Technique for analyzing SPME samples used by the Material Working Group's Materials Testing and Standards group

SPME Round-Robin Protocol - 2023

Instrumental parameters for the one required experiment are described below. Two samples are provided (~0.5 g per sample per 10 mL vial). The second sample is preferably for replication, however you may conduct other GCMS protocols with the second sample vial. Additional material is available on request.

For participants in the 2023 protocol: Samples will be sent in 10 mL SPME vials and any manipulation of samples for non-SPME testing should be handled only while wearing nitrile gloves. A blank 10 mL SPME vial is also included.

• Experimental parameters must be described when results are submitted.
• Datafiles for the runs should be submitted, preferably in netCDF format. Many newer GCMS software packages can export in this file format.

Materials, Supplies, and Procedure

SPME fiber

• Use a Supelco 100 um PDMS that is newly purchased for this experiment
• Condition the fiber for 30 minutes at 260°C before first use (per Supelco’s instructions)
• Heat using a sand or water bath up to the shoulder of the 10 ml vial
• Incubate sample for 10 minutes at 60°C
• Expose fiber to sample for 5 minutes at 60°C

GC-MS

• DB-5 column equivalent
• SPME liner
• Inlet temperature: 275°C
• No cryotrap
• 1 minute desorption with 10:1 split
• Leave fiber in inlet for 15 minutes with a 200:1 split after injection
• Heat column: 40°C for 5 minutes then heat at 10°C/minute to 250°C
• Hold at 275°C for 5 minutes to clean
• m/z: 29 – 450
• Run a blank vial before and after the sample is run

Report your detector when you submit your results

SPME Round-Robin Protocol - 2019 & 2020

Below is a protocol used by the Materials Working Group to ascertain whether the same material analyzed at different museums will give the same result. Seven materials were tested during this process.

• Instrumental parameters for the one required experiment are described below. Two samples are provided (~0.5 g per sample per 10 mL vial). The second sample is preferrably for replication.
  
• nb: You may conduct other GCMS protocols with the second sample vial
  
• Additional material is available on request
• Samples will be sent in 10 mL SPME vials and any manipulation of samples for non-SPME testing should be handled only while wearing nitrile gloves
• Experimental parameters must be described when results are submitted.
• A blank 10 mL SPME vial is included for any experiments the user wants to add. Be sure to describe the experimental parameters.
• Datafiles for the runs should be submitted, preferably in netCDF format. Many newer GCMS software packages can export in this file format.

Materials, Supplies, and Procedure

• Supelco 100 um PDMS that is newly purchased for this experiment
• DB-5 column equivalent
• SPME liner

SPME fiber preparation and sampling procedure

1. Condition the fiber for 30 minutes at 260°C before first use as per Supelco’s instructions
2. Heat using a sand or water bath up to the shoulder of the 10 ml vial
3. Incubate sample for 10 minutes at 60°C
4. Expose fiber to sample for 5 minutes at 60°C

GC-MS

1. Inlet temperature: 275°C
2. No cryotrap
3. 1 minute desorption with 10:1 split
4. Leave fiber in inlet for 15 minutes with a 200:1 split after injection
5. Heat column: 40°C for 5 minutes then heat at 10°C/minute to 250°C; at end of run, hold column at 275°C for 5 minutes to clean
6. m/z: 35 – 500
7. Run a blank vial before and after the sample is run
   

Report your detector when you submit your results