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

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SPME Round-Robin Protocol - 2019 & 2020[edit | edit source]

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 Equipment[edit | edit source]

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

Procedure[edit | edit source]

SPME fiber preparation and sampling procedure[edit | edit source]

  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[edit | edit source]

  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