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LONG TERM LEACHING FROM BOTTLES. Prepared by Giancarlo Boschi (Calp ) Presented by Pietro Stanghellini ( Calp ) 13 th ICF TECHNICAL EXCHANGE CONFERENCE. INDEX. MODEL A - AUTOMATIC BOTTLES : 9 YEARS STORAGE MODEL B - AUTOMATIC / HAND MADE BOTTLES:
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LONG TERM LEACHING FROM BOTTLES Prepared by Giancarlo Boschi (Calp) Presented byPietro Stanghellini(Calp) 13th ICF TECHNICAL EXCHANGE CONFERENCE
INDEX • MODEL A - AUTOMATIC BOTTLES: 9YEARS STORAGE • MODEL B - AUTOMATIC / HAND MADE BOTTLES: 3 YEARS STORAGE • MODEL C -AUTOMATIC BOTTLES: 4 CONTACTS OF DIFFERENT DURATION • MODEL D - ORDINARY AND PRETREATED BOTTLES: A 2nd CONTACT LASTING 4 YEARS • MODEL E - LEAD CRYSTAL AND BARIUM GLASS BOTTLES: LEAD AND BARIUM LEACHING 7 YEARS STORAGE
AUTOMATIC BOTTLES AFTER 9 YEARS STORAGE WITH BEVERAGES • VOLUME BEVERAGES - 700 ml 24 h ISO Test = 96mgr/Litre “new” bottles SA/V = 0.62 cm-1 TYPE BEVERAGES • WHISKY pH=3.4 • BRANDY pH=3.8 • ACETIC ACID 4% pH=2.4
AUTOMATIC PRODUCTION AFTER 9 YEARS STORAGE (Model A) • Lead leaching into HAc 4% is much higher than Whisky and Brandy after 6 years (+43%) • Leaching in Whisky after 6 years is over 600% than leaching after ISO (96 mgr/L) • After 6 years Whisky and HAc were degraded, the test continued with Brandy
AUTOMATIC vs HAND MADE PRODUCTION AFTER 3 YEARS STORAGE (Model B) “Automatic” ISO “new” 127 mgr/Litre “Hand made” ISO “new” 318mgr/Litre • After 3 years, Lead leaching from Hand made product is about 240% of leaching from Automatic pH BEVERAGES • WHISKY (A) -3,36 • WHISKY (H) - 3,87
REPEATED SHORT CONTACT PERIODS (2 MONTHS) WITH HAND WASHING AFTER EACH CONTACT (Model C1) AUTOMATIC PRODUCTION • ISO Test = 241 mgr/Litre for “aged” Bottles • Type beverage = Whisky • pH Whisky = 3.9 • SA/V = 0.62 cm-1 • Hand washing with mild detergent; time 30”
REPEATED SHORT CONTACT PERIOD (2 MONTHS) WITHDISHWASHING MACHINEAFTER EACH CONTACT (Model C2) AUTOMATIC PRODUCTION • ISO Test = 241 mgr/Litre for “aged” Bottles • Type beverage = Whisky • pH Whisky = 3.9 • SA/V = 0.62 cm-1 • Dishwashing machine, rinsing with tap water; time 30’
COMPARISON BETWEENHAND WASHING(C 1)ANDDISHWASHING MACHINE(C 2) • As known, after the 1st contact, Lead leaching is lower with hand washing than with dishwashing. • In both cases, Lead leaching after the 3rd contact is relatively low ( < 100 mgr/L ) .
4th CONTACT OF 3 YEARS AFTER 3 SHORT CONTACTSOF 2 MONTHS EACH (Model C3 and C4) • In the case C3 (hand washing) Lead leaching after the 3rd contact was: 33mgr/L • In the case C4 (dishwashing) Lead leaching after the 3rd contact was: 81mgr/L • After the 4th contact of 3 years Lead leaching is : C3 (hand washing) : 217mgr/L C4 (dishwashing) : 244mgr/L
COMPARISON BETWEEN A 1st CONTACT OF 3 YEARS vs 4 th CONTACT OF 3 YEARS AFTER 3 SHORT CONTACTS OF 2 MONTHS (Models B, C3 and C4) AUTOMATIC BOTTLES • In a 3 year contact, after 3 short contacts (2 months each), Lead leaching reduces more than 50 % in both cases C3 and C4
ORDINARY and PRETREATED (vinegar) BOTTLES:a 2nd CONTACT LASTING 4 YEARS (Model D) • AFTER THE 1st YEAR OF CONTACT WITH WHISKY, FOR EACH TYPE OF BOTTLE (ORDINARY AND PRETREATED), 2 SAMPLES HAVE BEEN WASHED BY HAND AND 2 SAMPLES BY WASHING MACHINE (STRONG CYCLE LASTING 1h,30’); THE 8 SAMPLES HAVE BEEN RINSED BY WATER AND THEN REFILLED WITH WHISKY (pH 3.9). • DURING THIS 2ND CONTACT, 1 cc HAS BEEN EXTRACTED FOR LEAD LEACHING DETERMINATION AT 1 YEAR TIMEINTERVALS.
