Agilent Technologies, Inc. · NYSE:A

Agilent Technologies — Technical Presentation (October 2017)

34 slides from Agilent Technologies's technical presentation, Oct 24, 2017

  1. Slide 1: The Future of Environmental Analysis by GC/MS

    The Future of Environmental Analysis by GC/MS: Combining New Deactivation Chemistries, Microfluidics, and Precision Pneumatics Agilent Intuvo 9000 GC Matthew Giardina, Ph.D. October 24, 2017 1

  2. Slide 2: Outline

    Outline • Brief review of the Intuvo flowpath • Guard chip modes of operation • Applying guard chip modes of operation to environmental analysis 2

  3. Slide 3: Intuvo 9000 GC Flow Path

    Intuvo 9000 GC Flow Path Modular Intuvo flow chips Disposable Guard chip Ferrule-free click-and- run connections No-trim column Direct heating 3

  4. Slide 4: Intuvo 9000 GC Flow Path

    Intuvo 9000 GC Flow Path guard chip Inlet flow chip guard chip heater 4

  5. Slide 5: Intuvo 9000 GC Flow Path – Guard Chip

    Intuvo 9000 GC Flow Path – Guard Chip Thermally conductive proprietary alloy Intuvo ultra inert treatment Intuvo Flow Chip cross section High purity Carrier silica channel gas 5

  6. Slide 6: Intuvo 9000 GC Pneumatics

    Intuvo 9000 GC Pneumatics Microfluidic-enabled 6th generation EPC modules. TPH Analysis: 250 C/min and 10 mL/min 6

  7. Slide 7: What is the guard chip trapping?

    What is the guard chip is trapping? Guard chip 40 C isothermal Guard chip 350 C isothermal 7

  8. Slide 8: What is the guard chip trapping?

    What is the guard chip is trapping? Guard chip 40 C isothermal Guard chip 350 C isothermal 8

  9. Slide 9: What is the guard chip trapping?

    What is the guard chip is trapping? Guard chip 40 C isothermal Pass Through Intermediate Trapped 9

  10. Slide 10: What about ramping the guard chip temperature?

    What about ramping the guard chip temperature? Guard chip following the column temperature program 10

  11. Slide 11: What about ramping the guard chip temperature?

    What about ramping the guard chip temperature? Isothermal guard chip 350 C - Peak broadening for some compounds - Better peak shape ramping guard chip 11

  12. Slide 12: What about pulsing the guard chip temperature?

    What about pulsing the guard chip temperature? Rapid guard chip heating and cooling 400 350 300 Temperature (C) 250 Oven Program 200 Guard Chip Program 150 100 50 0 0 5 10 15 20 Run Time (min) 12

  13. Slide 13: How do the peak area and height compare?

    How do the peak area and height compare? ∎ Guard Chip Fast Pulse (300 C/min) ∎ Guard Chip Follow Column Ramp (100 C/min) ∎ Guard Chip Isothermal (350 C) 20 16 Millions Millions 18 14 16 12 14 10 12 Peak Height Peak Area 10 8 8 6 6 4 4 2 2 0 0 C10 C12 C14 C16 C18 C20 C22 C24 C26 C28 C30 C32 C34 C3

  14. Slide 14: How selective is guard chip pulsing?

    How selective is guard chip pulsing? C10 C12 C14 C16 Pulse Guard Chip to 100 C 5.4 5.6 5.8 6 6.2 6.4 6.6 6.8 7 Retention Time (min) C18 Pulse Guard Chip to 110  C Pulse Guard Chip to 120 C Pulse Guard Chip to 125C Pulse Guard Chip to 130 C C20 14

  15. Slide 15: How selective is guard chip pulsing?

    How selective is guard chip pulsing? Pulsed guard chip to endpoints from 100 to 305 C 1.00 0.90 0.80 C18 C20 0.70 C22 Normalized Peak Area C24 0.60 C26 0.50 C28 C30 0.40 C32 C34 0.30 C36 0.20 C38 C40 0.10 0.00 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 2

  16. Slide 16: How selective is guard chip pulsing?

    How selective is guard chip pulsing? Pulsed guard chip to endpoints from 100 to 305 C T = 29.2 C Boiling point resolution about 30C at (~4 carbon units) 300 C/min T = 28.7 C (~3 carbon units) Distinguish between 2 to 4 carbon units T = 28.3 C depending on boiling point (~2 carbon units) 16

  17. Slide 17: Guard chip pulsing selectivity

    Guard chip pulsing selectivity What is gained with boiling point selectivity of the guard chip? I. Can be used trap heavy matrix on the guard chip while passing analytes to the column. II. In combination with post-column backflush can provide more efficient use of time and prevent high boilers from

  18. Slide 18: I. Can be used to trap heavy matrix

    I. Can be used to trap heavy matrix 350 Injection of 1 L 300 250 Temperature (C) 200 Oven Program 150 Guard Chip Program Trapped on guard chip 100 50 0 0 5 10 15 20 Run Time (min) 400 Injection Blank 350 300 Released from Temperature (C) 250 guard chip 200 Oven Program 150 Guard Chip Program 100

  19. Slide 19: I. Can be used to trap heavy matrix

    I. Can be used to trap heavy matrix Semivolatile Standard Indeno[1,2,3-cd]pyrene Benzo[g,h,i]perylene C22H12 C22H12 EIC 276 Soil Extract Likely PAH Isomers C24H14 Indeno[1,2,3-cd]pyrene C22H12 Benzo[g,h,i]perylene C22H12 EIC 276 EIC 302 19

