standard operation procedure - br 9200 spinning band
TRANSCRIPT
Rev 01 Issued By: Kat Lawrence
2020.09.14
Approved By:
Confidential Information
Standard Operation Procedure - BR 9200 Spinning
Band Distillation SOP
Document Number [####]
Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP [Doc
###]Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP
Rev 01 Issued By: Kat Lawrence
2020.09.15 Approved By: [Approvers Name]
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Table of Contents
Table of Contents .......................................................................................................................................... 1
1. Purpose ................................................................................................................................................ 2
2. Scope .................................................................................................................................................... 2
3. Terminology ......................................................................................................................................... 2
4. Safety .................................................................................................................................................... 2
5. Equipment ............................................................................................................................................ 3
6. Materials .............................................................................................................................................. 3
7. Chain of Custody .................................................................................................................................. 3
8. Record Keeping .................................................................................................................................... 4
9. Equipment Set-Up ................................................................................................................................ 4
10. Procedure ............................................................................................................................................. 6
11. Waste Handling .................................................................................................................................. 10
12. Calculations ........................................................................................................................................ 11
13. References .......................................................................................................................................... 11
14. Appendixes ......................................................................................................................................... 12
Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP [Doc
###]Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP
Rev 01 Issued By: Kat Lawrence
2020.09.15 Approved By: [Approvers Name]
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1. Purpose
The purpose of this SOP is to provide instruction for safe loading of the BR9200 Spinning Band
Distillation Unit.
2. Scope
This document is applicable to laboratory operations and employees preforming distillations with
the spinning band unit.
3. Terminology
This section should include abbreviations, definitions, acronyms, key words, or other special terms
contained within the procedure.
Term Definition
SOP Standard Operating Procedure
PPE Personal Protective Equipment
COC Chain of Custody
4. Safety
4.1. Required PPE
• Heat resistant gloves
• Flame Resistant long-sleeved shirts and jeans or pants.
• Latex/Nitrile disposable gloves
• Closed-toe shoes that are chemical resistant and have non-skid soles
• Safety glasses with side shields
• Goggles (where there is a potential for splashing liquids)
• Long hair should be tied back and tucked under lab coat.
Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP [Doc
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2020.09.15 Approved By: [Approvers Name]
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• Hanging/dangling jewelry should be tucked into clothing or removed prior to working with
equipment).
4.2. Other PPE may be required in addition to, or in place of, the above list.
4.3. General Safety Information
• Before following this SOP, you must review the user manual for the BR9200.
• Do not operate this equipment if you have not been trained to do so.
• Do not apply pressure to this system, it is designed to be used under a vacuum.
• Do not operate this equipment if it is in less than perfect condition.
• Do not plug or unplug anything unless all switches are in the off position.
4.4. HSE Risks
• Hot surfaces can cause scalding/burns. Always allow equipment and glassware to cool prior
to handling.
• Glass components can break, broken glass can cut/puncture the skin. Handle with caution
to avoid breakages.
• Malfunctions or hazardous operating conditions that may affect personnel safety require
shut down and disconnection from power. Equipment will require proper restoration to the
normal operational state before the equipment can be used.
5. Equipment
5.1. Required Equipment
• BR9200 Spinning Band Distillation Unit
• Heating Mantle (1L, 5L, and 22L depending on Batch Size)
• Boiling Flasks (1L, 5L, and 22L depending on Batch Size)
• 1 L Receiving Flasks
• 4 L Receiving Flasks
• Distillation Notebook
6. Materials
6.1. The following materials are examples of acceptable feeds for this SOP
6.1.1. Winterized, decarboxylated Extract
6.1.2. Extract that has passed through a 5um filter at -60C.
7. Chain of Custody
To be addressed according to state guidelines utilizing Metrc and Lab Databases.
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###]Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP
Rev 01 Issued By: Kat Lawrence
2020.09.15 Approved By: [Approvers Name]
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8. Record Keeping
8.1. Records are to be kept in the ‘Distillations’ Notebook and Lab Database:
8.1.1. Date
8.1.2. Feed Extract Metrc Tag Numbers and Quantities
8.1.3. Distillate Metrc Tag Number and Quantities
8.1.4. Terpene Fraction weights.
8.1.5. Pot Bottom Metrc Tag Numbers and Quantities
8.1.6. Product Batch ID (See Appendix B for instructions on Batch ID generation)
8.1.7. Production Batch Metrc Tag Number
8.2. Additional data is logged by the PC including temperatures, vacuum levels, and set points.
9. Equipment Set-Up
9.1. Please refer to BR9200 Manual for equipment set-up information.
9.2. The BR9200
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9.3. The Cold Trap
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9.4. The Fraction Collector
10. Procedure
10.1. Please refer to BR9200 Manual for operational procedure.
10.2. Turning on the system
10.2.1. Turn on the power to the controller. The switch is located on the front panel of the
microprocessor. 1 is for on and 0 is for off.
