SO2-Трета част

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SO2-Трета част

Мнениеот vinoirakia » Нед Юли 11, 2010 7:19 am

15. Removing Free SO2
Sometimes excessive SO2 is (accidentally) added to a wine. SO2 will slowly deplete during an oxidative ageing process, but sometimes winemakers wish to reduce the SO2 level in a short period of time. In any case, desulphiting may inevitably result in loss of aroma/flavour [Weger, 1956] and overdosing should be avoided at all costs. There are three methods commonly employed for such situations, and a fourth potential method.

15.1. Blending
Blending the high-SO2 wine with another wine low in SO2 is the safest method, ensuring the wine does not suffer from oxidation or further processing.

15.2. Aeration
SO2 is often removed from wine by aerating. This is based on the slow oxidation of the SO2 and is only really suitable for slightly excessive doses of SO2, since excessively high doses will not be successfully stripped by even multiple aerations.
Usually the wine is transferred from one vessel to another in a violent manner (with turbulence) to encourage oxygen contact. This method can be traumatic for a wine, potentially over-oxidising and "damaging" its delicacy. However, it remains a simple solution to reducing excessive SO2. A wine saturated with oxygen will contain 5-8 mg/l oxygen (see section "SO2 and Oxidation, Saturation level" above). Assuming a complete reaction (though somewhat chemically unrealistic), this amount of oxygen may remove 20-32 mg/l SO2. If the aim is to reduce SO2 by over 20-32 mg/l then this method can be used on a periodic basis more than once (with several days between successive operations). If the aim is to reduce the SO2 by less that 20 mg/l, the aerating should be done with less violence.

15.3. Hydrogen Peroxide
15.3.1. Theory
Free SO2 can be removed by adding hydrogen peroxide (H2O2) to wine. The use of H2O2 is considered too severe by many. Nevertheless, it remains one of the only real options for removing excessively high levels of SO2 from wine for the non-commercial winemaker.

The removal reaction is:
SO2 + H2O2 ===> SO4-- + 2H+

The molecular weight of SO2 is 64.1 and that of H2O2 is 34. Therefore, 0.5304 g (1/64.1*34) of H2O2 is required to react with 1 g of SO2.

The peroxide reacts with molecular SO2, changing the SO2 equilibrium. Since this equilibrium is continually re-establishing, the H2O2 should be added slowly. Additionally, since H2O2 is such a powerful oxidiser, the amount added should be calculated carefully. Analytically testing the SO2 content before and after H2O2 addition is advised.

Solutions of H2O2 commonly come as 3% solutions. If they are mass/mass solutions (this appears to be the typical case) they should contain about 30.3 mg/ml H2O2. If they are volume/volume solutions they should contain about 42.3 mg/ml H2O2. (See "Information on H2O2 content" below for more details.)
15.3.2. Example using H2O2
15 litres of wine has a free SO2 level of 70 mg/l. It is desired to reduce this to 40 mg/l. The reduction of 30 mg/l (70-40) requires an H2O2 addition of 16 mg/l (0.5304*30). Thus, the 15 litres requires an addition of 240 mg (15*16) of H2O2. Using a 3% mass/mass solution of H2O2, 7.9 ml (240/30.3) of the solution needs to be added to the 15 litres for the drop to 40 mg/l.

15.3.3. Information on H2O2 content
Pure (100%/weight) H2O2 has a density of about 1.41 g/ml.
Mass/mass solutions: 3 g H2O2 / (97 g H2O + 3 g H2O2) means a volume of 97 ml + (3 g / 1.41 g/ml = 2.13 ml) = 99.1 ml. This contains 3 g per 99.1 ml which is 30.3 mg H2O2/ml of the 3% solution.
Volume/volume solutions: 3 ml H2O2 / (97 ml H2O + 3 ml H2O2). 3 ml H2O2 provides (3 ml * 1.41 g/ml =) 4.23 g H2O2 per 100 ml solution, which is 42.3 mg H2O2/ml of the 3% solution.

