEASURES “ALL” ACID - FREE & NOT FREE
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ACID pH = 1 - 6 [LOWER VALUE] {E.G., LEMON JUICE, VINEGAR}
NEUTRAL pH = 7
{WATER}
BASIC pH = 8 - 14 [HIGHER VALUE] {E.G., AMMONIA, DRANO}
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GENERAL RELATIONSHIP BETWEEN ACIDITY AND pH
IN GENERAL: AS ACIDITY INCREASES / pH DECREASES AS ACIDITY DECREASES / pH INCREASES BUT NO DIRECT RELATION
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USUAL RANGE 3.0 - 3.5 > 3.6 [E.G. CALIF] UNDESIRABLE MICROBIOLOGICAL GROWTH, DULL TASTE, POORER FERMENTATIONS < 3.0 [E.G. EAST] SHARP TASTE, BETTER FERMENTATIONS
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SUMMARY pH OF MUST AND WINE OF CRITICAL IMPORTANCE TO WINE QUALITY LOW pH VALUES [3.0 - 3.4] A PRIME REQUISITE TO PRODUCING STABLE, HIGH QUALITY WINES pH CAN INCREASE EXCESSIVELY DURING GRAPE MATURATION, SO USE ALONG WITH SUGAR AND TOTAL ACIDITY IN HARVEST DECISIONS [BEELMAN, PW, 1-2/1984, 38-42]
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pH CAN INCREASE EXCESSIVELY ALSO DURING VINIFICATION [AND EVEN POSSIBLY DURING AGING?] SO PROPER MONITORING IS REQUIRED [BEELMAN, PW, 1-2/1984, 38-42]
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OTHER pH AND WINE EFFECTS PROTEIN STABILITY - PROTEINS PRECIPITATE FASTER AT LOWER pH WINES FERMENTED AT LOW pH GENERALLY CONTAIN LOWER AMOUNTS OF PROTEIN PROTEIN FINING WITH BENTONITE 25% LESS AT pH 3.0 THAN 3.6 LOW pH FOR WINE CHEMICAL STABILITY [METAL ION COMPLEXES, Ca & K TARTRATES] [BEELMAN, PW, 1-2/1984, 38-42]
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NOTE
IN 1980’S, pH METERS BECAME
LESS EXPENSIVE AND MORE READILY AVAILABLE
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[H] = CONCENTRATION OF H OR THE FREE PROTONS IN SOLUTION LOG = LOGARITHM = “VERY SIMPLY A “FORMULA” - CAN LOOK UP VALUES IN TABLES OR USE THE “LOG” KEY ON YOUR CALCULATOR
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LOG = LOGARITHM = THE EXPONENT OF THE POWER TO WHICH A FIXED NUMBER [THE BASE] MUST BE RAISED IN ORDER TO PRODUCE A GIVEN NUMBER [THE ANTILOGARITHM]
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OR X P = Y WHERE:
X = FIXED NUMBER [BASE] P = EXPONENT [A SUPERSCRIPT]
OF THE POWER [ A NUMBER] Y = A GIVEN NUMBER [ANTILOGARITHM]
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* NORMALLY THE BASE IS 10
* SO FOR 101 = 10, 10
2 = 100,
103 = 1000, 10
4 = 10000
* THE LOG OF 100 TO THE BASE 10
= 2 [OR THE ANTILOG OF 2 = 100]
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SO FOR 10-1
= 0.1, 10-2
= 0.01,
10-3
= 0.001, 10-4
= 0.0001
THE LOG OF 0.001 TO THE BASE 10 = -3 [OR THE ANTILOG OF -3 = 0.001]
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SO FOR 0.001 MOLAR [H+]: SINCE: pH = - {LOG [H+]}
= - {LOG [0.001]} BECAUSE LOG [0.001] = 3
= - {- 3} = +3
THUS: pH OF 0.001 MOLAR [H+] = 3
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OR:
10 + 3
EQUALS 10 + 3 DECIMAL
PLACES TO THE RIGHT → OF LAST DIGIT = 10000
10 - 3
EQUALS 10 + 3 DECIMAL
PLACES TO THE LEFT ← OF FIRST DIGIT = 0.001
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ALSO CAN EXPRESS pH AS:
[H+] = 10 –pH
SO: 0.001 MOLAR [H+] = 10 -3
SINCE: 0.001 = 10 -3
THUS: pH OF 0.001 MOLAR [H+] = 3
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ACID pH BASE Ph MOLAR [H+] =pH MOLAR [-OH] =pH 1.0 M [H+] = 0 1.0 M [-OH] = 14 0.1 M [H+] = 1 0.1 M [-OH] = 13 0.01 M [H+] = 2 0.01 M [-OH] = 12 0.001 M [H+] = 3 0.001 M [-OH] = 11 0.0001 M [H+] = 4 0.0001 M [-OH] = 10 0.00001 M [H+] = 5 0.00001 M [-OH] = 9 0.000001 M [H+] = 6 0.000001 M [-OH] = 8 0.0000001 M [H+] = 7 0.0000001 M [-OH] = 7
NOTE AT pH = 7, [H+] = [-OH] 08/08/99/© FRANK J. GADEK, PH.D., FAIC
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MUST / WINE
pH = QUALITY
ROBERT BEELMAN PRACTICAL WINERY JANUARY / FEBRUARY 1984 PAGES #38 - 42
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REDUCING RESIDUAL SUGAR IN WINEREDUCING RESIDUAL SUGAR IN WINE
RESIDUAL FERMENTABLE [REDUCING] SUGAR REMAINING IN A WINE [% RRS]
IF >0.2% - SOME “ACTION” MUST BE TAKEN TO PREVENT / MINIMIZE REFERMENTATION
MOST PRACTICAL FOR SMALL WINERIES IS THE PROPER USE OF POTASSIUM SORBATE
OTHER METHODS INCLUDE:A] STERILE FILTRATION [BUT ALSO NEED
COMPLETE STERILE CONDITIONS FOR BOTTLING]
B] PASTEURIZATION [USUALLY NOT ACCEPTABLE FOR TABLE WINES]
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ANOTHER OPTION:ANOTHER OPTION:
▓ COMMERCIAL MOBILE BOTTLING LINE THAT COMES TO YOUR WINERY TO STERILE BOTTLE AND INCLUDESA GUARANTEE
▓ COST?