ORDINARY BOTTLES 1 YEAR WHISKY - 426 gr/Litre D1 : HAND WASHING Pb WHISKY 1st year - 112 gr/Litre 2nd year - 198 gr/Litre 3rd year - 238 gr/Litre 4th year - 258 gr/Litre D2 :WASHING MACHINE Pb WHISKY 1st year - 362 gr/Litre 2nd year - 496 gr/Litre 3rd year - 521 gr/Litre 4th year - 548 gr/Litre PRETREATED BOTTLES 1 YEAR WHISKY - 7 gr/Litre D3 : HAND WASHING Pb WHISKY 1st year - 8 gr/Litre 2nd year - 8 gr/Litre 3rd year - 8 gr/Litre 4th year - 9 gr/Litre D4 : WASHING MACHINE Pb WHISKY 1st year - 16 gr/Litre 2nd year - 17 gr/Litre 3rd year - 19 gr/Litre 4th year - 21 gr/Litre 2nd CONTACT LASTING 4 YEARS AFTER 1stCONTACT OF 1 YEAR (Model D)
HAND WASHINGBOTTLES (D1) ORDINARY BOTTLES(O) 1st YEAR - 112 gr/Litre Pb 2ndYEAR - 198gr/Litre Pb 3rdYEAR - 238gr/Litre Pb 4thYEAR - 258gr/Litre Pb (D3) PRETREATED BOTTLES(P) 1st YEAR - 8gr/Litre Pb 2ndYEAR - 8 gr/Litre Pb 3rdYEAR - 8gr/Litre Pb 4thYEAR - 9gr/Litre Pb
DISHWASHING MACHINEBOTTLES (D2)ORDINARY BOTTLES(O) 1st YEAR - 362 gr/Litre Pb 2ndYEAR - 496gr/Litre Pb 3rdYEAR - 521gr/Litre Pb 4thYEAR - 548gr/Litre Pb (D4)PRETREATED BOTTLES(P) 1st YEAR - 16gr/Litre Pb 2ndYEAR - 17 gr/Litre Pb 3rdYEAR - 19gr/Litre Pb 4thYEAR - 21gr/Litre Pb
COMMENTS • The benefits of hand washing is confirmed after the 2nd contact, Lead leaching is : Hand washingD1 =258 gr/LD3 =9gr/L DishwashingD2 =548 gr/LD4 =21 gr/L D1 and D3 = about 50 % of D2 and D4 (respectively) • Pre-treated Bottles show an extremely low leaching also duringthe2nd contact; probably a pre-treatment lasting less than 24 hours can be sufficiently effective and more easy to be applied; this approach can be investigated with further tests.
LEAD AND BARIUM LEACHING FROM BOTTLES(Model E) Bottles in Barium Glass have been filled with whisky and stored for 7 years; sampling and analysis for Barium leaching determination have been carried out at 1 year time interval. The protocol is similar to Model A. Lead and Barium leaching are compared during the 7 years of test.
BARIUMLEACHINGfrom BARIUM GLASSBOTTLES AUTOMATIC BOTTLES ISO Ba = <10gr/L pH Whisky Model (E) = 4,2 BaO in Barium Glass = 19%
COMPARISON BETWEENLEADandBARIUMLEACHING ISOPb Lead Crystal - 96 gr/L ISOBa Barium Glass - <10 gr/L pH Whisky Model (A) - 3,4 pH Whisky Model (E) - 4,2 • PbOLead Crystal - 25% • BaOBarium Glass - 19%
COMMENTS • Although the Barium Glass has not been specifically designed with the purpose of limiting Barium leaching, it is surprising to observe the very high increase with time of Barium leaching. • Barium leaching appears to be extremely low during the ISO test (<10 gr/L), but it becomes very high in whisky after 7 years (2600 gr/L).