10.2.2. When power is applied, the controller will sound a brief audible alarm test. The
following screen will be displayed:
B/R Instrument M690
Please Wait
Running System Test
10.2.3. Once the system test is successfully completed, the following screen will be displayed.
B/R Instrument M690
Select a Command Key
10.2.4. Turn on the PC and open the B/R Icon on the desktop. The small keypad of the M690
will now read:
USB Operation
Keypad Disabled
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10.2.5. From the PC Desktop select the B/R Icon. From Manual Controls a vacuum test can be
performed, and the condenser bath can be turned on and pre-cooled.
10.3. Pre-Cooling the Distillation System and Vacuum Check
10.3.1. Make sure the distillation system is clean and dry.
10.3.2. Assemble the distillation system and perform a full vacuum test and achieve a vacuum
below 0.1 mmHg. If the distillation system does not pass the vacuum test, use the
procedure for finding a vacuum leak before proceeding.
10.3.3. Cool the cold trap for a minimum of 2 hours. Longer is better. If possible, leave the cold
finger on overnight.
10.3.4. Start the condenser bath in manual controls and make the set point -20 °C. Let it cool till
it reaches at least -10 °C.
10.4. Preparing the Distillation System
10.4.1. After ethanol recovery and decarboxylation, the warm extract shall be transferred into
an appropriately sized boiling flask for distillation. Flasks should never be filled past 80% of
their capacity, the following Table indicates appropriate sizing information for boiling pot
selection.
Boiling Flask
Size
Minimum Quantity of
Extract Required
Maximum Quantity
of Extract Allowed
1 liter 500 grams 800 grams
5 liter 2000 grams 4000 grams
22 liter 8500 grams 1900 grams
10.4.2. The heating mantle appropriate to the flask selected for the distillation should be placed
in the distillation unit and plugged into the control board.
10.4.2.1. The boiling flask containing decarboxylated distillate should be placed into the
mantle, and the platform should be raised to ensure a proper seal between the
boiling flask and the column.
10.4.2.2. Warning!!! Do not leave any residue on the exterior of the boiling flask. Do not
spill anything on the heating mantle. These can cause heating mantle failure.
10.4.2.3. Warning!! Do not overtighten the lab jack as this may damage the distillation
column.
10.4.2.4. Verify that the receivers in the fraction collector are in place and are empty.
10.4.2.5. Verify that the fraction collector is assembled and connected to the distillation
system.
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10.4.2.6. Verify Cold Fingers are in place and empty.
10.4.2.7. Make sure you have the thermowell and temperature probe in the boiling flask.
Apply vacuum grease to the boiling flask thermowell. Check the temperature probe
in the head for proper placement. Close door for safety.
10.4.2.8. If you are going to perform an atmospheric distillation, Open the Vent Valve.
10.4.2.9. If you are going to perform a vacuum distillation, Close the Vent Valve.
10.4.2.10. Correct Valve Positions for starting a Distillation:
10.4.2.10.1. Valve #1 in pointing upward means you have sealed off Distillation head
to allow full vac.
10.4.2.10.2. Valve #2 pointing to the left allows vac on collection vessel.
10.4.2.10.3. Valve #3 in the upright position means system is fully open to vac
10.4.2.10.4. Valve #3 in the closed position means you have isolated the collection
flask.
10.4.2.10.5. See BR Manual for troubleshooting and vacuum testing.
10.5. Performing a Distillation.
10.5.1. From the PC Desktop press the BR ICON. The main menu screen will appear on the PC.
10.5.2. Select the Start Distillation button and the library of distillation runs will appear.
10.5.3. Select the distillation run which corresponds to the material you are distilling. A series of
questions/reminders will be displayed. After acknowledging the questions, the Process
Run screen will appear. There are several options.
10.5.3.1. The Run Data Screen allows the distillation parameters to be viewed and edited.
10.5.3.2. The Run Tuning Screen allows certain “Hot Keys” to be accessed. The spinning
band motor, reflux valve, fraction collector and some other functions can have their
functions briefly tested.
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Rev 01 Issued By: Kat Lawrence
2020.09.15 Approved By: [Approvers Name]
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10.5.3.3. The Process Diagram allows the current state of the distillation to be viewed
along with the schematic of the distillation equipment. The actual schematic
displayed will depend on the configuration selected in System Options.
10.5.3.4. The Run Data Screen is the most common screen to use to operate the
distillation. The distillation can be paused at any time by selecting the Pause button.
Once paused, the distillation can be Aborted or Resumed.
10.5.3.5. You can edit any parameter during the distillation run in the Run Data screen.
Once you enter a new parameter you will need to press ENTER to confirm your
parameter change.
10.5.3.6. At the bottom of each screen is a bar which displays the real time parameters
of the distillation. Vapor, Pot and Condenser Temperatures, vacuum level and
heating rate are displayed.
10.5.3.7. Distillation begins at 50 mmHg vacuum set point.
10.5.3.8. As boiling flask heats up, you’re able to slowly reduce vacuum.
10.5.3.8.1. Caution- Only reduce vacuum in 10 unit increments or less.
10.5.3.9. Residual ethanol will come off first then Terpenes.
10.5.3.9.1. Properly winterized material will have minimal ethanol, we may see up
to 200mL ethanol collected in a large distillation of 19L of feed.
