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FAST GC WITH PID & FUV DETECTORS IN FIELD 
        ENVIRONMENTAL ANALYSES
        ENVIRONMENTAL ANALYSES

    Dr. Jack Driscoll & David Walsh
    Dr Jack Driscoll & David Walsh
   PID Analyzers, LLC, Sandwich, MA
              Booth #461
                   h 6
                   &

          Dr. Phillip Smith
          Dr. Phillip Smith
     OSHA Labs, Salt Lake City, UT
INTRODUCTION
• Field environmental labs are expected to
  Field environmental labs are expected to 
  Field environmental labs are 
  provide  rapid sample turnaround.  One 
  potential improvement is to utilize faster GC 
  potential improvement is to utilize faster GC
  columns in a portable GC like the PID 
  Analyzers Model GC312
  Analyzers Model GC312
• We are evaluating several types of columns & 
  detectors to provide faster and more accurate 
  detectors to provide faster and more accurate 
  detectors to provide faster and more accurate
  analyses in the field.
Types of Samples
                yp    f    p
•   BTEX
•   Chlorinated HC (TCA, TCE, PERC, MeCl2…)
    Chlorinated HC (TCA TCE PERC MeCl2 )
•   Gasoline HC’s
•   Solvents
• ===============================
• Columns selected‐ Thick film MS Cap (0.53) &  a Gas Pro 
  Columns selected‐ Thick film MS Cap (0.53
  PLOT (0.32
  PLOT (0.32)
• ===============================
• Pesticides & PCB’s‐ not considered here
  Pesticides & PCB’s‐
• Better with short (5‐10M) thin film capillary column
  Better with short (5‐
                    (      )            p     y
DETECTORS_ PID & FUV
   DETECTORS PID & FUV
Photoionization   Far UV Ansorbance
                  Far UV 
                  Far UV Ansorbance
Comparison of PLOT & Thick Film 
             Columns
                l
• Compare PLOT to Thick Film columns for
  Compare PLOT to Thick Film columns for 
  speed for C1‐C6 anes & enes
  speed for C1‐C6 anes & enes
• What are the advantages/disadvantages of
  What are the advantages/disadvantages of 
  each?
• A
  Any advantages of resistively heated 
       d           f i i l h         d
  columns?
  Heatup/cool down? Power utilized?
  Heatup/cool down? Power utilized?
• Advantages e.g comparison of sensitiviity
  Advantages e.g comparison of sensitiviity
          g     g    p                    y
GC312
Portable GC‐
Portable GC
Portable GC‐312                   Features
                     •   Battery operated –
                         Battery operated – 8 hours
                     •   Has external charger or
                         Has external charger or 
                         power from car battery
                     •   Carrier gas supply‐
                         Carrier gas supply‐ > 15 
                         hours
                         hours
                     •   1 or 2 Detectors
                     •   PID FID TCD Far UV FPD (S
                         PID, FID, TCD, Far UV, FPD (S 
                         or P)
                     •   Temperature Programming‐
                         Temperature Programming‐
                         NEW
GC Schematic
GC Schematic




     Focus is on the column/oven

     Small or no oven (direct heating of
     column) provides rapid temperature
     p g
     programming and faster analyses
                 g                y
Packed vs
Packed 
Packed vs Capillary


            Note the improved
            separation of BTX on
            capillary vs packed. The
            disadvantage is the
            analysis time is much
            longer.
            longer.

            Fast GC provides better
            separation & detection
            limits in a much shorter
            time period
Our Definitions
                     Our Definitions
•    #1 What is a FAST GC?
•    A FAST GC has a low mass or resistively heated column that
                  h     l                i ti l h t d l         th t
     can be heated and/or cooled faster than a conventional oven
•    Conditions-
     Conditions-
•    Improved heating efficiency is a must for battery operated GCs
•    Fast GC – run times in 5- 10 minutes instead of 20-30 minutes
                              5-                       20-
•    #2 What is a FAST GC column?
•    Depends on the application; two examples are:
    1. A 15m x 0.32 mm ID, PLOT that is resistively heated & can be
     cooled faster since it has a very small thermal mass
    2. A thick film (5-10 ) 7.5-30 M capillary column that can
                    (5-      7.5-
     separate gases & Solvents
FAST GC
              FAST GC‐Advantages
              FAST GC‐
•   Advantages of FAST GC
             g
•   Reduced run times 
•   Increased sample throughput 
•   Faster turnaround of results
•   Improved signal to noise ratio
•   Improved detection limits 
•   Wider range of analytes
    Wider range of analytes
•   More samples means a more accurate assessment of the site
    More samples means a more accurate assessment of the site 
•   Disadvantages of FAST GC
•   Minimal
Resistively Heated Column or Low 
            Mass Oven
Comparison of Oven Cool Down 
                                  times
                     120
                               Cool down times resistive (blue) & Low mass (red) ovens

