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25

2008 vol. 1

GC Accessories

Consider Resealability

Multiple injections can core the vial cap septum and lead to significant bleed.

Resistance to coring varies by septum material (Figure 5). Coring can be min-

imized by preparing separate vials for replicate injections, when feasible, and

by carefully considering the type of septum material when multiple injections

are necessary. Septum resealability also affects evaporative loss, which can be a

significant source of error for low volume samples. For example, a relatively

nonvolatile analyte in a volatile solvent can concentrate significantly due to

evaporative loss (Figure 6). Vials should be recapped when necessary for

extended runs or long term storage.

Conclusion

Septum bleed is not a very common occurrence, but when bleed does occur, it

is easy to assume the injection port septum is the source because the vial cap

septum often is not considered. However, correctly diagnosing the source of

bleed contamination can save time and effort by preventing unnecessary injec-

tion port maintenance. Effectively and efficiently reducing interfering peaks by

controlling septum bleed can significantly improve analytical performance,

particularly for trace analyses.

Figure 3

PTFE lining prevents bleed due to

solvent/septum interaction.

Figure 4

Unlined septa show bleed

contamination within 24 hours.

Figure 5

Bleed contamination increases

over multiple injections.

Figure 6

This bar graph shows the volume

of solvent lost for three septum types.

Crimp-Top Vials, Snap Seal™ Style—12 x 32mm, 11mm Crimp

Description

100-pk.

1000-pk.

2.0mL Clear Glass Vial w/White Graduated Marking Spot

24383

24384

2.0mL Amber Glass Vial w/White Graduated Marking Spot

24385

24386

2.0mL Clear Glass Vial without Graduated Marking Spot

21152

21153

2.0mL, 11mm Aluminum Crimp Seals with Septa

Description

100-pk.

1000-pk.

Silver Seal, PTFE/Natural Rubber Septa

21174

21175

Red Seal, PTFE/Red Rubber Septa

24355

24356

Silver Seal, PTFE/Silicone Septa

24359

24360

Limited Volume Inserts for 2.0mL Crimp-Top & Short-Cap,

Screw-Thread Vials

Description

100-pk.

1000-pk.

350µL Glass, Flat Bottom Insert w/ ID Ring

24692

24693

Rtx®-5MS—Low-bleed GC/MS Columns (fused silica)

(Crossbond

®

5% diphenyl/95% dimethyl polysiloxane)

ID

df (µm)

temp. limits

length

cat. #

price

0.25mm

0.25

-60 to 330/350°C

30-Meter

12623

Split Liners for Agilent GCs

ID* x OD & Length (mm)

qty.

cat.#

price

4mm Split w/ Wool

4.0 ID x 6.3 OD x 78.5

ea.

20781

4.0 ID x 6.3 OD x 78.5

5-pk.

20782

4.0 ID x 6.3 OD x 78.5

25-pk.

20783

*Nominal ID at syringe needle expulsion point.

Vials were prepared with methylene chloride and stored at room temperature.

Vials were prepared with methylene chloride, sealed with caps contain-

ing septa that were inserted upside down in order to expose the non-PTFE

lined septum surface to the solvent, and stored at room temperature.

Vials containing 300µL of methylene chloride were punctured and left

at room temperature for 24 hours.