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Pyrolysis
Purge & Trap
Thermal Desorption
Page 1
CDS ANALYTICAL, LLC
Your Single Source for Sample
Introduction
Pyrolysis
Purge & Trap
Thermal Desorption
2
• Expand the value of your GCMS
–Replace solvent extraction with
Thermal Extraction.
–Analyze polymers by Pyrolysis
–Concentrate VOC’s & increase sensitivity of
GC detectors with Thermal Desorption
–Condition aqueous samples for VOC
analysis with Purge & Trap
Pyrolysis
Purge & Trap
Thermal Desorption
ALL WITHOUT SOLVENTS
Make Your Analysis GREEN
3
Pyrolysis
Purge & Trap
Thermal Desorption
Volatilize Small Molecules Intact- SOLVENT FREE
Thermal Desorption, Dynamic Headspace
~ 50 – 300°C
4
Carrier Gas To
GC
Pyrolysis
Purge & Trap
Thermal Desorption
Pyrolysis of a Polymer
5
Polymer fragments
volatized and
transferred to GC
Heat greater
than 500°C
Pyrolysis
Purge & Trap
Thermal Desorption
What Can CDS Analyze?
6
• Plastics – films, foams, fibers, molded parts
• Coatings – paints, varnish, polyurethanes
• Rubber – tires, adhesives, building materials
• Energy Feedstock– oil, coal, biomass, algae
• Printing – inks and toners
• Consumer goods – cosmetics, surfactants, food, tobacco
• Forensics- paint, fiber, tapes, documents, drugs
• Environmental- air, water & soils
• All with your existing GCMS and WITHOUT SOLVENTS
Pyrolysis
Purge & Trap
Thermal Desorption
7
Resistively Heated Pyrolyzer
Analyze any polymers by
GCMS
Fast, Accurate, Reliable,
Consistent
Quantitate copolymers
Analyze for Trace additives
Deformulate samples
Connects to any GC
Pyrolysis
Purge & Trap
Thermal Desorption
8
Pyrolysis
Purge & Trap
Thermal Desorption
A Programmed
3 step run of
this lubricating
strip follows
CDS Pyrolyzers can be programmed to thermally extract
additives BEFORE analyzing for polymers
9
Pyrolysis
Purge & Trap
Thermal Desorption
UV light stabilizer
10
Pyrolysis
Purge & Trap
Thermal Desorption
5000 Series
11
5000
Injection port mounted
5150
Easy on/off sample
line connection
5200
Pyrolysis with built in
analytical trap for reactant
gas pyrolysis
• Heating up to 1400°C
• Programmable heat rates to 20,000°C/sec
• Includes Evolved Gas and Thermal Desorption capability
• All systems can have 8 unique temperature runs
• Connects to any model GC
Pyrolysis
Purge & Trap
Thermal Desorption
12
Pyroprobe Autosamplers
Carousel
Pyrolysis coil
Trapping
zone
Cryogenics
5250T Trapping Version 5250 Non-Trapping
Pyrolysis
Purge & Trap
Thermal Desorption
Analyze Biomass, Oils and
Coal
And experiment with Catalysts with
our New Pyrolysis Micro Reactor
13
Pyrolysis
Purge & Trap
Thermal Desorption
High Pressure Pyrolysis with Catalytic Reactor
• Sample can be pyrolyzed up to 1400°C
• Vary pyrolysis Pressure up to 500 PSI
14
• Designed to simulate reactor conditions
• Pyrolyze in carrier gas or in a reactive gas
• Test the catalyst on biomass, coal, or oils
• Reacted sample is automatically sent direct
to your GCMS for analysis
• Pyrolyzed sample flows through heated catalyst
reactor (to 800°C)
Pyrolysis
Purge & Trap
Thermal Desorption
15
High Pressure Pyrolysis with Reactor
Reactor
Reactor
on-line
Valve
Back
Pressure
Regulator
Pyroprobe
Pyrolysis
