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ultra inert and high efficiency

VIEWS: 11 PAGES: 50

									         New Capillary Column Technologies to
         Make Your Analyses Fast and Simple




                                       LAR Tour
                                       2010
Page 1
Presentation outline

         • Background and terminology for faster analyses

         • High Efficiency Capillary GC Columns

         • Utility of Method Translation Software

         • Faster GC application examples

         • Ultra Inert columns for difficult analytes

         • Why testing matters

         • Ultra inert application examples




Page 2
Resolution



                  N  k  a  1
             Rs =            
                         
                  4 k 1  a 
         Efficiency    N = (gas, L, rc)   L = Length
                                             rc = column radius
         Retention     k = (T, df, rc)
                                             df = film thickness
         Selectivity   a =  (T, phase)     T = temperature


Page 3
   Impact of Efficiency, Selectivity and Retention on
                      Resolution
                            7.00
                                                      Typical Method Development Parameters
                            6.00


                            5.00
               Resolution




                            4.00                                                                                        Increase N
                                                                                                                        Increase Alpha
                            3.00                                                                                        Increase k'



                            2.00


                            1.00
                                                                       Rs = N ½/4  ( a- 1)/ a  k’/(k ’+1)
                            0.00
                                    1     2   3   4    5     6     7     8    9   10    11    12   13   14   15    16     17   18    19   20    21
         Plates:                   5000                    10000                       15000                      20000                        25000
         Alpha:                    1.10                    1.35                        1.60                       1.85                          2.1
         k’:                       2.0                      4.5                         7.0                        9.5                         12.0



Page 4
Variables for Speeding Up an Analysis



   •Stationary Phase
   •Temperature Programming
   •Shorten Column Length
   •Decrease Film Thickness
   •Decrease Internal Diameter
   •Carrier Gas: type and linear
   velocity



Page 5
Column Diameter - Theoretical Efficiency
                       Total Plates    I.D. (mm)    n/m

                5m     N ~ 112,000         0.05    23,160

               10 m    N ~ 112,000         0.10    11,580

                      High-Efficiency GC   0.18    6,660
               20 m    N ~ 112,000         0.20    5830

                                           0.25    4630

               30 m    N ~ 112,000         0.32    3660
                                           0.45    2840
         k=5
                                           0.53    2060

Page 6
Column Diameter and Capacity

                         I.D. (mm)   Capacity (ng)
                           0.05           1-2
                           0.10          6-13
                           0.18         25-55

                           0.20         35-70
Like Polarity
Phase/Solute               0.25         80-160
0.25 µm film thickness
                           0.32        110-220
                           0.45        600-800
                           0.53       1000-2000

Page 7
Column Diameter - Inlet Head Pressures (Helium)

                            I.D (mm)   Pressure (psig)
                              0.05        275-400
                              0.10         90-130

                              0.18          30-45
                              0.20          25-40

                              0.25          15-25
 30 meters
 Hydrogen pressures x 1/2
                              0.32          10-20

                              0.45           3-7
                              0.53           2-4
Page 8
DECREASE THE LENGTH

 DB-5                                                              1                                                                                                      4
 30 m
                                                                                                           2                                                          3
 0.53 mm I.D., 0.5 µm                                                                                                                                                                     5




                     .5
                    0 0          .0
                                1 0      .5
                                        1 0          .0
                                                    2 0      2 0
                                                              .5          .0
                                                                         3 0      .5
                                                                                 3 0            .0
                                                                                               4 0          .5
                                                                                                           4 0     5 0
                                                                                                                    .0          .5
                                                                                                                               5 0     .0
                                                                                                                                      6 0          .5
                                                                                                                                                  6 0          .0
                                                                                                                                                              7 0         7 0
                                                                                                                                                                           .5      .0
                                                                                                                                                                                  8 0          .5
                                                                                                                                                                                              8 0           .0
                                                                                                                                                                                                           9 0
                     .5         1.0     1.5         2.0       2.5        3.0     3.5           4.0         4.5     5.0         5.5    6.0         6.5         7.0         7.5     8.0         8.5          9.0




 DB-5                                                                                                1.          Benzene
 15 m                                                                                                2.          Toluene
 0.53 mm I.D., 0.5 µm                                                                                3.          Ethylbenzene                                     4
                                                                                                     4.          m,p-Xylene
                                                    1                                2               5.          o-Xylene                               3
                                                                                                                                                                                      5




              0 0
               .2   0 0
                     .4
                      1.00.60    0 0
                                  .8   1 0
                                        .0     .2
                                              1 0    .4
                                                    1 0
                                                        2.01.60    1 0
                                                                    .8   2 0
                                                                          .0   2 0
                                                                                .2
                                                                                           3.02.60
                                                                                         2 0
                                                                                          .4         2 0
                                                                                                      .8    3 0
                                                                                                             .0   3 0
                                                                                                                   .2    3 0
                                                                                                                           4.03.60
                                                                                                                          .4         3 0
                                                                                                                                      .8     .0
                                                                                                                                            4 0   4 0
                                                                                                                                                   .2       4 0
                                                                                                                                                             .4
                                                                                                                                                              5.0 4.60    4 0
                                                                                                                                                                           .8   5 0
                                                                                                                                                                                 .0    .2
                                                                                                                                                                                      5 0
                                                                                                                                                                                                6.0 5.60
                                                                                                                                                                                               .4
                                                                                                                                                                                              5 0            .8
                                                                                                                                                                                                            5 0