                     100



                      80
   n Temperature C




                      60
                                                                                             Series1
Oven




                                                                                             Series2
                      40



                      20



                      0
                           0      1           2            3          4         5        6
                                                     Cool down min.
                                                     Cool down min
C1 to C6 Alkanes w FUV on 0.32 mm thick 
C1 to C6 Alkanes
            (5   film Capillary
            (  f l       ll
PLOT Column (15M 00.32 mm)with TP
PLOT Column (15M 00.32 mm)with TP
PLOT Column 
 (30M 00.32 
 (30M 00 32
mm)with TP
    )
Alkanes & BTEX on 7u MXT1 w PID
        & BTEX on 7u MXT1 w PID
Differences Between TF Cap and PLOT for 
                 C1‐C6 HC
• Main differences are for C1‐C3 HC
  Main differences are for C1‐C3 HC
                           C1
  – Separation of CH4 & C2H6‐ better on PLOT
  – Separation of C2H6 & C2H4‐ better on PLOT
    Separation of C     &C     better on PLOT
  – Separation of C3H8 & C3H6‐ better on PLOT
    Separation of C     & C
  – El ti
    Elution of  C4 t C6 HC – much shorter on TFC
             f C to C HC 
                        HC –    h h t        TFC
Comparison of PLOT to Wide Bore Thick 
               Film Cap sensitivity
                il          ii i
WCOT Sensitivity Thick Film 7u x 0.53 mm x 7.5M; 15 cc &  35C; PID 0.2 cc inj. X100
 Compound          Run            PH
C2H4 25 ppm Avg             3306 cts/ppm
        pp
H2S  25 ppm   Avg
                g           1453 cts/ppm
                                    /pp
Gaspro Sensitivity 30M x 0.32 mm; 5 cc &  35C: PID 
0.2cc  inj. X 100
C2H4  25 ppm Avg.           1519 cts/ppm 
H2S  25 ppm   Avg.          1739 cts/ppm 
SUMMARY
•   The thick film caps can provide faster analyses with excellent separations 
    for a wide variety of HC & solvents  than PLOT columns
•   The sensitivity for the thick film column for gases (C2H4 & H2S) is similar to 
    the PLOT
•   A Resistively heated column can provide faster analyses than a small GC 
    oven because of its  low mass
•   If we program from 30C to 100C, the total time for the RHC is 10 min., 
    whereas, a small oven (fan cooled) will take nearly 20 min to run this 
    program.
•   These two detectors FUV & PID can provide sub ppm or ppb detection of 
    CH4, TCA to the xylenes or decane in air, water or soil (headspace for the 
    latter two)
•   If we use a thick film 30M x 0.32 mm column that is resistively heated, we 
    can do most analyses in 10‐12 min and nearly double the volume of 
    samples done in a normal work day.

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Fast Gc With Pid %26 Fuv Pc 2011[1]

