ASTM E1510 - 95(2013)e1

    Standard Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs

    Active Standard ASTM E1510 | Developed by Subcommittee: E13.19

    Book of Standards Volume: 03.06


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    Significance and Use

    5.1 This practice is intended to be used by all analysts using fused silica capillary chromatography. It contains the recommended steps for installation, preparation, proper installation, and continued column maintenance.

    1. Scope

    1.1 This practice covers the installation and maintenance of fused silica capillary columns in gas chromatographs that are already retrofitted for their use. This practice excludes information on:

    1.1.1 Injection techniques.

    1.1.2 Column selection.

    1.1.3 Data acquisition.

    1.1.4 System troubleshooting and maintenance.

    1.2 For additional information on gas chromatography, please refer to Practice E260. For specific precautions, see 7.2.2.2(1), 7.2.2.2(2), 7.2.7, and 7.2.7.2.

    1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

    1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific safety information, see Section 6, 7.2.2.2(1), 7.2.2.2(2), 7.2.7, and 7.2.7.2.2

    TABLE 1 Typical Splitter Vent Flow Rates (50 to 1 split ratio) (at optimum linear velocity)

    Carrier gas

    0.25-mm ID,
    cm3 /min

    0.32-mm ID,
    cm3 /min

    0.53-mm ID,
    cm3 /min

      helium
      hydrogen

    35
    70

     80
    160

    125
    250


    Van Deemter Profile for Hydrogen, Helium, and Nitrogen
Carrier Gases
    Note 1The curves were generated by plotting the height equivalent to a theoretical plate (length of column divided by the total number of theoretical plates, H.E.T.P.) against the column's average linear velocity. The lowest point on the curve indicates the carrier gas velocity in which the highest column efficiency is reached.
    Note 2Gases information available from Compressed Gas Association (CGA), 4221 Walney Rd., 5th Floor, Chantilly, VA 20151-2923, http://www.cganet.com.
    FIG. 1 Van Deemter Profile for Hydrogen, Helium, and Nitrogen Carrier Gases
    Hydrogen Versus Helium (Isothermal Analysis)

    Carrier gas: Hydrogen

    Carrier gas: Helium

    Linear velocity: 40 cm/s

    Linear velocity: 20 cm/s


    Note 1Fig. 2 shows that the resolution is similar but the analysis time is reduced by 50 % when comparing hydrogen to helium in an isothermal analysis using optimum flow velocities.
    Note 2Hydrogen provides similar resolution in one-half the analysis time of helium for an isothermal analysis.
    Note 3

     

    1. Tetrachloro-m-

     8. Heptachlor epoxide

    15. Endosulfan II

     

      xylene

     9. γ-chlordane

    16. DDD

     

    2. α-BHC

    10. Endosulfan I

    17. Endrin aldehyde

     

    3. β-BHC

    11. α-chlordane

    18. Endosulfan sulfate

     

    4. γ-BHC

    12. Dieldrin

    19. DDT

     

    5. δ-BHC

    13. DDE

    20. Endrin ketone

     

    6. Heptachlor

    14. Endrin

    21. Methyoxychlor

     

    7. Aldrin

     

     


    Note 430 m, 0.25-mm ID, 0.25 μm 5 % diphenyl − 95 % dimethyl polysiloxane 0.1-μL split injection of chlorinated pesticides.

     

    Oven temperature: 210°C isothermal

     

    Injector and detector temperature: 250°C/300°C

     

    ECD sensitivity: 512 × 10 −11

     

    Split vent: 100 cm 3 /min


    FIG. 2 Hydrogen Versus Helium (Isothermal Analysis)
     Capping Silanol Groups with Dimethyl Dichlorosilane
(DMDCS)
    FIG. 3 Capping Silanol Groups with Dimethyl Dichlorosilane (DMDCS)
    ECD Septum Bleed
    Note 1Septum bleed can obscure or co-elute with compounds of interest, thus decreasing the analytical accuracy.
    Note 2

     

    1. 2,4,5,6-tetrachloro-

     8. Heptachlor

    16. p,p-DDD

     

     m-xylene (IS)

        epoxide

    17. Endrin aldehyde

     

    2. α-BHC

     9. γ-chlordane

    18. Endosulfan sul-

     

    3. β-BHC

    10. Endosulfan I

        fate

     

    4. γ-BHC

    11. α-chlordane

    19. p,p-DDT

     

    5. δ-BHC

    12. Dieldrin

    20. Endrin ketone

     

    6. Heptachlor

    13. p,p-DDE

    21. Methyoxychlor

     

    7. Aldrin

    14. Endrin

    22. Decachlorobi-

     

     

    15. Endosulfan II

       phenyl (IS)


    Note 330 m, 0.53-mm ID, 0.50 μm 5 % diphenyl − 95 % dimethyl polysiloxane 0.1 μL direct injection of 50 pg pesticide standard.

    Oven temperature: 150 to 275°C at 4°C/min,
     hold 15 min

     

    Injector temperature: 250°C

    Detector temperature: 300°C

    Carrier gas: Helium

     

    Linear velocity: 40 cm/s (Flow rate: 10 cm 3 /min)

     

    ECD sensitivity: 8 × 10 −11 AFS

     


    FIG. 4 ECD Septum Bleed


    2. Referenced Documents (purchase separately) The documents listed below are referenced within the subject standard but are not provided as part of the standard.

    ASTM Standards

    E260 Practice for Packed Column Gas Chromatography

    E355 Practice for Gas Chromatography Terms and Relationships

    CGA Publications

    HB-3 Handbook of Compressed Gases


    ICS Code

    ICS Number Code 71.040.50 (Physicochemical methods of analysis)

    UNSPSC Code

    UNSPSC Code


    Referencing This Standard

    DOI: 10.1520/E1510-95R13E01

    ASTM International is a member of CrossRef.

    Citation Format

    ASTM E1510-95(2013)e1, Standard Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs, ASTM International, West Conshohocken, PA, 2013, www.astm.org

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