Dutch pilot experiment: LEGALLY growing organic female hemp flowers high in CBD

[Santalum]

Hi Grassomatic, Where can we read more about the Eletta strain? And what about seed suppliers? Thanks in advance

For many Finola appeals because of the dwarf nature of its grow and short season. That means it can be grown over many parts of the world where the taller longer season varieties will not.

 

[HFT]

Hi HFT,

I was wondering.. how much would you pay per kilo of feminized seeds of a registered (UE) dioecious strain with an average content of 6-7% CBD? and how much if it were a very early flowering with CBD > 10%??

ps - come si dice in bocca al lupo tra canapicoltori?... pare che finalmente stanno lavorando a un decreto legge, con limite di THC all' 1%. )

Ciao Grass-O-Matic!
I think that we are able to pay the right price for those seeds
But we don't need of some feminized hemp seeds but regulars... Regulars but dioecious to make a manual selection of female plants and do extractions of essential oils and CDB with the best conditions...
This year we paid 4,50€/kg. for uso-31, around 5euro for Futura-75 but they are monoecious...
The autoflowering Finola prize is 10euro/kg. ... Do you have some good but legal strain to plant in Italy?
We are open to every possibility

Speriamo porti bene 'sto lupo! Abbiamo tutte le carte in regola per fare prodotti anche di canapa, di qualità con il nostro micro-clima italiano...

Good luck also to you and yours seed bank. Some time ago I've tried maxi gom and sugar gom...very sweet taste and grow very easy and without much water in guerrilla growing...

 

[DutchHempCBD]

UPDATE

UPDATE

Here's an update.

Harvest 2014 processing
Some months ago we experimented with using a rotary sieve mounted with a 250 micron stainless steel mesh to obtain trichome rich concentrate. This was done by combining dried plant material (leaves and flowers with seeds) with dry ice nuggets. The dry ice nuggets with a temperature around -79°C (-109°F) cool the trichomes to such an extent that they become brittle and get dislodged from the plant material. However in the process some of the already brittle dried plant material also gets crushed and falls through the 250 micron mesh together with the trichomes. Using this approach we obtained a powder with a relatively high trichome content. From this trichome concentrate oil can be obtained by ethanol alcohol extract. Oil yield is around 10 to 15 wt% of trichome concentrate weight. By the smell and taste of it the oil contains terpenes and so also most likely cannabinoids. On ingesting no psychoactive effect is noticed, however at higher doses a clear relaxation of muscles can be noticed. It's quite likely that the oil contains cannabinoids, of which the most prominent are CBD and CBDA.


Even though in principal the technique worked the screen clogged often with combination of frozen moisture from the air, tiny pieces of dry ice and small plant material. On top of that the technique was quite inefficient in the use of dry ice. Dry ice is brittle and thus gets pulverized and easily lost among the processed plant material. This complicates the separation of the dry ice from the plant material after a batch is processed.

To prevent/minimize screen clogging and increase cooling efficiency we designed a rotary sieve system with a 2 mm screen and liquid nitrogen (-196°C, -321°F ). Though we haven't completed construction we have made some progress. This sieve has a 2 mm stainless steel mesh. The idea is to spray the plant material with a liquid nitrogen air mixture. This should cool the trichomes to such an extent that together with the tumbling motion of the sieve should dislodge the trichomes. The screen will stop seeds and larger plant matter (>2 mm) and let's through trichomes and small plant material. The latter is than collected and dried at ambient temperature to wick of the frozen moisture. This <2 mm trichome concentrate is further refined by sieving this through a 250 micron screen to minimize non-tricome content. The collected <250 micron trichome rich material can then be extracted using ethanol (super critical CO2 is also and option) into an oil. As I said we are not done yet, but have made some good steps in design and construction.



Research:
As I touched on earlier in post #294 we are in the process of conducting quantitative research. As a base we are planning to determine the cannabinoid and terpene content and ratio in the freshly frozen plant material at harvest. Further more we are quantitatively comparing two alcohol (ethanol) extraction methods of trichome concentrate (<250 micron).

