Section: 8 | Solid-Phase Microextraction Sorbents |
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John R. Rumble, ed., CRC Handbook of Chemistry and Physics, 103rd Edition (Internet Version 2022), CRC Press/Taylor & Francis, Boca Raton, FL.
If a specific table is cited, use the format: "Physical Constants of Organic Compounds," in CRC Handbook of Chemistry and Physics, 103rd Edition (Internet Version 2022), John R. Rumble, ed., CRC Press/Taylor & Francis, Boca Raton, FL.


Thomas J. Bruno and Paris D. N. Svoronos

While trapping sorbents have been used for many years in headspace analysis (most commonly with gas chromatography), the modern techniques of solid-phase microextraction (SPME) are particularly applicable to survey analyses (Ref. 1). In the following tables, we provide information for the selection and application of the various fibers, modifications to fiber materials and data on salting out reagents (Refs. 1–5). For information on other trapping sorbents, chelating agents, resins, and polymeric phases used for headspace analysis, see Ref. 1.


  1. Bruno, T. J., and Svoronos, P. D. N., CRC Handbook of Basic Tables for Chemical Analysis – Data-Driven Methods and Interpretation, Fourth Edition, CRC Press/Taylor & Francis, Boca Raton, FL, 2021. []
  2. Rumble, J. R., Ed., CRC Handbook for Chemistry and Physics, 102nd Edition, CRC Press, Boca Raton, FL, 2021.
  3. NIST Chemistry Web Book, <>.
  4. Machata, G., Clin. Chem. Newsletter 4, 29, 1972.
  5. Ioffe, B. V., and Vitenberg, A. G., Head Space Analysis and Related Methods in Gas Chromatography, Wiley Interscience, New York, 1983.
  6. Fritz, J.S., Solid Phase Extraction, Wiley-VCH, New York, 1999.

Fiber Selection Criteria

The main fiber selection parameters are polarity and relative molecular mass. Table 1 provides general guidelines on the applicability of available fibers relative to these two parameters. The fibers are characterized by the extraction mechanism, either adsorption or absorption. Adsorbent fibers contain particles suspended in polydimethyl siloxane (PDMS) or polyethylene glycol (PEG, Carbowax). The column definitions for Table 1 are as follows.

Column heading Definition
Fiber Name of acronym of fiber; see below for list of acronyms
Type of fiber Indication of whether fiber extraction mechanism is adsorption or absorption
Polarity Indication of polarity of fiber
RMM range Relative molecular mass range that is the ideal range for optimum extraction. Ranges can be extended by varying extraction times, but results will not be optimized

PDMS – Polydimethylsiloxane
DVB – Divinylbenzene (3 μm to 5 μm particles)
PEG – Polyethylene glycol
Carboxen – Carboxen 1006 (contains micro-, meso-, and macro-tapered pores) (3 μm to 5 μm particles)

Table 1. Polarity and Relative Molecular Mass Range of Selected Fibers

FiberType of fiberPolarityRMM range
7 μm PDMSAbsorbentNonpolar150–700
30 μm PDMSAbsorbentNonpolar80–600
85 μm PolyacrylateAbsorbentModerately polar60–450
100 μm PDMSAbsorbentNonpolar55–400
50 μm Carbowax (PEG)AdsorbentPolar50–400
Carbopak Z-PDMSAdsorbentNonpolar50–500

Phase Material Characteristics

Polydimethylsiloxane (PDMS):

Similar in properties to the OV-1 or SE-30 silicone phases (Ref. 1); nonpolar fluid suitable for nonpolar or slightly polar analytes; thicker coatings extract more analyte, but require longer extraction times; thicker coatings may show carryover effects; useful for hydrocarbons, aldehydes, ketones, and esters.


Rigid solid material; moderate polarity; diffusion of analytes through bulk is relatively slow because of rigidity of material; relatively higher desorption temperatures required because of rigidity of material; can be oxidized easily at higher temperatures; must use oxygen-free carrier gas and ensure gas chromatographic system is leak-free; fibers are very solvent resistant; darkens to a brown color upon exposure to temperatures in excess of 280 °C, but fiber is generally still usable until color becomes black; useful for alcohols.

