G. Ordinneau, On the nature of the Ethers of the Brandy and on the causes that influence it’s quantity

[This is such a mess and one of the first foreign language documents I ever collected. I should probably properly translate it and collect the other writings of the author.]

A big thank you to Christine Eslao for getting the document from the Harvard Library.

ordinneau in french PDF

This is crude OCR to babel fish English translation of a late 19th century French study of Cognac. The paper was widely cited by writers like Maynard Amerine and Peter Valaer. Unfortunately the PDF is in french but I think an english version exists somewhere. My understanding is the works of the seventh international congress of applied chemistry in 1909 were translated into other languages as well (I’ve seen english and German but never of the section that contains this paper). I do not know how useful this translation will be to readers because it is so poor but it will at least let people know that researchers such as Ordinneau were taking the chemistry of spirits quite seriously as far back as the 1890’s. These old works can still provide a lot of insights to the distillation renaissance that is happening.

The significance of the study was that Ordinneau showed that the acidity of the distilling material was very important to the formation of esters in Cognac. He also showed how the pace of distillation formed aroma compounds. I think he distilled a base wine to strip much of the aroma and alcohol, then re-added a neutral alcohol to the non-volatile fraction then re-distilled that fraction again. What Ordinneau finds is that he produces even more aroma compounds because of the increased opportunity for esterification (a reaction of an alcohol with an acid to produce an ester and water). I thought that esterification happened mainly through fermentation but I guess it also happens to a large degree by time spent in the still, with a pot still providing the most opportunity for esterification.

