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ASTM International - ASTM E1510-95(2013)e1

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

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Organization: ASTM International
Publication Date: 1 January 2013
Status: inactive
Page Count: 13
ICS Code (Physicochemical methods of analysis): 71.040.50
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... View More

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,
cm

3 /min

0.32-mm ID,
cm

3 /min

0.53-mm ID,
cm

3 /min

  helium
  hydrogen
35
70
 80
160
125
250


Note 1-The 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 2-Gases 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

Carrier gas: Hydrogen Carrier gas: Helium
Linear velocity: 40 cm/s Linear velocity: 20 cm/s

Note 1-Fig. 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 2-Hydrogen 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 4-30 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)
FIG. 3 Capping Silanol Groups with Dimethyl Dichlorosilane (DMDCS)
Note 1-Septum 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 3-30 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

Document History

April 1, 2021
Standard Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
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:...
ASTM E1510-95(2013)e1
January 1, 2013
Standard Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
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:...
February 1, 2005
Standard Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
1.1 This practice is intended to serve as a general guide for the installation and maintenance of fused silica capillary columns in gas chromatographs which are already retrofitted for their use....
January 1, 2000
Standard Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
1.1 This practice is intended to serve as a general guide for the installation and maintenance of fused silica capillary columns in gas chromatographs which are already retrofitted for their use....
January 1, 2000
Standard Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs
1.1 This practice is intended to serve as a general guide for the installation and maintenance of fused silica capillary columns in gas chromatographs which are already retrofitted for their use....
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