 BTEX
 Carrier: Helium, 36 cm/sec at 40°c
 Oven : 40°C for 3 min, 5°/min to 100°C

Page 9
Column Length VS Resolution and Retention:
Isothermal


          R=0.84                  R=1.16                  R=1.68
          2.29 min                4.82 min                8.73 min




          15 m                    30 m                    60 m

                     Double the plates, double the time
                     but not double the the resolution



Page 10
Combining a change in Length
with a change in Diameter


                  Decrease Length
                  Decrease Diameter
     Efficiency




                     Analysis Time

Page 11
 PHASE RATIO ()
          β= r/2 df where
               r = column radius in mm
               df = film thickness in µm

          Column Dimensions            Phase Ratio β
          30 m x 0.25 mm x 0.25 m          250
          20 m x 0.18 mm x 0.18 m          250
           Example calculation for 0.32 mm ID column
                     β = 125 mm /(2 x 0.25 m) = 250

Page 12
          Carrier Gas Considerations
          Best velocity?
            Optimal range of velocities

            Too low or high results in loss of resolution

            Balance resolution and analysis time

            Faster still works? Go faster.




Page 13
    Carrier Gas Considerations
                                 Van Deemter Curve

                     Excessive Diffusion
              1.00

                                                             He
              0.75
          h                                                   Poor Mass Transfer
              0.50
                                                             H2
              0.25
                     ūopt                                OPGV

                            10        20    30     40   50    60
                                           u (cm/sec)

Page 14
Easy Options with Method Translation Software


    Different Column Dimensions


    Same Column & Gas Type but Faster Velocities


    Switch He to H2 Carrier Gas and Try Faster Velocities


    Combination of all of the above




Page 15
      Method Translation Software

                                                    • Four translation modes

                                                                               Lock all carrier gas
                                                      – Translation only
                                                                            parameters, making the
                                                      – Best efficiency           flow rate an
                                                      – Fast analysis       independent parameter.

                                                      – None (unlock all carrier gas
                                                        parameters)




      • If translating to a different ID column, phase ratio should be maintained for the most
        reliable results
      • If there are significant differences in phase ratio, Method Translation Software can
        still be used but elution order should be confirmed.
      • Stationary phase of a new column must be the same as the original – the Method
        Translation Software cannot account for differences in selectivity.



Page 16
Method Translation Made Simple
  • Agilent Method Translation Software
    – A FREE, stand-alone software running on a PC
    – Download at: http://www.chem.agilent.com/cag/servsup/usersoft/files/GCTS.htm
    – Method Translation allows easy “tweaking” of method parameters to speed up run time.
    – It preserves relative elution order by properly scaling gas velocity and temperature
      program to maintain equivalent elution pattern.

  • Can Change
    – column dimensions (i.e. ID, column length, film thickness, or phase ratio)
    – carrier gas type (i.e. hydrogen, helium, nitrogen)
    – pneumatic set points (i.e. flow rates, head pressure, or holdup time).
    – The software then generate a translated method (new temperature program), which will
      attempt to maintain the resolution and selectivity of the original method.

  • Benefits
    - reduces method development time
    - helps assess if GC method is compatible with hardware




Page 17
CLP-Pesticides - Original “Improved” Method
0.32mm I.D., Helium Carrier Gas
                                                                                Column:   Agilent J&W DB-XLB
                                    5,66                                                  30m x 0.32mm i.d., 0.25µm
                        G   C   3    -     7   0   7       . D    \ E   C   D    2 B
                                                                                Carrier:  He, constant flow, 38 cm/s at 120°C
                    2                                                           Injector: Pulsed Splittless, 220 °C
                        3                                                                 Pulse pressure & time: 35psi for 1.15min
                                                                                          2µL, 50ppb
                                                                                Oven:     120°C for 1.17min
                                           7                     10                       120°C to 160°C at 25°/min
                                                                                          160°C to 260°C at 10°/min
                                                             9        12                  260°C to 300°C (4min) at 15°/min
          1                                                                     Detector: µ-ECD, 320°C
                                                       8          11 13                   Ar/CH4 (P5) makeup gas at 60mL/min
                                                                                                    21
                                                                              15
                                                                            14 16 18
                                4
                                                                                          19                       <16 minutes
                                                                                                                           22
                                                                                    17


                                                                                               20




      6   . 0   0           8   . 0   0            1   0    . 0   0         1   2   . 0   0         1    4   . 0   0   1   6    . 0   0




