Distilling liquor

 

If your talking about distilling it's a separation method based on different boiling points. In the dutch language 'distilleren' means distilling alcohol. To also get acquainted with distilling I have followed a course during the past few weeks given by Pieter Rijneveel in Dordrecht.

Pieter has a distillery http://www.slijterij-vwk.nl/  and according to traditional methods  he distills with a single-walled copper kettle. During one evening we visited a distillery of van Toorn in Vlaardingen

The photo above is a still from the distillery. Distiller Leo Fontijne gives some explanation about the production process of liqueur, genever, brandewijn and advocaat. He is the only producer of  'schelvispekel'. See the website http://www.schelvispekel.nl/





In addition to theory there was also room for making liquor. I got a jerry can, yeast, a bag of sugar and a water lock . The intention was to ferment  a sugar solution for 3 to 4 weeks and and distill the alcohol off.

fermentation of sugar solution


Here is the recipe for fermentation, including:

1 kg sugar in 1 liter water and simmer for 5 minutes

dissolve the sugar water to a total volume of 5 liters in a fermentation tank, then let cool

Take about a half liter of solution and solve 1 gramof yeast and a crushed vitamin C tablet in it.
Bring this mixture back into the fermentation tank and end it with an airlock.
Shake the tank daily.

 

equation for the fermentation






ethanol model


 

A few weeks later the sugar solution, now about 10% fermented into alcohol, could be brought into the still. This is the smallest still Pieter has and is made from parts of a central heating boiler.

In the proces of distilling  alcohol a good cooling and separation of water and alcohol is important. The separation of the alcohol and water is made possible by a vertical column filled with marbles.



top of the still




After this separation column and the thermometer are some water coolers that make that alcohol vapor is condensed well.

 After some 20 liters of fermented sugar is transported in the still Pieter closes the boiler off and closes the cracks with a paste of flour and water.

Then the gas burner under the boiler is lit. After about half hour, the first distillate from the condenser drips into a beaker. Of course we throw the first 200 mL of distillate away because of traces of methanol in it.

Meanwhile we are working on skinning and filleting of an orange.

The essential oil in the peel with cinnamon and cloves maak sure we get a good taste of the liqueur. The sugar content of the liquor is achieved by 1 kg of sugar to 1 liter to resolve.

To make a good liquor we have 1 liter sugar 1 liter water, 1 liter of alcohol plus the orange rind and cinnamon cloves needed. This mixture must be left at least for 4 days to extract and then filter and divide into bottles. The result: an orange liqueur with an alcohol content of about 33% and 25% sugar content.

 In total, there are 2.5 liters orange liqueur made. Enough to get some bottles to give away for Christmas. I have not yet had any comments from people who have tasted the liqueur.

 When I poured the  liquor in smaller bottles it smelled very good! Do you want to know more about where liquor and beverages in general are produced click on this link:

http://www.pdcg.nl/left/drankenbank/introductie.php?grp=17&pg=846

Distillation of pine needles

Sunday, October 10, 2010I live in a wooded area and had planned a while  to distil the leaves of pine for essential oil. The weather cooperated this weekend to get back to distil.

For this distillation I had chosen the spruce. I  took some branches of very young trees growing naturally in the forest. With a folding crate full of freshly cut branches I went to work.




left and right spruce and pine

 

This is the silver fir Albies alba. http://www.bomengids.nl/zilversparren.html

The difference with the pine, which are very common and mostly does well on poor sandy soils, is very obvious.

 

As preparation for the distillation, I cut the branches into smaller pieces of mostly young twigs with needles.

 After having stuffed the Alembic with freshly cut spruce branches distillation could begin. At a temperature of about 90 degrees Celsius (in the top of the alembic) the first drops came from the cooling bucket

Setting the cooling gave no problems and after more than two hours, I stopped distilling.At that point there was no oil left, and I had six bottles filled with hydrosol.

The amount of spruce branches in the alembic was not weighed. So a exact yield was incalculable. What I know is that I filled the alambic with about 7 liters of spruce twigs and distilled  about 7 mL of essential oil.

The oil had a very surprising pleasant smell. I had expected a more pine-like odor. The spruce essential oil had a citrus odor. If you read the books about it is this true. Fir needle oil contains pinene Santen and over 30% limonene, a terpene that a major constituent of citrus oils. Reason enough for me in the near future to distil more conifer species .

Steamdistillation of lavender, eucalyptus and citruspeel

Thursday, August 26, 2010

steam distillation of citrus peel

Last school year , two groups of students from the Mgr Frencken College, Oosterhout , as part of their profile, concerned themselves with fragrances. One group of high school students have investigated the effect of lemon oil and the influence of concentration. The other group of 5- HAVO pupils experimented with  fragrances in general views.

