Excellent, that was my next question. Wonder if @Shadownaught has that blend yetđ¤
Do you know a brand or type you can share with us?
Hey, so I kind of have two questions. When filtering through an acidic clay, you would be dealing with surface/solid state chemistry not solution right? So the acid can only work for as long as you are filtering the material through (unless you filter improperly and some solid makes it into whatever container)? In other words, you arenât creating the ions in the solution because like chromatography you are just dealing with the acidic end groups. Hope that makes sense.
@Shadownaught xtractordepot carries your products i believe! Im pretty close to them. Ill try the bleaching clay soon! Is the neutral ph clay as affective as the acidic one?
@Photon_noir so because it has some acidic site it will still cause isomeriation?
Several people, and loads on ig, have mentioned they prefer proper prep instead of clay/ac in the boiling flask. I never get the same results in terms of color with pre processing. Maybe im doing something wrong? I usually just winterize, degum and then distill but when i was testing no clay in the boiling flask i followed this method.
Winterize - Degum - Carbon and Clay scrub at around 60C - 1st pass - Ethanol to Hexane partition - Saline scrub - 2nd pass. With all that, the color is way more gold than water clear and has way more of an azulene taste. I can never pull a dark blue azulene out with no absorbents in the flask. I get some for sure but not nearly as much as with clay in the flask. Suggestions?
FYI to all, when explaining, i may ask several questions as im not a chemist. Just an average guy trying to wrap my brain around this. This all way so much easier back in 2015 lol
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I do exactly this, except I move the adsorbent scrubs to post degum. Those phosphatides like to âgum upâ the adsorbents (thatâs actually where the term degumming comes from) which makes them less effective. Also, most of them work better in an alkane solution vs an ethanol solution, which tends to leach pigment from the adsorbents
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And that gives you close to water clear Delta 9? Iâll try again with your recommendations. Just trying to get a light color high d9 without chroma. Chroma seems like the best option now a days.
@Future silaceous minerals like hydrated silica are used for degumming processes, just fyi.
@xizqu Only âactivatedâ materials (which includes acid activated carbon and clays) have the potential to isomerize from the scrub, since they can and do sometimes leach excess acid into the solution.
Naturally, they can certainly catalyze isomerization of CBD and Î9 both to Î8-THC in the distillation boiling flask.
However, the Lewis acidity of neutral clay will only have the potential to isomerize CBD to Î9-THC under anhydrous conditions in the distillation boiling flask. This is a more valuable process, so if you try it, keep it on the down low, but please share your results with me!
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You know me! Iâll try it out and shoot over the lab tests! Whatâs your favorite lab in la?
Second, would you still recommend decarbing prior to adding the clay in the boiling flask? We always do it but want to make sure.
I donât have a favorite in LA, but my favorite in CA is Anresco.
Yes, I would always recommend vacuum decarbing in an oven prior to putting crude into the boiling flask. Also, warm decarboxylated crude is much easier to hand-mix dry ingredients into with a thin rubber spatula to make sure it is all wetted before pouring it into the boiling flask. That prevents any dust clouds suddenly emerging from your mixture while under vacuum.
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Okay, I tried lol
What, you donât remember me sending you a photo of carbon coating the entire system? First time trying the Tek. Yeah mixing isnât a problem anymore. Will have results sometime this week! Want to try nuetral ac too so Iâll have to look for that.
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I vaguely remember that under a different name on ig? But, yes, thatâs why you must pre-mix any dry additives.
âActivatedâ carbon is always acidic with carboxylic acid groups all over each particle. Thatâs what makes it work. You will have better luck with neutral clay.
Different name. I was your first client.
Some mentioned neutral ac in this thread so I got the idea. You know better than I! Will report back the results when I have them! Same number or should I shoot it via email?
Thanks everyone for all the help! Itâs greatly appreciated! 
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Hey! I thought that was you! Hope youâve been well! Good luck with the project! By the way, neutral charcoal is just charcoal⌠which I have tested and it doesnât do anything useful.
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The laymanâs lowdown on activated charcoal/carbon can be quickly perused by clicking on the links listed to the right of the page the following link takes you toâŚ
A little data dump:
RECRYSTALLISATION Techniques
The most commonly used procedure for the purification of a solid material by recrystallisation from a solution involves the following steps:
(a) The impure material is dissolved in a suitable solvent, by shaking or vigorous stirring, at or near the boiling point, to form a near-saturated solution.
(b) The hot solution is filtered to remove any insoluble particles. To prevent crystallisation during this filtration, a heated filter funnel can be used or the solution can be diluted with more of the solvent.
(c) The solution is then allowed to cool so that the dissolved substance crystallises out. (d) The crystals are separated from the mother liquor, either by centrifuging or by filtering, under suction, throughasinteredglass,aHirscho raBiichner,funnel. Usually,centrifugationisprefer redbecauseof the greater ease and efficiency of separating crystals and mother liquor, and also because of the saving of time and effort, particularly when very small crystals are formed or when there is entrainment of
solvent. (e) The crystals are washed free from mother liquor with a little fresh cold solvent, then dried.