10.5.3.10. Only lower vacuum set points as Distillation slows down to speed up the run. Be
careful not to push the limits.
10.5.3.11. At approximately 30 mmHg and 105c boiling flask temperature the
decarboxylation begins. CO2 will emit from the sample and the vacuum will not be
able to be reduced further until Decarboxylation is completed.
10.5.3.11.1. If feed material was previously decarboxylated, there will be no
vacuum/ temperature plateau and the run will continue to the next step.
10.5.3.12. Typically, residual ethanol will continue until you reach 160-170c. at this point
terpenes will roll off until oil starts to run.
10.5.3.13. Set points on chiller start at -20C through residual ethanol distillation.
10.5.3.14. As terpenes roll off the chiller temp should be increased to -10C briefly before
increasing the temperature to 0C.
10.5.3.15. As terpenes begin to slow down its time to raise chiller temperature 20c.
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###]Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP
Rev 01 Issued By: Kat Lawrence
2020.09.15 Approved By: [Approvers Name]
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10.5.3.16. When boiling flask reaches 190C vac set points should be as low as possible;
0.01 mmHg. Chiller should be set to 55C.
10.5.3.17. Look for smoke rings with a controlled light pops in boiling flask. This means
THC9 is ready to come out. Always remember that either green oil or azuline comes
off fist followed by main body.
10.5.3.18. When collecting oil make sure to collect main body with no tails.
10.6. Finishing a Distillation
10.6.1. When the distillation is complete, you can hit pause and then abort of the run.
10.6.2. Turn off the vacuum pump, and chillers. This will stop heating the unit; however it will
remain under vacuum until you open the vent.
10.6.3. You can isolate your fraction collector and receivers from the remainder of the system
by closing valve 3.
10.6.4. Then open valve 2 slowly to equalize the pressure in the fraction collector.
10.6.5. You are now able to open the fraction collector to remove the distillate product while
leaving the bulk of the system under vacuum to cool.
10.6.5.1. The distillate in the receivers is now ethanol free delta 9 THC distillate, it is no
longer considered hazardous. Weights and volumes should be recorded. The
distillate can be warmed and transferred to a large beaker for homogenization and
testing.
10.6.6. Once the distillation unit is cool, open valve 1 to eliminate the vacuum.
10.6.7. At this point you can remove the boiling pot flask and determine the mass of material
still in the flask. This is the heavies from the distillation, and the heavies will be combined
with other distillation heavies for future re-distillation.
11. Waste Handling
All solvents shall be recycled internally; undergo purification via additional rotary evaporator distillation
or by distillation in the spinning band unit, once purity can be confirmed the purified solvent can be
used again. Solvent waste shall be handled according to state and federal guidelines, following the Lab
Waste Handling SOP.
Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP [Doc
###]Standard Operation Procedure - BR 9200 Spinning Band Distillation SOP
Rev 01 Issued By: Kat Lawrence
2020.09.15 Approved By: [Approvers Name]
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12. Calculations
12.1.
13. References
13.1.1. Operating Manual Model 9200 Fractional Spinning Band Distillation System; BR
Instrument Corporation
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2020.09.15 Approved By: [Approvers Name]
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14. Appendixes
14.1. Appendix A. Production Batch ID:
14.1.1. The production batch ID will consist of the strain abbreviation (if more than one list all
separated by periods), followed by an underscore, then either Terp1, Terp2, Terp#,
THC9Dist1, THC9Dist2, etc for the distillate cut or Heavies for the pot bottoms , then the
date YYYY.MM.DD, followed by an underscore, then the last 4 digits of the New Metrc
batch tag ID. Cold Fingers will be labeled CFLT, CFMT, CFHT in the same mannor.
14.1.1.1. Example 1: You are labelling your main body of distillate for the day, and the
New Batch Metrc tag will end in 2127. The date is 2020.08.15, this distillate was from
99 Problems, the Batch ID would look like this:
99D1_THC9Dist1.2020.08.15_2127
14.1.1.2. Example 2: You are labelling your pot bottoms (heavies) August 15th, 2020. The
feed was 99 Problems extract and the batch Metrc tag will end in 2128. The Batch ID
would look like this:
99D1_Heavies.2020.08.15_2128
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14.2. Appendix B. Cloud Cover Strain Abbreviations
Strain Abbreviation
99 Problems #1 99D1
Alien Pie AP
Cherry Punch CP
Coogies CG
Do-Si-Dos DSD
Flo FLO
Frozen Dessert FD
Ghost Dawg GD
GMO GMO
Gorilla Glue #4 GG4
Grape Stomper GS
Headbanger HB
GSC GSC
Headbanger HB
Ice Cream Cke ICC
Katsu Bubba Kush BK
Lemon Ozium LO
Lemon Ozium #1 LO1
Mentoz MTZ
Orange Ghost OJG
Power Nap PN
Presidential Kush PREZ
Queso Perro QP
Sour Tangie ST
Triangle Kush TK
UK Cheese UK
White 99 W99
Wookie Girl '91 WG