▓ SCHEDULING?
▓ RELIABILITY / CONFIDENCE / ETC.
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REDUCING RESIDUAL SUGAR [% RRS] REDUCING RESIDUAL SUGAR [% RRS] ANALYSIS METHODSANALYSIS METHODS
¤CLINITEST KIT ™ [FORMERLY DEXTROCHECK KIT™ IS MOST PRACTICAL FOR SMALL WINERIES
¤ ALSO USED TO TEST FOR GLUCOSE IN URINE
¤ READILY AVAILABLE IN DRUGSTORES
¤ VALIDATION
¤ COLORIMETRIC METHOD – ADD “PILL OF REAGENTS”TO A CERTAIN AMOUNT OF WINE
““BTN” – BETTER THAN NOTHING!BTN” – BETTER THAN NOTHING!
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VERY SIMPLY –
¶ METHOD INVOLVES OXIDATION – REDUCTION REACTIONS
¶ REDUCING SUGARS [ARE OXIDIZED AND CAN CAUSE REDUCTION, E.G., GLUCOSE] REDUCE THE BLUE CUPRIC, Cu +2 CATION TO THE REDCUPROUS, Cu +1, [CUPROUS OXIDE, (Cu)2O]
¶ ACTUAL COLOR GET IS FROM BLUE [0 % RRS] TOORANGE [UP TO 2 – 5% RRS] TO OLIVE DRAB [> 2 – 5% RRS, DEPENDING ON HOW YOU DO THE TEST]
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OTHER ANALYSIS OPTIONS FOR % RRSOTHER ANALYSIS OPTIONS FOR % RRS
‡ ENZYMATIC BUT REQUIRES EXPENSIVE [~$2000] SPECTROPHOTOMETER
‡ COMPLEX & INVOLVED TITRATIONS:
∆ LANE-EYNON METHOD – CUPRIC SULFATE SOLUTION, METHYLENE BLUE INDICATOR
∆ REBELEIN [GOLD COAST METHOD – THIOSULFATE / IODINE / STARCH TITRATION
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ALCOHOL DETERMINATION * EBULLIOMETER - DIFFERENCE IN BOILING POINT OF WINE AND DISTILLED WATER * DISTILLATION [REGULAR] + HDROMETRY [PROOF / TRALLE] AND TEMPERATURE CORRECTION
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ALCOHOL
* MAINLY ETHANOL + OTHER LOW M.W. VOLATILE ALCOHOLS [E.G., METHANOL, PROPANOLS, BUTANOLS, PENTANOLS, {FUSEL OILS} ETC.]
* RANGE 10 - 14%
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PROOF SPIRIT = OLD METHOD OF TESTING WHISKEY BY POURING IT
ON SOME GUNPOWDER AND LIGHTING IT - IGNITION OF THE
GUNPOWDER AFTER THE ALCOHOL BURNED AWAY WAS CONSIDERED “PROOF” THAT THE WHISKEY DID NOT CONTAIN TOO MUCH WATER.
[P122, NOLLER, “TOOC”]
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EXTRACT * DISTILLATION [ REGULAR] + HYDROMETRY [BRIX / BALLING] OR REFRACTOMETRY + TEMPERATURE CORRECTION * NOMOGRAPH
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SOME EXTRACT DETAILSSOME EXTRACT DETAILS
► EXTRACT = NONVOLATILE MATERIALS IN WINE
► “DRY” EXTRACT = EXTRACT - % SUGAR
► CAN BE USED TO DETECT FALSIFIED [“DILUTED”] WINES
► HIGHER INITIAL SUGAR CONTENT OF “MUST,” HIGHER NONALCOHOLIC RESIDUE OF RESULTING WINE
► RED WINE > ROSE WINE > WHITE WINES
► DEPENDS ON VARIETY, HANDLING CONDITIONS, ETC.
