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ASTM E 1510 : 1995 : R2013 : EDT 1

Superseded

Superseded

A superseded Standard is one, which is fully replaced by another Standard, which is a new edition of the same Standard.

View Superseded by

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

Available format(s)

Hardcopy , PDF

Superseded date

26-04-2021

Language(s)

English

Published date

25-01-2013

£63.73
Excluding VAT

CONTAINED IN VOL. 03.06, 2015 Defines the installation and maintenance of fused silica capillary columns in gas chromatographs that are already retrofitted for their use.

Committee
E 13
DocumentType
Standard Practice
Pages
13
ProductNote
Reconfirmed EDT 1
PublisherName
American Society for Testing and Materials
Status
Superseded
SupersededBy
Supersedes

1.1This 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:

1.1.1Injection techniques.

1.1.2Column selection.

1.1.3Data acquisition.

1.1.4System troubleshooting and maintenance.

1.2For 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.

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

1.4This 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 NitrogenCarrier 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. 1Van 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. 2Hydrogen 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. 4ECD Septum Bleed

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