Page 19
                                                                                                                   Agilent J&W DB-XLB
                                                                                                             Column:
Final Method Used at EPA                                                                                 Carrier:
                                                                                                                   20m x 0.18mm i.d., 0.18µm
                                                                                                                   H2, constant flow, 77.3cm/s at 120°C
                                                                                                         Injector: Pulsed Splittless, 220 °C
                                                                                                                   Pulse pressure & time: 35psi for 0.5min
                                                                                                                   Flow ramp at 6.25min of 99mL/min2 to 3mL/min
                                23                                                                                 2mm i.d. liner
              G       C     8   -    3       6       7   . D       \ E     C       D   2   B
                                                                                                                   0.5µL, 50ppb
                                                                                                         Oven:     120°C for 0.49min
                                                               5                                                   120°C to 160°C at 59.4°/min
                                         3                                                          12             160°C to 260°C at 23.7°/min
                                                                           7                                       260°C to 300°C (1.69min) at 35.6°/min
                                                                                                 10
                  1                                                                            9         Detector: µ-ECD, 320°C
                                                                                           8          13           Ar/CH4 (P5) makeup gas at 60mL/min
                                                                                                                                      21
                                                                                                   11
                                                                                                                            19                           22
                                                                   6
                                                                                                             14 15
                                                                                                                 16 18
                                                         4

                                                                                                                       17

                                                                                                                                  20




2   . 5   0   3       . 0   0    3   . 5         0       4     . 0     0       4   . 5     0   5   . 0   0   5   . 5   0    6   . 0   0    6   . 5   0   7    . 0   0




Page 20
          CLP Pesticide Standard Key List

          1. TCMX                12. 4,4’ DDE
          2. Alpha BHC           13. Dieldrin
          3. Gamma BHC           14. Endrin
          4. Beta BHC            15. 4,4’ DDD
          5. Delta BHC           16. Endosulfan II
          6. Heptachlor          17. 4,4’ DDT
          7. Aldrin              18. Endrin Aldehyde
          8. Heptachlor Epoxide 19. Endosulfan Sulfate
          9. Gamma Chlordane     20. Methoxychlor
          10. Alpha Chlordane    21. Endrin Ketone
          11. Endosulfan I 22. DCB


Page 21
    Final Method Used at EPA
             2     G       C     8   -   3       3     6       7   . D         \ E     C       D       2       B


                                                                           5
                                                     3                                 7                                      12
                       1                                                                                   8        9
                                                                                                                        10
                                                                                                                               13
                                                                                                                                          DB-XLB
                                                                                                                         11                                              21
                                                                               6                                                                              19                                       22
                                                                                                                                      14 15
                                                                                                                                          16 18
                                                                   4
                                                                                                                                                    17
                                                                                                                                                                        20


                   G       C     8   -   3       3     6       7   . D         \ E     C       D       1       A
0    2   . 5   0   3       . 0   0       3       . 5       0       4       . 0     0       4   . 5         0        5   . 0   0       5   . 5       0         6    . 0   0           6    . 5      0   7    . 0   0



                                             2                 3                     5 7
                                                                                                   V       i   e    w
                                                                                                                     9 10 12
                                                                                                                         M        o   d   e     :       I n       t e    g       r   a   t i
                                                                                                                                                                                         21
                                                                                                                                                                                               o   n


                                                                                                                   8
                   1
                                                                                                                            13            DB-17ms
                                                                                                                        11                                               19

                                                                           6                                                                                                                                22
                                                                                                                                                14 16
                                                                                                                                                  15
                                                                                                                                                     17 18
                                                                       4
                                                                                                                                                                                     20



0    2   . 5   0   3       . 0   0       3       . 5       0       4       . 0     0       4   . 5         0        5   . 0   0       5   . 5       0         6    . 0       0       6    . 5      0   7    . 0   0




    Page 22
          Semi-Volatile Example-U.S EPA Method 8270
     30 m x 0.25 mm x 0.5 um DB 5.625




              4.00   6.00      8.00   10.00     12.00   14.00   16.00     18.00   20.00   22.00   24.00


     20 m 0.18 mm x 0.18 um DB 5.625




             4.00           6.00         8.00           10.00           12.00        14.00         16.00



Page 23
Application Examples – Aromatic Solvents
  • ASTM Unified aromatic solvent methods D16
    – Combines 10 ASTM aromatic methods into one
    – One method can be used for up to 16 different sample types
    – One capillary GC column replaces up to 6 different columns.

          – Due to demands for increased productivity, many QC / QA laboratories need to
            analyze large number of samples every day. Faster analysis is highly desirable for
            increased sample throughput and therefore lower cost per sample.

