Sampling and sample-preparation strategies
based on solid-phase microextraction for
analysis of indoor air
Jacek A. Koziel*, Inman Novak
Texas A&M University Agricultural Research and Extension Center, 6500 Amarillo Blvd. West, Amarillo,
TX 79106, USA
Applications of solid-phase microextraction (SPME)
to the sampling and analysis of volatile organic
compounds in indoor air are reviewed, including a
summary of quantification methods, coatings, com-
pounds, concentrations, sampling locations and
times, and detection limits. Strategies for on-site and
off-site sampling and analysis, advantages and
challenges associated with SPME for air sampling
are discussed. # 2002 Published by Elsevier Science
B.V. All rights reserved.
Keywords:
Air sampling; Environmental analysis; Gas chromato-
graphy; Indoor air; Solid-phase microextraction; Volatile organic
compounds
1. Introduction
1.1. SPME resources
SPME is an extraction technology that com-
bines sampling and sample preparation. Since it
conception, SPME has been widely used for
research applications in pharmaceutical, food,
aroma, forensic, environmental and physico-
chemical properties. Three books on SPME
summarize the theory, applications and many
practical considerations [1–3]. Several SPME
review articles include: new trends [4]; the evo-
lution of the technology [5]; a promising technique
for sample preparation [6]; trends in determination
of organic pollutants in environmental samples
[7]; biomedical analysis [8]; headspace for
analysis of biological fluids and samples [9]; and,
microextraction of drugs [10]. This journal has
published several SPME reviews [7,11], includ-
ing applications to chemical analysis of live bio-
logical
samples
[12].
SPME
manufacturer
application guides [13] and several Internet-
based literature databases [14] attempt to gauge
and to follow the wealth and breadth of SPME-
based publications.
1.2. Indoor air quality
In the past four decades, an increased aware-
ness of the indoor air quality (IAQ) in both
occupational and residential settings and its
impact on human health has encouraged the
development of new air-sampling methods.
Major indicators of IAQ include volatile organic
compounds (VOCs), particulates, CO, CO
2
,
NO
x
, SO
x
, ozone, environmental tobacco
smoke, radon, and biological agents. The
assessment of IAQ is challenged by the
presence of multiple sources, compounds,
interactions with building materials, the effects
of ventilation and occupant activities, and the
highly variable, and often low, concentrations of
analytes
[15,16].
The
sampling/analysis
approach has to be adjusted to the individual
case and optimize the choice of target pollu-
tants,
appropriate
sampling
and
analysis
method, budget and number of samples,
sampling
locations,
sampling
times
and
duration, and sample-preservation and custody
protocols [17].
0165-9936/02/$ - see front matter
# 2002 Published by Elsevier Science B.V. All rights reserved.
P I I : S 0 1 6 5 - 9 9 3 6 ( 0 2 ) 0 1 2 0 4 - 9
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trends in analytical chemistry, vol. 21, no. 12, 2002
*Corresponding
author.
Tel.:
+1
(806)
677-5619;
Fax: +1 (806) 677-5644.
E-mail: ja-koziel@tamu.edu
1.3. Indoor air sampling
Sampling and sample-preparation strategy are
the major part of an IAQ assessment. The
strategy considers:
(1) type of effect, e.g. acute vs. chronic;
(2) patterns of occupant or worker exposure;
(3) pollutant type and potential health risks;
(4) pollutant sources;
(5) applicable regulations (for occupational air);
(6) applicable sampling/analysis methods;
(7) site selection;
(8) the number of samples and their statistical
significance; and,
(9) budgetary, site access, and logistical limitations [17].
The relatively small air volume in IA makes
it difficult to sample without disturbing the
sampled microenvironments. For this reason,
some outdoor air-sampling methods are not
suitable for IA.
IA samplers can be personal, portable and
stationary. Samplers can also be classified as
analyzers (for real-time monitoring) and collectors
(for time-weighted average (TWA) or long-term
monitoring).
Sampling methods may be passive or active.
Conventional air-sampling methods use a wide
variety of real-time analyzers, passive samplers,
whole air samplers and sorbent tubes. Inexpen-
sive multi-analyte analysis of residential IA
combining direct (instantaneous, real-time) and
integrated (long-term, TWA) is still in its
infancy.
SPME is well suited to IAQ assessment.
