Restek 27490 User manual

Restek PAL SPME Manual Injection Kit

cat.# 27490

1. Description

The Restek PAL SPME manual injection kit will allow the end user to extract samples using SPME

Arrows or SPME fibers and then inject the samples into a GC inlet. The Restek PAL SPME manual

injection kit includes the components shown in Figure 1. SPME Arrows, SPME fibers, GC-specific

conversion kits (including adaptor cups), and additional adaptor cups are sold separately.

Due to the relatively large diameter of Restek PAL SPME Arrows, it will be necessary to modify

the GC inlet prior to use. Conversion kits include the following instrument-specific parts: a GC

injection port weldment, an adaptor cup, a 5-pack of liners, a 3-pack of septa, and a septum

nut. Conversion kits are available for the following types of GCs:

2. Installing a SPME Arrow or SPME Fiber in the Syringe

2.1 Loosen the cap (6) at the base of the syringe (8) and remove it (Figure 2).

2.2 Depress the black plunger completely and screw the hub of a SPME Arrow or SPME fiber

(7) into the bottom of the plunger at the end of the syringe body (8).

2.3 Slide the cap (6) over the SPME Arrow or SPME fiber and tighten it onto the syringe (8) as

shown in Figure 3.

2.4 Slide the locking screws (4 and 5) onto the syringe (8) from the plunger side (the right

side as shown in Figure 4). First, install the large ID locking screw (4) onto the silver body of the

syringe; then, install the small ID locking screw (5) onto the wider portion of the black plunger.

2.5 Tighten the locking screws until finger tight. Do not overtighten, as they will be adjusted

in subsequent steps.

Figure 1: Parts Included in the Restek PAL SPME Manual Injection Kit

1Extraction guide

2Injection guide

3Arrow/ﬁber syringe

4Large inner diameter (ID)

locking screw

5Small inner diameter (ID)

locking screw

Figure 2: Disassembled View of Syringe and SPME Arrow (or

Fiber) Prior to Installation

Figure 3: SPME Arrow/Fiber Installed in Syringe

Figure 4: Attaching the Locking Screws to the Syringe

GC Conversion Kit Cat.#

Thermo TRACE Ultra 27495

Thermo TRACE 1300/1310 27494

Agilent GC 6890 27492

Agilent GC 7890 27493

Shimadzu GC 2010 27491

slide the locking screws onto the

syringe from the plunger side

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3. Setting the Extraction Depth using the Extraction Guide

As shown in Figure 5, the extraction guide has two positions in which the syringe can be

installed. Use the upper position (9) for headspace extraction and the lower position (10) for

immersion extraction. For fine adjustment of the extraction depth, please refer to section 3.1

for headspace extraction and section 3.2 for immersion extraction. The extraction guide is de-

signed for use with 18 mm and 20 mm headspace vials.

3.1 Fine Depth Adjustment for Headspace Extraction

3.1.1 Raise the syringe plunger to the fully extended position and insert the syringe and

lower locking screw (4) into the upper position of the extraction guide. Lock the syringe

into place by rotating it until the locking screw is positioned in the notch (Figure 6).

3.1.2 Loosen the lower locking screw (4).

3.1.3 Adjust the syringe so that the SPME Arrow or SPME fiber is protruding ~1 cm beyond

the inner base of the extraction guide. When in proper position, the tip of the SPME Arrow or

SPME fiber will be recessed at least 1 mm in from the end of the extraction guide (Figure 7).

3.1.4 Tighten the lower locking screw (4) securely onto the silver body of the syringe. Do

not tighten the screw against the black plunger or you will not be able to move the SPME

Arrow or SPME fiber into position for sampling (Figure 8).

The septum penetration depth is now set. Proceed with steps 3.1.5 and 3.1.6 to the set the proper

exposure depth for headspace extraction.

3.1.5 Place the extraction guide (with the syringe in place) on an empty headspace

sampling vial and loosen the upper locking screw (5).

3.1.6 Adjust the SPME Arrow or SPME fiber to the desired exposure depth by moving the

black plunger up and down (Figure 9). Choose a depth that ensures the SPME Arrow or

SPME fiber will be in the gas phase and not submerged in the liquid phase of the sample.