  • 1. FAST GC WITH PID & FUV DETECTORS IN FIELD  ENVIRONMENTAL ANALYSES ENVIRONMENTAL ANALYSES Dr. Jack Driscoll & David Walsh Dr Jack Driscoll & David Walsh PID Analyzers, LLC, Sandwich, MA Booth #461 h 6 & Dr. Phillip Smith Dr. Phillip Smith OSHA Labs, Salt Lake City, UT
  • 2. INTRODUCTION • Field environmental labs are expected to Field environmental labs are expected to  Field environmental labs are  provide  rapid sample turnaround.  One  potential improvement is to utilize faster GC  potential improvement is to utilize faster GC columns in a portable GC like the PID  Analyzers Model GC312 Analyzers Model GC312 • We are evaluating several types of columns &  detectors to provide faster and more accurate  detectors to provide faster and more accurate  detectors to provide faster and more accurate analyses in the field.
  • 3. Types of Samples yp f p • BTEX • Chlorinated HC (TCA, TCE, PERC, MeCl2…) Chlorinated HC (TCA TCE PERC MeCl2 ) • Gasoline HC’s • Solvents • =============================== • Columns selected‐ Thick film MS Cap (0.53) &  a Gas Pro  Columns selected‐ Thick film MS Cap (0.53 PLOT (0.32 PLOT (0.32) • =============================== • Pesticides & PCB’s‐ not considered here Pesticides & PCB’s‐ • Better with short (5‐10M) thin film capillary column Better with short (5‐ ( ) p y
  • 4. DETECTORS_ PID & FUV DETECTORS PID & FUV Photoionization Far UV Ansorbance Far UV  Far UV Ansorbance
  • 5. Comparison of PLOT & Thick Film  Columns l • Compare PLOT to Thick Film columns for Compare PLOT to Thick Film columns for  speed for C1‐C6 anes & enes speed for C1‐C6 anes & enes • What are the advantages/disadvantages of What are the advantages/disadvantages of  each? • A Any advantages of resistively heated  d f i i l h d columns? Heatup/cool down? Power utilized? Heatup/cool down? Power utilized? • Advantages e.g comparison of sensitiviity Advantages e.g comparison of sensitiviity g g p y
  • 6. GC312 Portable GC‐ Portable GC Portable GC‐312 Features • Battery operated – Battery operated – 8 hours • Has external charger or Has external charger or  power from car battery • Carrier gas supply‐ Carrier gas supply‐ > 15  hours hours • 1 or 2 Detectors • PID FID TCD Far UV FPD (S PID, FID, TCD, Far UV, FPD (S  or P) • Temperature Programming‐ Temperature Programming‐ NEW
  • 7. GC Schematic GC Schematic Focus is on the column/oven Small or no oven (direct heating of column) provides rapid temperature p g programming and faster analyses g y
  • 8. Packed vs Packed  Packed vs Capillary Note the improved separation of BTX on capillary vs packed. The disadvantage is the analysis time is much longer. longer. Fast GC provides better separation & detection limits in a much shorter time period
  • 9. Our Definitions Our Definitions • #1 What is a FAST GC? • A FAST GC has a low mass or resistively heated column that h l i ti l h t d l th t can be heated and/or cooled faster than a conventional oven • Conditions- Conditions- • Improved heating efficiency is a must for battery operated GCs • Fast GC – run times in 5- 10 minutes instead of 20-30 minutes 5- 20- • #2 What is a FAST GC column? • Depends on the application; two examples are: 1. A 15m x 0.32 mm ID, PLOT that is resistively heated & can be cooled faster since it has a very small thermal mass 2. A thick film (5-10 ) 7.5-30 M capillary column that can (5- 7.5- separate gases & Solvents
  • 10. FAST GC FAST GC‐Advantages FAST GC‐ • Advantages of FAST GC g • Reduced run times  • Increased sample throughput  • Faster turnaround of results • Improved signal to noise ratio • Improved detection limits  • Wider range of analytes Wider range of analytes • More samples means a more accurate assessment of the site More samples means a more accurate assessment of the site  • Disadvantages of FAST GC • Minimal
  • 12. Comparison of Oven Cool Down  times 120 Cool down times resistive (blue) & Low mass (red) ovens 100 80 n Temperature C 60 Series1 Oven Series2 40 20 0 0 1 2 3 4 5 6 Cool down min. Cool down min
  • 14. PLOT Column (15M 00.32 mm)with TP PLOT Column (15M 00.32 mm)with TP
  • 15. PLOT Column  (30M 00.32  (30M 00 32 mm)with TP )
  • 16. Alkanes & BTEX on 7u MXT1 w PID & BTEX on 7u MXT1 w PID
  • 17. Differences Between TF Cap and PLOT for  C1‐C6 HC • Main differences are for C1‐C3 HC Main differences are for C1‐C3 HC C1 – Separation of CH4 & C2H6‐ better on PLOT – Separation of C2H6 & C2H4‐ better on PLOT Separation of C &C better on PLOT – Separation of C3H8 & C3H6‐ better on PLOT Separation of C & C – El ti Elution of  C4 t C6 HC – much shorter on TFC f C to C HC  HC – h h t TFC
  • 18. Comparison of PLOT to Wide Bore Thick  Film Cap sensitivity il ii i WCOT Sensitivity Thick Film 7u x 0.53 mm x 7.5M; 15 cc &  35C; PID 0.2 cc inj. X100 Compound Run PH C2H4 25 ppm Avg 3306 cts/ppm pp H2S  25 ppm Avg g 1453 cts/ppm /pp Gaspro Sensitivity 30M x 0.32 mm; 5 cc &  35C: PID  0.2cc  inj. X 100 C2H4  25 ppm Avg. 1519 cts/ppm  H2S  25 ppm Avg. 1739 cts/ppm 
  • 19. SUMMARY • The thick film caps can provide faster analyses with excellent separations  for a wide variety of HC & solvents  than PLOT columns • The sensitivity for the thick film column for gases (C2H4 & H2S) is similar to  the PLOT • A Resistively heated column can provide faster analyses than a small GC  oven because of its  low mass • If we program from 30C to 100C, the total time for the RHC is 10 min.,  whereas, a small oven (fan cooled) will take nearly 20 min to run this  program. • These two detectors FUV & PID can provide sub ppm or ppb detection of  CH4, TCA to the xylenes or decane in air, water or soil (headspace for the  latter two) • If we use a thick film 30M x 0.32 mm column that is resistively heated, we  can do most analyses in 10‐12 min and nearly double the volume of  samples done in a normal work day.