the polyarc system workshop - activated research company · swagelok brass tees and copper tubing...
TRANSCRIPT
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
The Polyarc® SystemWorkshop
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
Agenda
• Polyarc® Overview (10 min.)
• Installation and User Experience (30 min.)
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
Polyarc®
System: Catalyzing the FutureAn add-on technology to provide better data and higher throughput.
Microreactor Design and
Stainless Steel 3D Printing
Expertise in Catalysis
Design and Synthesis
First and Only Commercial 3D Printed
Microreactor
Made in the U.S.A.
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
GC with flame ionization detection (GC/FID)
GC with Polyarc®
and FID
Polyarc®
System: How it WorksPost-column and pre-detector conversion to methane.
https://www.activatedresearch.com/technology/
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
Agenda
• Polyarc® overview (10 min.)
• Installation and User Experience (30 min.)
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Installation
1. Position of Polyarc
2. Air and Hydrogen Supply lines
3. Polyarc inlet and outlet
4. Heater
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Polyarc Position
• Detector (1)
• Inlet (2)
• Valve box (3)
• MS (4)
• Other
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
Air and Hydrogen Supplies
• Splice supply lines to FID using Swagelok brass tees and copper tubing
• Controller:
• ARC EFC
• ARC MFC
• GC Aux EPC
• Flow rates:
• Air 2.5 sccm
• Hydrogen 35 sccm
• Different if hydrogen as a carrier gas
• Verify flows out of FID
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Polyarc Inlet and Outlet
• Inlet connects to column via Agilent Zero Dead Volume union• UltiMetal swaging
• Outlet connects straight to FID• 0.8mm graphite ferrule
0.1 – 0.5 mm (column sticking out)
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Heater
• Setpoints• Operate at 293 °C setpoint
(450 °C actual)• Condition at 350 °C setpoint
(550 °C actual)
• ARC PID Controller
• GC Heater• A1/A2 with heater adapter
cable assembly• Detector position• Inlet position
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
User Experience
• No additional software
• Same GC methods
• Polyarc heater at 293 °C setpoint
• Initial bakeout period at 350 °C setpoint
• Polyarc air at 2.5 sccm, H2 at 35 sccm
• FID H2 at 1.5 sccm
• “Quantification with the Polyarc” document
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Polyarc Shutdown Procedure
Shut off the FID.
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Cool the reactor to room temperature (turn off auxiliary temperature).
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Shut off air and H2flows to the reactor.
3
Perform maintenance or shut down GC.
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
Quantification with the Polyarc
•𝑟𝑒𝑠𝑝𝑜𝑛𝑠𝑒𝐴
𝑚𝑜𝑙𝑒𝑠 𝑐𝑎𝑟𝑏𝑜𝑛𝐴=
𝑟𝑒𝑠𝑝𝑜𝑛𝑠𝑒𝐵
𝑚𝑜𝑙𝑒𝑠 𝑐𝑎𝑟𝑏𝑜𝑛𝐵for all molecules
• 𝑅𝐹 𝑐𝑎𝑟𝑏𝑜𝑛 − 𝑏𝑎𝑠𝑒𝑑 =ൗ
𝑟𝑒𝑠𝑝𝑜𝑛𝑠𝑒𝐴𝑚𝑜𝑙𝑒𝑠 𝑐𝑎𝑟𝑏𝑜𝑛𝐴
ൗ𝑟𝑒𝑠𝑝𝑜𝑛𝑠𝑒𝐵
𝑚𝑜𝑙𝑒𝑠 𝑐𝑎𝑟𝑏𝑜𝑛𝐵
= 1
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𝐶𝐴 = 𝐶𝑆𝐴𝑟𝑒𝑎𝐴𝐴𝑟𝑒𝑎𝑆
𝑀𝑤𝐴𝑀𝑤𝑆
#𝐶𝑆#𝐶𝐴
Polyarc® System: Quick & Easy Data AnalysisSame GC. Same Software. Simplified Data Analysis.
