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Everything That’s Old is New
           Again

    Introducing HALO-5
    A Truly “High Performance”
             5µ Particle
How Much Does a
Theoretical Plate Weigh?
Introduction
 HALO core-shell particles are unique high-purity silica
  particles for stable high efficiency packed columns that
  are capable of very fast separations with modest back
  pressures
 Original HALO particles are 2.7-microns with 90 Å pores
 HALO provides the efficiency of sub-2-micron particles at
  half the pressure
 New HALO-5 particles are ~ 5-microns with 90 Å pores
 HALO-5 provides the efficiency of 3-micron particles with
  the pressure of 5-micron particles
HALO -5 Fused-Core Particles
                ®




                                                                  ~ 5 µm




                                                        0.6 µm



SEM of ~ 5 µm HALO Fused-core   Graphical representation of ~ 5 µm HALO Fused-core
• As predicted by theory, the smaller the particle, the smaller the plate height
   (e.g., the sharper the peaks)
• The 4 µm and 2.2 µm particles are from R&D batches
• The reduced plate height, h (same plate height data divided by the particle
               size), provides a measure of packed bed quality.
 • The larger-particle HALO packings exhibit lower values for h, indicating
   more homogeneous packed beds. HALO(2.7) h = 1.5, HALO-5 h = 1.2!
More Theoretical Plates at Lower Pressure




• When operated at optimum flow rates, HALO-5 columns provide the
      highest number of theoretical plates per unit of pressure
So how much does a
theoretical plate weigh?
Based on the previous graph, a theoretical plate from
a column packed with 1.8µ particles weighs 0.025 bar.
 A theoretical plate from a column packed with HALO-
5 weighs 0.0028 bar.

Practical significance: You get 10X as many HALO-5
plates per pound!
HALO-5 Bonded Phases

                              Available November 2012
                                      - Phenyl-Hexyl
                                      - C8
                                      - ES-CN
    C18 (octadecyl)
                              Available February 2013

  PFP                                 - HILIC
  (pentafluorophenylpropyl)           -Penta-HILIC
Who Should Use HALO-5 Columns?

 Users who currently use 3- or 5-micron
  particle columns and want to increase their
  efficiency and speed
 Anyone wanting to transfer a method to a
  routine laboratory
 Users who want more speed or who want
  more separation power but are owners of
  pressure-limited HPLC instruments (400 bar
  max pressure)
Conclusions
Regarding HALO-5 Columns

 Produce unusual column efficiency; reduced plate
  heights h of ~1.2 for small molecules making them the
  first high-performance 5-micron columns in the world.
 Efficiency and separation speed rivals that of
  3-μm columns, but with about one-half the pressure.
 Thin porous outer shell results in superior mass
  transfer kinetics and better efficiency at high mobile
  phase velocities, especially for larger molecules.
 2-μm porosity frits allow the convenience and
  ruggedness of columns with 5 μm particles.
 Strong particles allow pressures of at least 600 bar.
The line it is drawn, the curse it is cast
The slow one now will later be fast
As the present now will later be past
The order is rapidly fadin’
And the first one now will later be last
For the times they are a-changin’

Bob Dylan 1964
Easy Transfer from Existing Methods




  • HALO-5 Columns Can be Substituted for 5-Micron Totally
Porous Columns to Provide Sharper Peaks and Shorter Analysis
         Times Under Identical Method Parameters
Obtain 5-Micron Benefits for 3-Micron Methods




• HALO-5 Columns Provide the Same Efficiency as 3-Micron
Columns at about Half the Pressure
Comparable Selectivity with 2.7-Micron HALO
                                        PEAK IDENTITIES (in order):
                                        1. Uracil
                                        2. Resorcinol
                                        3. Aniline
                                        4. 4-Chloroaniline
                                        5. Acetoacetanilide
                                        6. Dimethylphthalate
                                        7. Cinnamyl alcohol
                                        8. 2,6-Dinitrotoluene
                                        9. Tolbutamide
                                        10. 4-Chloro-3-nitroanisole




• Methods are easily transferred from HALO 2.7-micron
columns to HALO-5 Columns with only minor adjustment
              to mobile phase strength
HALO-5 Columns Exhibit the Same Sample Loadability as 2.7-Micron
HALO Columns and are Similar to 5-Micron Totally Porous Columns

            35000



            30000



            25000

                           2.7 µm Fused-Core, 0.5 µm shell
            20000
                           5 µm Fused-Core, 0.6 µm shell

                           5 µm Totally porous
            15000
        m
        N
        b
        u
        P
        e
        a
        r
        t
        l




            10000



             5000
                    0.01           0.1                    1                  10   100
                                                 µg of 1-Cl-4-Nitrobenzene
Back Pressure Plots for Columns of Different
                              Particle Sizes
                600
                             2.7 µm Halo fused-core
                             3 µm totally porous
                             4 µm Halo fused-core
                500
                             5 µm Halo fused-core
                             5 µm totally porous
                             Linear regression
                400
Pressure, bar




                300



                200
                                                                              •Columns: 150 x 4.6 mm, C18
                                                                              •Mobile Phase:
                                                                                    50% ACN, 50% Water
                100
                                                                              •Temperature: 30°C
                                                                              •Instruments: Agilent 1100 or
                                                                                            Agilent 1200 SL
                  0
                      0.0   0.5     1.0     1.5       2.0   2.5   3.0   3.5       4.0     4.5     5.0