[A&O, MFAOMAW, P#26-27]
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SOME EXTRACT VALUESSOME EXTRACT VALUES
◘ 0.7 G / 100 ML FOR LOW ALCOHOL GERMAN WINES
◘ 3 G / 100 ML FOR LATE HARVEST RED WINES
◘ AVERAGE = 2.0 G / 100 ML[A&O, MFAOMAW, P#26-27]
NOW EXPRESSED IN UNITS OF G / L
DRY WHITE WINES 20 – 30 G / L [2 – 3%, OR G / 100 ML]
DRY RED WINES > 30 G / L, SINCE HIGHER LEVELS OF PHENOLS
[ZOECKLEIN, WAAP, P#113]
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< 20 G / L [2%] THIN, LIGHT BODIED DRY WINES
> 30 G / L [> 3%] FULL BODIED WINES
ZOECKLEIN, WAAP, P#113]
EXTRACT ALSO RELATES TO EXTRACT ALSO RELATES TO THE “BODY” [MOUTH FULLNESS]THE “BODY” [MOUTH FULLNESS]
OF A WINEOF A WINE
POINTS:AMELIORATED WINES CAN HAVE LOW EXTRACTS
TYPE OF PRESS CAN AFFECT EXTRACT VALUE
INCREASED PRESSING CAN INCREASE EXTRACT
PECTIC ENZYMES CAN INCREASE EXTRACT
BARREL FERMENTATION CAN INCREASE EXTACT
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SULFUR DIOXIDE TOTAL = FREE + FIXED TOTAL - 350 PPM BATF MAXIMUM FREE - NO REGULATION, BUT 20 - 30 PPM RECOMENDED
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FORMATION OF ETHANOL AND / OR ACETIC ACID [VINEGAR] IN WINE
FERMENTATION
C6H12O6 CH3 - C = O YEASTS / ENZYMES | H SUGAR ACETALDEHYDE ----
| REDUCTION CH3 CH2 - O - H -------- ETHANOL
| OXIDATION CH3 C = O ---- | ACETIC ACID O - H 09/01/99 FRANK J. GADEK, PH.D., FAIC
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ANTIOXIDANT ACTION OF SULFUR DIOXIDE
NaSO3 NaHSO3 | CH3 - C - H CH3 - C - H || SODIUM | O BISULFITE O - H ACETALDEHYDE ADDITION PRODUCT
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EFFECT OF pH ON SULFUR DIOXIDE USE IN WINEMAKING
THE PRIMARY ANTIMICROBIAL AGENT USED IN WINE THE DESIRED ACTIVE FORM IS
MOLECULAR SO2 [BEELMAN, PW, 1-2/1984, 38-42]
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SOME EQUILIBRIA INVOLVED WHEN SO2 IS DISSOLVED IN WATER / WINE -
SO2 + H20 MOLECULAR [SO2] + FREE SO2 +
FIXED / BOUND SO2 + H2SO3 HSO3 + H SULFUROUS ACID
SO3 + H 09/01/99 FRANK J. GADEK, PH.D., FAIC
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BISULFITE HSO3 AND SULFITE
SO3 IONS HAVE NO ANTIMICROBIAL PROPERTIES RELATIONSHIP OF pH, FREE AND
MOLECULAR SO2:
pH % FREE SO2 IN MOLECULAR FORM 3.0 61% 3.3 3.1% 4.0 0.6% [BEELMAN, PW, 1-2/1984, 38-42] 09/01/99 FRANK J. GADEK, PH.D., FAIC
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RECOMMEND WINE HAVE 0.8 PPM
MOLECULAR SO2 =
26 PPM FREE SO2 AT pH 3.3 79 PPM AT pH 3.8 120 PPM AT pH 4.0 [BEELMAN, PW, 1-2/1984, 38-42] 09/01/99 FRANK J. GADEK, PH.D., FAIC
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SULFUR DIOXIDE [SO2]
SOME COMMENTS BY LISA VAN DE WATER, DIRECTOR, THE WINE LAB, NAPA, CA ON
“A TECHNICAL REVOLUTION IN WINEMAKING”
SHE ENTERED CA WINE INDUSTRY IN 1974 FEW WINERIES MEASURED pH in 1974 OR
EVEN KNEW WHAT IT WAS SUPPOSE TO BE HIGH pH WINES FADED SOONEST
“DIED LIKE A DOG” [ZOECKLEIN’S LAB BOOK, P9]
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pH PROBABLY MOST IMPORTANT TEST CAN DO ON JUICE OR WINE
1982 RELATIONSHIP BETWEEN pH AND SO2
AND “MOLECULAR SO2” ESTABLISHED BEFORE 1982, WINERIES JUST TRIED TO
REACH A CERTAIN LEVEL OF FREE SO2
DID NOT ADUST SO2 LEVEL WITH RESPECT TO pH OR EVEN WINE TYPE [ZOECKLEIN’S LAB BOOK, P9]
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MEASUREMENT OF SO2 CHANGED SINCE 1980’S RIPPER METHOD HAS SIGNIFICANT
INTERFERENCES AERATION – OXIDATION [VACUUM
ASPIRATION] GREATER ACCURACY CONSUMERS BECAME MORE AWARE OF
SO2
SO2 USE PLUMMETED! [ZOECKLEIN’S LAB BOOK, P9]
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1975 ABOUT 75 – 100 PPM SO2 ADDED TO WHITE JUICE AT HARVEST & SLIGHTLY LESS IN REDS
LATE 1970’S NO SO2 FERMENTATION OF WHITE WINES WAS INTRODUCED
BY END OF 1980’S CA WINERIES SELDOM
ADDED ANY SO2 AT ALL TO REDS BEFORE FERMENTATION
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NOW PENDULUM SWUNG BACK A LITTLE AFTER EXPLOSION OF DEVASTATING SPOILAGE FROM SPONTANEOUS LACTOBACILLUS GROWTH DURING YEAST FERMENTATION
QUICKLY REALIZED THIS PROBLEM COULD BE CONTROLLED BY RESUMING SMALL SO2 ADDITIONS [ZOECKLEIN’S LAB BOOK, P9]
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DETERMINATION OF SULFUR DIOXIDE IN WINEDETERMINATION OF SULFUR DIOXIDE IN WINE
RIPPER METHOD – TRADITIONAL / STANDARD IODINE TITRATION / STARCH INDICATORDIFFICULT FOR RED WINESOTHER COMPONENTS REACT BESIDES SO2
AERATION / OXIDATION METHOD –
OXIDIZE SO2 TO SULFURIC ACID AND TITRATE WITH SODIUM HYDROXIDE WITH SPECIAL MIXED INDICATOR
MORE ACCURATE / PRECISE
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KITS / TEST PAPERS –
TITRETS, QUANTOFIX, REFLECTOQUANT, ETC.
NEED VALIDATION
““BBTTNN”” – BETTER THAN NOTHING!