15.4. Inert Gas Stripping
This technique is used to remove SO2 from large-scale commercial fruit juices. On a small scale, it might be done by sparging a receiving vessel with CO2 (or nitrogen or argon). The wine is then sprayed against the vessel wall in an attempt to volatise the SO2. Alternatively, bubbling inert gas through the wine might be practised. The effectiveness of this method is, however, questionable without the use of sophisticated equipment.

16. Adding SO2: Practical Considerations
When adding SO2, it is important to ensure that it is evenly distributed in the must or wine. Injecting SO2 solution steadily (rather than in a single hit) during pumping/transfer/racking procedures presents an ideal method of homogenous SO2 addition.
Due to the rapid enzymatic oxidation reactions in musts, SO2 ought to be in contact with the juice as soon as possible after crushing the fruit. This is the principal which should be followed in any SO2 additions to musts. Exactly how this is practised may vary from set-up to set-up. In the case where fruit is partially crushed upon harvesting, SO2 should be added to the fruit with the aim to take action within the juice resulting from partial crushing.
Addition of SO2 to the uncrushed fruit in the case of reds, or crushed and unpressed fruit in the case of whites, will result in SO2 binding with fruit solids. Such binding should be accounted for, and higher SO2 additions may be required in such situations.
Oxidation of draining press juice will be significant in the absence of SO2 and SO2 might therefore be added to the marc of the post-free run press fraction. Delteil [2001] argues that this practise results in increased aromatics and varietal expression, greater palate volume and decreased sensations of palate dryness.

Post crush additions in a liquid form are recommended, since they assist in SO2 distribution and help prevent combination with solids. SO2 is most effective when added to individual portions of the must during, or within quick succession of, pressing (or crushing, in the case of reds). This method presents a more effective use of SO2 than a number of consecutive additions to must storage vessels (e.g. must receptacle tanks/vessels).

High point-concentrations of SO2 indicate that SO2 has not been mixed thoroughly. In practise, this can sometimes be seen in crushed fruit or fresh must as a localised discolouration of the pomace or juice. Figure 11 shows this phenomenon.

According to some, adding small concentrations of SO2 to must sequentially results in more oxidation than would occur in an unsulphited juice. Additionally, SO2 doses are more effective on yeast and microbes if the dose is given as a single high dose, rather than a number of small sequential doses.

Since a portion of any previously added SO2 is in the bound form and therefore not effective, SO2 solutions used for additions should be relatively dilute.
After fermentation, corrective SO2 additions should only be made under conditions of potential contamination or volatilisation (e.g. during transfer or under high temperatures) or when molecular SO2 levels are far from the required effective dose.
17. Typical SO2 Additions
Winemakers who add SO2 pre-fermentation typically add around 25-50 mg/l at crush. This is followed by a post alcoholic fermentation (or post malolactic fermentation) addition sufficient to, having accounted for binding, maintain the desired molecular SO2 level. (Some estimate this as 120-150% of the amount required to maintain the desired molecular SO2 level.) During bulk ageing, and for bottling, the wine is maintained at this same molecular SO2 level.
As mentioned previously, molecular SO2 levels are pH dependent. However, many winemakers cannot assess pH in their wines and, therefore, quantities of total SO2 to add at particular times or procedures of winemaking are made based on rough guidelines. Exact quantities vary from winemaker to winemaker (and on wine type/style and set-up). However, dosages can be amplified or reduced depending on the circumstances surrounding the quality of the fruit, juice, and wine. For fruit and musts, the following situations will require increased SO2 dosages: high suspended solids, ruptured/diseased fruit, violent or prolonged fruit transport, increased handling, higher temperatures, or a longer duration between crush and fermentation. For wines, increased temperatures and increased exposure to air tend to call for increased SO2 dosages. At bottling, wine style and the intended duration of ageing dominate dosage decisions.