                                            Mobile Phase Flow Rate, mL/min

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09 everything that’s old is new again introducing 5 mm hplc particles carl zimmerman - mac-mod analytical

  • 1. Everything That’s Old is New Again Introducing HALO-5 A Truly “High Performance” 5µ Particle
  • 2. How Much Does a Theoretical Plate Weigh?
  • 3. Introduction  HALO core-shell particles are unique high-purity silica particles for stable high efficiency packed columns that are capable of very fast separations with modest back pressures  Original HALO particles are 2.7-microns with 90 Å pores  HALO provides the efficiency of sub-2-micron particles at half the pressure  New HALO-5 particles are ~ 5-microns with 90 Å pores  HALO-5 provides the efficiency of 3-micron particles with the pressure of 5-micron particles
  • 4. HALO -5 Fused-Core Particles ® ~ 5 µm 0.6 µm SEM of ~ 5 µm HALO Fused-core Graphical representation of ~ 5 µm HALO Fused-core
  • 5.
  • 6. • As predicted by theory, the smaller the particle, the smaller the plate height (e.g., the sharper the peaks) • The 4 µm and 2.2 µm particles are from R&D batches
  • 7. • The reduced plate height, h (same plate height data divided by the particle size), provides a measure of packed bed quality. • The larger-particle HALO packings exhibit lower values for h, indicating more homogeneous packed beds. HALO(2.7) h = 1.5, HALO-5 h = 1.2!
  • 8. More Theoretical Plates at Lower Pressure • When operated at optimum flow rates, HALO-5 columns provide the highest number of theoretical plates per unit of pressure
  • 9. So how much does a theoretical plate weigh? Based on the previous graph, a theoretical plate from a column packed with 1.8µ particles weighs 0.025 bar. A theoretical plate from a column packed with HALO- 5 weighs 0.0028 bar. Practical significance: You get 10X as many HALO-5 plates per pound!
  • 10. HALO-5 Bonded Phases Available November 2012 - Phenyl-Hexyl - C8 - ES-CN C18 (octadecyl) Available February 2013 PFP - HILIC (pentafluorophenylpropyl) -Penta-HILIC
  • 11. Who Should Use HALO-5 Columns?  Users who currently use 3- or 5-micron particle columns and want to increase their efficiency and speed  Anyone wanting to transfer a method to a routine laboratory  Users who want more speed or who want more separation power but are owners of pressure-limited HPLC instruments (400 bar max pressure)
  • 12. Conclusions Regarding HALO-5 Columns  Produce unusual column efficiency; reduced plate heights h of ~1.2 for small molecules making them the first high-performance 5-micron columns in the world.  Efficiency and separation speed rivals that of 3-μm columns, but with about one-half the pressure.  Thin porous outer shell results in superior mass transfer kinetics and better efficiency at high mobile phase velocities, especially for larger molecules.  2-μm porosity frits allow the convenience and ruggedness of columns with 5 μm particles.  Strong particles allow pressures of at least 600 bar.
  • 13. The line it is drawn, the curse it is cast The slow one now will later be fast As the present now will later be past The order is rapidly fadin’ And the first one now will later be last For the times they are a-changin’ Bob Dylan 1964
  • 14. Easy Transfer from Existing Methods • HALO-5 Columns Can be Substituted for 5-Micron Totally Porous Columns to Provide Sharper Peaks and Shorter Analysis Times Under Identical Method Parameters
  • 15. Obtain 5-Micron Benefits for 3-Micron Methods • HALO-5 Columns Provide the Same Efficiency as 3-Micron Columns at about Half the Pressure
  • 16. Comparable Selectivity with 2.7-Micron HALO PEAK IDENTITIES (in order): 1. Uracil 2. Resorcinol 3. Aniline 4. 4-Chloroaniline 5. Acetoacetanilide 6. Dimethylphthalate 7. Cinnamyl alcohol 8. 2,6-Dinitrotoluene 9. Tolbutamide 10. 4-Chloro-3-nitroanisole • Methods are easily transferred from HALO 2.7-micron columns to HALO-5 Columns with only minor adjustment to mobile phase strength
  • 17. HALO-5 Columns Exhibit the Same Sample Loadability as 2.7-Micron HALO Columns and are Similar to 5-Micron Totally Porous Columns 35000 30000 25000 2.7 µm Fused-Core, 0.5 µm shell 20000 5 µm Fused-Core, 0.6 µm shell 5 µm Totally porous 15000 m N b u P e a r t l 10000 5000 0.01 0.1 1 10 100 µg of 1-Cl-4-Nitrobenzene
  • 18. Back Pressure Plots for Columns of Different Particle Sizes 600 2.7 µm Halo fused-core 3 µm totally porous 4 µm Halo fused-core 500 5 µm Halo fused-core 5 µm totally porous Linear regression 400 Pressure, bar 300 200 •Columns: 150 x 4.6 mm, C18 •Mobile Phase: 50% ACN, 50% Water 100 •Temperature: 30°C •Instruments: Agilent 1100 or Agilent 1200 SL 0 0.0 0.5 1.0 1.5 2.0 2.5 3.0 3.5 4.0 4.5 5.0 Mobile Phase Flow Rate, mL/min