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╬ CONVERSION OF MALIC ACID TO LACTIC ACID BY BACTERIA IN WINE
╬ CONVERSION OF A DICARBOXYLIC ACID [MALIC ACID] TO A MONOCARBOXYLIC ACID [LACTIC ACID] WITH THE EVOLUTION OF CARBON
DIOXIDE [FROM SECOND CARBOXYLIC ACID GROUP]╬ DECREASES ACIDITY OF WINE
╬ CAN ADD “COMPLEXITY” TO THE WINE ESPECIALLY RED WINES]
MALOLACTIC FERMENTATIONMALOLACTIC FERMENTATION
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FOR THOSE WHO
SPEAK & UNDERSTAND
ORGANIC CHEMISTRY
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CO2H l CO2H
l l l H - C* - OH l HO - C* - H
| l |
H - C - H l H- C - H
l l l CO2H MIRROR CO2H MALIC ACID D, DEXTRO, + , d L, LEVO, - , l DEXTROROTATORY LEVOROTATORY “UNNATURAL” “NATURAL”
[P632, MERCK]08/08/99/© FRANK J. GADEK, PH.D., FAIC
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“REVISED+” CO2H CO2H
l l l HO - C* - H l HO - C* - H
| l |
H - C - H l H - C - H
l l l CO2H l H
MIRROR + CO2 L (-, l) MALIC ACID L (+,d) LACTIC ACID “MLF”
[P1012, MERCK]08/08/99/© FRANK J. GADEK, PH.D., FAIC
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CO2H CO2H
l l l H - C* - OH l HO - C* - H
| l |
H - C - H l H- C - H
l l l H MIRROR H LACTIC ACID D, (- , l) L, (+, d) LEVOROTATORY DEXTROROTATORY FROM FERMENTATION FROM “MLF”
[P593, MERCK]08/08/99/© FRANK J. GADEK, PH.D., FAIC
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NOMENCLATURE d, l, +, - HAVE TO DO WITH OPTICAL ROTATION OF A BEAM OF PLANE POLARIZED LIGHT [PPL] BEING ROTATED TO THE LEFT [LEVO] OR TO THE RIGHT [DEXTRO] D & L HAVE TO DO WITH COMPARISON TO D & L GLYCERALDEHYDE, A REFERENCE COMPOUND FOR “RELATIVE CONFIGURATION” [WHICH LATER TURNED OUT TO ALSO BE THE CORRECT ABSOLUTE CONFIGURATION] [NOLLER,TOOC,310] 09/01/99 FRANK J. GADEK, PH.D., FAIC
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SIMPLE MALOLACTIC SIMPLE MALOLACTIC FERMENTATION FERMENTATION
PAPER CHROMATOGRAPHYPAPER CHROMATOGRAPHY
Ж SEPARATION OF MAIN NONVOLATILE ORGANIC ACIDS IN WINE
ж SPECIAL SOLVENT MIXTURE
ж BROMCRESOL GREEN INDICATOR
ж ACIDS YELLOW ON BLUE BACKGROUND
ж QUALITATIVE AND SEMIQUANTITATIVE
ж PRACTICAL FOR SMALL FARM TYPE WINERIES
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WINE TOTAL PHENOLS IMPORTANCE: COLOR AGEING TASTE OXIDATION - REDUCTION RESERVOIR OTHER
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TYPES OF WINE PHENOLS: ANTHOCYANINS - FLAVONOID TANNINS HYDROLYZABLE - NONFLAVONOID CONDENSED - FLAVANOL, FLAVANDIOL OTHER - NONFLAVANOID
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TOTALTOTAL PHENOLS PHENOLS
COMPLEX – TANNINS + PIGMENTS + ???COMPLEX – TANNINS + PIGMENTS + ???
CRUDE ANALYSIS –
POTASSIUM PERMANGANATE [KMnO4] / INDIGO CARMINE INDICATOR TITRATION
BEFORE AND AFTER TREATMENT WITH “CARBON”
OF DEALCOHOLIZED WINE SAMPLE [FROM EXTRACT DETERMINATION?]
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MORE PROFESSIONAL , MORE PROFESSIONAL , BUT MORE COMPLEX AND BUT MORE COMPLEX AND EXPENSIVE, METHODSEXPENSIVE, METHODS
FOLIN – CIOCALTEU COLORIMETRIC METHOD, BUT NEED A SPECTROPHOTOMETER
HPLC – HIGH PRESSURE [PERFORMANCE] LIQUID CHROMATOGRAPHY
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LOWENTHAL-NEUBAUER METHODLOWENTHAL-NEUBAUER METHOD
× FOR TANNIN & COLORING MATTER [“T + CM”]
× RELATIVELY EASY FOR SMALL WINERIES TO DO
× WAS OFFICIAL A.O.A.C [1950] METHOD FOR MANY YEARS
× TITRATE WITH PURPLE POTASSIUM PERMANGANATE - A DEALCOHOLIZED WINE SAMPLE [FROM
EXTRACT DETERMINATION?] - BEFORE AND AFTER TREATMENT WITH
ACTIVATED CARBON TO REMOVE TANNINS & PIGMENTS
- IN ORDER TO CORRECT FOR OTHER
MATERIALS THAT REACT WITH KMnO4
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AT THE ENDPOINT OF THE TITRATION, THE DEEP OPAQUE BLUE BLACK INDIGO CARMINE INDICATOR DRAMATICALLY TURNS -
BRIGHT CLEAR YELLOW
SO THE ENDPOINT IS VERY EASY TO DETECT PRECISELY & ACCURATELY
PURPLE KMnO4 + BLUE BLACK INDICATOR →YELLOW
[AMERINE, LPFE, P#28-29]
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EQUATION:[T + CM, G / 100 ML] = {C X [N KMnO4] X [0.0416] X