 1 heptane              8 1,4-dioxane      15 o-xylene          22 tridecane
 2 cyclohexane          9 undecane         16 propylbenzene     23 diethylbenzene isomer
 3 octane              10 ethylbenzene     17 p-ethyltoluene    24 diethylbenzene isomer
 4 nonane              11 p-xylene         18 m-ethyltoluene    25 n-butylbenzene
 5 benzene             12 m-xylene         19 t-butylbenzene    26 a-methylstyrene
 6 decane              13 cumene           20 s-butylbenzene    27 phenylacetylene
 7 toluene             14 dodecane         21 styrene




Page 24
    Application Examples – Aromatic Solvents
     Unified Aromatics Method 1

                                Column                    HP-INNOWax, 60m × 0.32mm × 0.50 mm
                                Carrier Gas               Helium @ 20.00 psi constant pressure mode

                                                          Split/Splitless @ 250°C
                                Inlet
                                                          100:1 split ratio

                                                          75°C (10 min); 3 °C/min to 100 °C (0 min)
                                Oven Temp
                                                          10 °C/min to 145 °C (0 min)
       1                        Detector                  FID @ 250 °C
                                Data acquisition rate     @ 20 Hz
                                Injection Size            1 L                                                                          26


              3
        2         4
                                                                                                                                   25
                          6                                                                                                      24            27
                      5             7                            11                      15   16       18 19             22 23
                                                 9             10 12          13                                    21
                                                                                    14                         20
                                                                                                      17
                                           8

5                 5           7.5                    10             12.5                 15                17.5           20                 22.5




    Page 25
     Application Examples – Aromatic Solvents
       Unified Aromatics Method 2
                                   Column                       HP-Innowax, 20 m x 0.18 mm x 0.18 m

                                   Carrier Gas                  Helium @ 33.00 psi constant pressure mode

                                                                Split/Splitless @ 250 °C
                                   Inlet
                                                                100:1 to 600:1 split ratio

                                   Oven Temp                    70 °C ( 3 min); 45 °C/min to 145 °C (1 min)
                                   Detector                     FID @ 250 °C

pA                                 Data acquisition rate        @ 50 Hz
               1
25                                 Injection Size               0.2 to 1.0 L

00

75
                   3       4                                                                                                                  23 24    26
50
                                      6
25                             5                                                                                         19     21                25
               2                                                                                                                                             27
00                                                                                                                                       22
                                                    7       9                   11                            16     18       20
                                                                         10          12           14 15
75                                                                                           13                    17
50

25
                                                        8

0
 0.5                   1                   1.5              2                    2.5              3                3.5               4                 4.5        min




     Page 26
Food/Fragrance – Method translation




Page 27
Spearmint Oil




                          17.7 min
                                   Δ -9.7 min (0.18 mm, He Carrier)



                                               (0.25 mm, He
                                               Carrier)
                                                        27.4 min


    3     8     13            18              23              28


                     Time (min)




Page 28
Spearmint Oil


                10.6 min
                              Δ -16.8 min (0.18 mm, H2
                              Carrier)



                                17.7 min
                                         Δ -9.7 min (0.18 mm, He Carrier)



                                                     (0.25 mm, He
                                                     Carrier)
                                                              27.4 min


    3     8          13             18              23              28


                           Time (min)



Page 29
Spearmint Oil – Resolution Check

                   Δ -16.8 min (0.18 mm, H2 Carrier)

                                                            10.6 min




                   Δ -9.7 min (0.18 mm, He carrier)

                                                            17.7 min




                          (0.25 mm, He Carrier)

                                                            27.4 min


          8   13                      18               23       28




Page 30
Resolution Maintained



                        Compound Resolution
          Compound      0.25 mm   0.18 mm     0.18 mm
          s
                        Helium    Helium      Hydrogen
          Sabinene
                         1.52      1.59         1.56
          β-Pinene
          α-Terpinene
                         1.61      1.73         1.86
          p-Cymene
          Speed Gain      N/A      35%          61%




Page 31
          Agilent J&W Ultra Inert Capillary GC Columns

          Raising the Bar for CONSISTENT
          Column Inertness Performance


Page 33
Section Outline
           Back ground, Evolution of capillary column QC
              Grob’s type mix, test for the 80
              “DB-5ms mix”, test for the 90s
              “UI” mix, test for today


           Value of inertness consistency


           Application examples


           Take away messages



Page 34
Grob-type Test Mix Results on Restek Rxi-5SIL ms
   pA                                 2

   35
                                                             not probative                         1. 1-Octanol
                                                       6                                           2. n-Undecane
   30
                                  1
                                           3       5                                               3. 2,6-Dimethylphenol
                                               4
   25                                                                                              4. 2,6-Dimethylaniline

                                                                             8                     5. n-Dodecane
   20
                                                                    7                              6. Naphthalene
   15                                                                                              7. 1-Decanol
                                                                                    9
                                                                                                   8. n-Tridecane
   10
                                                                                                   9. Methyl decanoate

    5
        0        1          2          3           4          5          6          7        8          9         min




    Sampler:     Agilent 7683B, 5 µL syringe (Agilent part # 5181-1273), 1.0 µL split injection, 4 ng each component
    Carrier:     Hydrogen constant pressure 37 cm/s
    Inlet:       Split/splitless; 250 ºC, 1.4 ml/min. column flow, split flow 140 ml/min.
    Liner:       Deactivated single taper w glass wool (Agilent part # 5183-4647)
    Oven:        120 ºC isothermal
    Detection:   FID at 325 ºC, 450 ml/min. air, 40 ml/min. hydrogen, 45 ml/min. nitrogen makeup