NOTE: Above equation applies to quantification with mass concentrations, and other variants exist for other concentration units (e.g. molar). Additional information can be found on the Documents page of ARC’s website in ‘Quantification with the Polyarc’.
Any compound of interest can be quantified using an internal standard and the integrated peak areas
from a single injection.
The response per carbon atom is equivalent for all organic molecules.
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http://www.activatedresearch.com/Public_Documents/Quantification with the Polyarc.pdf
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
𝐶𝐴 = 𝐶𝑆𝐴𝑟𝑒𝑎𝐴𝐴𝑟𝑒𝑎𝑆
𝑀𝑤𝐴𝑀𝑤𝑆
#𝐶𝑆#𝐶𝐴
Polyarc® System: Quick & Easy Data AnalysisSimplified Data Analysis in a Single Injection.
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Quantification Example:Crude Isoprene
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Quantification Example:Crude Isoprene
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
Paul Dauenhauer, University of Minnesota, Twin Cities
Sulfur Limitations
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Tailing and reduction in peak areas signals the need for a replacement reactor.
New Reactor
Replacement Reactor Needed
Polyarc System: LifetimeEasy to reactor replace cartridges
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Replacement reactors
4 Step Replacement
1. Cool reactor, shut off gas flows and turn off GC2. Disconnect gas fittings (2 external, 2 in GC oven)3. Unplug heater cable from GC electronics4. Replace module and repeat steps in reverse order
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Resources
• https://www.activatedresearch.com/documents/
• Installation Manuals
• Quantification Guide
• Installation Video
• More…
• https://www.activatedresearch.com/technical-literature/
• Application Notes
• Technical Publications
• Contact Us
• 612-787-2721
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https://www.activatedresearch.com/documents/https://www.activatedresearch.com/technical-literature/mailto:[email protected]?subject=Polyarc Question
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
“The Polyarc is the future of FID. It is to carbon as the SCD is to sulfur without the complexity.”
Jean-Paul Schirle-Keller, Flavor Research and Education Center, University of Minnesota, Twin Cities
Questions
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Appendix
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Data Analysis
• FID Area = Carbon %
• See “Quantification with the Polyarc” for more information
𝑹𝑭 𝒄𝒂𝒓𝒃𝒐𝒏 − 𝒃𝒂𝒔𝒆𝒅 =ൗ
𝒂𝒓𝒆𝒂𝟏𝒄𝒂𝒓𝒃𝒐𝒏 𝒄𝒐𝒏𝒄𝒆𝒏𝒕𝒓𝒂𝒕𝒊𝒐𝒏𝟏
ൗ𝒂𝒓𝒆𝒂𝟐
𝒄𝒂𝒓𝒃𝒐𝒏 𝒄𝒐𝒏𝒄𝒆𝒏𝒕𝒓𝒂𝒕𝒊𝒐𝒏𝟐
= 𝟏
𝒎𝒐𝒍 𝑪 = 𝒎𝒐𝒍 𝑪𝑰𝑺 ∙𝒂𝒓𝒆𝒂
𝒂𝒓𝒆𝒂𝑰𝑺
𝒘𝒕.% = 𝒘𝒕.𝑰𝑺% ∙𝒂𝒓𝒆𝒂
𝒂𝒓𝒆𝒂𝑰𝑺
𝑴𝑾
𝑴𝑾𝑰𝑺
#𝑪𝑰𝑺#𝑪
Molar:
Mass:
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Quantification Example:Solvents in Paints and Coatings
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
Quantification Example:Solvents in Paints and Coatings
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
Quantification Example:Crude Isoprene
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
Quantification Example:Crude Isoprene
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Quantification Example:Fragrances
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Quantification Example:Fragrances
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Quantification Example:Paints and Coatings
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Quantification Example:Paints and Coatings
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LimitationsRecovery
• Leak• Inlet Discrimination• Adsorption/Reaction• Sample issues
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LimitationsRecovery
ASTM Methods D6729, D6730, D6733 and more
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4
1.6
1.8
0.0 50.0 100.0 150.0 200.0 250.0 300.0
No
rma
lize
d C
on
ce
ntr
ati
on
Boiling Point [°C]
PiONA Standard
Custom Mix
PiONA MixC5-C15
133 compounds
Dauenhauer, P., University of Minnesota, Twin Cities
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LimitationsSulfur
Paul Dauenhauer, University of Minnesota, Twin Cities
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Tailing and reduction in peak areas signals the need for a replacement reactor.