100} / [ML WINE USED]WHERE:T + CM = TANNIN + COLORING MATTERC = A – BA = TITRATION OF WINEB = TITRATION OF WINE AFTER CHARCOAL TREATMENT TO REMOVE [T + CM], FOUND TO BE ALMOST CONSTANT FOR SAME REAGENTS AND CHARCOALN = NORMALITY OF KMnO4
0.0416 = EMPIRACAL FACTOR, ASSUME 1 ML OF 0.1N KMnO4 = 0.00416 G OF TANNIN, BUT FACTORS FROM 0.00173 TO 0.00588 HAVE BEEN USED
[AMERINE, LPFE, P#28-29]
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SOME VALUES OF TANNIN + COLORING SOME VALUES OF TANNIN + COLORING MATTER [“T + CM”]:MATTER [“T + CM”]:
WHITE WINES = < 0.05 G / 100 ML [%]
PINK WINES = < 0.01 G / 100 ML [%]
RED WINES = < 0.20 G / 100 ML [%]
HIGHLY COLORED NEW RED WINES = MAY BE AS HIGH AS 0.40 G / 100 ML [%]
VALUES USEFUL IN STANDARDIZING RED WINES, INDICATING RATE / EXTENT OF AGING, FINING AGENTS,ETC. [AMERINE, LPFE, P#28-29]
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EQUATION:PI = PERMANGANATE INDEX = 5 [A – B]
WHERE:A = TITRATION OF JUST INDICATOR,
ML KMnO4
B = TITRATION OF WINE + INDICATOR,
ML KMnO4
[WINE NOT DEALCOHOLIZED][ZOECKLEIN, WAAP, P#458]
PERMANGANATE INDEX [POLYPHENOL INDEX, “PERMANGANATE INDEX [POLYPHENOL INDEX, “PIPI”] ”] {FROM ZOECKLEIN}{FROM ZOECKLEIN}
- - NOT THE SAME AS NEUBAUER – AS NEUBAUER – LOEWENTHAL PROCEDURE LOEWENTHAL PROCEDURE
– – GIVES ONLY GIVES ONLY “CRUDE”“CRUDE” EVALUATION} EVALUATION}
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VALUES:35 – 50 FOR LOW PHENOLIC WINES> / = 100 FOR HIGH PHENOLIC CONTENT
– “HARD / BITTER”
25 = 320 MG / L, GAE [GALLIC ACID EQUIVALENT]
OR 0.320 G / L OR 0.0320 G / 100 ML [%]
NOTE: IN ESSENCE, VALUES ARE JUST ML OF KMnO4 USED IN TITRATIONS
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FOLIN - CIOCALTEU COLORIMETRIC METHOD FOR TOTAL PHENOLS
OXIDATION OF PHENOLS WITH YELLOW TUNGSTATE / MOLYBDATE COMPLEX
[W+6
Mo+6
] TO FORM BLUE TUNGSTATE /
MOLYBDATE COMPLEX [W+5
Mo+6
/
W+6
Mo+5
] BY REDUCTION, GAIN OF ELECTRONS, + e-] MIXTURE IS GREEN [765 NM]
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OXIDATION [LOSS OF ELECTRONS, - e-] H-O-Ph-O-H O=Ph=O [Ph = BENZENE RING, O-H GROUPS IN 1,2 OR 1,3 OR 1,4 POSITIONS]
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SOME WINE ANALYSES VALUES SOME WINE ANALYSES VALUES FROM MY ENOLOGY RESEARCH FROM MY ENOLOGY RESEARCH
PROJECTSPROJECTS
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MUST COMPOSTION VINEYARD/ HARV YIELD
B %TTA pH
VARIETY DATE [T/A] CHESTER SEYVAL 9/14 2 16.9 0.83 2.81
VILLARD 10/8* 3 16.9 1.05 2.80 NORTHAMPTON CHELOIS 9/15 8 17.0 0.92 3.28 [YIELDS ESTIMATED BY GROWERS]
[* HARVESTED EARLY DUE TO FROST] 09/01/99 FRANK J. GADEK, PH.D., FAIC
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“AVERAGE” WINE COMPOSITION VALUES
%TTA pH %VA %RRS %ALC EXT TP SEYVAL 0.75 3.16 0.008 0.26 11.2 2.04 298 VILLIARD 0.71 3.15 0.016 0.15 12.1 1.87 274 CHELOIS 0.77 3.82 0.007 0.13 10.8 2.37 831
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RANGE OF WINE COMPOSTION VALUES
%TTA pH %VA %RRS %ALC EXT TP 0.69 2.95 0.001 0.07 10.1 1.71 220 0.81 3.99 0.022 0.50 12.2 2.63 925 [EXT = DRY EXTRACT = G / 100ML] [TP = TOTAL PHENOLS = MG / L]
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420 NM – BROWNING COLOR
520 NM – RED COLOR
420 NM + 520 NM = DENSITY OR INTENSITY
420 NM / 520 NM = HUE OR TINT
WINE COLORWINE COLOR
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SOME VALUES FOR COLOR FROM SOME VALUES FOR COLOR FROM MY ENOLOGY RESEARCH PROJECTSMY ENOLOGY RESEARCH PROJECTS
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“AVERAGE COLOR VALUES OD OD % BRIGHT HUE 420NM 520 NM [420 + 520][420 / 520] SEYVAL 0.053 VILLARD 0.068 CHELOIS 0.34 3.30 3.60 0.0920
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RANGE OF COLOR VALUES
OD OD % BRIGHT HUE 420 NM 520 NM [420+520] 420 / 520] 0.034 2.58 2.77 0.0752 0.352 3.82 4.17 0.1085
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SOME OTHER WINE ANALYSES THATSOME OTHER WINE ANALYSES THATLARGE WINERIES MAY DOLARGE WINERIES MAY DO
METALS – BY ATOMIC ABSORPTION [AA] – K, Ca, Fe, Cu, ETC.