If the solution contains extraneous coloured material likely to contaminate the crystals, this can often be removed by adding some activated charcoal (decolorising carbon) to the hot,but not boiling, solution which is then shaken frequently for several minutes before being filtered. (The large active surface of the carbon makes it a good adsorbent for this purpose.) In general, the cooling and crystallisation steps should be rapid so as to give small crystals which occlude less of the mother liquor. This is usually satisfactory with inorganic material, so that commonly the filtrate is cooled in an ice-water bath while being vigorously stirred. In many cases, however, organic molecules crystallise much more slowly, so that the filtrate must be set aside to cool to room temperature or left in the refrigerator. It is often desirable to subject material that is very impure to preliminary purification, such as steam distillation, Soxhlet extraction, or sublimation, before recrystallising it. A greater degree of purity is also to be expected if the crystallisation process is repeated several times, especially if different solvents are used. The advantage of several crystallisations from different solvents lies in the fact that the material sought, and its impurities, are unlikely to have similar solubilities as solvents and temperatures are varied.
For the final separation of solid material, sintered-glass discs are preferable to filter paper. Sintered glass is unaffected by strongly acid solutions or by oxidising agents. Also, with filter paper, cellulose fibres are likely to become included in the sample. The sintered-glass discs or funnels can be readily cleaned by washing in freshly prepared chromic acid cleaning mixture. This mixture is made by adding 10OmL of concentrated sulfuric acid slowly with stirring to a solution of 5g of sodium dichromate (CARE: cancer suspect) in 5mL of water. (The mixture warms to about 70°, see p 3).
For materials with very low melting points it is sometimes convenient to use dilute solutions in acetone, methanol, pentane, diethyl ether or CHC13-CC14. The solutions are cooled to -78° in a dry-ice/acetone bath, to give a slurry which is filtered off through a precooled Biichner funnel. Experimental details, as applied to the purification of nitromethane, are given by Parrett and Sun [/ Chem Educ 54 448 1977].
Where substances vary little in solubility with temperature, isothermal crystallisation may sometimes be employed. This usually takes the form of a partial evaporation of a saturated solution at room temperature by leaving it under reduced pressure in a desiccator. However, in rare cases, crystallisation is not a satisfactory method of purification, especially if the impurity forms crystals that are isomorphous with the material being purified. In fact, the impurity content may even be greater in such recrystallised material. For this reason, it still remains necessary to test for impurities and to remove or adequately lower their concentrations by suitable chemical manipulation prior to recrystallisation.
Filtration. Filtration removes paniculate impurities rapidly from liquids and is also used to collect insoluble or crystalline solids which separate or crystallise from solution. The usual technique is to pass the solution, cold or hot, through a fluted filter paper in a conical glass funnel. If a solution is hot and needs to be filtered rapidly a Biichner funnel and flask are used and filtration is performed under a slight vacuum (water pump), the filter medium being a circular cellulose filter paper wet with solvent. If filtration is slow, even under high vacuum, a pile of about twenty filter papers, wet as before, are placed in the Biichner funnel and, as the flow of solution slows down, the upper layers of the filter paper are progressively removed. Alternatively, a filter aid, e.g. Celite, Florisil or Hyflo-supercel, is placed on top of a filter paper in the funnel. When the flow of the solution (under suction) slows down, the upper surface of the filter aid is scratched gently. Filter papers with various pore sizes are available covering a range of filtration rates. Hardened filter papers are slow filtering but they can withstand acidic and alkaline solutions without appreciable hydrolysis of the cellulose (see Table 5). When using strong acids it is preferable to use glass micro fibre filters which are commercially available (see Table 5 and 6).
Freeing a solution from extremely small particles [e.g. for optical rotatory dispersion (ORD) or circular dichroism (CD) measurements] requires filters with very small pore size. Commercially available (Millipore, Gelman, Nucleopore) filters other than cellulose or glass include nylon, Teflon, and polyvinyl chloride, and the pore diameter may be as small as O.Olmicron (see Table 6). Special containers are used to hold the filters, through which the solution is pressed by applying pressure, e.g. from a syringe. Some of these filters can be used to clear strong sulfuric acid solutions.
As an alternative to the Biichner funnel for collecting crystalline solids, a funnel with a sintered glass-plate under suction may be used. Sintered-glass funnels with various porosities are commercially available and can be easily cleaned with warm chromic or nitric acid (see above).
When the solid particles are too fine to be collected on a filter funnel because filtration is extremely slow, separation by centrifugation should be used. Bench type centrifuges are most convenient for this purpose. The solid is placed in the centrifuge tube, the tubes containing the solutions on opposite sides of the rotor should be balanced accurately (at least within 0.05 to O.Ig), and the solutions are spun at maximum speed for as long as it takes to settle the solid (usually ca 3-5 minutes). The solid is washed with cold solvent by centrifugation, and finally twice with a pure volatile solvent in which the solid is insoluble, also by centrifugation. After decanting the supernatant,the residue is dried in a vacuum, at elevated temperatures if necessary. In order to avoid âspittingâ and contamination with dust while the solid in the centrifuge tube is dried, the mouth of the tube is covered with aluminium foil and held fast with a tight rubber band near the lip. The flat surface of the aluminium foil is then perforated in several places with a pin and the tube and contents are dried in a vacuum desiccator over a desiccant.
