WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 1 SOME CHEMICAL WINE ANALYSES FRANK J. GADEK, Ph.D., FAIC ENOLOGY EDUCATION SERVICES.

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 1 SOME CHEMICAL WINE ANALYSES FRANK J. GADEK, Ph.D., FAIC ENOLOGY EDUCATION SERVICES

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 2 TOPIC – “ SOME CHEMICAL WINE ANALYSES “ SCIENCE, TECHNOLOGY & SOCIETY { “STS” } BY FRANK J. GADEK, PH.D.

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 3

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 20 WINE ANALYSES OPTIONS § DO AT WINERY § COMMERCIAL LABS § COMBINATION ¥ ONLY ABOUT 10 TO 20 ¢ / BOTTLE ¥ INEXPENSIVE INSURANCE!

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 30 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

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 33 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]

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 55 NOTE NOTE: 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]

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 58 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

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 60 REFLECTOQUANT TITRETS CLINITEST OR DEXTROCHECK GALLARD-SCHLESSINGER QUANTOFIX AND EMSCIENCE TEST PAPERS VARIETY OF SPECIALTY KITS, ETC.

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 115 REDUCING 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]

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 116 ANOTHER OPTION: ▓ COMMERCIAL MOBILE BOTTLING LINE THAT COMES TO YOUR WINERY TO STERILE BOTTLE AND INCLUDES A GUARANTEE ▓ COST? ▓ SCHEDULING? ▓ RELIABILITY / CONFIDENCE / ETC.

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 117 REDUCING RESIDUAL SUGAR [% RRS] ANALYSIS 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!

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 118 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 RED CUPROUS, Cu +1, [CUPROUS OXIDE, (Cu) 2 O] ¶ ACTUAL COLOR GET IS FROM BLUE [0 % RRS] TO ORANGE [UP TO 2 – 5% RRS] TO OLIVE DRAB [> 2 – 5% RRS, DEPENDING ON HOW YOU DO THE TEST]

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 119 OTHER 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

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 124 SOME 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]

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 125 SOME 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]

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 126 < 20 G / L [2%] THIN, LIGHT BODIED DRY WINES > 30 G / L [> 3%] FULL BODIED WINES ZOECKLEIN, WAAP, P#113] EXTRACT ALSO RELATES TO THE “BODY” [MOUTH FULLNESS] OF 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

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 139 DETERMINATION OF SULFUR DIOXIDE IN WINE RIPPER METHOD – TRADITIONAL / STANDARD IODINE TITRATION / STARCH INDICATOR DIFFICULT FOR RED WINES OTHER COMPONENTS REACT BESIDES SO 2 AERATION / OXIDATION METHOD – OXIDIZE SO2 TO SULFURIC ACID AND TITRATE WITH SODIUM HYDROXIDE WITH SPECIAL MIXED INDICATOR MORE ACCURATE / PRECISE

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 140 KITS / TEST PAPERS – TITRETS, QUANTOFIX, REFLECTOQUANT, ETC. NEED VALIDATION “BTN” “BTN” – BETTER THAN NOTHING!

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 141 ╬ 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 FERMENTATION

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 147 SIMPLE MALOLACTIC FERMENTATION PAPER 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

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 150 TOTAL PHENOLS COMPLEX – TANNINS + PIGMENTS + ??? CRUDE ANALYSIS –  POTASSIUM PERMANGANATE [KMnO 4 ] / INDIGO CARMINE INDICATOR TITRATION  BEFORE AND AFTER TREATMENT WITH “CARBON”  OF DEALCOHOLIZED WINE SAMPLE [FROM EXTRACT DETERMINATION?]

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 151 MORE PROFESSIONAL, BUT MORE COMPLEX AND EXPENSIVE, METHODS FOLIN – CIOCALTEU COLORIMETRIC METHOD, BUT NEED A SPECTROPHOTOMETER HPLC – HIGH PRESSURE [PERFORMANCE] LIQUID CHROMATOGRAPHY

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 152 LOWENTHAL-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 KMnO 4

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 153 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 KMnO 4 + BLUE BLACK INDICATOR → YELLOW [AMERINE, LPFE, P#28-29]

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 154 EQUATION: [T + CM, G / 100 ML] = {C X [N KMnO 4 ] X [0.0416] X 100} / [ML WINE USED] WHERE: T + CM = TANNIN + COLORING MATTER C = A – B A = TITRATION OF WINE B = TITRATION OF WINE AFTER CHARCOAL TREATMENT TO REMOVE [T + CM], FOUND TO BE ALMOST CONSTANT FOR SAME REAGENTS AND CHARCOAL N = NORMALITY OF KMnO 4 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]

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 155 SOME VALUES OF TANNIN + COLORING 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]

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 156 EQUATION: PI = PERMANGANATE INDEX = 5 [A – B] WHERE: A = TITRATION OF JUST INDICATOR, ML KMnO 4 B = TITRATION OF WINE + INDICATOR, ML KMnO 4 [WINE NOT DEALCOHOLIZED] [ZOECKLEIN, WAAP, P#458] PERMANGANATE INDEX [POLYPHENOL INDEX, “PI”] {FROM ZOECKLEIN} - AS NEUBAUER – LOEWENTHAL PROCEDURE - NOT THE SAME AS NEUBAUER – LOEWENTHAL PROCEDURE – GIVES ONLY “CRUDE” EVALUATION}

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 157 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

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 160 SOME WINE ANALYSES VALUES FROM MY ENOLOGY RESEARCH PROJECTS

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 164 420 NM – BROWNING COLOR 520 NM – RED COLOR 420 NM + 520 NM = DENSITY OR INTENSITY 420 NM / 520 NM = HUE OR TINT WINE COLOR

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 165 SOME VALUES FOR COLOR FROM MY ENOLOGY RESEARCH PROJECTS

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 168 SOME OTHER WINE ANALYSES THAT LARGE 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

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 173 SOME VERY SOPHISTICATED AND EXOTIC WINE ANALYSES

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 179 NUCLEAR MAGNETIC RESONANCE [NMR] AJEV 2003 ARTICLE ACETIC ACID [VINEGAR] DETECT THRU NECK OF UNOPENED BOTTLE OTHER WINE COMPONENTS POSSIBLE

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 180 FOSS FOURIER TRANFORM INFRARED SPECTROPHOTOMETRY [FT-IR] FOR: GRAPES - GRAPESCAN WINE - WINESCAN ALMOST ALL MAJOR COMPONENTS!

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 184 COMPLEX LIKE A SPIDER WEB !

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 207 TO BE CONTINUED AS INTEREST & RESOURCES PERMIT JUST LET ME KNOW !

WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 1 SOME CHEMICAL WINE ANALYSES FRANK J. GADEK, Ph.D., FAIC ENOLOGY EDUCATION SERVICES.

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WINE ANALYSISCOPYRIGHT F. GADEK 04/18/2003 1 SOME CHEMICAL WINE ANALYSES FRANK J. GADEK, Ph.D., FAIC ENOLOGY EDUCATION SERVICES.

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