GAS CHROMATOGRAPHY [GC] – MANY WINE COMPONENTS
HIGH PERFORMANCE / PRESSURE LIQUID CHROMATOGRAPHY[HPLC] – MANY WINE COMPONENTS
GRAPE AMINO ACIDS – ESPECIALLY WITH RESPECT TO “STUCK” FERMENTATION, PROTEIN STABILITY, ETC.
MANY PROPRIETARY ANALYSES FOUND TO BE IMPORTANT FOR A PARTICULAR WINERY
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ACCURACY OF VOLUMETRIC PROCEDURES
ABOVE RESULTS BASED ON: ACCURACY UNLIKELY MORE THAN +/- 0.5% IN MOST ANALYTICAL WORK ALLOWABLE ERROR +/- 0.1% TO +/- 1.0% FOR CONSTITUENTS MAKING UP MORE THAN 1% OF THE SAMPLE BRUER, BRUER & BRIEN,AJEV,33(3),159-163,1982]
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ACCEPTED PERMISSABLE
CHEMICAL ANALYSIS ERRORS
* FOR ROUTINE ANALYSIS
+/- 0.05% * CHOICE OF METHOD
- RAPID - SIMPLE
- APPROXIMATE - APPROPRIATE FOR PURPOSE
[E.G., CELLAR, LEGAL, COMMERCIAL, ETC.]
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INDIVIDUAL CHEMICAL ANALYSIS PERMISSABLE LIMITS OF
ERRORS * % TOTAL SOLUBLE SOLIDS [%TSS] - + / - 0.2% * % TOTAL TITRATABLE ACIDITY [%TTA] - + / - 0.03% * pH [DEPENDING ON PARTICULAR INSTRUMENT] + / - 0.04 pH UNITS
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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* % REDUCING RESIDUAL SUGAR [%RRS] - + / - 0.05% * % ALCOHOL {ETHANOL} [%ALC] - + / - 0.25% * % EXTRACT - + / - 0.2% * % VOLATILE ACIDITY {VINEGAR} [%VA] - + / - 0.006% * SULFUR DIOXIDE TOTAL [DIST] - + / - 10 PPM FREE [RIPPER] - + / - 5 PPM * TOTAL PHENOLS {TANNIN, COLORING} [PERMANGANATE] - + / - 0.15%
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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SOME VERY SOPHISTICATED SOME VERY SOPHISTICATED AND EXOTIC WINEAND EXOTIC WINE
ANALYSESANALYSES
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”CLASSIFICATION OF WINE SAMPLES ACCORDING TO ORIGIN
AND GRAPE VARIETIES ON THE BASIS OF INORGANIC AND
ORGANIC TRACE ANALYSES” BY DANZER, GARCIA, THIEL & REICHENBACHER, AMERICAN LABORATORY, VOL. 31, NO.20, ISSN 0044-7749, 26-34, 10/99 GC OF VOLATILE AROMATIC COMPONENTS CAN BE USED TO DETERMINE GRAPE VARIETY
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USED 165 WINES, FROM 6 GERMAN WINE-GROWING REGIONS, 21 GRAPE VARIETIES, VINTAGES 1986 - 1996 MEASURED 16 ELEMENTS - Al, B, Ba, Ca, Cr, Cu, Fe, Mn, Mg, P, Pb, Si, Sn, Sr, V & Zn BY ICP-AES [INDUCTIVELY COUPLED PLASMA-ATOMIC EMISSION SPECTROMETRY] SPME [SOLID PHASE MICROEXTRACTION] USED AS SAMPLE PREPARATION METHOD FOR GC ANALYSIS, MORE THAN 90 FLAVOR COMPONENTS COULD BE ANALYZED
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90.2 % OF WINES CAN BE CORRECTLY PREDICTED AS TO ORIGIN WITH RESPECT TO: * ELEMENTS - Ba, Si, & V * ORGANIC COMPOUNDS - 2- FURANCARBOXALDEHYDE [CONTENT INFLUENCED BY AGING], 4-METHYL-1- PENTANOL [DEPENDS ON FERMENTATION] & 1-OCTANOL [MATURITY INFLUENCED]
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>99 % OF WINES CAN BE CORRECTLY PREDICTED AS TO GRAPE VARIETY OVER VINTAGES 1988 - 1996 WITH RESPECT TO: * TERPENES [DEPEND ON AGING] & VINTAGE-DEPENDENT COMPONENTS SUCH AS 1-HEXANOL, 2-FURANCARBOXALDEHYDE, DIETHYL SUCCINATE, PHENYLETHYL ALCOHOL, BENZYL ALCOHOL & HEXANOIC ACID 09/01/99 FRANK J. GADEK, PH.D., FAIC
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* TERPENES = TRANS-LINALOOL OXIDE, NEROL OXIDE, CIS-LINALOOL OXIDE, NEROL, LINALOOL, HOTRIENOL, ALPHA-TERMINEOL, TERPENDIOL, CITRONELLOL, GERANIOL, 2-ETHYLTETRAHYDRO-2H-PYRAN ROLE OF INORGANIC CONSTITUENTS FOR VARIETAL CHARACTERIZATION DO NOT SIGNIFICANTLY IMPROVE CLASSIFICATION RESULTS BUT DISCRIMINATION OF ORIGIN CAN BE IMPROVED BY ADDITION OF SELECTED ORGANIC COMPOUNDS TO THE INORGANIC DATA 9 FRANK J. GADEK, PH.D., FAIC
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NUCLEAR MAGNETIC RESONANCE [NMR]NUCLEAR MAGNETIC RESONANCE [NMR]
AJEV 2003 ARTICLE
ACETIC ACID [VINEGAR]
DETECT THRU NECK OF UNOPENEDBOTTLE
OTHER WINE COMPONENTSPOSSIBLE
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FOSS FOURIER TRANFORM INFRAREDFOSS FOURIER TRANFORM INFRAREDSPECTROPHOTOMETRY [FT-IR]SPECTROPHOTOMETRY [FT-IR]
FORFOR::
GRAPES - GRAPESCANGRAPES - GRAPESCAN
WINE - WINESCANWINE - WINESCAN
ALMOST ALL MAJOR COMPONENTS!ALMOST ALL MAJOR COMPONENTS!