* Low temperature ethanol extract at 30°C in vacuum (using rotary evaporator).
* High temperature ethanol extract at 87°C at atmospheric pressure.

Using HPLC and GC we are aiming at quantifying the cannabinoids CBD, CBDA, CBN and terpenes b-caryophyllene, limonene and myrcene. As measuring THC(a) is problematic due to legal restrictions we are measuring CBN to get an estimate of the THC content. By prolonged heating we convert THCA -> THC -> CBN. With all this testing we are hoping to get an idea of what the best extraction technique is for maintaining the original cannabinoid - terpene ratio found in the plant.

Due to some technical challenges we don't have any data yet from the HPLC or GC. Shoulnd't be to long though before we do have some data.

 

[DutchHempCBD]

Extraction pictures

 

[Santalum]

Hi DH, Have you explored the economics of doing extraction abroad? We get our sandalwood kernels supercritically extracted (CO2) in India by Proderna. We explored all the toll providers and they came up trumps on professionalism and cost. Very reliable and ever keen to take on new business. We're producing an oil that wholesales for around $150-180/kg, so if the margins are working there I'm sure they'd be working on CBD rich feedstock. Thanks for the updates. S

 

[HFT]

Here's an update.

Harvest 2014 processing
Some months ago we experimented with using a rotary sieve mounted with a 250 micron stainless steel mesh to obtain trichome rich concentrate. This was done by combining dried plant material (leaves and flowers with seeds) with dry ice nuggets. The dry ice nuggets with a temperature around -79°C (-109°F) cool the trichomes to such an extent that they become brittle and get dislodged from the plant material. However in the process some of the already brittle dried plant material also gets crushed and falls through the 250 micron mesh together with the trichomes. Using this approach we obtained a powder with a relatively high trichome content. From this trichome concentrate oil can be obtained by ethanol alcohol extract. Oil yield is around 10 to 15 wt% of trichome concentrate weight. By the smell and taste of it the oil contains terpenes and so also most likely cannabinoids. On ingesting no psychoactive effect is noticed, however at higher doses a clear relaxation of muscles can be noticed. It's quite likely that the oil contains cannabinoids, of which the most prominent are CBD and CBDA.
[URL=https://www.icmag.com/ic/picture.php?albumid=59810&pictureid=1419962&thumb=1]View Image[/url]
[URL=https://www.icmag.com/ic/picture.php?albumid=60084&pictureid=1420049&thumb=1]View Image[/url]
Even though in principal the technique worked the screen clogged often with combination of frozen moisture from the air, tiny pieces of dry ice and small plant material. On top of that the technique was quite inefficient in the use of dry ice. Dry ice is brittle and thus gets pulverized and easily lost among the processed plant material. This complicates the separation of the dry ice from the plant material after a batch is processed.

To prevent/minimize screen clogging and increase cooling efficiency we designed a rotary sieve system with a 2 mm screen and liquid nitrogen (-196°C, -321°F ). Though we haven't completed construction we have made some progress. This sieve has a 2 mm stainless steel mesh. The idea is to spray the plant material with a liquid nitrogen air mixture. This should cool the trichomes to such an extent that together with the tumbling motion of the sieve should dislodge the trichomes. The screen will stop seeds and larger plant matter (>2 mm) and let's through trichomes and small plant material. The latter is than collected and dried at ambient temperature to wick of the frozen moisture. This <2 mm trichome concentrate is further refined by sieving this through a 250 micron screen to minimize non-tricome content. The collected <250 micron trichome rich material can then be extracted using ethanol (super critical CO2 is also and option) into an oil. As I said we are not done yet, but have made some good steps in design and construction.
[URL=https://www.icmag.com/ic/picture.php?albumid=59810&pictureid=1419961&thumb=1]View Image[/url] [URL=https://www.icmag.com/ic/picture.php?albumid=59810&pictureid=1419960&thumb=1]View Image[/url]


Research:
As I touched on earlier in post #294 we are in the process of conducting quantitative research. As a base we are planning to determine the cannabinoid and terpene content and ratio in the freshly frozen plant material at harvest. Further more we are quantitatively comparing two alcohol (ethanol) extraction methods of trichome concentrate (<250 micron).