SPME has several qualities that are superior to
conventional methods. This review attempts to
summarize applications of SPME to VOCs in
occupational and residential IA, as reported in
recent years. Types of sample and sample-
preparation strategies based on SPME are iden-
tified and illustrated with references. Sampling
locations, sampling times, SPME coatings,
detected
compounds,
concentrations,
and
method
detection
limits
are
summarized.
Advantages and limitations of SPME-based
methods for IA sampling and analysis are also
discussed.
2. SPME
2.1. General characteristics
The original SPME design comprised poly-
mer-coated fused silica fiber housed inside a
needle [1–3]. Other SPME geometries and
phases have also evolved and are described
elsewhere [1–5].
SPME is a solvent-less sampling/extraction
and pre-concentration of analytes and is based
on partitioning between the polymeric phase
and the sample matrix. There are currently eight
SPME coatings commercially available. The
most popular for air sampling include poly-
dimethyl siloxane (PDMS), PDMS/divinyl-
benzene (DVB) and Carboxen/PDMS. The
PDMS coating is a non-porous, viscous liquid-
like polymeric phase, while the latter two can be
considered predominantly porous polymeric
phases. Extraction of analytes on PDMS is via
absorption, while it is adsorption for PDMS/
DVB and is likely to be capillary condensation
for Carboxen/PDMS. Although all analytes in
air will partition with the polymeric phase, each
coating has a different sensitivity and can be
used to provide selective air sampling, as was
demonstrated for on-fiber derivatization of
formaldehyde [18,19].
2.2. Sampling time and sampling modes
Typically, the sampling time is determined by
detector sensitivity and quantification require-
ments. Sampling times for SPME can range
from a few seconds to days for assessment of
short-term and long-term exposures, respec-
tively. Occupational exposures for gaseous pol-
lutants, such as threshold limit value (TLV),
recommended exposure limit (REL), and per-
missible exposure limit (PEL) are typically
defined in 8-hr intervals. Occupational short-
term exposure limits (STEL) are based on a
15-min TWA concentrations. The ‘‘immediately
dangerous to life and health’’ levels reflect an
instantaneous concentration. The occupational
thresholds can in some cases serve as surrogate
reference, although there are no regulations for
trends in analytical chemistry, vol. 21, no. 12, 2002
841
residential IA in the USA. SPME-fiber position
with the reference to the needle can be either
‘‘exposed’’ with the fiber outside the needle or
‘‘retracted’’ with the fiber inside the needle
(Fig. 1). The latter lends itself to long-term
sampling, while the former is used for spot
sampling. Selection of the sampling time and the
sampling mode is crucial for quantification.
2.3. Quantification with SPME
Quantification with SPME is complicated by
its variable sensitivity to all analytes and coating
types, and the effects of sampling time, air
temperature, relative humidity and air velocity.
2.3.1. Liquid (absorptive) coatings
For liquid (absorptive) coatings, such as
PDMS, sampling is typically conducted until
a partitioning equilibrium is reached between
target analytes in air and the SPME coating. The
main challenge is establishing the value of the
partitioning coefficient (K
fg
) for an individual
analyte and then adjusting it for the actual field-
sampling temperature and pressure. The values
of K
fg
can be determined through a series of
experiments involving the sampling of standard
gases or from their physicochemical properties
[20].
A more elegant way to establish the values of
K
fg
is based on the use of the linear temperature-
programmed retention index (LTPRI) system
first developed by Martos and Pawliszyn [20].
The LTPRI system is based on the chromato-
graphic
retention
of
n-alkanes.
A
linear
relationship allows for the determination of K
fg
at 25
C as a function of the LTPRI [20]. No
calibration is needed, and values of the K
fg
can
be established using chromatographic retention
times only. This approach was tested on the
standard gas mixture of 29 isoparaffinic and 33
aromatic compounds in air [21]. To date, the
LTPRI approach has been used for quantifica-
tion of VOCs in few applications involving real
IA [22,23].
A similar approach for establishing values of
K
fg
for the PDMS fiber coating was developed
by Bartelt [24]. He introduced a ‘‘calibration
factor’’, which is a surrogate equivalent of the
product of the K
fg
for the individual analyte and
the fiber-coating volume. Bartelt and Zilkowski
proposed a semi-empirical model for the cali-
bration factor as a function of LTPRI, sampling
temperature and a functional group [25]. The
functional groups include n-alkanes, esters,
ketones, aldehydes, alcohols, carboxylic acids,
amines and others [24]. This model was
developed based on sampling from moving air
streams with 71 standard gases and is applicable
to
both
equilibrium
and
non-equilibrium
conditions [25,26]. To date, no field applications
of this approach have been reported.