  20. Slide 20: I. Can be used to trap heavy matrix

    I. Can be used to trap heavy matrix How high a temperature do you need to pulse the guard chip to release the last compounds of interest? 0.90 0.80 0.70 Relative Response (perylene-d12) 0.60 Pulse lower than 250 C 0.50 analytes are retained on the guard chip 0.40 Indeno[1,2,3-cd]pyrene 0.30 Dibenz[

  21. Slide 21: I. Can be used to trap heavy matrix

    I. Can be used to trap heavy matrix Injection of 1 L 350 300 250 Target Temperature (C) PAHs 200 Oven Program 150 Guard Chip Program Trapped on guard chip 100 50 0 0 5 10 15 20 Run Time (min) 350 Released from guard chip Injection Blank 300 250 Target PAHs Temperature (C) 200 Oven Program 150 Gua

  22. Slide 22: I. Can be used to trap heavy matrix

    I. Can be used to trap heavy matrix How can selectivity be further increased with guard chip pulsing? Guard Chip Pulse Add Short Isothermal Period 22

  23. Slide 23: Injection Blanks After Pulsing

    I. Can be used to trap heavy matrix – Injection Blanks After Pulsing Target PAHs Too short! Matrix PAHs (EIC 276) (EIC 302) Hold Time 1.5 seconds Best Compromise! ~1% carryover Hold Time 3.0 seconds Hold Time 6.0 seconds Too long! Hold Time 12.0 seconds 23

  24. Slide 24: II. Guard chip pulsing with backflush

    II. Guard chip pulsing with backflush Traditional Air Bath Oven Backflush EPC Inlet EPC Backflush EPC Inlet EPC Vent ~2 psi ~12 psi ~10 psi ~2 psi MSD MSD Column Column Analysis Cycle Backflush Cycle 24

  25. Slide 25: II. Guard chip pulsing with backflush

    II. Guard chip pulsing with backflush Inlet EPC Intuvo Inlet EPC ~12 psi ~12 psi Backflush EPC Inlet Inlet Backflush EPC Vent ~2 psi ~2 psi Guard Guard Chip Chip Inlet Inlet Flow Flow MSD MSD Chip Chip Post-Column Post-Column Backflush Chip Backflush Chip Analysis Cycle Backflush Cycle 25

  26. Slide 26: II. Guard chip pulsing with backflush

    II. Guard chip pulsing with backflush Temperature Programs Pressure Programs 450 50 Backflush Begin Backflush End Backflush Begin Backflush End 400 45 Column 40 Column 350 35 300 Temperature (C) Guard Chip Backflush Restrictor Pressure (psi) 30 250 25 200 20 150 15 100 10 50 5 0 0 0 1 2 3 4 5 6 7 8

  27. Slide 27: II. Guard chip pulsing with backflush

    II. Guard chip pulsing with backflush Without Backflush Injection blank 1 L injection With Backflush (1 min duration) Injection blank 1 L injection C28 – C40 backflushed from guard chip 27

  28. Slide 28: II. Guard chip pulsing with backflush

    II. Guard chip pulsing with backflush Pulse guard chip backflush – 7x improvement in time required to backflush 1.2 1 Pulsed Guard Chip Traditional Post Column Backflush Normalized Area Sum (C28-C40) 0.8 0.6 0.4 Backflush Complete Backflush Complete 0.2 0 0 0.5 1 1.5 2 2.5 3 3.5 4 4.5 Backflush Dura

  29. Slide 29: II. Guard chip pulsing with backflush

    II. Guard chip pulsing with backflush Matrix backflushing pulsed guard chip with 3 second hold. Temperature Program Flow Program 450 16 Backflush 1 minute Bacflush 1 minute 400 Oven Program 14 Column Backflush Restrictor 350 Guard Chip Program 12 300 Temperature (C) 10 Flow (mL/min) 250 8 200 6 150

  30. Slide 30: II. Guard chip pulsing with backflush – matrix injections

    II. Guard chip pulsing with backflush – matrix injections Without Backflush 1 L injection Injection blank With Backflush (1 min duration) Injection blank 1 L injection backflushed from guard chip 30

  31. Slide 31: II. Guard chip pulsing with backflush

    II. Guard chip pulsing with backflush Pulse guard chip backflush – 5x improvement in time required to backflush 1.2 Traditional Backflush 1 Pulsed Guard Chip Normalized Area Sum (EIC 302) 0.8 0.6 0.4 Backflush Complete Backflush Complete 0.2 0 0 1 2 3 4 5 6 Backflush Duration (min) 31

  32. Slide 32: III. Pseudo heart-cutting – requires two GC runs

    III. Pseudo heart-cutting – requires two GC runs Sample loading and backflushing below 80 C (~C18-C10) Analyze and backflush above 200 C (C28-C40) Temperature Program Temperature Programs 160 450 140 400 Column Column 350 Temperature (C) Temperature (C) 120 100 Guard Chip 300 Guard Chip 250 80 2

  33. Slide 33: III. Pseudo heart-cutting

    III. Pseudo heart-cutting intermediate backflushed Sample cut backflushed Heart-Cut 33

  34. Slide 34: Conclusions

    Conclusions • Provided some fundamental information on how the guard chip functions in the Intuvo • How precise temperature control can be used to selectively trap compounds on the guard chip • Combining guard chip temperature pulsing with precise flow programing can be used to backflush lower volat

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