It is worth noting that, because of the differences in environmental conditions and typical practises in different countries, typical additions vary among different countries and regions. The additions in France, for example, are often much higher than what is considered necessary or normal in California. Likewise, hotter climates tend to receive higher doses (e.g. Languedoc Roussillon vs Burgundy). Common SO2 levels for addition to must are presented in Table 4 and levels for addition to wines are presented in Table 5. Note that these values are not the dosage additions themselves, but are the quantity of free SO2 that should exist in the must/wine after addition (binding should be taken into account upon addition to ensure that these levels are met). Table 6 shows recommended maximum values of total SO2. On an international scale, these values are relatively conservative.

(For typical Campden tablet additions, see the Campden Tablets section below.)

Table 4. Recommended free SO2 levels for musts
Circumstance Free SO2 (mg/l)
white, healthy fruit, low pH 25-50
white, healthy fruit, high pH 60-80
white, fruit with some rot 80-100
red, healthy fruit, low pH 50
red, healthy fruit, high pH 50-80
red, fruit with some rot 80-100

Table 5. Recommended free SO2 levels for wine
Circumstance Free SO2 (mg/l)
before MLF none / under 20
dry white, maintenance 30-40
sweet white, maintenance 40-80
red, maintenance 20-40
dry white, bottling 20-30
sweet white, bottling 30-50
red, bottling 10-30


The range in the values corresponds to the pH of the wine. If the wine is an acidic style the lower values should be used, whilst the higher values should be used for less acidic wines. Wines which will be travelling or stored in unfavourable conditions often have 1.5 to 2 times the bottling values above (Table 5) added at bottling.

Table 6. Recommended total SO2 levels for wine
white (conservative) under 150
red (conservative) under 150
white, dry (liberal) under 200
white, white (liberal) under 400
red (liberal) under 300


It is sometimes claimed that SO2 additions without reference to pH is sufficient. Whilst this is generally true, there are exceptions. Figure 13 shows three different levels of free SO2 (20, 30, and 50 mg/l) and their corresponding molecular SO2 levels at varying pHs. Assuming that molecular SO2 must be kept below the sensory threshold (2 mg/l) and above 0.8 mg/l for microbial stability (see Section 6), then "safe zones" are molecular SO2 levels between these two values (i.e. 0.8-2 mg/l). It can be seen from the figure that these zones still vary over the typical pH values encountered in wine. For example, whilst 30 mg/l free SO2 is sufficient for pH values ranging 3.0 to 3.4, it is not suitable for pHs outside this range (below this level it is above sensory threshold, above this level it is below levels suitable for microbial stability). Based on this information, it might be suggested that red wines (which typically have a pH > 3.2) be kept around 50 mg/l free SO2 and white wines (which typically have a pH < 3.3) be kept above 30 but below 50 mg/l free SO2. Of course, awareness of the pH is always preferable to such estimates.
18. Storage and Purity
Dry sulphur dioxide (in the metabisulphite form, or otherwise) is sensitive to high temperatures and humidity. It will lose its strength under such conditions. It is important to replace SO2 stores reasonably frequently.

Additionally, the strength of SO2 is sometimes weak upon purchase. For example, upon making up an aqueous solution of metabisulphite and testing its SO2 concentration, it is not uncommon to find only 90% of the expected SO2 value present. This is most likely due to the conditions experienced by the SO2 prior to purchase. It is therefore important to check the strength of the SO2 stock being used for winemaking additions.
19. Stock Solutions
Stock solutions of dissolved sodium or potassium metabisulphite salts provide a fast and simple way of adding sulphite to a wine. This is especially the case when a gram scale is not available and measuring a volume of stock solution is preferential to weighing out very small quantities of powder.

It is important to keep a stock solution in an air tight container since contact with air will decompose the sulphite. (It should also be noted that plastic is breathable to some extent, and stock solutions stored in plastic bottles should therefore be remade relatively frequently.)