Photo : Wikipedia

This was a great opportunity for me as facilitator to let the students do a steam distillation of essential oil.The steam distillation arrangement of laboratory glass ( see previous post) was excellent for this . Therefore , the pre-university students had cut the shells of 12 lemons into small pieces and placed them in the biomass flask. After 40 minutes distillation they had a yield of about 2 mL.

Photo : Wikipedia

The pupils of 5 havo  where distilling orange peels. This group has previously the peels derived from 8 of oranges adjusted this was later yield calculated. The steam - distillation of 454 g peel yielded 2.12 g oil.

The scan of TLC plate (silica gel G) with 10 essential oils Developed with mobile phase toluene - ethyl acetate ( 93:7 v / v) , next sprayed with vanillin in H2SO4 and heated . From left to right oils from : bergamot , cedar , eucalyptus , Syzygium , malaleuca , Lavandula , mint , orange , pine, spruce . Identified components : B1 and L1 - linalool, B2 and L2 - linalyl acetate , E1 - cinneol , G1 - eugenol , G2 - carryophyllene . Doubt Fully Identified components - C1 - cedrol , M3 - menthol , P1 - limonene .
Thin Layer Chromatography
photo : wikipedia

This group has also succeeded in their oil to be analyzed at a company laboratory IFF ( International Flavors & Fragrances IFF ( Netherlands ) BV ) in Tilburg . This was a unique opportunity because the equipment in schools is not sufficient to change the oil in a reliable way to investigate. The oil was analyzed using a gas chromatograph , this technique is derived from the separation method chromatography.
With this technique you get information about the composition of the oil. It would be excessive to state the whole chemistry of the essential oil treatment. A comprehensive story of the composition can be read on ; http://www.gielenaroma.nl/index.php?page=werkzame-bestanddelenA database on the composition of essential oil can be found at : http://www.thegoodscentscompany.com/essentlx.html

Source : Kennislink

The types of substances ( molecules) in essential oil can roughly be divided into:

ALCOHOLS

Aldehydes

ALKANES

Carboxy - ACIDS

Terpenes

ESTERS

ETHERS

FURANOIDEN

KETONES

Lactones

Oxides

PHENOLS

Orange oil is an important fragrance determining substance the terpene ( R )- Limonene . This molecule is the mirror image of ( L )- Limonene a substance that is characteristic of the smell of lemon oil. The following gas chromatogram is the result of a measurement with the gas chromatograph of the orange oil that the students had made .

gas chromatogram orange oil

Each peak in the chromatogram represents a substance . The results of this chromatogram was compared (computer)  with existing data of the substances. The measurement yielded 23 identified substances .

I have compared the results with the average composition of orange oil in the book 'The chemistry of essential oils made simple '. The results I have rankedin the following table

Citrus sinensis

sweet orange
                                                              measurement IFF

monoterpenes 90-95 %                                                      

d- limonene 85-90 %                              86.16 %

myrcene 1.3 %                                     3.61 %

terpinolene 1-2 %                                    0.01 %

tetracyclic terpenes 4-8 %                      -----

aldehydes 3-8 %      

citral                 1.2 %                                -----

decanal             1-2 %                            0.88 %

citronellal           0-1 %                           0.10 %

Dead canal         0-1 %                          0.25 %   

alpha sinensal      0-1 %                          0.13 %

geranial              ------                           0.26 %

                                                                                           

Alcohols 2-6 %

carveol              1-2 %

linalool               1.2 %                        1.85 %

alpha- terpineol   0-1 %                      0.25 %

geraniol               0-1 %                      0.22 %

1- octanol          ------                         0.66 %

1- nonanol         ------                        0.10 %

1- decanol         ------                         0.35 %

sesquiterpenes --------                                                     

beta ylangeen     -------                       0.11 %

beta - farnesene   -------                     0.03 %

ketones 1-4 %                                   --------

esters 2-3 %

citronellylacetaat 0-1 %                      -------

geranylacetaat     0-1 %                0.02 %

Furanoides        1-2 %                --------

Sesquiterpenones 0-1 %

nootkatone         0-1 %                         0.06 %

In addition to large contracts , for example the amount of d - limonene , decanal and linalool are also some differences in composition . This may be the origin and production of oil. The percentages given are cold-pressed orange peel. The oil of the students is by steam distillation obtained .