Page 35
Grob-type Test Mix Results on a DB-5ms Ultra Inert
     pA
                                      2
      35
                                                             not probative                       1. 1-Octanol
                                                                                                 2. n-Undecane
                                  1                   6                                          3. 2,6-Dimethylphenol
      30                                  3
                                                  5                                              4. 2,6-Dimethylaniline
                                              4
      25                                                                                         5. n-Dodecane
                                                                                                 6. Naphthalene
      20
                                                                          8
                                                                 7                               7. 1-Decanol
                                                                                 9               8. n-Tridecane
      15
                                                                                                 9. Methyl decanoate
      10


          5
              0            2                  4                  6                   8              10              min


    Sampler:      Agilent 7683B, 5 µL syringe (Agilent part # 5181-1273), 1.0 µL split injection, 4 ng each component
    Carrier:      Hydrogen constant pressure 37 cm/s
    Inlet:        Split/splitless; 250 ºC, 1.4 ml/min. column flow, split flow 140 ml/min.
    Liner:        Deactivated single taper w glass wool (Agilent part # 5183-4647)
    Oven:         120 ºC isothermal
    Detection:    FID at 325 ºC, 450 ml/min. air, 40 ml/min. hydrogen, 45 ml/min. nitrogen makeup




Page 36
DB-5ms test Mix on a Restek Rxi-5SIL-ms
          pA
                               1
                                        3                  more probative                        1. 2-Ethylhexanic acid
          35
                                   2
                                                      4                                          2. 1,6-Hexanediol
                                                           5                                     3. 4-Chlorophenol
          30

                                                                                                 4. Tridecane
          25                                                          6         7                5. 1-Methylnaphthalene

                                                                                        8
                                                                                                 6. 1-Undecanol
          20

                                                                                                 7. Tetradecane
          15
                                                                                                 8. Dichlorohexylamine

          10



           5

               0          2                 4             6               8                 10        min



    Sampler:       Agilent 7683B, 5 µL syringe (Agilent part # 5181-1273), 1.0 µL split injection, 4 ng each component
    Carrier:       Hydrogen constant pressure 38 cm/s
    Inlet:         Split/splitless; 250 ºC, 1.4 ml/min. column flow, split flow 100 ml/min.
    Liner:         Deactivated single taper w glass wool (Agilent part # 5183-4647)
    Oven:          125 ºC isothermal
    Detection:     FID at 320 ºC, 450 ml/min. air, 40 ml/min. hydrogen, 45 ml/min. nitrogen makeup




Page 37
DB-5ms Mix on DB5-msUI
          pA


          35
                               1
                                        3
                                                        4
                                                                more probative                 1. 2-Ethylhexanic acid
                                   2                                                           2. 1,6-Hexanediol

          30
                                                                5                              3. 4-Chlorophenol
                                                                                               4. Tridecane
          25                                                             6        7            5. 1-Methylnaphthalene

          20                                                                             8     6. 1-Undecanol
                                                                                               7. Tetradecane
          15
                                                                                               8. Dichlorohexylamine

          10


          5
               0          2                 4               6             8              10          min


    Sampler:       Agilent 7683B, 5 µL syringe (Agilent part # 5181-1273), 1.0 µL split injection, 4 ng each component
    Carrier:       Hydrogen constant pressure 38 cm/s
    Inlet:         Split/splitless; 250 ºC, 1.4 ml/min. column flow, split flow 100 ml/min.
    Liner:         Deactivated single taper w glass wool (Agilent part # 5183-4647)
    Oven:          125 ºC isothermal
    Detection:     FID at 320 ºC, 450 ml/min. air, 40 ml/min. hydrogen, 45 ml/min. nitrogen makeup




Page 38
UI Mix Results on Restek Rxi-5SIL ms

     pA                                                            5     fully probative                                    1.      1-Propionic acid
     20                                       3                                                                             2.      1-Octene
                                         2
                                                         4                                                                  3.      n-Octane
     18
                                                                                        8                                   4       4-Picoline
     16
                                 1                                                                                          5.      n-Nonane

     14
                                                                                                                   11       6.      Trimethyl phosphate
                                                                                                        10                  7.      1,2-Pentanediol
                                                                                                9
     12
                                                                                                                            8.      n-Propylbenzene
     10                                                                                                                     9.      1-Heptanol
                                                                                7                                           10. 3-Octanone
          8
                                                                           6                                                11. n-Decane
          6
              0                      2                       4                      6                     8                         10      min

              Sampler:     Agilent 7683B, 0.5 µL syringe (Agilent part # 5188-5246), 0.02 µL split injection
              Carrier:     Hydrogen constant pressure, 38 cm/s
              Inlet:       Split/splitless; 250 ºC, 1.4 ml/min. column flow, split flow 900 ml/min., gas saver flow 75 ml/min. on
                           at 2.0 min.
              Liner:       Deactivated single taper w glass wool (Agilent part # 5183-4647)
              Oven:        65 ºC isothermal
              Detection:   FID at 325 ºC, 450 ml/min. air, 40 ml/min. hydrogen, 45 ml/min., nitrogen makeup