On the nature of the Ethers of the water of life of
Wine and on the causes that influence the
quantity that it owns
By Ch. ORDINNEAU.
There is a lack of specific information on the nature of the contained ethers in eau-de-vie of wine; also I think interesting to publish the results of research made a long time ago already on the distillation of wines of the Charentes products.
I will indicate first of all in a succinct manner the means by which I used to get these results I will provide in the suite. In 1897, I distilled about 10 hectolitres of dregs of the “Borderies” of Cognac, which provided 225 litres of phlegm or “brouillis” 15° which served as base for my tests. This brouillis, saturated by the carbonate of soda and distilled, provided free vi3 water of free acids, and one residue or vinasse that evaporated to dry and gave the volatile acids, sodium salts.
Eau-de-vie has been processed by the soda caustic to décom­poser ethers, and then distilled. Vinasse evaporated then dry provided etherified acid soda salts.
The separation of volatile acids was made by their industries in ethyl ethers and their rectification and split with a Henninger device to six balls. Low fractions were studied specifically; CROTONIC acid was obtained crystallized and caproic acid was separated as a calcium salt.
The lactic acid that comes from the fermentation of the Malic acid in wine
the summer separated from sodium salts by drinking alcohol, which easily dissolved.
The results concerning the nature of volatile acids and their quantity, either free State or the State of ethers, in the procedure of wine, are recorded in the following table
ordinneau table
• The Lees of wine contained about 70% of wine, the rest was repré­senté by the yeast, pectic substances and the potassium bitartrate, constituting a deposit that distillation provides especially heavy ethers or oenanthique ether. The amount of this last ether is variable in the waters of life; It corresponds on average to 10 gr. per hectolitre of alcohol at 100 ° by direct measurements made on different types of eau de vie des Charentes. Assuming this amount of 10 gr. I established in a special column total ethers provided by current distil­lation wine with obtained living water.
Ethers are almost entirely as ethyl ethers; I to was assured me in a previous operation that had allowed me to remove the head of 20 hectolitres of brandies by splitting 20 gr. of formic ether and 3 kg. 400 gr. of acetic ether. The column of ethers is therefore ethy­liques ethers, acids mentioned.
We see by this painting that volatile acids in wine are the same those who combined alcohol provide the ethers. However the lactic ether is not stable there. are found in the distilled product that fast free.
Acetic ether in water studied life represents 92% of
ethers of the wine; He is accompanied by small amounts of ethers
formic and 7% approximately of oenanthique ether. other ethers
very fragrant intermediaries are found in very low quantities.
Acetic ether being more volatile than alcohol, because it boils at 73% must meet head especially during the distillation process and this is what actually takes place.
Since brandy ethers are formed by the combination with alcohol the volatile acids, their quantity is dependent on several factors according to the laws of etherification. the main are: ‑
10. The amount of volatile acids in the wine. – known for a long time that this amount is variable depending on the nature of yeast and especially the abundance of organisms or bacteria furnished by the grapes at harvest. These bacteria are abon­dantes grapes stung by wasps and birds and those with rot. Their action is slow and produces the General diseases of the wines. As soon as the complete fermentation the wines are little wealth in volatile acids and ethers, so what it is about bookbinding in the following spring, especially with wines that are not separated from their lie. The acetic acid bacteria is one that provides the most volatile acids. It is in the wines of the Charentes, which are mainly in white; on the other hand it causes in noon wine the large amount of ethers are sometimes found.
The water of life no.. 1 was prepared with a hectolitre wine clear made specially by the wort to the Khun device sterilization and fermented with a pure yeast. The distillation has been rapid.
The water of life no.. 3 was provided by a wine disorder, turned but not pitted, and load of bacteria.
The water of life no.. 4 from the Champagne region, was considered to be of poor quality in the tasting.
2′ Extended the time that lasted distillation. – heating wine, that is to say a slow distillation, éthérifie volatile acids and subsequently increases the amount of ether, and this amount, which is difficult to establish with a laboratory device, it is not when using the boiler charentais alembic.
• For example, by adding to the vinasse that remains in the still after the distillation of wine yields a quantity of neutral alcohol equal to that contained in the primitive wine a vinous alcohol loaded in ethers. An operation is made with an aircraft first jet and second provided an alcohol containing 27 gr. of ethers / HL to 100 °, while the alcohol being implemented had only 6 gr., hence gain of 21 gr. due to distillation.
A stillage distilled by brouillis after Champagne mixed with alcohol containing 5 gr. of ethers provided 44 gr. of ethers, where 39 gr. gain provided by the boiler. However, vinasse necessarily less volatile acids than the wine itself, so as such less than product distillation contains ethers than wine. We are forced to admit that during the slow distillation by brouillis charentaise method are made with certain wines
40 gr. of ethers at a minimum, ethers found in the water of life and which did not exist in the wine, or that an eau de vie made so with 120 gr. of ether comes from a wine that contained only 80 gr. maximally.
This amount of ether produced depends on the heating time, so that a slow distillation is most advantageous for their Production as a quick distillation and a simple or brouillis apparatus is greater than this point of view to a first draft with second device, and the latter greater than the device without second.
We wanted to assign to the separation of varying amounts of the head of the good heating or grinding the cause of poverty in certain waters of life of Cognac ethers. This explanation is not acceptable. It does not exist in water of life free ethers by rectification, Charentes whereas this operation does not in fact occur. A few litres withdrawn at the beginning of each heating and which are rich in acetic ether are added to the liquid to be distilled by the next operation, and always end up, whatever the importance do the amount of separate head.
Elsewhere the distillation of wine with the area methods does not residue alcoholic as the indus­trielle alcohol rectification, and in distilleries more often the latter was obtained at low title containing the mixture of the last head and the last tail remains to be added to the first barrel of the operation of the following year, so that in can admit that there is no loss of ethers during distillation.
3 ° The total acidity of the wine. – This acidity is important, because it
Bele. r 2
228
promotes the formation of ethers. As a result wines obtained with little ripe grapes that are distilled on their lie that contains potassium acid tartrate, are advantageous for the preparation of ethers.
It follows from these considerations that the pure waters of life less rich in ether are those which are distilled: as soon as the wine fermentation finished and are produced quickly to single unit or with the first jet with wines of Lees apparatus and from very ripe, healthy grapes.
Many ethers assays I’ve done over the last 15 years have provided me less than 100 grams per hectolitre of alcohol at 1000 only operating on waters of life from the harvest of 1894. The minimum was 92 Gr., the average has varied between 105 gr. and 120 gr. All life waters examined were obtained by slow distillation to the simple device.
The eaux de vie made with first jet machines used in secondary wines provide, from what has been said above, a lower amount of ethers, but I own point safe figures concerning these waters of life.
Be that as it may it is easy to realize as such that the presence of ethers in an an alcoholic liquid cannot be proof of the existence of real life water in this liquid, since it is possible to form ethers by neutral alcohol to the charentais alembic distillation under certain circumstances. But as it is recognized that the best eaux de vie are obtained by slow distillation to the primitive device one can conclude that for the
Cognac real low-ethers more often involves poor distillation, while elevated, if it may not indicate exceptional quality, because some waters of life of
damaged wine are responsible for ethers, it provides nonetheless completed by the tasting, which can see the source of the first matter, of nranignemants pracieux on the value of the product considered.
CONCLUSIONS.
1. In the analysis of alcohols and spirits group of components by chemical functions: acids, ethers, aldehydes, higher alcohols, appears to be generally adopted.
2 For determination methods and their details, there is not yet agreement. The doubts are referent;
(a) for acids and ethers: choice of alkaline liquor and the flag.
(b) for aldehydes: colori­metriques and volumetric methods, and for them, the choice between processes Uayon, Jandrier Baker, and others.
(c) for the higher alcohols: separation and determination methods, process color French (Saliu-Girard). German prorede physico-chemical (Itiise-Hybiscus-Sell); English (Marquardt-Allen-Schidrowitz) oxidation process.
3. It is likely that different methods should be used for the analysis of various classes of alcohols, spirits and alcoholic beverages. For the classification, it. will be used in the first place of the tasting.
4. For the experimental study of all these excessive­ment complex issues, we propose the creation of three independent special laboratories of the national rivalries that are currently felt: one for countries where there is balance of industrial alcohol (Switzerland or Belgium); the second in one of the countries where pré­dominent the so-called natural spirits (Portugal or Romania); the third in North America.

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