2.3.2. Solid (adsorptive) SPME coatings
Solid (adsorptive) SPME coatings are typically
more efficient in the sampling of highly volatile
organic
compounds
and
VOCs
[1,2,27].
Naturally, these coatings should be preferred
in some applications, particularly where short
sampling times are required.
In the past, quantification with solid SPME
coatings was often complicated by non-linear
extractions [27]. A possible solution based on
very short sampling times and extractions con-
trolled by diffusion through the boundary layer
(thickness ) surrounding the fiber was pro-
posed by Koziel et al. [28]. Constant extraction
conditions are maintained by exposing the fiber
to fast-moving air at constant velocity. The
main challenge in this method is establishing
Fig. 1. Schematic of sampling with exposed (for spot
sampling) and retracted (for TWA sampling) SPME fibers.
n
f
=amount of an analyte; K
fg
=air/coating partition coeffi-
cient (at equilibrium); V
f
=coating volume; C
g
=concentration
of analyte in air; D
g
=gas-phase molecular diffusion coeffi-
cient; A=needle opening area; Z=diffusion path length; and,
t=sampling time.
842
trends in analytical chemistry, vol. 21, no. 12, 2002
as a function of fiber-coating dimensions, dif-
fusion coefficients, air velocity, air temperature
and air viscosity. This approach was originally
developed
for
standard
gas
mixtures
of
benzene, toluene, xylenes and ethylbenzene
(BTEX) in air and later field tested in occu-
pational IA surveys [29].
2.3.3. On-fiber derivatization
On-fiber derivatization allows for very effi-
cient
extraction
of
formaldehyde
from
IA [18,19]. The derivatizing agent, water-soluble
o-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine
(PFBHA), is first doped in excess on the
PDMS/DVB 65-mm coating using headspace
Fig. 2. Strategies for SPME-based sampling and sample preparation for indoor air.
trends in analytical chemistry, vol. 21, no. 12, 2002
843
extraction immediately before exposing the fiber
to air. Formaldehyde in air reacts with the
PFBHA forming a stable derivative (PFBHA-
HCHO oxime). The on-fiber reaction is the
rate-controlling step and the amount of oxime
formed is proportional to the formaldehyde
concentration. This method has reported detec-
tion limits of less than 5 ppbv, well below the
current occupational TLVs. This on-fiber deri-
vatization method was tested in several IA
locations using 10-min. spot sampling and 8-hr
TWA sampling modes [19]. Martos
and
Pawliszyn suggested that the same approach
could be used for sampling and analysis of
acetaldehyde and other airborne aldehydes [18].
Velikonja et al. presented a similar approach
for the determination of formaldehyde [30].
This method used doping of PDMS 7-mm fiber
via
direct extraction of dinitrophenylhydrazine
(DNPH) or acetylacetone derivatizing agents.
Doping was followed by sampling of formalde-
hyde from vial headspaces. Limited field appli-
cations to the interior of new furniture have
been reported [30]. However, method detection
limits of approximately 140 ppbv were too high
to detect concentrations in a room with new
furniture.
Quantification of VOCs using the TWA-
sampling mode with retracted SPME fiber was
first described by Martos and Pawliszyn [31].
The distance between the fiber opening and the
fiber tip serves as the diffusion barrier/path.
The sampling rate is much reduced compared
to the exposed fiber mode, allowing for sig-
nificant extension of the sampling time. TWA
sampling is non-equilibrium sampling, since the
SPME sorbent cannot be affected by saturation
throughout the sampling session for quantifica-
tion purposes. The diffusion path-length can be
reduced or increased, providing flexibility in
extending or reducing the sampling time in the
field. Thus, the use of SPME devices for TWA
sampling presents the potential user with flex-
ibility in choosing a time appropriate for both
short-term and long-term sampling.
A commercial SPME holder can be modified
for TWA sampling by adding additional notches
for precise retraction of the SPME fibers (Fig. 1)
[22]. The use of TWA sampling for VOCs in IA
applications has been demonstrated in several
publications [22,23,31-33] and there has been one
on on-fiber derivatization of formaldehyde [19].
3. Applications to indoor air
3.1. Historical perspective
SPME evolved from initial applications to
direct extractions from aqueous samples to
Table 1
Summary of SPME applications to air sampling of laboratory air
Location
Sampling
time (min)
SPME coating
GC
detector
Analytes
Reported (range of)
concentrations
Method
Detection
Limit (MDL)
Environmental
conditions
Ref.