New Reactor
Replacement Reactor Needed
LimitationsReactor degradation
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Short Long Name Area (pA·s) mol C/mL µg/mL
MeOH Methanol 159220 24115 772660
TBA Tert-butanol 3651 553 10246
MTBE methyl-tert-butyl ether 740 112 1977
DIPE diisopropyl ether 759 115 1957
ETBE ethyl-tert-butyl ether 771 117 1988
TAME tert-amyl methyl ether 781 118 2015
TAEE tert-amyl ethyl ether 809 122 2033
Example calculation – VOCs in gasoline
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
Short Long Name Area (pA·s) µmol C/mL µg/mL
MeOH Methanol 159220 24115 772660
TBA Tert-butanol 3651 553 10246
MTBE methyl-tert-butyl ether 740 112 1977
DIPE diisopropyl ether 759 115 1957
ETBE ethyl-tert-butyl ether 771 117 1988
TAME tert-amyl methyl ether 781 118 2015
TAEE tert-amyl ethyl ether 809 122 2033
Example calculation – VOCs in gasoline
𝑚𝑜𝑙 𝐶 = 𝑚𝑜𝑙 𝐶𝐼𝑆 ∙𝑎𝑟𝑒𝑎
𝑎𝑟𝑒𝑎𝐼𝑆
112 ൗµ𝑚𝑜𝑙 𝐶
𝑚𝐿 = 117 ൗµ𝑚𝑜𝑙 𝐶
𝑚𝐿 ∙740 𝑝𝐴 ∙ 𝑠
771 𝑝𝐴 ∙ 𝑠
MTBE ETBE
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Short Long Name Area (pA·s) µmol C/mL µg/mL
MeOH Methanol 159220 24115 772660
TBA Tert-butanol 3651 553 10246
MTBE methyl-tert-butyl ether 740 112 1977
DIPE diisopropyl ether 759 115 1957
ETBE ethyl-tert-butyl ether 771 117 1988
TAME tert-amyl methyl ether 781 118 2015
TAEE tert-amyl ethyl ether 809 122 2033
Example calculation – VOCs in gasoline
MTBE ETBE
𝑤𝑡.% = 𝑤𝑡.𝐼𝑆% ∙𝑎𝑟𝑒𝑎
𝑎𝑟𝑒𝑎𝐼𝑆
𝑀𝑊
𝑀𝑊𝐼𝑆
#𝐶𝐼𝑆#𝐶
1977 ൗµ𝑔
𝑚𝐿 = 1988 ൗµ𝑔
𝑚𝐿 ∙740 𝑝𝐴 ∙ 𝑠
771 𝑝𝐴 ∙ 𝑠
88 ൗ𝑔𝑚𝑜𝑙
102 ൗ𝑔𝑚𝑜𝑙
6 𝐶
5 C
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Short Long Name Area (pA·s) µmol C/mL µg/mL
MeOH Methanol 159220 24115 772660
TBA Tert-butanol 3651 553 10246
MTBE methyl-tert-butyl ether 740 112 1977
DIPE diisopropyl ether 759 115 1957
ETBE ethyl-tert-butyl ether 771 117 1988
TAME tert-amyl methyl ether 781 118 2015
TAEE tert-amyl ethyl ether 809 122 2033
Example calculation – VOCs in gasoline
1.7% average error
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© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC
© 2016 Activated Research Company
Our solution simplifies analysis
Traditional analysis vs. ARC Polyarc® technology
98% 80% 86%
>100 customers have validated value proposition
By reducing all molecules to methane
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