Page 39
UI Mix Results on Varian VF-5 ms
  pA

   20
                                                                    5
                                      2
                                            3                               fully probative                               1.
                                                                                                                          2.
                                                                                                                                    1-Propionic acid
                                                                                                                                    1-Octene
   18                                                  4

                                                                                          8
                                                                                                                          3.        n-Octane
   16
                                                                                                                          4         4-Picoline
                            1
                                                                                                                          5.        n-Nonane
   14                                                                                                                11
                                                                                                                          6.        Trimethyl phosphate
                                                                                                             10
   12                                                                                              9                      7.        1,2-Pentanediol
                                                                                                                          8.        n-Propylbenzene
   10

                                                                                                                          9.        1-Heptanol
                                                                                    7
    8                                                                                                                     10. 3-Octanone
                                                                            6
                                                                                                                          11. n-Decane
        0                       2                     4                         6                      8                       10        min



            Sampler:     Agilent 7683B, 0.5 µL syringe (Agilent part # 5188-5246), 0.02 µL split injection
            Carrier:     Hydrogen constant pressure, 38 cm/s
            Inlet:       Split/splitless; 250 ºC, 1.4 ml/min. column flow, split flow 900 ml/min., gas saver flow 75 ml/min. on
                         at 2.0 min.
            Liner:       Deactivated single taper w glass wool (Agilent part # 5183-4647)
            Oven:        65 ºC isothermal
            Detection:   FID at 325 ºC, 450 ml/min. air, 40 ml/min. hydrogen, 45 ml/min., nitrogen makeup




Page 40
UI Mix Results on GL Science 5MS/SIL
     pA
                                                                 5                                                          1.      1-Propionic acid
      22                                                                 fully probative                                    2.      1-Octene
                                         2
      20                                      3                                                                             3.      n-Octane
                                                                                  8
                                                                                                                            4       4-Picoline
      18                                              4
                                                                                                                            5.      n-Nonane
      16                                                                                                  11
                                                                                                                            6.      Trimethyl phosphate
      14                         1                                                                                          7.      1,2-Pentanediol
                                                                                                 10
                                                                                          9
      12
                                                                                                                            8.      n-Propylbenzene
                                                                                                                            9.      1-Heptanol
      10
                                                                             7                                              10. 3-Octanone
                                                                        6
          8
                                                                                                                            11. n-Decane
          6

               0                     2                      4                         6                    8                         10        min

              Sampler:     Agilent 7683B, 0.5 µL syringe (Agilent part # 5188-5246), 0.02 µL split injection
              Carrier:     Hydrogen constant pressure, 38 cm/s
              Inlet:       Split/splitless; 250 ºC, 1.4 ml/min. column flow, split flow 900 ml/min., gas saver flow 75 ml/min. on
                           at 2.0 min.
              Liner:       Deactivated single taper w glass wool (Agilent part # 5183-4647)
              Oven:        65 ºC isothermal
              Detection:   FID at 325 ºC, 450 ml/min. air, 40 ml/min. hydrogen, 45 ml/min., nitrogen makeup




Page 41
UI Mix Results on an Agilent J&W DB-5ms Ultra Inert
                                                                                                                         1.        1-Propionic acid
  pA
                                    2
                                                  4          5        fully probative                                    2.        1-Octene
  35                                       3                                                                             3.        n-Octane
                                                                                                                         4         4-Picoline
  30
                                                                                   8                                     5.        n-Nonane

  25                                                                                                                     6.        Trimethyl phosphate
                           1                                                                                   11        7.        1,2-Pentanediol
                                                                                           9        10
  20
                                                                                                                         8.        n-Propylbenzene
                                                                          7                                              9.        1-Heptanol
  15
                                                                                                                         10. 3-Octanone
                                                                     6
  10                                                                                                                     11. n-Decane

   5
       0                       2                      4                       6                      8                        10        min
           Sampler:     Agilent 7683B, 0.5 µL syringe (Agilent part # 5188-5246), 0.02 µL split injection
           Carrier:     Hydrogen constant pressure, 38 cm/s
           Inlet:       Split/splitless; 250 ºC, 1.4 ml/min. column flow, split flow 900 ml/min., gas saver flow 75 ml/min. on
                        at 2.0 min.
           Liner:       Deactivated single taper w glass wool (Agilent part # 5183-4647)
           Oven:        65 ºC isothermal
           Detection:   FID at 325 ºC, 450 ml/min. air, 40 ml/min. hydrogen, 45 ml/min., nitrogen makeup




Page 42
Test Mix Observations

           Grob’s style mix not probative for inertness


           DB-5ms text mix good test for the 90s


           UI mix probes inertness and differentiates an excellent
            column from a mediocre one

           Well designed test mix uncovers potential adsorption of
            acid and base analytes and raises the bar in inertness QC


           Same selectivity as corresponding DB-5ms, HP-5ms,DB-1ms or HP-
            1ms columns


Page 45
 Why Does this new Testing Matter?


