DpTek1

Important Update (June 23)  - A  batch of coarsely shredded root proved  extremely difficult to work with in recent tests.  A writeup of the tests will be made available in due course, but in the meantime we strongly suggest using finely powdered only.  If this genuinely impossible to obtain then choose the root which is the most finely shredded available. See also powdered vs shredded

Equipment & Ingredients

Note: this tek can be used with 1L containers & 50g of root, simply by dividing the quantites of lye/salt/water etc by two.  Suggest using a little more than half the quantity of solvents for pulls, since it's easier to pippette out. 

• Powdered root base 75-100g, this tek is designed especially for powdered (See Powdered vs shredded root)  How much root is optimum to use? 

• Vinegar, approx 250ml Regular 5% white (i.e. clear). Citric acid crystals can also be used by dissolving approx 30g in 300ml of water. Exact PH is not expected to be critical

• Water, tap or purified water as preferred.  Purified Vs Tap Water For DpTek

• 180g Salt table salt or 100% NaCl as preferred Why use salt? Is iodised salt OK to use?

• Lye pearls or crystals: 110g (aka sodium hydroxide, caustic soda). How much lye is best to use in this tek? Lye demands serious safety precautions, please familiarise yourself

•   Solvent:  approx 400ml, e.g. naphtha (e.g.Clipper, Ronsonal, Azure Naphtha) or Petroleum Ether 40/60 is recommended. Heptane is also an option but be aware that solvent sold as "Heptane" can have wildly varying properties so it's vital to be aware of which you have.  See  Naphtha vs Pet Ether vs Heptane for more details.

• 2L (or larger) container – e.g. media bottle (called reagent bottle in UK). Preferably heat resistant to allow lye to be added faster without risking heat damage to the glass) Note: Erlenmayer flasks are not recommended ( why not? )

• A safe means of thoroughly shaking/mixing the 2L container when containing corrosive lye solution, e.g. a secure stopper/lid, ptfe stirring rod (or similar). Magnetic stirrers are not recommended.

• Pipette, e.g. 10ml glass pippette with rubber bulb. Kitchen turkey basters are not recommended owing to their proneness to dribble during transfer

• Thermometer (optional but highly desirable), e.g. generic infra red thermometer is ideal

• Small fan, e.g. usb powered (optional but desirable)

• Shallow glass dish(es), pie dishes are ideal

• A few sundry containers, old jars of various sizes, shot glasses etc.

• Safety equipment, safety goggles, rubber gloves, nearby supply of running fresh water, a tidy, well lit & ventilated work area

• A good attitude, sufficient time allocated, no disturbances, no rushing, no corner-cutting, prior research, planned breaks
  
  

Procedure

The acidification stage

Why a complete acidification stage is essential to DpTek1

1. Place 75g-100g powdered root into a container (e.g. a glass jar) and cover with vinegar or citric acid solution (takes approx 200-300ml depending on the root). Stir until a mud-like paste is achieved.

2. Freeze/thaw the jar 3 times (is the freeze/thaw worthwhile?). It's done for "cell disruption" purposes as described in this article .  Stir well at each thaw adding a little more vinegar to maintain the wet mud texture, then leave the jar at room temperature (not less than about 20°C) for a few hours before re-freezing.

Preparing the water/salt/lye solution

3. Dissolve 110g of lye into approx 1.0L water (add lye slowly to the water, stirring or swirling gently throughout). Owing to the large amount of water, heat build up is unlikely to be a problem but still worthy of care, especially with any clumps of lye adhering to the bottom of the containerand causing localised heat spots.

4. Dissolve 180-200g salt in approx the lye water. Residual heat from lye reaction will speed this. Allow the water/salt/lye to cool before proceeding

Adding the bark to the salt/lye solution to make the “soup”

When the acidified root has thawed from its final freeze, we’re ready to mix with our pre-prepared water/lye/salt solution to make the “soup”

5. Add the acidified bark to the lye/salt salt water.  Swirl/stir to form an even mixture (roughly 1-3 minutes)  with a long kitchen knife ptfe stirring rod (don't attach to drill) or similar.

6. Add more water to bring the fluid level in the flask to a point where it will have sufficient spare capacity to add 130ml of solvent and still a margin to be able to agitate properly when shaken (add hot/cold to bring the final temp to 20°C). Suggest a total level of approx 1.75L in a 2L flask. Some of this added water can be used to rinse remaining traces of acidified bark from its jar before pouring into the soup.

