The Polyarc System Workshop - Activated Research Company · Swagelok brass tees and copper tubing •Controller: •ARC EFC •ARC MFC •GC Aux EPC •Flow rates: •Air 2.5 sccm

© 2018 Activated Research Company, LLC© 2018 Activated Research Company, LLC

The Polyarc® SystemWorkshop

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Agenda

• Polyarc® Overview (10 min.)

• Installation and User Experience (30 min.)

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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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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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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

1 2

3

4

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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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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.

1

Cool the reactor to room temperature (turn off auxiliary temperature).

2

Shut off air and H2flows to the reactor.

3

Perform maintenance or shut down GC.

4

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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


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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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

• [email protected]

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https://www.activatedresearch.com/documents/https://www.activatedresearch.com/technical-literature/mailto:[email protected]?subject=Polyarc Question


“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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Quantification Example:Solvents in Paints and Coatings

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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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Short Long Name Area (pA·s) µmol C/mL µg/mL

MeOH Methanol 159220 24115 772660








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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MeOH Methanol 159220 24115 772660








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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MeOH Methanol 159220 24115 772660








1.7% average error

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© 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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