ACS 2018 New Orleans: The Effect of Grinding on SFE
1. GRINDING: THE DELICATE DANCE BETWEEN OPTIMIZATION
AND REPETITION TO CONTROL EXTRACTION OUTCOMES
S 1F R I T S C H MI L L I N G & S I Z I N G , I N C .
• Pre-processing
• Considerations
• Physical characterization
BARRY SCHUBMEHL
TECHNICAL MANAGER
FRITSCH MILLING & SIZING, INC.
DR. MARKUS ROGGEN
VP EXTRACTIONS
OUTCO
• Overview
• Parameters
• Findings
3. PRE-PROCESSING - CONSIDERATIONS
S 3F R I T S C H MI L L I N G & S I Z I N G , I N C .
PREVENT LOSSES
• Physical / Chemical
IMPROVE CONTROL & CONSISTENCY
• Packing density
• Extraction efficiency
ALSO IMPORTANT
• Worker safety
• Validatable cleaning SOP – reduce risk
of batch rejection
• Energy & labor costs
4. MOLECULAR CHANGES THROUGH MILLING
S 4F R I T S C H MI L L I N G & S I Z I N G , I N C .
Does milling effect the substrate quality?
0%
1%
2%
%decarb by Size
0
0.2
0.4
0.6
0.8
1
1.2
1.4
%wt. Terpenes by Size
5. EXTRACTION EFFECTS THROUGH MILLING
S 5F R I T S C H MI L L I N G & S I Z I N G , I N C .
What method gives the highest yield?
20
22
24
26
28
30
32
34
Non-Ground Food
Blender
2 mm 6 mm 10 mm
%Recovery
Cannabinoid Recovery by Size
75
80
85
90
95
Non-Ground Food
Blender
2 mm 6 mm 10 mm
%Recovery
Terpene Recovery by Size
6. EXTRACTION PARAMETERS
S 6F R I T S C H MI L L I N G & S I Z I N G , I N C .
• 3 kg of plant matter
• Terpene Fraction (F1): 1100 psi, 34˚C, 5 h
• Cannabinoid Fraction (F2): 1900 psi, 60˚C, 12 h
7. EXTRACTION PRECISION TERPENES
S 7F R I T S C H MI L L I N G & S I Z I N G , I N C .
30
35
40
45
50
55
Non-Ground Food Blender 2 mm 6 mm 10 mm
%conc.
Terpene Concentration F1
Higher is better, Food Blender wins
0
1
2
3
4
5
Non-Ground Food Blender 2 mm 6 mm 10 mm
%conc.
Terpene Concentration F2
Lower is better, 2mm wins
• 3 kg of plant matter
• Terpene Fraction (F1): 1100 psi, 34˚C, 5 h
• Cannabinoid Fraction (F2): 1900 psi, 60˚C, 12 h
8. EXTRACTION PRECISION CANNABINOIDS
S 8F R I T S C H MI L L I N G & S I Z I N G , I N C .
0
2
4
6
Non-Ground Food
Blender
2 mm 6 mm 10 mm
%conc.
Cannabinoid Concentration F1
Lower is better, 10mm wins
55
60
65
70
75
Non-Ground Food
Blender
2 mm 6 mm 10 mm
%conc.
Cannabinoid Concentration F2
Higher is better, 2mm wins
• 3 kg of plant matter
• Terpene Fraction (F1): 1100 psi, 34˚C, 5 h
• Cannabinoid Fraction (F2): 1900 psi, 60˚C, 12 h
9. PHYSICAL CHARACTERIZATION
S 9F R I T S C H MI L L I N G & S I Z I N G , I N C .
NEW METHOD
• Laser particle sizer
ANALYSETTE 22 NanoTec
• Wet dispersion
• Propylene glycol,
IPA
WHY?
To determine the particle size
distribution of material going
into the extractor
HOW?
• Visual / sensory - No
• Sieving - Limited
• Optical based- Yes
• Laser based - Yes
Contributors: Dr. Günther Crolly, Jeff Scott
11. PARTICLE SIZE DISTRIBUTION - EXAMPLES
S 1 1F R I T S C H MI L L I N G & S I Z I N G , I N C .
Example 1: Food Blender Example 2: Milled Cannabis leaves
12. PARTICLE SIZE DISTRIBUTION - EXAMPLES
S 1 2F R I T S C H MI L L I N G & S I Z I N G , I N C .
Example 3: Trichome heads Example 2: Milled Cannabis leaves
14. QUESTIONS
S 1 4F R I T S C H MI L L I N G & S I Z I N G , I N C .
Hinweis der Redaktion
Good morning everyone & welcome. My name is Barry Schubmehl, Technical Manager with Fritsch Milling & Sizing. Thank you to Dr. King & Dr. Roggen for the opportunity to be here. Over the past years, we’ve been asked to provide new solutions by LCPs, and have been working closely with the industry to do that. It has been an honor for us to collaborate with companies like OutCo, who are taking a pioneering role in the science of cannabis production. As an introduction to the research studies conducted by Dr. Roggen & his team, I will share some concepts & considerations regarding the optimization process, and a new analytical method that was developed to allow physical characterization of the samples.
This pre-processing step is typical across industries, and is necessary to allow for optimal packing density in the extraction column. There are many options available for doing this, and the choice is dependent on the material, and desired final particle size. For a given material, we can expect that the output from a given mill may have different physical & chemical characteristics. This study was aimed at exploring these potential differences, and the impact on the extraction process.
The true “starting batch” on which a hypothetical maximum yield can be calculated, is the material that enters a production suite, before processing or extraction. The goal of this pre-processing (or material preparation) step can be viewed as an opportunity to:
1. Prevent physical or chemical losses from the starting batch of material
2. Optimize particle size & distribution to maximize packing density & extraction efficiency
Here I talk about the effects of milling on the cannabinoid and terpene composition of the plant substrate. We cannot point at any effect. But the terpene concentration will decrease quickly with milled material. It is important to extract quickly after milling.
Smaller particle give higher yields. In both cannabinoids and terpenes.
Even more important then total yield is extraction precision. Therefore we do two fractions and assess “Trennschärfe”
Non-Ground is so horrible.
Non-Ground is really bad. And 2mm is great.
Laser particle size analyzers have been used for many decades across a wide-range of industries as a tool in quality control, process development, or basic research. This method development for analyzing cannabis samples involved determining the optimal dispersion method, and subsequently, the appropriate solvent.
Smaller particle give higher yields. In both cannabinoids and terpenes.
The diagrams above are data outputs from the laser particle sizer, showing particle size distribution from a particular milling system. The sharp peak indicates that the majority of particles are concentrated around the same size range. The shape of the curve can vary widely depending on the milling system used. Detection range shown on the X-axis is from 10 nanometers, up into the millimeter scale.
The diagrams above are data outputs from the laser particle sizer, showing particle size distribution from a particular milling system. The sharp peak indicates that the majority of particles are concentrated around the same size range. The shape of the curve can vary widely depending on the milling system used. Detection range shown on the X-axis is from 10 nanometers, up into the millimeter scale.
Data from the ANALYSETTE 28 Image Sizer shows tighter particle size distribution using the cutting mill compared to kitchen blender.