• The most consistent column inertness performance

         Features                     Advantages                                 Benefits
   Unique QC testing      Consistent column inertness
                                                            More predictable and reliable results
   procedure              performance
                          Better peak shape
                          Greater signal and noise ratios   More accurate peak identification, more accurate
   Highest degree of
                          Minimum compound loss or          quantification
   column inertness
                          degradation
                          Extended column lifetimes         Reduced costs and instrument downtime
   Support of 0.18mm ID
                          Higher sample througput           Analyze more samples in less time
   configuration


• Critical for analysis of active compounds, trace level samples, and
  screening of unknown samples

                             Improved sensitivity and performance
                       higher productivity – the right answer the first time
                                  with the utmost confidence

Page 46
Ultra Inert Application Examples

           Semi Volatile Analysis


           Brominated Fire Retardants


           Pesticides in Orange Oil


           PAHs




Page 47
     Ultra Inert Application - Semi Volatile Analysis
                                        GC :         Agilent 6890N/5975B MSD
                                        Sampler :    Agilent 7683B, 5.0 µL syringe (Agilent part # 5188-5246), 1.0 µL splitless injection, 5 ng on
                                                     column
                                        Carrier:     Helium constant flow 30 cm/s
                                        Inlet:       Split/splitless; 260% C, 53.7 ml/min. total flow, purge flow 50 ml/min. on at 0.5 min., gas saver
1.   N-nitrosodimethylamine                          off
2.   Aniline                            Inlet Liner: Deactivated single taper w glass wool (Agilent part # 5183-4647)
3.   1,4 dichlorobenzene-D4             Column:      Agilent J &W DB-5ms Ultra Inert 30m x 0.25mm x 0.25µm (Agilent part # 122-5532UI)
4.   Benzoic acid                       Oven:        40% C (1 min) to 100%C (15% C/min), 10% C to 210% C (1 min), 5% C/min. to 310% C (8 min)
                                        Detection: MSD source at 300% C, quadrupole at 180% C, transfer line at 290% C, scan range 50-550 AMU
5.   Naphthalene- D8
6.   Acenapthene-D10
7.   2,4-dinitrophenol                                       6                                                                         16   17
                                                      5                          11    12
8.   4-nitrophenol
9.   2-methyl-4,6-dinitrophenol
10. pentachlorophenol                                                                                                                        18
                                        3                                                                          14
11. 4-aminobiphenyl
                                    2
12. Penanthrene-D10
13. Benzidine
14. Chrysene-D12
15. 3,3’-dichlorobenzidine                                                                          13                  15
16. Benzo [b] fluoroanthene                                                       10

17. Benzo [k] fluoroanthene
18. Perylene-D12

                                                                             9
                         1                                           8

                                               4                 7




                             5.00             10.00                  15.00                  20.00          25.00               30.00




Page 48
“Large Mix” 5 ng on Column AccuStandard 8270 Mixes 1,2,3,4a,4b,5 &6 (93
Compounds) Select compound highlighted

     1. n-Nitrosodimethylamine           GC/MSD Conditions

     2. 2-methyl pyridine                Column:            Agilent J&W DB-5ms Ultra Inert 30 m x 0.25 mm x 0.25 µm part # 122-5532UI
                                         Carrier:           He 30 cm/sec constant flow
     3. Benzidene
                                         Oven:              40% C (1min) to 100 % C (15 % C/min), 10 % C /min to 210% C (1min), 5 % C/min to 310% C (8
     4. Flouranthene                     min)
                                         Inlet:             splitless 260 % C purge flow 50 % ml/min at 0.5 min, gas saver 80 ml/min on at 1 minute
     5. Benzo (g,h,i) perylene
                                         MSD:               transfer line 290 % C, source 300 % C, quad 180 % C




                                                                                     4
                                                                                                                                             5




                           2

                                                                                    3
                     1


                    5.00         10.00              15.00                 20.00              25.00                30.00           35.00




Page 49
Pesticides and Fire Retardants (US EPA 527)
                                    GC/MSD Conditions
1.    1,2-Dimethyl-2-nitrobenzene
                                    Sample:                 Pesticide/PBDE standards 1 ng with 5ng IS/SS on column
2.    Acenaphthalene-D10
3.    Dimethoate                    Column:                 Agilent J&WDB-5ms Ultra Inert 30m x 0.25mm x 0.25um (Agilent part # 122-5532UI)
4.    Atrazine
5.    Propazine                     Carrier:                Helium 52cm/sec, constant flow
6.    Anthracene-D10                Oven:                   60oC (1min) to 210OC (25O/min), 20OC/min to 310OC (3 min)
7.    Vinclozoline
8.    Prometryne                    Injection:              Splitless, 250oC, purge flow 50ml/min at 1min, gas saver 80ml/min on at 3 min
9.    Bromacil                      MSD:                    Transfer Line 290OC , Source 300OC, Quad 180OC
10.   Malathion
11.   Thiazopyr
12.   Dursban                   1                2                            6                                                           23      25                           30