Purge & Trap
Thermal Desorption
16
High Pressure Pyrolysis with Reactor
Reactor
Catalyst tube
Reactor valve
(manual)
Pyroprobe valve
(automatic)
Pyrolysis
Purge & Trap
Thermal Desorption
17
5200HPR Pyrolysis Microreactor Flow Path
Pyrolysis
Purge & Trap
Thermal Desorption
18
5200HPR Pyrolysis Microreactor Flow Path
Carrier Gas
Pyrolysis
Purge & Trap
Thermal Desorption
19
Wood Pyrolyzed in He & H₂ through Pt
Reactor
Pyrolyzed in He
at 650°C
Pyrolyzed in H₂
at 300 PSI
through reactor
Pyrolyzed in H₂
at 400 PSI
through reactor
Pyrolysis
Purge & Trap
Thermal Desorption
NEW 5500 Fixed Gas Analyzer
20
• Analyze for Fixed Gases that pass through the Analytical
Trap
• Pre-programmed for H2, CO, CO2, CH4, H2O, C2H2, C2H4
• A True Plug & Play Analyzer for any CDS Trapping Pyrolyzer
• Includes an Industry Standard
Chromatography Software Package
Pyrolysis
Purge & Trap
Thermal Desorption
Environmental
21
• Air
– TO-1/2
– TO-17
• CW Agent Monitoring
• Product Emissions
• Water
• Solids
● Purge & Trap
– Trace VOC’s in water &
waste water, soils
● Thermal Desorption
– Monitor for trace air
pollutants
• Water
– EPA 624, 524.2/3
• Soil/Waste
– SW 846 8260 8021
5030 5035
Pyrolysis
Purge & Trap
Thermal Desorption
Thermal Desorption
22
CDS 9350 with Purge & Trap accessory on
your favorite GC
Pyrolysis
Purge & Trap
Thermal Desorption
23
Pyrolysis
Purge & Trap
Thermal Desorption
Ambient Air Monitoring (TO-17)
65 component
mixture
1. Propylene
2. Dichlorodifluoro
methane
3. Chloromethane
4. Vinyl chloride
.
.
.
.
64. 1,2,4-Trichloro
Benzene
65. Hexachlorobutadiene
24
Sorbent Tubes
Column: CP-Select 624Column: CP-Select 624
Pyrolysis
Purge & Trap
Thermal Desorption
CW Agent Run
25
Pyrolysis
Purge & Trap
Thermal Desorption
PAHs in Soil
• 0.5 grams of soil
thermally extracted at
325ºC
– Empty TD tube
– Pre-dry sample or Dry
Tube
– 1 ppm standard (~ 0.5 ug)
Phenanthene
Fluoranthene & Pyrene
Benzanthracene & Chrysene
Benzo (a) Pyrene
Thermal Extraction
26
Pyrolysis
Purge & Trap
Thermal Desorption
27
Dynatherm Thermal Desorption
Benefits
• Focusing tube allows 100% of absorbed
compounds to be transferred to GC; No GC Split
Needed
• No peltier or cryo cooling needed
– Lower cost of ownership
– Eliminates H2O problems w/ dry purge
– Peltiers may freeze with high moisture samples
• No Special Dry gas needed
• Sensitivity to sub PPT
• Simple flow path increases reliability
Pyrolysis
Purge & Trap
Thermal Desorption
NEW Soil/Water PT Autosampler
28
• 72 Position pick & place Autosampler
• Water capability
–Moves vial to water station
• Soil Capability
–Moves vial to soil Heater with
magnetic stirrer
• Internal Standard addition
Pyrolysis
Purge & Trap
Thermal Desorption
NEW Soil/Water PT Autosampler
29
• System prepared blanks (Water only)
• Programmable rinse cycles
• REPLACE YOUR AGING ARCHONS!
• Compatible with any PT Concentrator
Pyrolysis
Purge & Trap
Thermal Desorption
Water Analysis: EPA Method 524.2
30
Gases
Pyrolysis
Purge & Trap
Thermal Desorption
7300/7400 Advantages
31
• Reliable, Durable and Reproducible
• Low cost advantage
• Soils (Solids) and waters
• Internal standard addition
• What more do you the customer really need?