* Low temperature ethanol extract at 30°C in vacuum (using rotary evaporator).
* High temperature ethanol extract at 87°C at atmospheric pressure.

Using HPLC and GC we are aiming at quantifying the cannabinoids CBD, CBDA, CBN and terpenes b-caryophyllene, limonene and myrcene. As measuring THC(a) is problematic due to legal restrictions we are measuring CBN to get an estimate of the THC content. By prolonged heating we convert THCA -> THC -> CBN. With all this testing we are hoping to get an idea of what the best extraction technique is for maintaining the original cannabinoid - terpene ratio found in the plant.

Due to some technical challenges we don't have any data yet from the HPLC or GC. Shoulnd't be to long though before we do have some data.

Thanks Dutch CBD! Wonderful work!

 

[KiefSweat]

dry ice busts up to much plant material to then not be collecting a ton of chlorophyll through a 250 micron screen. You may want to think about a cold ethanol extraction to mitigate some of that.

 

[oldchuck]

Your extract looks very green, Dutch. Yours is a pretty color but mine comes out a rich amber.

 

[DutchHempCBD]

Thank you for all the reply's.

@Santalum: That's an option that I had not considered. I'll keep it in mind!

@KiefSweat: Yes, super cooled ethanol extract might be interesting. Especially considering that ethanol only freezes at −114 °C. Do any of you know of any quantification based literature on low temperature (<0°C) ethanol extraction?

@oldchuck: how did you perform your extraction? Do you have pictures? Are you also talking about industrial hemp extraction or about drug type cannabis?


What is the problem with ingesting chlorophyll at the rate that is in these extracts? I understand if you are smoking it that you don't want (to much) chlorophyll. As this oil is primarily intended for oral use, is there a problem? Can chlorophyll cause problems at concentrations of maximum of a milliliter of extracts per day? Doesn't one mouthful of spinach have way more chlorophyll?! Or does the chlorophyll cause other problems like limiting bio-availability, rancidity, etc?!

 

[KiefSweat]

the chlorophyll can lead to slight digestion problems. Ive found with a lot of ethanol extracts you will def notice a heavier feeling in your stomach.

I'm not sure if any of the studies i've read are on cold extracts or warm ones, Hazenkamp i think had a few papers with some good relevant info, GWpharm is the only other ones i know that use ethanol but its for winterization.

 

[oldchuck]

@Dutch, the green caught my eye because you did your extraction at super cold temperatures which surprised me.

I do a low tech kitchen chemistry small batch ethanol extraction. I've had it come out the very same pretty green when I don't chill anything and leave the plant material steep in the ethanol for a while. Tastes terrible. When I chill everything to ordinary freezer temps (a few degrees above 0 F) and only steep for about 30 seconds it comes out amber. Why, do you suppose, yours comes out green at much lower temps?

 

[mexcurandero420]

Not only digestion problems can occur, but it has a bad influence on the taste as well.Kind of bitterness.

Keep on growing

 

[DutchHempCBD]

Thanks for the input.

I've never had problems with the chlorophyll and digestion. Like I said in my last post, an average spinach salad would likely introduce more chlorophyll (though maybe a different type of chlorophyll?!) than a couple of ml alcohol extract. But the bitter/weird taste is a factor for sure!

@KiefSweat: here's an excerpt of an article co-authored by Hazekamp which amongst others describes the reduction of chlorophyll extraction by ethanol.

Unfortunately, pure ethanol efficiently extracts chlorophyll from cannabis, which will give the final extract a distinct green color, and often unpleasantant taste. Removing chlorophyll by filtering the ethanol extract over activated charcoal was found to be very effective, but it also removed a large proportion of cannabinoids and terpenes, and is therefore not advised.

