Updated: Jul 13, 2020
Emergencies, Spill Procedures, and Exposures/Unintended Contact
Details of Process
Preparation and Use:
Hot CBD distillate will be loaded onto a prepared column and eluted with a blend of 70% Ethanol and 30% Water. The distillate will be run through a column of packed media. A less diluted volume of ethanol will be passed over the column after CBD has eluted to release THC into a separate fraction.
Concentration- Use HPLC grade Ethanol and HPLC grade Water
Quantity- One column volume for prep, two to four column volumes for elution, two column volumes to flush.
Frequency- Ethanol: Initial saturation, media slurry, column feeding and flushing
Location- All procedures are to occur in the fume hood.
Note: If identified as a process, provide additional detailed procedural steps for the use of each hazardous chemical in Section 5, below.
Potential Hazards and Risk:
See Ethanol MSDS for detailed risks. The boiling point of ethanol lends to its evaporation at room temperature. Pouring Ethanol can lead to spills.
Potential Acute Health Effects:
Causes severe eye irritation. Causes respiratory tract irritation. This substance has caused adverse reproductive and fetal effects in humans. May cause central nervous system depression. May cause liver, kidney and heart damage. Causes moderate skin irritation.
Animal studies have reported the development of tumors. Prolonged exposure may cause liver, kidney, and heart damage. Laboratory experiments have resulted in mutagenic effects
Selection and Purchasing:
Use only HPLC grade ethanol
Provide exhaust ventilation or other engineering controls to keep airborne concentrations of vapors below their respective threshold limit value. Ensure that eyewash stations and safety showers are proximal to the work-station location.
Administrative and Work Practice Controls:
Special handling requirements:
Keep away from heat. Keep away from sources of ignition. Ground all equipment containing material
Special equipment requirements:
Mop and Bucket easily accessible.
Chemical-specific antidotes or first aid treatments:
Eye Contact: Check for and remove any contact lenses. In case of contact, immediately flush eyes with plenty of water for at least 15 minutes. Cold water may be used. WARM water MUST be used. Get medical attention.
Skin Contact: In case of contact, immediately flush skin with plenty of water. Cover the irritated skin with an emollient. Remove contaminated clothing and shoes. Wash clothing before reuse. Thoroughly clean shoes before reuse. Get medical attention.
Serious Skin Contact: Wash with a disinfectant soap and cover the contaminated skin with an anti-bacterial cream. Seek medical attention.
Inhalation: If inhaled, move individual to fresh air. If not breathing, provide artificial respiration. If breathing is difficult, provide oxygen. Provided medical attention if symptoms appear or reappear.
Serious Inhalation: Evacuate the victim to a safe area as soon as possible. Loosen tight clothing such as a collar, tie, belt or waistband. If breathing is difficult, administer oxygen. If the victim is not breathing, perform mouth-to-mouth resuscitation. Seek medical attention.
Ingestion: If swallowed, do NOT induce vomiting. Never give anything by mouth to an unconscious person. Aspiration hazard if swallowed- can enter lungs and cause damage. Loosen tight clothing such as a collar, tie, belt or waistband. Get medical attention.
Serious Ingestion: Not available. Section Chemical segregation strategies (also address in sub-section 2e: Storage and Transportation).
Describing additional safe work practices:
Always keep Ethanol containers closed and cool
How will the work surface and other items be decontaminated after use?
Use clean ethanol and a shop towel to clean any surfaces contaminated with solvent/distillate solution.
Personal Protective Equipment (PPE):
Splash goggles. Lab coat. Vapor respirator. Be sure to use an approved/certified respirator or equivalent. Gloves.
Personal Protection in Case of a Large Spill:
Splash goggles. Full suit. Vapor respirator. Boots. Gloves. Suggested protective clothing might not be sufficient; consult a specialist BEFORE handling this product.
Storage and Transportation:
Precautions: Keep away from heat. Keep away from sources of ignition. Ground all equipment containing material. Do not ingest. Do not breathe gas/fumes/ vapor/spray. Wear suitable protective clothing. In case of insufficient ventilation, do not proceed. If ingested, seek medical advice immediately and show the container or the label. Avoid contact with skin and eyes. Keep away from incompatibles such as oxidizing agents.
Storage: Store in a segregated and approved area. Keep container in a cool, well-ventilated area. Keep container tightly closed and sealed until ready for use. Avoid all possible sources of ignition (spark or flame). Do not store above 25°C (77°F).
EMERGENCIES, SPILL PROCEDURES, AND EXPOSURES/UNINTENDED CONTACT
Absorb with an inert material and put the spilled material in an appropriate waste disposal.
Flammable liquid. Keep away from heat. Keep away from sources of ignition. Stop leak if without risk. Absorb with DRY earth, sand or other non-combustible material. Do not touch spilled material. Prevent entry into sewers, basements or confined areas; dike if needed. Be careful that the product is not present at a concentration level above TLV. Check TLV on the MSDS and with local authorities.
NIOSH: The recommended airborne exposure limit (REL) is 1,000 ppm averaged over a 10-hour workshift. ACGIH: The threshold limit value (TLV) is 1,000 ppm as a STEL (short-term exposure limit).
Ecotoxicity: Not available.
BOD5 and COD: Not available.
Products of Biodegradation:
Possibly hazardous short term degradation products are not likely. However, long term degradation products may arise.
Toxicity of the Products of Biodegradation:
The product itself and its products of degradation are not toxic.
DETAILS OF PROCESS
1. Begin by deciding the amount of media necessary to remediate. Your resin load should be eight to ten percent of the mass of the media used. For this example we will assume you want to remediate eight grams of oil, and we will use 100 grams of media, this gives a column volume of 125ml.
2. Prepare work area. Clean all surfaces, clean entire chromatography column, clean all fraction collection flasks.
3. Create a 70:30 solution of Ethanol and Water for a total volume of 500 ml. Create a second solution of 50:50 Ethanol:Water for a total of 250 ml.
4. Add 100 grams media to the 250ml 50:50 ethanol:water solution and stir well, creating a slurry. Allow media to expand for 12 hours in slurry before packing column.
5. Place column into stand, close stopcock, and place a flask below the column
Note: A 14-20mm inside diameter x 800mm column is recommended for a 100 gram run.
6. Rapidly mix slurry to reduce settling, then pour into column until full.
7. Open stopcock and and use vibrating motor to vibrate column.
8. Collect solution until media is fully settled in column then repeat Step 6 to Step 7 until all media is fully loaded into the column.
9. When all media is fully loaded into the column, close stopcock when solution level is about one centimeter above the media level, your column is now ready for use.
10. Mix eight grams distillate with just enough hot ethanol to make it a liquid
Note: no more than 2:1 oil:ethanol.
11. Load distillate solution into column.
12. Open stopcock and collect into new flask until solution level is just above media level.
13. Load one column volume of ethanol blend on top of the oil load.
14. Feed 70:30 ethanol blend through column 125 ml at a time. (It will most likely require approximately an for 125ml to pass through) You should use a slight vacuum, below 200mmhg, do not feed more than one column volume per hour.
15. Fraction into 20 ml fractions.
16. Test all fractions, early fractions will contain only CBD, later fractions will contain a mixture of CBD and THC, these will be recycled and run again later. The end fractions will contain mostly THC and can be recycled or disposed of.
17. To reuse the column flush with two column volumes of pure ethanol, then equilibrate the column with one volume of 50:50 ethanol:water
All personnel are required to complete the online General Lab Safety session thru the OESO website. This session includes an introduction to general chemical safety. Furthermore, all personnel shall read and fully adhere to this SOP when handling the chemical.