Steam Distillation in glass

Last year I started steamdistillation using a distillation apparatus of laboratory glassware

I had seen a picture on the Internet of some steam distillation set. The price that was asked , over $ 400 plus shipping , far over my budget. Therefore, I  asked a glass supplier ( http://www.lgsbv.com/ ) if he was able to supply this type of glassware.

boiling flask 2 liters

This was possible for the amount of € 220 , - . One month later I was the proud owner of this glass distilling unit. The setup consists of a boiling flask with a capacity of 2 liters, a Biomass flask (Pyrex®; 2-litre

biomass flask 2000 mL with distillation structure

The connection to the coil cooler is made with a distillation setup.

coil condenser

For boiling I use an electric cooker .
In the months June , July and August of 2009 I started working with the distillation of a number of plant parts. For this I filled the biomassflask with the plant parts and caught the distillate .
The revenues were disappointing , but could be explained . A volume of 2 liters fresh picked herbs  is little ground when you know that the most essential oil containing herbs give a yield of 1% of the plant parts.

distillation design

In the months June , July and August I went to work with a number of plants .
The distillation of chamomile resulted in a pretty strong hydrosol , but chamomile oil only visible as a pair of little blue strings floating in the hydrosol . A hemisphere filled with freshly picked rosemary gave it a fragrant distillate but not a drop of oil. On distillation of coin the same story. Only distilling faded lavender gave a yield of approximately 2 mL fragant oil.
The disadvantage was that a portion of the proceeds remained in the distillation bridge. It is possible to produce oil with this setup !

Tuesday, August 3, 2010

Eucalyptus in the Netherlands

Gustavo Iglesias (git - forestry ), expressed in his own way the story of the Eucalyptus Festival  held on July 17 and 18 in Steenwijkerwold. The story is posted on the weblog eucalyptologics .

For the interested a must to read. Gustavo has many links contained with background information about Eucalyptus . Includes a story about the oil glands in Eucalyptus leaf .

More information via the link below:

 http://git-forestry-blog.blogspot.com/2010/07/eucalyptus-oil-distillation-hi-tech.html

Friday, July 23, 2010

Lavandin distill

On Friday, July 9 , I picked a large amount of lavandin at the lavender farm Viva - Lavandula  farm. The Lavandin official Lavandula intermedia var . was dryed in 24 mesh trays in a well ventilated area.

I expected that during the drying the essential oil of lavender for a part would be released. That did not happen .   Only when touching the drying plant parts , the typical lavender scent escaped.

On Wednesday 21 and Thursday, July 22 , I decided to distill a part of the dried Lavandin.

It was exactly 800 grams Lavandin in the alembic .

During the eucalypt feast in Steenwijkerwold  a visitor had told me that he used aluminium tape for sealing his still. Thus far, I used a paste made from rye flour and water. Works well but is rather laborious .

Photo : Frank Stolvoort

So every reason to try this method in the distillation of Lavandin .

Steam leaks were easy to solve by the tape (with a glove ) just to press the tape or tape around to leak. 

Lavandin , has greater yield of essential oil compared with lavandula, this was during distillation actually already visible.

On Wednesday and Thursday I have distilled 4 times a quantity of 800 grams. 

The essential oil , I per day collected was filtered and put in dropper bottles. To increase yields I've collected the hydrosol , 15 filled wine bottles with a total volume of 12

Liter , and distilled in the alembic cast. It gained another 5 mL extra of oil.

In total  I produced 80 mL lavender oil which is converted 2.5 % yield of the dried Lavandin .

I 'm not sure , but I think there is not much distilled lavender and in the Netherlands cultivated Lavandin oil available!

A collector's item?

Tuesday, July 20, 2010

Eucalyptus distilling

On Friday, July 16th was the day. I was able to work with fresh flown in eucalyptus leaves from Galicia . Gustavo had the leaves airtight in plastic bags and numbered.

On Friday it was not clear wich bags the eucalyptus species were in. I have therefore decided to start with bag 1 to 4 to start.

The total weight of 2000 grams  of leaves were firmly  pressed into the column of the alembic

After Catherina sealed the alembic with rye flour paste the burner could be ignited.

Just before the water in the kettle began to boil actually something inevitable happened ! The glass table was not withstand as much heat from the burner and broke into pieces .

Fortunately remained damage was so limited that after clearing the shards the distillation apparatus could be put together. The alembic did have some badly damaged.

The two kilograms of eucalyptus leaves ( E.globulus ) were distilled for over 2 hours .

The total volume produced essential oil was 18 mL . With a quick calculation to get off to a yield of 1 % .

The witch Eucalypta was obviously right on the scent of fresh eucalyptus oil !

She liked the smell . The proceeds of the oil , I have divided into two vials.

The distilled leaves were then removed with a new load of eucalyptus leaves to start .

The new batch of leaves were in the pockets 5 to 8 and had a total weight of 1550 grams. After 2 hours distilled I produced 6 mL of essential oil. It later appeared that this leaves were a mixture of two species eucalyptus included E. nitens and E. globulus .

SATURDAY 17 JULY

 

Photo : Frank Stolvoort

This day attracted most visitors to the Eucalyptus Festival.

photo Frank Stolvoort

A photographer from the local paper had come and made the following report: http://www.steenwijkercourant.nl/?n_id=154361&s_id=668

There were plenty of eucalyptus leaves about for two distillations . From an email from Gustavo I read that the bags 9 to 13 E.nitens contain the small pockets 14 and 15 young leaves of E.nitens .