As an example of the calculations used in making and using a stock solution, a 10% stock solution can be made up by adding enough water to 100 grams of potassium metabisulphite to make up a total volume of 1 litre (100 grams / 1000 mls * 100 = 10%). This solution contains 100 mg/ml of potassium metabisulphite. Since potassium metabisulphite is only 57.6% SO2, this solution then contains 5.76% SO2 (10% * 0.576 = 5.76%) or, alternatively stated, it contains 57.6 mg/ml of SO2 (100 mg/ml * 0.576 = 57.6 mg/ml).
10 ml of this 10% stock solution added to 20 litres gives 50 mg/l of potassium metabisulphite (100 mg/ml * 10 ml / 20 L = 50 mg/l) which gives 28.8 mg/l of SO2 (50 mg/l * 0.576).
Alternatively, to obtain 30 mg/l of SO2 in 15 litres, this requires 781 mg of potassium metabisulphite (30 mg/l * 15 l / 0.576 = 781 mg) for which 7.8 ml of the 10% stock solution is required (450 mg / 100 mg/ml / 57.6 % SO2 = 4.5 / 0.576 = 7.81 ml).

20. Campden Tablets
Campden tablets are designed to have a mass of 0.44 grams. However, consistency of the tablet size in manufacturing is questionable, and many winemakers claim there is little certainty that tablets contain the amount of metabisulphite they are intended to (expected concentrations have been seen to deviate by up to 25%). Additionally, some winemakers claim that the "fillers" used in Campden tablets to increase the bulk size of the tablet, taint wine flavour and affect clarity. Nevertheless, Campden tablets remain a simple way of adding a small (if rough) quantity of sulphite to a must or wine.

Rules of thumb for the use of Campden tablets are generally quoted as:
One tablet should be added per gallon (Imperial or US) initially and then one at each of the 2nd, 4th, 6th, etc rackings.
Or, if heat is used in preparing the must, none initially but one per gallon at each of the 1st, 3rd, 5th, etc rackings.

Assuming one Campden tablet contains 0.44 grams of potassium/sodium metabisulphite, the following sulphite levels are obtained by the addition of 1 tablet to the given volumes:
Table 7. SO2 Equivalent Campden Tablet Dosages
Salt per Imperial gallon per US gallon per litre
Sodium 65 mg/l 78 mg/l 297 mg/l
Potassium 56 mg/l 67 mg/l 254 mg/l

In practise, these figures may vary by up to 25%, possibly more.

21. Sulphur Wicks and Rings
Sulphur wicks or rings are usually comprised of cellulose coated sulphur or a mineral (aluminium or calcium silicate) mixed with sulphur. They are generally only used for dosing barrels or small wooden tanks. They are not recommended for use in concrete tanks or stainless steel, due to the subsequent chemical attack on the surfaces of these vessels.

Sulphur wicks and rings are heterogeneous and their exact SO2 content varies due to the manufacturing process and storage conditions (again, humidity reduces their effectiveness) [Chatonnet et al., 1993]. Sulphur rings are more sensitive to storage conditions than wicks.

In theory, the burning of a sulphur wick or ring follows the reaction:
S + O2 ===> SO2

However, in reality around 20-30% of the sulphur is lost due to (1) part of the sulphur falling from the wick before it burns and (2) part of the sulphur producing sulphuric acid. In an enclosed space like a barrel, the amount of sulphur which can be burnt is limited by the presence of sulphurous gas which inhibits combustion. For example, in a 225 litre barrel around 20 g of sulphur is the limit which can be burnt. In addition to this, humid barrels hinder combustion. In general, 5 g of sulphur burnt in a 225 litre barrel will increase the SO2 by 10-20 mg/l (by burning a sulphur ring) or by 10 mg/l (by burning a sulphur wick) [Chatonnet et al., 1993].

SO2 is not usually distributed evenly during the filling of sulphured barrels, nor does it homogenise well afterwards. A thorough mixing is therefore recommended after barrel filling (e.g. by rolling the barrel).

22. Acknowledgements
The author would like to thank Dr. John Danilewicz for his assistance in accurately describing the reactions regarding the oxidation of wine in the presence of sulphur dioxide. There is much debate with regards to the theories expounded in the literature in this area and Dr. Danilewicz's cutting edge input in this area is much appreciated.
Additionally, the author would like to thank Lum Eisenman for his communication of AO and Ripper test data results.

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