3.1.7 Once the SPME Arrow or SPME fiber is at the proper depth, hold the plunger in place

and slide the upper locking screw (5) until it is flush against the top of the silver syringe

body. Then tighten the upper locking screw (5) securely as shown in Figure 10.

3.2 Fine Depth Adjustment for Immersion Extraction

3.2.1 Insert the syringe into the lower position (10) of the extraction guide (Figure 5).

3.2.2 Penetrate a vial and fully expose the SPME Arrow or SPME fiber within the vial

(Figure 11).

3.2.3 Adjust the lower locking screw (4) and upper locking screw (5) in order to obtain the

desired exposure depth (one that ensures immersion in the sample liquid). Note: If using

a SPME fiber, set a depth that prevents the tip of the fiber from hitting the bottom of the

vial as this can damage the fiber. If using a SPME Arrow, this is not a concern due to the

Arrow’s protective tip.

4. Adjusting the Injection Guide

Note: The positions of the upper (4) and lower (5) locking screws are set based on the extraction

technique and the depths used in either section 3.1 or 3.2. Do not change the position of the

locking screws during the following steps.

4.1 Carefully insert the syringe (3) into the injection guide (2). Use caution and avoid damaging

the SPME Arrow or SPME fiber when threading it through the hole in the base of the injection

guide.

4.2 Lock the syringe into place by rotating it until the locking screw is positioned in the notch

(Figure 12).

4.3 With the appropriate GC-specific adaptor cup on the end of the injection guide, measure

the distance from the tip of the SPME Arrow or SPME fiber to the groove inside the adaptor cup

(Figure 13).

4.4 Adjust the desorption depth by screwing the body of the injection guide up or down.

4.5 Set the depth to a maximum of 67 mm.

4.6 Twist the locking ring down until it locks on the body of the injection guide (Figure 14).

Figure 7: Proper Positioning

of a SPME Arrow in the

Extraction Guide

Figure 9: Exposure Depth for

Headspace Extraction

Figure 10: Upper Locking

Screw (5)

Figure 5: The extraction

guide has two extraction

positions (notches).

Figure 6: Syringe Installed in

the Extraction Guide

9 5

Figure 8: Incorrect and

Correction Position of the

Lower Locking Screw

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Figure 12: Injection Guide

with GC-Specific Adaptor Cup

Figure 11: Exposure Depth

for Immersion Extraction

Figure 13: Distance from Lower Groove of the Adaptor Cup to

Tip of SPME Arrow or SPME Fiber

Figure 14: Adjusting the Desorption Depth

5. Typical Workflow with Restek PAL SPME Manual Injection Kit

5.1 Extraction

5.1.1 Attach a SPME Arrow or SPME fiber to the syringe (3) and install the syringe (3) into

the extraction guide (1) at the appropriate depth settings.

5.1.2 Penetrate the sample vial septum with the black plunger up so that the SPME Arrow

or SPME fiber is fully retracted.

5.1.3 Push the black plunger down until it rests on the silver body of the syringe (3) to

expose the SPME Arrow or SPME fiber for sampling.

5.1.4 Extract for the prescribed length of time.

5.1.5 Pull the black plunger all the way up to fully retract the SPME Arrow or SPME fiber.

5.2 Remove the syringe (3) from the extraction guide (1) and place the syringe (3) into the

injection guide (2).

5.3 Injection

5.3.1 Install the syringe (3) in the injection guide (1) and set the appropriate desorption

depth using the correct GC-specific adaptor cup for your GC.

5.3.2 Penetrate the septum on the GC inlet with the black plunger up so the SPME Arrow

or SPME fiber is fully retracted.

5.3.3 Push the black plunger down until it rests on the silver body of the syringe (3),

exposing the SPME Arrow or SPME fiber in the GC inlet.

5.3.4 Desorb for the prescribed length of time.

5.3.5 Pull the black plunger all the way up to fully retract the SPME Arrow or SPME fiber.

5.3.6 Remove the injection guide and syringe from GC inlet.

Injection Guide

Body

Locking

Ring

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#500-60-003 Rev. date: 03/17

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