13.   Benthiocarb
14.   Parathion
15.   Terbus sulfone
16.   Bioallethrin                                                                        9-14
17.   Oxychlordane
                                                                                                                                                       27
18.   Fenamiphos
                                                                                      8
19.   Nitrophen                                                                                          17
20.   Norflurazone                                                                                                                           24
                                                                                                                                                                                32
21.   Kepone
                                                                                  7                                                               26
22.   Hexazinone
                                                                                                                                                                    28   29
23.   Triphenyl phosphate
                                                                                                 15,16                          20
24.   Bifenthrin
25.   Chrysene-D12                                                 3
                                                                                                                                 21                                                33
26.   BDE-47                                                                                                                                                                            34
27.   Mirex                                                                                                   18
28.   BDE-100                                                          4,5
                                                                                                                                                                              31

29.   BDE-99                                                                                                               19
30.   Perylene-D12
31.   Fenvalerate                                                                                                                    22

32.   Esfenvalerate
33.   Hexabromobiphenyl
34.   BDE-153
                             5.00   6.00             7.00              8.00               9.00                     10.00                  11.00             12.00             13.00




Page 50
Pesticides in Orange Oil
          Analysis was carried out on the Agilent 7890A/5975 GC/MS or 7890A/7000 A (Prototype) GC/MS/MS equipped with either a 7683 or 7683B
          Series ALS, split/splitless injection port and triple-axis detector. An Agilent J&W DB-5ms Ultra Inert 15 m x 0.25 mm x 0.25 um column
          (Agilent part # 122-5512UI) was used. The initial GC oven temperature was 70°C, which was held for 0.67 minutes. The oven was then
          ramped by 75°C/minute to 150°C, held for 0 minutes and ramped by 9°C/minute to 200°C and held for 0 minutes before ramping by
          24°C/minute to 280°C and holding for 3 minutes. A six-minute post-run at 320°C was used. Pressure was held constant at 10 psi
          throughout the run and a split ratio of 10:1 for a 1uL injection. An open ended 4 mm helical liner was used (Agilent #5188-5396). The inlet
          temperature was 250°C and transfer line was set to 280°C. In the case of both detectors the source temperature was set to 300°C and
          the analyzer to 180°C.

                                                                                                                                         Tetradifon

                                                            Carbaril         200 ppb Tetradifon in Orange Oil (1:10 split)

                                                                             S/N for quantitating transition m/z 356 → 229
                                                                             Signal to Noise ratio: 400:1




                         Phenanthrene-D10 (2 ppm)




                                                                   Chlorpyrifos

               2,4 D Ethyl ester
                                                                                                                     Ethion
                                                                                                                                          Tetradifon




Page 51
Ultra Inert Application - PAH Analysis
 GC/MSD Conditions
 Sample:           10ug/ml PAH Standard
 Column:           DB-5ms Ultra Inert 30m x 0.25mm x 0.25um (Agilent part # 122-5532UI)
 Carrier:          Helium 45cm/sec, constant flow
 Oven:             55oC (1min) to 320OC (25O/min), hold 3 min
 Injection:        Pulsed splitless, 300oC, 40psi until 0.2 min, purge flow 30ml/min at 0.75 min
                   Gas saver 80ml/min on at 3 min                                                                                             12
                                                                                                                     8     9     10
 MSD:              Transfer Line 280OC , Source 300OC, Quad 180OC
                                                                                                             7                         11
                                                                                                                                                   13
                                                                                              5   6                                                             14
                                                                                                                                                                     15
                                                                               3   4
                                                1                   2                                                                                                        16




 1.       Naphthalene
 2.       Acenaphthylene
 3.       Acenaphthene                                6.00              7.00           8.00           9.00       10.00   11.00        12.00             13.00        14.00
 4.       Fluorene
 5.       Phenanthrene
 6.       Anthracene
 7.       Fluoranthene                          1                   2          3   4          5   6          7       8     9     10    11     12   13           14   15      16

 8.       Pyrene
 9.       Benz[a]anthracene
 10.      Chrysene
 11.      Benz[b]fluoranthene                       Enlarged View
 12.      Benz[k]fluoranthene
 13.      Benz[a]pyrene
 14.      Indeno[1,2,3-cd]pyrene
 15.      Dibenzo[a,h]anthracene
 16.      Benzo[g,h,i]perylene


                                                       6.00             7.00           8.00           9.00       10.00   11.00        12.00             13.00        14.00




Page 52
Take Home Message


 Consider high efficiency columns for faster analyses
 Method translation software make it easy
 Use Ultra Inert columns for critical applications
 Excellent performance over a range of applications
 The Bottom Line
 Quality innovation for our customers to get the right
  answer the 1st time




Page 55
Thank You.   Questions?




Page 58

								
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