Pyrolysis
Purge & Trap
Thermal Desorption
NEW 7500 Thermal Desorption
Autosampler
32
• Ability for the user to change between TD tubes for air and VOA
vials for soil and/or water analysis
• Pick and Place robotic arm
• 72 position autosampler, with 3 removable trays
• Leak Checking
• Ability to desorb other manufacturers’ tubes (consult factory)
• Automated IS Addition (optional)
• Sample Saver (optional)
• Compatible with the Dynatherm 9300 Series
• Compatible with the Purge & Trap 7000 E and most
standard/commercial P&T systems
Pyrolysis
Purge & Trap
Thermal Desorption
CDS Analytical - Your
Partner in Sample
Preparation for GCMS
33

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Pittcon Powerpoint (2014)

  • 1. Pyrolysis Purge & Trap Thermal Desorption Page 1 CDS ANALYTICAL, LLC Your Single Source for Sample Introduction
  • 2. Pyrolysis Purge & Trap Thermal Desorption 2 • Expand the value of your GCMS –Replace solvent extraction with Thermal Extraction. –Analyze polymers by Pyrolysis –Concentrate VOC’s & increase sensitivity of GC detectors with Thermal Desorption –Condition aqueous samples for VOC analysis with Purge & Trap
  • 3. Pyrolysis Purge & Trap Thermal Desorption ALL WITHOUT SOLVENTS Make Your Analysis GREEN 3
  • 4. Pyrolysis Purge & Trap Thermal Desorption Volatilize Small Molecules Intact- SOLVENT FREE Thermal Desorption, Dynamic Headspace ~ 50 – 300°C 4 Carrier Gas To GC
  • 5. Pyrolysis Purge & Trap Thermal Desorption Pyrolysis of a Polymer 5 Polymer fragments volatized and transferred to GC Heat greater than 500°C
  • 6. Pyrolysis Purge & Trap Thermal Desorption What Can CDS Analyze? 6 • Plastics – films, foams, fibers, molded parts • Coatings – paints, varnish, polyurethanes • Rubber – tires, adhesives, building materials • Energy Feedstock– oil, coal, biomass, algae • Printing – inks and toners • Consumer goods – cosmetics, surfactants, food, tobacco • Forensics- paint, fiber, tapes, documents, drugs • Environmental- air, water & soils • All with your existing GCMS and WITHOUT SOLVENTS
  • 7. Pyrolysis Purge & Trap Thermal Desorption 7 Resistively Heated Pyrolyzer Analyze any polymers by GCMS Fast, Accurate, Reliable, Consistent Quantitate copolymers Analyze for Trace additives Deformulate samples Connects to any GC
  • 9. Pyrolysis Purge & Trap Thermal Desorption A Programmed 3 step run of this lubricating strip follows CDS Pyrolyzers can be programmed to thermally extract additives BEFORE analyzing for polymers 9
  • 10. Pyrolysis Purge & Trap Thermal Desorption UV light stabilizer 10
  • 11. Pyrolysis Purge & Trap Thermal Desorption 5000 Series 11 5000 Injection port mounted 5150 Easy on/off sample line connection 5200 Pyrolysis with built in analytical trap for reactant gas pyrolysis • Heating up to 1400°C • Programmable heat rates to 20,000°C/sec • Includes Evolved Gas and Thermal Desorption capability • All systems can have 8 unique temperature runs • Connects to any model GC
  • 12. Pyrolysis Purge & Trap Thermal Desorption 12 Pyroprobe Autosamplers Carousel Pyrolysis coil Trapping zone Cryogenics 5250T Trapping Version 5250 Non-Trapping
  • 13. Pyrolysis Purge & Trap Thermal Desorption Analyze Biomass, Oils and Coal And experiment with Catalysts with our New Pyrolysis Micro Reactor 13
  • 14. Pyrolysis Purge & Trap Thermal Desorption High Pressure Pyrolysis with Catalytic Reactor • Sample can be pyrolyzed up to 1400°C • Vary pyrolysis Pressure up to 500 PSI 14 • Designed to simulate reactor conditions • Pyrolyze in carrier gas or in a reactive gas • Test the catalyst on biomass, coal, or oils • Reacted sample is automatically sent direct to your GCMS for analysis • Pyrolyzed sample flows through heated catalyst reactor (to 800°C)
  • 15. Pyrolysis Purge & Trap Thermal Desorption 15 High Pressure Pyrolysis with Reactor Reactor Reactor on-line Valve Back Pressure Regulator Pyroprobe
  • 16. Pyrolysis Purge & Trap Thermal Desorption 16 High Pressure Pyrolysis with Reactor Reactor Catalyst tube Reactor valve (manual) Pyroprobe valve (automatic)