Laboratory 15 min
100-mm PDMS MS
11 VOCs
identified
N/A
N/A
T=24.5
C
RH=54%
[54]
Organics
laboratory
35 min
95-mm PDMS
MS
Dichloromethane N/A
N/A
N/A
[55]
Organics
laboratory
20 min
100-mm PDMS MS
5 chlorinated
VOCs
Toluene
26-420 ng/L
0.05-2 ppb
0.2 ppb
N/A
[56]
Laboratory 60 min
100-mm
PDMS,
C18-bonded,
silica-coated
multifibers
MS
N/A
N/A
< 1 ppb
N/A
N/A
[57]
844
trends in analytical chemistry, vol. 21, no. 12, 2002
Table 2
Summary of SPME applications to off site indoor air sampling followed by analysis in a laboratory
Location
Sampling time
(min)
SPME coating
GC
detector
Analytes
Measured
concentrations
Method
Detection
Limit
(MDL)
Comments
Environmental
conditions
Ref.
Laminated
particle board
Hair gel
20-60 sec
65-mm PDMS/
DVB
FID
Formaldehyde
640 ppb
4.6 ppb
HCHO derivatized
with PFBHA
N/A
[18]
Acrolein
72000 ppb
N/A
n-Valeraldehyde
45000 ppb
N/A
6 residential/
occupational
sites
10 min-
8 hr (TWA)
65-mm
PDMS/DVB
FID
Formaldehyde
11-376 ppb
1 ppb
HCHO derivatized
with PFBHA and
collocated w/
NIOSH-2451
T=19.5-28.5
C
RH=34-76%
[19]
Indoor area of
an industry
5-30 min
100-mm PDMS
PID
Styrene
56-130 mg/L
N/A
Spot and TWA
sampling
T=23
C
RH=25%
[20]
House,
apartment,
industrial
shops
10 min-
7 hrs (TWA)
65-mm
PDMS/DVB,
100-mm PDMS
FID
Formaldehyde
TVOCs
(C8-C12 range)
11-90 ppb
0.5-28 mg/m
3
1 ppb
N/A
HCHO derivatized
with PFBHA and
collocated w/
NIOSH-2451
N/A
[22]
Technological
laboratories
30-840 min
100-mm PDMS
FID
Acetone
1.76 mg/m
3
N/A
T=27-33
C
[23]
n-alkanes
(C5 to C15)
0.01-12.86
mg/m
3
N/A
RH=N/A
Chloroform
TEX
0.60-1.37
mg/m
3
N/A
0.12-22.27
mg/m
3
N/A
Vehicle and
mechanical
shops
30 sec
65-mm
PDMS/DVB
FID
BTEX
BDL- 249 ppb
2-18 ppb
Use of forced air
for quantitative
screening
Collocated with
NIOSH-1501
method
N/A
[29]
Room with
new & old
furniture
1 min
7-mm PDMS
ECD
Formaldehyde
1.3 mg/m
3
0.17 mg/m
3
HCHO found in
interior of new
furniture
T=23-24
C
RH=N/A
[30]
Unidentified
industrial site
7 hr
65-mm
PDMS/DVB
FID
Formaldehyde
57- 152 ppb
12.5 ppb
HCHO derivatized
with PFBHA
Co-located with
NIOSH-2451. TWA
sampling
T=23
C
RH=25%
[31]
(continued)
trends
in
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chemistry,
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12,
2002
845
Table 2 (continued)
Location
Sampling time
(min)
SPME coating
GC
detector
Analytes
Measured
concentrations
Method
Detection
Limit
(MDL)
Comments
Environmental
conditions
Ref.
