Decarb Experiment: Lid vs No Lid

In this experiment, we explored how decarboxylation conditions affect the chemical composition of hash rosin by manipulating temperature and duration as follows:

  1. Control Group (No Decarb)
  2. Low & Slow(sealed): Sealed vial at 160°F for 142 hours.
  3. Hot & Fast(sealed): Sealed vial at  240°F for 10 hours with a lid.
  4. Hot & Fast (open vial): Open vial  at 240°F for 10 hours without a lid.

The results can be seen below:

Compound %wtControl160f lid240f lid240f no lid
CannabinoidsTHCA79.58963.94678.187214.8435
THC1.161971.172166.189156.9531
THC/THCa sum86.266975.118874.376371.7966
TerpenesTrans-caryophyllene1.8862.01282.0541.9374
Farnesene1.25661.36291.37831.2531
(R (+)-Limonene0.68830.77190.76490.367
Alpha-Humulene0.49840.53870.54470.5194
Linalool0.42520.45410.46610.4029
Beta-Myrcene0.31380.32790.32860.1203
Alpha-Bisabolol0.13120.1580.15510.1572
Caryophyllene Oxide0.12140.0250.03650.352
Beta-Pinene0.08690.0250.04450.025
Alpha-Terpineol0.07480.0910.08850.0772
Alpha Pinene0.0660.14230.12360.0451
(R-Endo-(+)-fenchyl alcohol0.06040.07770.07410.0652
trans-Nerolidol0.05710.06420.06370.0626
Total Terpenes5.66616.05156.12265.3844

Weight loss Analysis:

The following table shows the loss of mass observed due to the decarb reaction.

Test GroupInput Weight (g)Output Weight (g)Loss (g)Theoretical CO2 loss (g)
160f lid4.0133.6430.370.37
240f lid2.0911.9310.160.18
240f no lid2.0881.9070.180.16

The observed losses are nearly identical to the theoretical loss expected due to CO2 off gassing for the 160f lid group. Whereas, the 240f lid group falls a bit short, however this is expected because the decarb reaction was not fully complete. The 240f no lid group overshot expectations, suggesting that loss was attributed to more than just CO2 off gassing.

Cannabinoid Analysis:

The following table presents the cannabinoid composition, expressed in percentage weights, for the control and various test conditions:

CompoundControl (%wt)160°F with lid (%wt)240°F with lid (%wt)240°F without lid (%wt)
THCa79.593.958.1914.84
THC1.1671.1766.1956.95
Sum of THC & THCa86.2775.1274.3871.80

The results reveal variance in reaction completeness among the different setups. Specifically, the 160°F condition with a lid achieved the highest degree of conversion(THCa consumed by the reaction) at 95%, followed by the 240°F condition with a lid at 90%, and the 240°F condition without a lid at 85%. Additionally, there are notable differences in the sum of THC and THCA across the test conditions, with the unlidded 240f sample showing a slightly lower value that the lidded groups which were similar. 

These findings suggest that a sealed environment may play a crucial role in driving the decarb reaction. The presence of a lid creates internal pressure due to the off gassing of CO2, the resulting pressure seems to aid in both the  conversion of THCA to THC as well as retention of these compounds, highlighting the importance of maintaining a pressurized environment to optimize the decarboxylation processes.

Terpene Results:

The following table highlights the changes in terpene composition, expressed as percentage differences from the control, across different decarboxylation setups:

Compound160f lid, percent difference240f lid, percent difference240f no lid, percent difference
Trans-caryophyllene-3%1%-5%
Farnesene-2%1%-8%
(R) (+)-Limonene2%3%-51%
Alpha-Humulene-2%1%-4%
Linalool-3%1%-12%
Beta-Myrcene-5%-3%-65%
Alpha-Bisabolol9%9%11%
Caryophyllene Oxide-81%-72%168%
Beta-Pinene-74%-53%-73%
Alpha-Terpineol10%9%-5%
Alpha Pinene96%73%-37%
(R-Endo-(+)-fenchyl alcohol17%13%0%
trans-Nerolidol2%3%1%
Total Terpenes-3%0%-12%

These results underscore the beneficial impact of a sealed environment on terpene preservation. Both lidded setup showed minimal terpene loss and in some cases, slight gains, which contrasts sharply with the substantial losses observed in the unsealed 240°F setup. The exception to this being that Caryophyllene Oxide surged by 168% in the unsealed setup, an anomaly potentially indicative of chemical transformations influenced by exposure to open air at high temperatures.

The 160°F with lid setup, despite its lower temperature, did not always result in superior terpene retention compared to the 240°F with lid setup, challenging the assumption that lower temperatures universally preserve terpenes better.

These findings suggest that while decarboxylation temperature is critical, the duration and the maintenance of a closed environment are equally vital, probably due to the effect of internal pressure on terpene boiling points. The outcomes indicate potential for further optimization of decarboxylation parameters to enhance both cannabinoid conversion and terpene retention.

Control Group (No Decarb)

high_north_coa_00471341

240F No Lid

high_north_coa_00471339

240F with Lid

high_north_coa_00471340

160F with Lid results

high_north_coa_00471342

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