Source: Cannabis Oil: chemical evaluation of an upcoming
cannabis-based medicine http://www.bedrocan.nl/userfiles/file/cannabs%20oil%20hazekamp%20Romano.pdf

@oldchuck: the reason our oil is green is because we perform 30 minutes ultrasonic agitation at just above 0°C. It makes sense that it would also give it enough time to dissolve chlorophyll. Here's a video showing cold ethanol extract of cannabis with little chlorophyll extraction. https://www.youtube.com/watch?v=JIaA6N9dELY This is along the lines of how you did it I believe, and that is to reduce the contact time of alcohol and plant matter. However what I found from personal experience is that the cannabis plant material still contains a good portion of cannabinoids! So this is an effective method of reducing chlorophyll, just not very efficient in terms of extracting all cannabinoids.

I wonder what would happen if you did 30 minutes of sonication of ethanol and plant material at close to −114 °C. This could be done I guess by cooling the bath occasionally with liquid nitrogen (-198°C) or mixing dry ice with ethanol to create dry ice ethanol sludge.

Maybe the 30 minutes sonnication is not even necessary if you would submerge the trichome concentrate (with leaf contamination) in liquid nitrogen and agitate shortly to break open the trichome heads and release cannabinoids with minimal soak time in ethanol at -114°C. Sounds like a nice experiment.

 

[KiefSweat]

a water filtration step may work too between the sieving and ethanol soak.

 

[DutchHempCBD]

a water filtration step may work too between the sieving and ethanol soak.

That could work, but I wouldn't do that as lot of compounds like cannabinoids and terpenes partially dissolve in water. Granted this loss is most likely very small as water solubility is very low, but still it's not something I would stand for in my extracts.

 

[KiefSweat]

there is some loss even with cold water but its pretty minimal from what ive seen comparing tests on water hash vs solvent extracts.

there are some other tricks you can use with water to separate and even refine your extracts so its something that I wouldn't rule out. if your further processing your extracts into a neutral form a lot of the terps will volatilize off in the process

 

[karl.uk]

Is THCA a controlled substance in the UK ?

 

[Santalum]

Here is a question for you Dutchy coming from a growing perspective. Do you think it would be possible to get two 'cuts' out of a crop? In other words if you cut the top third when you are happy with flower stage, could the remaining crop then go on to reflower and provide another cut before the season closed out on you? I'm interested how the hemp plant responds to being cut before it sets seed.

If you look at annual forage crops like oats, they will generally reshoot if moisture is available following cutting.

 

[GlandualFever]

Is THCA a controlled substance in the UK ?

YES, Its THC-Acid. Read the following as a good starting point!

http://www.legislation.gov.uk/uksi/2008/3130/pdfs/uksiem_20083130_en.pdf

Strangely enough, the legislation makes note of CBN

 

[DutchHempCBD]

there is some loss even with cold water but its pretty minimal from what ive seen comparing tests on water hash vs solvent extracts.

there are some other tricks you can use with water to separate and even refine your extracts so its something that I wouldn't rule out. if your further processing your extracts into a neutral form a lot of the terps will volatilize off in the process

Hi, I appreciate your input. Do you have some info on 'some other tricks'? You're right that I shouldn't rule water refinement out. As for decarboxilating into neutral form you're right that a lot of terpenes are lost in this process. Hazekamp had some research results (see report mentioned in post #373) showing that already after 5 minutes at 100°C a good chunck (like 3/4th) of the terpenes where lost. Especially the more voaltile/fragile monoterpes where no longer present in the plant material. As acid cannabinoids have a different effect in the body than neutral cannabinoids my intention is to produce both acid and neutral forms of cannabinoids.

@Santalum: mhhhh interesting point. I'm don't have a lot of experience or knowledge about growing hemp/cannabis. For Finola I think it might interesting to harvest already as early as day 60 yielding quite some trichomes already. Assuming sowing around half of May already This means that that harvest will take place around half of July. Still providing something like one extra month for growth of new shoots to take place. I don't know if plants can do that. Something to try out his year, at least on a small yet significant scale. Though I don't know how quickly flowers would form again. I have my doubts. Anyone, OO?!