  • 17. Pyrolysis Purge & Trap Thermal Desorption 17 5200HPR Pyrolysis Microreactor Flow Path
  • 18. Pyrolysis Purge & Trap Thermal Desorption 18 5200HPR Pyrolysis Microreactor Flow Path Carrier Gas
  • 19. Pyrolysis Purge & Trap Thermal Desorption 19 Wood Pyrolyzed in He & H₂ through Pt Reactor Pyrolyzed in He at 650°C Pyrolyzed in H₂ at 300 PSI through reactor Pyrolyzed in H₂ at 400 PSI through reactor
  • 20. Pyrolysis Purge & Trap Thermal Desorption NEW 5500 Fixed Gas Analyzer 20 • Analyze for Fixed Gases that pass through the Analytical Trap • Pre-programmed for H2, CO, CO2, CH4, H2O, C2H2, C2H4 • A True Plug & Play Analyzer for any CDS Trapping Pyrolyzer • Includes an Industry Standard Chromatography Software Package
  • 21. Pyrolysis Purge & Trap Thermal Desorption Environmental 21 • Air – TO-1/2 – TO-17 • CW Agent Monitoring • Product Emissions • Water • Solids ● Purge & Trap – Trace VOC’s in water & waste water, soils ● Thermal Desorption – Monitor for trace air pollutants • Water – EPA 624, 524.2/3 • Soil/Waste – SW 846 8260 8021 5030 5035
  • 22. Pyrolysis Purge & Trap Thermal Desorption Thermal Desorption 22 CDS 9350 with Purge & Trap accessory on your favorite GC
  • 24. Pyrolysis Purge & Trap Thermal Desorption Ambient Air Monitoring (TO-17) 65 component mixture 1. Propylene 2. Dichlorodifluoro methane 3. Chloromethane 4. Vinyl chloride . . . . 64. 1,2,4-Trichloro Benzene 65. Hexachlorobutadiene 24 Sorbent Tubes Column: CP-Select 624Column: CP-Select 624
  • 25. Pyrolysis Purge & Trap Thermal Desorption CW Agent Run 25
  • 26. Pyrolysis Purge & Trap Thermal Desorption PAHs in Soil • 0.5 grams of soil thermally extracted at 325ºC – Empty TD tube – Pre-dry sample or Dry Tube – 1 ppm standard (~ 0.5 ug) Phenanthene Fluoranthene & Pyrene Benzanthracene & Chrysene Benzo (a) Pyrene Thermal Extraction 26
  • 27. Pyrolysis Purge & Trap Thermal Desorption 27 Dynatherm Thermal Desorption Benefits • Focusing tube allows 100% of absorbed compounds to be transferred to GC; No GC Split Needed • No peltier or cryo cooling needed – Lower cost of ownership – Eliminates H2O problems w/ dry purge – Peltiers may freeze with high moisture samples • No Special Dry gas needed • Sensitivity to sub PPT • Simple flow path increases reliability
  • 28. Pyrolysis Purge & Trap Thermal Desorption NEW Soil/Water PT Autosampler 28 • 72 Position pick & place Autosampler • Water capability –Moves vial to water station • Soil Capability –Moves vial to soil Heater with magnetic stirrer • Internal Standard addition
  • 29. Pyrolysis Purge & Trap Thermal Desorption NEW Soil/Water PT Autosampler 29 • System prepared blanks (Water only) • Programmable rinse cycles • REPLACE YOUR AGING ARCHONS! • Compatible with any PT Concentrator
  • 30. Pyrolysis Purge & Trap Thermal Desorption Water Analysis: EPA Method 524.2 30 Gases
  • 31. Pyrolysis Purge & Trap Thermal Desorption 7300/7400 Advantages 31 • Reliable, Durable and Reproducible • Low cost advantage • Soils (Solids) and waters • Internal standard addition • What more do you the customer really need?
  • 32. Pyrolysis Purge & Trap Thermal Desorption NEW 7500 Thermal Desorption Autosampler 32 • Ability for the user to change between TD tubes for air and VOA vials for soil and/or water analysis • Pick and Place robotic arm • 72 position autosampler, with 3 removable trays • Leak Checking • Ability to desorb other manufacturers’ tubes (consult factory) • Automated IS Addition (optional) • Sample Saver (optional) • Compatible with the Dynatherm 9300 Series • Compatible with the Purge & Trap 7000 E and most standard/commercial P&T systems
  • 33. Pyrolysis Purge & Trap Thermal Desorption CDS Analytical - Your Partner in Sample Preparation for GCMS 33

Editor's Notes

  1. Benzophenone is used to prevent ultraviolet light from damaging scents and colors in products such as perfumes and soaps. This allows the manufacturer to package the product in clear glass or plastic. Without it, opaque or dark packaging would be used. It can also be added to the plastic packaging as a UV blocker.