SHORT PATH DISTILLATION STANDARD OPERATION PROCEDURE (SOP)


SUMMARY:

  1. Hazard Identification

  2. Hazard Control

  3. Emergencies, Spill Procedures, and Exposures/Unintended Contact

  4. Waste

  5. Details of Process




HAZARD IDENTIFICATION


PREPARATION & USE:Crude oil, Ethanol, Butane, Propane, other residual solvents


Concentration - Residual amounts in crude solution


Quantity - Batch dependent, use only fully degassed/evaporated crude


Location - All procedures are to occur in the fume hood. All crude oil should be kept in appropriately sealed and stored media containers.



Note: If identified as a process, provide additional detailed procedural steps for the use of each hazardous chemical in Section 5, below.


POTENTIAL HAZARD & RISK:


See Butane MSDS (CAS#106-97-8) Ethanol MSDS (CAS#64-17-5) for detailed risks. These solvents create flammable vapor at room temperature. Transferring crude oil can lead to exposure to solvent vapors.


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.


Carcinogenic Effects: Animal studies have reported the development of tumors. Prolonged exposure may cause liver, kidney, and heart damage. Laboratory experiments have resulted in mutagenic effects.

HAZARD CONTROL

SELECTION & PURCHASING:Only use fully de-gassed and winterized crude oil to distill. Make sure to safely degas and recover your solvent fully before attempting short path distillation.


ENGINEERING CONTROLS:Provide exhaust ventilation or other engineering controls to keep the airborne concentrations of vapors below their respective threshold limit value. Ensure that eyewash stations and safety showers are proximal to the work-station location. Wear fire-resistant lab coat, wear vapor respirator, wear eye protection, use high heat gloves


ADMINISTRATIVE & WORK PRACTICE CONTROLS


Special handling requirements:Keep away from heat. Keep away from sources of ignition. Ground all equipment containing material.


Special equipment requirements:Vacuum Oil Mist Filter on Vacuum Apparatus


Chemical-specific antidotes or first aid treatments:


Eye Contact: p. 2 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, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult, give oxygen. Get medical attention if symptoms appear.


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 crude containers closed and coolHow will the work surface and other items be decontaminated after use?Use clean ethanol


PERSONAL PROTECTIVE EQUIPMENT (PPE):Splash goggles or Face Mask. Fire-Resistant Lab coat. Vapor respirator. Be sure to use an approved/certified respirator or equivalent. High Heat Gloves.


Personal Protection in Case of a Large Spill: Splash goggles. Full suit. Vapor respirator. Boots. Gloves.STORAGE & 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, wear suitable respiratory equipment. 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 SMALL SPILL: Absorb with an inert material and put the spilled material in an appropriate waste disposal.


LARGE SPILL: 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 p. 3 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.


EXPOSURE LIMITS: Ethanol (CAS#64-17-5) IDLH: 3300 ppm, Butane (CAS#106-97-8) IDLH: 1,600 ppm


WASTE

ECOTOXICITY:

Not available.


BOD5 & 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 BIODEGREDATION:

The product itself and its products of degradation are not toxic.



DETAILS OF PROCESS Clean and prepare all glassware completely (clean solvent wash, acidic water wash, basic water wash, neutral water wash)


Properly grease all glassware joints, enough to create a good vacuum seal, without squeezing grease out of the joints and into the inside of the distillation unit


Load boiling flask to no more 60 percent of the total flask volume with crude oilInsert mag-stir bar into boiling flask if your mantle has a stir function


Place boiling flask into heating mantle


Begin to assemble glassware, use lab stands where necessary, from beginning to end short path distillation units normally go boiling flask>distillation head>condenser>receiving flask adapter with receiving flask>cold trap>cold trap>vacuum gauge>vacuum apparatus


Depending on receiving flask adapter style there are multiple ways to setup fraction collection. With a single straight vacuum adapter, you will rotate the main fraction flask upward and support it with a scissor stand, allowing the heads to pass through and collect in your first cold trap. With a cow style receiving adapter you will rotate the cow so that the heads fraction goes into the smaller collection flask first and support it with a scissor stand. With a bung and screw type adapter you will simply put the first flask on the adapter and support it with a scissor stand, and have more clean flasks cleaned, greased and ready to change.


Once all glassware is assembled; grease and insert thermometer probes


Apply cooling to cold trap systems (dry ice or chilling recirculator)


Apply vacuum to system


Monitor vacuum depth gauge, you should quickly reach below 100 microns and it should hold steady, if you are not below 100 micron or if numbers do not steadily go down and continue to bounce up and down you have a leak or your vacuum needs maintenance


Once you are sure your distillation system has no leaks, insulate your boiling flask with fire-rope or a boiling flask jacket


Set heating mantle to 110°C and set mag stirrer to low setting (200-400 rpm)As mantle heats up to 110°C it will boil off any minuscule amounts of residual solvent, terpenes and water left in the crude into your first receiving flask or first cold trap


When first fraction is nearly collected and begins to drip instead of flowing, turn mag stirrer to a medium setting (800-1000 rpm) to eject the last bits of volatiles


When fraction stops collection completely turn mag stirrer back to low setting and raise mantle temperature to 180°C


Continue collecting into first flask or first cold trap


Based on the purity of your crude, and quality of your vacuum, fraction switch temperature can vary from as low as 195°C to as high as 230°C and sometimes even higher if the crude oil is low purity


Before the heart fraction you may see a blue, green, purple, or clear fraction. These are unwanted compounds. If you have a colored fraction hold temperature and collect until completely distilled.Slowly dial temperature up 5 degrees at a time, watching fraction color, head temperature, and distillation rate.Allow mantle to reach temp fully before raising temperature


Signs that you have reached the heart fraction: an increase in distillation speed, color change to golden, higher viscosity at receiving adapter, temperatures at distillation head become much closer to mantle temperature, and higher reflux at distillation head


Change flask once heart fraction is distilling. With a single flask adapter simply lower the scissor stand until the fraction collects into receiving flask. With a cow adapter carefully hold cow with gloved hand while lowering scissor stand, rotate to collect in hearts flask, and raise scissor stand back up to support main body flask. With bung and screw type adapter screw down seal screw, release vacuum from flask with vacuum release port, lower scissor stand and remove flask, place new flask on, close vacuum release port, raise scissor stand to support flask, and unscrew the seal screw


Monitor fraction collection it may begin to slow as boiling flask reaches set temperature


Continue to raise set temp 3°C to 5°C at a time once mantle has reached set temp and distillation speed begins to slow


Signs that the heart fraction is nearly done collecting: slowing of reflux at distillation head, darkening of fraction color, and distillation head temps exceeding 230°C


Once you have collected all your hearts fraction change to a clean flask


With a single flask adapter you will have to shut down heating mantle and allow it to cool significantly, disconnect vacuum, replace flask, reapply vacuum, and turn mantle back on. If you do not let mantle cool enough you may get bump-over when reapplying vacuum


Once flask has been changed set mantle to 250°C and set mag stirrer to medium


Tails fraction will be darker and less pure but worth reprocessing for cannabinoids


Once mantle reaches temperature and fraction begins to slow raise mantle temperature 5°C


Continue raising mantle temp 5°C until tails fraction stops collecting or you reach 280°C


When finished collecting tails fraction turn off heating mantle and leave vacuum applied


Allow mantle to cool to near room temperature


Remove vacuum from distillation apparatus


Carefully disassemble all glassware


Empty fractions from flasks into media containers


Clean all glassware (clean solvent wash, acidic water wash, basic water wash, neutral water wash)Put glassware and equipment away


Clean workstation

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