7. Bring the mix to the required temperature depending upon your chosen solvent 

• naphtha/pet ether this is 20°C.

• Heptane around mid 40s°C or even higher (currently under investigation). 

Heptane apparently needs a much higher temperature for optimal yield and can tolerate this without goo forming in the extracted product. Very Important: pulling at this temperature with naphtha is not recommended as much goo will also be absorbed into the solvent.  

To achieve this temperature, heat baths are OK for larger temp changes. For fine tuning temperature, consider adding hot/cold water as desired in step 6. above.  Adding the ingredients in step 5 appears to raise the temperature, so if using naphtha it may be necessary to cool it. If stronger acid solutions have been used (e.g. by using concentrated citric acid) then the temp rise can be considerable. This important step has a remarkable effect on the levels of impurities/whiteness of the Purity Flakes

 “Quick, pulls” for a clean product 

 What do we mean by quick pulls

8. Once at the correct temperature for your solvent (see 7. above), add around 130-150ml of solvent to the soup. Now we need to mix /shake (gentle swirling is insufficent) in the solvent into the soup for approx 40-50 seconds. Be aware that over-vigorous mixing can sometimes cause problems Just how hard do I shake/mix my soup/solvent mix?

 One of the following methods can be used depending upon available equipment/preference

• Seal the 2L container and taking extreme care, shake or otherwise manually agitate (e.g.with stirring rod). If sealed during shaking expect a slight pressure difference (normally a very slight in-rush of air) when removing the stopper/lid.

• Use your chosen mixing tool thoroughly mix (take care not to over-mix as described above)

9. Wait for the layers to fully separate (solvent on top), ~3-5 minutes and then carefully pipette solvent into a pie dish. If some soup is inadvertently sucked into the pipette, it can be removed by first squirting the contaminated solvent first into a shot glass where the lye will stick to the insides, and then the clean solvent poured into the dish.
   
   Note: if the layers didn’t readily separate in step 9, add approx 100ml of water and stir gently with a long kitchen knife or similar, especially at the surface and wait a little longer, Repeat as necessary. If an emulsion (layer of oily bubbles between solvent and soup) is visible when viewed in torch light, adding water also helps with this, but first try gently agitating the surface until eliminated. The commonly-reported tip of adding more salt to has invariably proved to greatly exacerbate the problem for this tek (probably owing to increased viscosity).

10. Perform the remainder of your pulls (how many pulls are optimum?) immediately one after another (a pull is defined as adding solvent, shaking/mixing, separation, pipetting out).  Slightly less solvent may be used after the first (e.g. 80-100ml). The solvent from pulls can be combined in a single dish or kept separate if preferred (All pulls are remarkably clean but the first is often pristine)

Preparing the solvent for freezing 

Can I leave simply the fan blowing over the mix until it all evaporates leaving only spice, thus eliminating the freezer? 

11.  In a well ventilated workspace, evaporate the solvent in your dish down with a usb fan or similar blowing gently on the dish until the crystals just are beginning to form on the bottom. Can I place the solvent directly in the freezer without evaporating? 

12. Optionally, when crystals begin to form in the solvent, it can be gently heated (e.g. by covering and placing the dish in a heat bath) to re-dissolve the crystals so that during freezing, they can re-precipitate at the edge of the dish (by placing it at a slight angle).  This can result in easier scraping of the Purity Flakes.

Freezing & harvesting the Purity Flakes

13.  Fit the lid to the dish (or cover with cling film) and place it in the freezer.  If the dish is kept at slight angle, the solvent collects on one side and and a thicker layer of crystals will result, facilitating scraping and reducing losses

14.  Leave the dish in the freezer for at least 4 hours and preferably overnight. 

15.  Remove and pour off the excess solvent to leave the precipitated crystals. If there are any floating crystals, angle the dish so the solvent collects at one side and carefully pipette away the clear solvent, leaving the crystals behind

16.  Gently fan these wet crystals for a few hours to thoroughly dry, ready for scraping.

17.  If you were careful to perform pulls at 20-21°C then there should be almost no trace of goo. But when scraping, do this very lightly at first and try to cream off the top later. Afterwards you may scrape up right to the glass and evaluate for purity.

Useage of the Purity Flakes From DpTek1

When dried, the finished Purity Flakes may be added directly to the purificator for testing on standard 30°C laundry washing cycle.  250mg of flakes per 9kg wash should be sufficient to produce desired results, but will be dependent upon garment soiling, fabric types and levels of dissolved calcium salts in the washine machine's source water.