The leaves of 9 to 13 had a total weight of 3585 grams and fits perfect in the alembic .

After 3.5 hours distilled I had 15 grams of oil produced.

Converted  a yield of about 0.5% . There was a difference in yield between E.globulus 1 % and E. nitens 0.5 % . The final distillation of young leaves was not really carry out . The amount of 320 grams of leaves was not enough essential oil to drain . The produced oil about 0.5 mL was increasing to funnel down.

photo Frank Stolvoort

According to Gustavo:

Your results for E. globulus are similar to Those quoted by Bosisto today : 0.75 to 1.25 % richness in crude oil . Lower Than what is quoted in scientific literature , but there is always a difference Between fully controlled laboratory conditions and industrial operations (even if at a small scale ) . Your results for E. nitens are Useful too .

Eucalyptus Festival in Steenwijkerwold

Nursery Green Prince and Eucalyptus Nursery Koala organized a Eucalyptus party on 16 and July 17 .

During these two days I would give a demonstration of the distillation of eucalyptus leaves.

Steenwijkerwold is not next door so I had to pack the alembic and accessories and mounted them on the bike and traveled by train to Steenwijk.

The Eucalyptus Festival was held on the grounds of Nursery Green Prince of Kwikkel 3 in Steenwijkerwold . This nursery Hans Prince specializes in growing exotic plants.

For more information about this farm at:http://www.degroeneprins.nl/

Besides guided tours , there were plenty of other activities organized click http://www.eucalyptuskwekerijkoala.nl/eucalyptusfeest.htm for details.

During the two days the visitors more information to give , I had a brochure about the technique of steam distillation and eucalyptus oil itself.

What is Eucalyptus oil and how are you?

Eucalyptus oil is by steam distillation made of the large-leaved eucaluptus tree or Eucalyptus globulus . Besides this variation , other eucalyptus oils used, especially the lemon eucalyptus (E. citriodorata ) , mint eucalyptus (E. radiata ) and the E. polybractea .

Indication of the composition:

> 25 % - 1.8 cineol

5-10 % - Limonene

3-5 % - alpha pinene

1-2 % - Alpha Terpineol

Eucalyptus is in perfumes often used because it is a strong medicinal smell. It is in such cases essentially a top note . The top is fresh with the characteristic odor of cineol in the heart , the freshness largely disappeared , but caused some green notes .

Eucalyptus can in soaps be used , it gives a certain freshness , but is a strong fixative need . It is also an important oil in aromatherapy and also as a home remedy for colds . Eucalyptus oil supports breathing. They regenerate lung tissue, mucus problems and the drain promote . Also works sedative in strong cough stimuli . In the spiritual domain the refreshing and stimulating. It increases concentration and supports logical thinking .

Eucalyptus oil is often used in medications for respiratory illnesses, asthma , bronchitis , colds and laryngitis.

Furthermore, eucalyptus oil a the powerful natural disinfectant that is often added to detergents .

eucalyptus oil:

Do not use in children and pregnant women. used topically is Eucalyptus oil ( diluted ) is not toxic. Internally , however , a small amount of 3.5 ml can be fatal.

Attention ! essential oils are highly concentrated. use them Never purely on the skin unless explicitly stated that it does. For intake of essential oils or other specific medications , we recommend a qualified aromatherapist to consult .

Eucalyptus oil is irritating to eyes , skin and respiratory tract. Furthermore, flammable , so take care with aroma burners : get here enough water in it . When swallowed may cause lung damage. limonene , a substance that some people are allergic response.

STEAM DISTILLATION

Steam Distillation is a chemical separation method used for the purification of substances. This method was first (in the middle ) used by the Arabs who steam distillation used to make of essential oils .

An important application of steam distillation is the extraction of essential oils . This is steam through a barrel of the processing plant parts resulted . The steam cools then down and condenses. The volatile components of the plant with the steam it and condensing too. Some of these volatile compounds dissolved in water and some not, it separates . Because this water insoluble part mostly lighter than water remains on water float and can there be gutters this called the ethereal oil. The water is called hydrosol . This hydrosol is primarily used to combat respiratory infections, upper respiratory infections, colds , flu , coughs and hay fever allergies. Good to gargle , as mouthwash or to cough syrup make , if necessary with a drop eo Not for use in children. The stabililteit of the hydrosol is not known. Best before 18 months if in a cool place stored , freeze can .

Important for the distillation process , the distribution of plant material . The cell walls of some plants are very thin , so that steam, water , solvents , the ability to penetrate . Other materials should be prepared. The materials are prepared , then the distillation begin immediately associated with the volatility of the material.