Carbowax (polyethylene glycol, PEG):

Similar in properties to the PEG coatings used extensively in chromatography; moderately polar; highly cross-linked to counteract water solubility; sensitive to attack by oxygen at temperatures in excess of 220 °C, at which point the fiber will darken and become powdery; requires use of high purity carrier gas (typically He at 99.999 % mass/mass) treated for oxygen contamination.

Divinylbenzene (DVB):

Similar to the properties of divinylbenzene porous polymer phases; higher polarity than Carbowax, and when combined with Carbowax results in a more polar phase; like polyacrylate, it is a solid particle that must be carried in a liquid to coat on a fiber.


Similar to the material used in Carboxen porous-layer open tubular (PLOT) columns; structure has an approximately even distribution of macro-, meso-, and micropores, making it valuable for smaller analytes; larger analytes can show hysteresis that must be addressed by desorption at 280 °C; useful for hydrocarbons, ethers, aldehydes, and ketones.

Extraction Capability of Solid-Phase Microextraction Sorbents

Table 2 shows the extraction capability of the fibers for acetone, a small, moderately polar analyte, for 4-nitrophenol, a medium size polar analyte, and benzo(GHI)perylene, a large nonpolar analyte. This provides a general guideline for fiber selection.


Table 2. Approximate Linear Concentration Ranges for Acetone, 4-Nitrophenol, and Benzo[ghi]perylene

FiberAcetone 10 min exta (FID)4-Nitrophenol 20 min extb (GC/MS)Benzo[ghi]perylene 20 min ext
7 μm PDMS100 ppm and upNot extracted100 ppt to 500 ppb
30 μm PDMS10 ppm and up10 ppm and up100 ppt to 10 ppm
85 μm Polyacrylate1 ppm to 1000 ppm5 ppb to 100 ppm500 ppt to 10 ppm
100 μm PDMS500 ppb to 1000 ppm500 ppb to 500 ppm500 ppt to 10 ppm
50 μm Carbowax (PEG)1 ppm to 1000 ppm5 ppb to 50 ppm25 ppb to 10 ppm
PDMS-DVB50 ppb to 100 ppm25 ppb to 10 ppm10 ppb to 1 ppm
Carbowax-DVB100 ppb to 100 ppm5 ppb to 10 ppm50 ppb to 5 ppm
PDMS-DVB-Carboxen25 ppb to 10 ppm50 ppb to 10 ppm100 ppb to 1 ppm poorly desorbed
PDMS-Carboxen5 ppb to 5 ppm100 ppb to 10 ppmNot desorbed
Carbopak Z-PDMS10 ppm to 500 ppm5 ppm to 100 ppm500 ppt to 100 ppb
  • Note: In each case, the concentration is expressed on a mass basis (e.g., ppm mass/mass).
  • aWater sample contains 25% NaCl (mass/mass)
  • bWater sample contains 2% NaCl (mass/mass) acidified to pH = 2 with 0.05 M phosphoric acid
  • 1 ppm = 1 part in 1 × 106
  • 1 ppb = 1 part in 1 × 109
  • 1 ppt = 1 part in 1 × 1012

Table 3. Typical Phase Volumes of SPME Fiber Coatings

Fiber coating thickness/typeType of fiber coreFiber core diameter/mmPhase volume/mm3
Continued on next page...
PDMSFused silica0.1100.612
100 μm PDMSMetal0.1300.598
30 μm PDMSFused silica0.1100.132
30 μm PDMSMetal0.1300.136
7 μm PDMSFused silica0.1100.028
7 μm PDMSMetal0.1300.030
85 μm PAFused silica0.1100.543
60 μm PEGMetal0.1300.358
15 μm Carbopack Z/PDMSMetal0.1300.068
65 μm PDMS/DVBFused silica0.1200.418
65 μm PDMS/DVBProprietary0.1300.440
65 μm PDMS/DVBMetal0.1300.440
75 μm Carboxen-PDMSFused silica0.1200.502
85 μm Carboxen-PDMSProprietary0.1300.528
85 μm Carboxen-PDMSMetal0.1300.528
50/30 μm DVB/CarboxenMetal
Carboxen layer0.1300.151
DVB layer0.1900.377
50/30 μm DVB/CarboxenMetal

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