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JUST DOING WINE ANALYSES MAY BE THE EASIEST PART
PROPER INTERPRETATION OF WINE ANALYSES RESULTS DEVELOPING PROPER, APPROPRIATE EFFICIENT & EFFECTIVE “ACTION PLANS” TO IMPLEMENT IN DETAIL TO MAKE
BETTER WINE MORE CONSISTENTLY TO MAKE BEST USE OF THE RESULTS & INTERPRETATION OF WINE ANALYSES
MAY BE THE MOST DIFFICULT 09/01/99 FRANK J. GADEK, PH.D., FAIC
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NEED: “ILLUMINATION” DATA TESTS PROPER INTERPRETATION OF DATA / TESTS APPROPRIATE “ACTION PLAN” DEVELOPED FROM ABOVE PROPER INTERPRETATION PROPER IMPLEMENTATION OF “ACTION PLAN” 09/01/99 FRANK J. GADEK, PH.D., FAIC
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EVALUATION OF EFFECTIVENESS OF “ACTION PLAN” CONTINUOUS FEEDBACK TO MODIFY “ACTION PLAN” CONTINUOUS IMPLEMENTATION OF MODIFIED “ACTION PLANS” UNTIL SUITABLE AND ACCEPTABLE RESULTS ARE OBTAINED
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08/08/99/© FRANK J. GADEK, PH.D., FAIC
COMPLEX LIKE A SPIDER WEB !COMPLEX LIKE A SPIDER WEB !
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SHELF LIFE OF WINERY LAB REAGENTS
SODIUM HYDROXIDE, NaOH, 0.1N, FOR TOTAL ACIDITY - 46 DAYS IN GLASS, 37 DAYS IN PLASTIC - DO NOT USE SODA- LIME GUARD TUBE NOTE 0.01N NaOH FOR ASPIRATION SULFUR DIOXIDE ANALYSIS - ONLY 7 DAYS IN PLASTIC COMMERCIAL pH BUFFERS, pH 4.01 & 7.00 - 4 MONTHS AFTER OPENING [BRUER, BRUER & BRIEN,AJEV,33(3),159-163,1982]
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IODINE, I2, 0.1N, FOR RIPPER METHOD FOR SULFUR DIOXIDE - 3 MONTHS
HYDROGEN PEROXIDE, H2O2, 0.3%, FOR ASPIRATION SULFUR DIOXIDE ANALYSIS - 3 MONTHS IN GLASS, BUT SHOULD BE REFRIGERATED [BRUER, BRUER & BRIEN,AJEV,33(3),159-163,1982]
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OPTIONS FOR WINE LAB REAGENTS MAKE YOUR OWN AND STANDARDIZE ? - CAN BE “VERY TRICKY” AND ULTIMATELY MORE EXPENSIVE AND
LESS RELIABLE RESTANDARDIZE OUTDATED REAGENTS - SEE ABOVE PURCHASE PROPER NEW REAGENTS AT BEGINNING OF EACH VINTAGE AND THEREAFTER AS NEEDED - OVERALL MAY BE THE BEST [GADEK,WINE EAST,9(1), 14-20 (1981).VINIFERA WINE GROWERS JOURNAL, 15(2), 71-81 (1988)]
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SOME “TIPS / HINTS / TRICKS”
ON
WINE ANALYSES
LABORATORY TECHNIQUES
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SOME LAB “TIPS” REFRACTOMETRY
RINSE LENSES AND APPLICATOR WELL WITH DISTILLED WATER WIPE LENSES DRY AND CLEAN WITH “KIMWIPES” TO MINIMIZE SCRATCHING TEMPERATURE CORRECTION - ESPECIALLY IMPORTANT AT EXTREME TEMPERATURES PERIODIC CALIBRATION USEFUL WITH DISTILLED WATER FOR ZERO VALUE AND FRESHLY PREPARED KNOWN % SUGAR SAMPLES
09/01/99 FRANK J. GADEK, PH.D., FAIC
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SOME LAB “TIPS” HYDROMETRY
MAKE SURE HYDROMETER & GRADUATED CYLINDER ARE CLEAN & DRY RINSE WITH DISTILLED WATER AND LET DRAIN DRY AFTER USE CHECK FOR CHIPS AND CRACKS MAKE SURE IT FLOATS PROPERLY FILTER SAMPLE IF IT HAS A LOT OF SUSPENDED MATTER
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DIP & SPIN HYDROMETER IN SAMPLE TO WET SURFACE AND DISPERSE ANY GAS BUBBLES READ BOTTOM OF MENISCUS TEMPERATURE CORRECTION - ESPECIALLY IMPORTANT AT EXTREME TEMPERATURES PERIODIC CALIBRATION USEFUL WITH DISTILLED WATER FOR ZERO VALUE AND FRESHLY PREPARED KNOWN % SUGAR SAMPLES 09/01/99 FRANK J. GADEK, PH.D., FAIC
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INVEST IN A SPECIAL HYDROMETER CYLINDER WITH AN OVERFLOW CATCH AREA INVEST IN A SERIES OF HYDROMETERS TO BETTER MEASURE DIFFERENT RANGES [E.G., 0 - 5%, 5 - 10%, 10 - 15%, 15 - 20 %, 20 - 25%, 25 - 30%] HAVE SPARES, ESPECIALLY FOR COMMON RANGES
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SOME LAB “TIPS” THERMOMETERS
USE ALCOHOL THERMOMETERS [FILLED WITH RED COLORED ALCOHOL INSTEAD OF SILVER COLOR MERCURY] SPECIAL MERCURY SPILL / CLEANUP KITS ELECTRONIC THERMOMETERS - PROBE FOOD GRADE OR PROTECTED HAVE SPARES 09/01/99 FRANK J. GADEK, PH.D., FAIC