Choice of solvents. The best solvents for recrystallisation have the following properties: (a) The material is much more soluble at higher temperatures than it is at room temperature or below. (b) Well-formed (but not large) crystals are produced. (c) Impurities are either very soluble or only sparingly soluble. (d) The solvent must be readily removed from the purified material. (e) There must be no reaction between the solvent and the substance being purified. (f) The solvent must not be inconveniently volatile or too highly flammable. (These are reasons why diethyl ether and carbon disulfide are not commonly used in this way.)
The following generalisations provide a rough guide to the selection of a suitable solvent: (a) Substances usually dissolve best in solvents to which they are most closely related in chemical and physical characteristics. Thus, hydroxylic compounds are likely to be most soluble in water, methanol, ethanol, acetic acid or acetone. Similarly, petroleum ether might be used with water-insoluble substances. However, if the resemblance is too close, solubilities may become excessive. (b) Higher members of homologous series approximate more and more closely to their parent hydrocarbon. (c) Polar substances are more soluble in polar, than in non-polar, solvents.
Although Chapters 4, 5 and 6 provide details of the solvents used for recrystallising a large portion of commercially available laboratory chemicals, they cannot hope to be exhaustive, nor need they necessarily be the best choice. In other cases where it is desirable to use this process, it is necessary to establish whether a given solvent is suitable. This is usually done by taking only a small amount of material in a small test-tube and adding enough solvent to cover it. If it dissolves readily in the cold or on gentle warming, the solvent is unsuitable. Conversely, if it remains insoluble when the solvent is heated to boiling (adding more solvent if necessary), the solvent is again unsuitable. If the material dissolves in the hot solvent but does not crystallise readily within several minutes of cooling in an ice-salt mixture, another solvent should be tried.
Petroleum ethers are commercially available fractions of refined petroleum and are sold in fractions with about 20° boiling ranges. This ensures that little of the hydrocarbon ingredients boiling below the range is lost during standing or boiling when recrystallising a substance. Petroleum ethers with boiling ranges (at 760mm pressure) of 35â60°, 40â60°, 60â80°, 80â100°, and 100â120° are generally free from unsaturated and aromatic hydrocarbons. The lowest boiling petroleum ether commercially available has b 30-40°/760mm and is mostly n-pentane. The purer spectroscopic grades are almost completely free from olefinic and aromatic hydrocarbons. Petroleum spirit (which is sometimes used synonymously with petroleum ether or light petroleum) is usually less refined petroleum, and ligroin is used for fractions boiling above 100°. The lower boiling fractions consist of mixtures of n-pentane (b 36°), n-hexane (b 68.5°) and n-heptane (b 98°), and some of their isomers in varying proportions. For purification of petroleum ether b 35-60° see p. 324.
Solvents commonly used for recrystallisation, and their boiling points, are given in Table 7. For comments on the toxicity and use of benzene see the first pages of Chapters 4, 5 and 6.
From pages 14-16 of PURIFICATION OF LABORATORY CHEMICALS Fifth Edition
Wilfred L. E Armarego/Christina Li Lin Chai
Download link page,
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Damn thats a mouthfull! thanks for the nice write up!
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@Photon_noir Iâve been well! Thanks! Iâm looking forward to figuring out a workflow that yields little Delta 8!
ive also read if you make the boiling flask basic in PH you will receive a purple distillate. @Future and columbolabs were testing this IRC. Anyone know anything about this? What additive would you use thats safe for distillation?
Most boiling flask additives that have color reducing activity are also reactive in various ways; usually acidic. You can add MgO to make purple distillate, only if it also has a small air leak in situ.
Just for everyoneâs safety, please note that the first instruction in that recrystallizing tek can be very dangerous in any sealed container! A solvent near itâs boiling point will rapidly expand into gas phase as it gets shaken. Try it with just plain hot tap water in a milk jug. Youâll see!
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Btw, have you tried the hot condenser tech? Thatâs is supposed to yield very light colored product. Using carbon scrubbing, pale yellow results have been posted on ig just recently. No winterizing, degumming, clay or other product used by the poster. I believe it was helana buds that posted it.
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With regard to purple colored products and high pH, you may be observing the âalkaline Beam testâ in action. Purple products are formed when CBD comes in contact with alkali. Saw this repeatedly when cleaning glassware with 2N KOH in ethanol, a less gruesome alternative to the chromic acid cleaning solutions mentioned above. As always with intensely colored products, a little goes a long way!
The Beam test was one of the presumptive field tests for cannabis in the âoldâ daysâŚ
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