Home/garage
120-
60-mm PDMS/
DVB
FID
n-alkanes
(C7-C12)
ND-0.78 mg/L
N/A
TWA sampling
collocated with
NIOSH-1550 method
N/A
[32]
Classroom,
210 min
grinding shop
Computer,
polymer
laboratories,
mailroom
75 min
10 min
100-mm PDMS,
PDMS/DVB(65)
FID
n-alkanes
(C5, C6, C12)
Formaldehyde
0.70-878 ppb
8.3 ppb
N/A
Spot/TWA sampling
collocated with
NIOSH-1550
method; HCHO
derivatized with PFBHA
N/A
[33]
Underground
parking lot
4 min
180-mm
MS
BTEX
4-33 ppb
1-10 ppb
Novel PDMS fiber
design
N/A
[45]
PDMS
n-Hexane
357 ppb
N/A
i-Octane
8 ppb
N/A
Organic
laboratory,
lilac bush
3 min
100-mm PDMS,
PDMS/DVB (65)
Carboxen/PDMS
FID
N/A
N/A
N/A
Commercial and novel
field samplers tested
for sample retention
N/A
[53]
Living room,
bedroom, and
laboratory air
15 min
100-mm PDMS
MS
BTEX
0.19-71.05
mg/m
3
0.002
mg/m
3
T=18-25
C
[58]
Chlorobenzene
2.15-18.65
mg/m
3
0.002
mg/m
3
RH=35.5-56%
n-Decane
0.05-3.84
mg/m
3
0.005
mg/m
3
TVOCs
1.8-63.9
mg/m
3
N/A
Indoor
swimming
pool
5 min
100-mm PDMS
MS
Trichloromethane
1.4-2.9 ppb
0.02 ppb
T=N/A
[59]
Tetrachloromethane
0.7-0.35 ppb
0.02 ppb
RH=N/A
Trichloroethylene
0.11-0.15 ppb
0.02 ppb
BTEX=benzene, toluene, ethylbenzene, and xylenes; TEX=toluene, ethylbenzene, and xylenes; ND=no detectable amounts; BDL=below detection limits.
846
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in
analytical
chemistry,
vol.
21,
no.
12,
2002
Table 3
Summary of SPME applications to sample preparation in conventional air-analysis methods, where the SPME was used only as a pre-concentrating device is in the
laboratory
Location
Sampling
time (min)
SPME
coating
GC
detector
Analytes
Measured
(range of)
concentrations
Method
Detection
Limit (MDL)
Comments
Environmental
conditions
Ref.
Headspace of
sewage tank
20 min
95-mm PDMS
ECD
6 chlorinated VOCs,
toluene
122-1959 ng/L
0.01-0.9 ppb Air sample collected
in SUMMA canisters
T=25
C
RH=25%
[56]
Gas-treatment
facility
10 min
100-mm PDMS
FID
BTEX
BDL- 189 mg/m
3
0.1 mg/m
3
Air samples collected
using Tedlar bags
T=23
C
RH=N/A
[60]
Smoking/non-
smoking rooms,
inside/outside of
laboratory bench,
car interior
30 min-
24 hr
75-mm Carboxen
PDMS
FID
BTEX
BDL- 70.0 mg/m
3
0.36-2.02
mg/m
3
SPME was used to
sample the headspace
of the solvent extraction
of charcoal tubes and
pads
T= 10-60
C
RH=N/A
[61]
Industrial area
(indoor/outdoor
not specified)
10 min
100-mm PDMS
MS,
CI, EI
14-Aromatic HCs
N/A
67 ng
SPME was used to
extract VOCs from
headspace of sorbent
tube adsorbent placed
in a sealed vial
T=100
C
RH=N/A
[62]
5-Chlorinated VOCs N/A
67 ng
8-Ketones
N/A
67 ng
4-Oxygenated VOCs N/A
67 ng
3-VOCs
N/A
67 ng
BTEX=benzene, toluene, ethylbenzene, and xylenes; BDL=below detection limits.
trends
in
analytical
chemistry,
vol.
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no.
12,
2002
847
headspace extractions, standard gases, spot
sampling of laboratory air, and eventually to
field air sampling [1–5]. Several studies using
headspace extractions could provide an insight
(coating
and
analytical
method
selection,
method detection limits, effects of temperature
or sampling time) to the development of
methods for VOCs that are important to IAQ.
Extractions of specific groups of VOCs from
vial headspaces include volatile amines [34],
ammonia and methylamine [35], volatile fatty
acids [36,37], and aromatic and halogenated
VOCs [38–40].
Studies with standard gases provided impor-
tant SPME characteristics including those listed
for headspace extraction and others, such as
humidity, air velocity, and sample-preservation
time. Specific groups of VOCs involving gas
standards and SPME include: sulfur VOCs
[41,42]; formaldehyde [18]; benzene, toluene,
ethylbenzene, xylenes (BTEX) [27,28,43–45],
isoparaffins and aromatic VOCs [21], halogen-
ated VOCs [43–45], n-alkanes, esters, ketones,
aldehydes, alcohols, carboxylic acids, amines
[24–26,46], and n-alkanes [32,47].
Several research articles involving SPME
sampling from moving/dynamic standard gas
samples
are
also
available
[18,20,21,24–
26,28,46,48,49]. In addition, SPME has also
been used to sample human breath [50,51], and
bovine breath [52].