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SOME LAB “TIPS” pH METER & ELECTRODE
GLASS ELECTRODE TIP IS “VERY DELICATE” PROTECT FROM MECHANICAL DAMAGE KEEP IN BUFFER SOLUTION WHEN NOT IN USE MAKE SURE pH METER IS OFF WHEN ELECTRODE IS OUT OF SOLUTION
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CALIBRATE IN BUFFER SOLUTIONS [pH 4 and 7???] BEFORE USE & PERIODICALLY DURING USE
USE SATURATED SOLUTION OF KHT [CREAM OF TARTAR, POTASSIUM ACID TARTRATE] AS A BUFFER pH = 3.56 AT ROOM TEMPERATURE 20 - 25 C HAVE SEVERAL SPARE ELECTRODES
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SOME LAB “TIPS” REPRESENTATIVE SAMPLE
MIX CONTENTS WELL BEFORE SAMPLING TAKE SEVERAL SAMPLES FROM DIFFERENT AREAS / DEPTHS [E.G., TANKS] MEASURE AS SOON AS POSSIBLE AFTER TAKING SAMPLE IF SAMPLES MUST BE STORED UNTIL MEASURED - REFRIGERATE OR FREEZE & THAW TO ROOM TEMPERATURE TO MEASURE - CHECK FOR DEPOSITS [KHT]
09/01/99 FRANK J. GADEK, PH.D., FAIC
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SOME LAB “TIPS” TITRATION
MAKE SURE PIPET & BURET ARE CLEAN & DRY RINSE WITH DISTILLED WATER & LET DRAIN DRY INVERTED AFTER USE CHECK FOR CHIPS & CRACKS MAKE SURE TEFLON STOPCOCK ON BURET IS WORKING PROPERLY USE SPECIAL PIPET BULBS & MAGNETIC STIRRERS
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USE FRESH 0.1 N SODIUM HYDROXIDE, NaOH INITIALLY RINSE BURET WITH 0.1 N SODIUM HYDROXIDE FILL BURET WITH 0.1 N SODIUM HYDROXIDE & REMOVE ANY AIR BUBBLES IN TIP OF BURET PHENOLPHTHALEIN IS A LAXATIVE! CORRECTION FOR BACKGROUND ACIDITY IN DISTILLED WATER MAY BE NECESSARY
REMOVE DISSOLVED CO2 FROM SAMPLE BY VACUUM OR HEATING 09/01/99 FRANK J. GADEK, PH.D., FAIC
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RINSE PIPET WITH SAMPLE READ BOTTOM OF MENISCUS OF PIPET & BURET “TD” ON PIPET MEANS TO DELIVER - DO NOT BLOW OUT REMAINING SAMPLE IN TIP ADD 100 - 200 ML OF DISTILLED WATER TO PIPETTED SAMPLE IN ERLENMEYER FLASK ASSISTS IN SEEING PINK ENDPOINT WHEN USING PHENOLPHTHALEIN AND IN OPERATION OF pH ELECTRODE
09/01/99 FRANK J. GADEK, PH.D., FAIC
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ERLENMEYER FLASK [500 ML, WIDE MOUTH] MINIMIZES SPLASHING DURING TITRATION, RINSE SIDES OF ERLENMEYER FLASK WITH DISTILLED WATER USING PLASTIC SQUEEZE WASH BOTTLE “CREEP UP” ON ENDPOINT SLOWLY WHEN NEAR END OF TITRATION BY ADDING A DROP AT A TIME 0F 0.1 N NaOH FROM THE BURET
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LIGHT PINK COLOR OF PHENOLPHTHALEIN ENDPOINT WILL FADE WITH TIME pH USING A METER WILL TEND TO SLOWLY DRIFT BACK TO LOWER VALUES FROM ENDPOINT OF pH = 8.2 THUS, SOME “JUDGEMENT” WILL BE REQUIRED TO MAKE SURE YOU ARE ACTUALLY AT THE ENDPOINT OF THE TITRATION
09/01/99 FRANK J. GADEK, Ph.D., FAIC
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NOTE COLOR OF RED WINES AT ENDPOINT OF TITRATION OF pH = 8.2 - SOMETIMES THIS COLOR CAN INDICATE THE ENDPOINT TITRATION IS ONE OF THE MORE COMPLEX WINE ANALYSIS TECHNIQUES MUCH PRACTICE REQUIRED FOR PROFICIENCY, APPROPRIATE REPRODUCIBILITY, PRECISION & ACCURACY
09/01/99 FRANK J. GADEK, PH.D., FAIC
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CONFIGURATION OF “SPECIAL
STILL” FOR DETERMINATION OF ALCOHOL, EXTRACT AND SULFUR
DIOXIDE
REGULAR DISTILLATION
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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CONFIGURATION OF “SPECIAL STILL” FOR DETERMINATION OF
VOLATILE ACIDITY
STEAM DISTILLATION
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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DRINK AND
ENJOY WINE !!!
08/08/99/© FRANK J. GADEK, PH.D., FAIC
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TO BE CONTINUED AS TO BE CONTINUED AS
INTEREST &INTEREST &
RESOURCES PERMITRESOURCES PERMIT
JUST LET ME KNOW !JUST LET ME KNOW !