Another important characteristic for field
applications, i.e. the retention of air samples on
SPME fiber coatings, has been researched
[22,41,49,53].
Comparison of novel SPME-based field
samplers with a commercial SPME field
sampler has also been described [53].
3.2. Strategies
To date, several strategies have been used in
applications of SPME to sampling and analysis
of IA (Fig. 2).
The first strategy is to use SPME for test
sampling of laboratory air (Table 1). Several
authors report sampling laboratory air [54–57].
In this case, no sample preservation is needed,
Table
4
Summary
of
SPME
applications
where
fi
eld
SPME
sampling
was
combined
with
on-site
analysis
with
a
portable
GC
Location
Sampling
time
(min)
SPME
coating
GC
detector
Analytes
Reported
(range
of)
concentrations
Method
Detection
Limit
(MDL)
Comments
Environmental
Ref.
Paint,
grinding,
carpenter,
and
vehicle
shops
1
min
65-
m
m
PDMS/DVB
Mobile
GC/PID
BTEX
Hexane
BDL-953
ppb
BDL-468
ppb
1.3-1.9
ppb
8.6
ppb
Collocated
sampling
with
the
NIOSH-1501
method
T=N/A
RH=N/A
[22]
Garage,
hall,
of
fi
ce,
solvent
storage
1
min
65-
m
m
PDMS/DVB
Mobile
GC/PID
BTEX
Hexane
BDL-573
ppb
BDL-575
ppb
1.3-1.9
ppb
8.6
ppb
Collocated
sampling
with
the
NIOSH-1501
method
T=N/A
RH=N/A
[27]
Living
room,
kitchen,
bedroom
1
min
65-
m
m
PDMS/DVB
Mobile
GC/PID
Toluene
24.1-35.8
ppb
1.3
ppb
Collocated
sampling
with
the
NIOSH-1501
method
T=35-40
C
RH=N/A
[33]
BTEX=benzene,
toluene,
ethylbenzene,
and
xylenes;
BDL=below
detection
limits.
848
trends in analytical chemistry, vol. 21, no. 12, 2002
because sample analysis was performed within a
very short time following the sample collection.
Chemicals found included aromatic and chlori-
nated hydrocarbons. A summary of these
applications including locations, sampling time,
SPME coating, compounds detected and their
range of concentrations is presented in Table 1.
The second strategy is the use of SPME as a
field sampler followed by analysis in the labora-
tory [18–20,22,23,29–33,45,53,58,59] (Table 2).
In such cases, some means of sample preserva-
tion was used, such as novel field samplers, low
temperature, or selection of a SPME coating
with high affinity for a particular group of
analytes. Several researchers studied sample
preservation on SPME fibers [22,41,49,53,55].
However, relatively little is known about SPME-
sample stability.
The third strategy is to use SPME as a sample
pre-concentration device in the laboratory
[56,60–62] (Table 3). In this case, sampling is
conducted with conventional methods, such as
Summa canisters [56], Tedlar bags [60] or sor-
bent tubes [61,62]. SPME served only to extract
analytes from Tedlar bags, Summa canisters, or
the headspace of sorbent tube extracts to
enhance the method detection limits or to speed
up the extraction process.
Finally, SPME can also be used for field
sampling combined with on-site analysis with a
portable GC [22,27,33] (Table 4). This approach
allows for collection and fast analysis of multiple
samples in the field. This is likely to be the most
efficient use of SPME to result in high sample
throughput and low cost per sample. On-site
analysis allows for greater flexibility in conduct-
ing an IA survey. This is because it makes
possible spot and TWA sampling, on-site
investigations of leaks and sources [27]. The
number of samples that can be collected within
a given sampling period and the relatively low
cost of such sampling serves are advantages.
The lower sensitivity of a portable GC (as
compared to stationary, full-scale GC) can be
offset by the sensitivity of SPME.
SPME
offers
many
advantages
for
air
sampling. These relate to its high sensitivity and
precision, speed of extraction, wide range of
sampling times, applicability to a wide rage of
compounds, reusability, possibility of automa-
tion, and compatibility with conventional analy-
tical equipment. To date, SPME remains best
suited to a research setting in which sampling
and analysis are typically conducted by the same
person/team.
Some
of
the
disadvantages
include coating-quality issues [19,32], lack of
comprehensive
guides
to
quantification
methods, and the relative lack of field com-
parisons with conventional methods.
4. Summary and conclusions
SPME has great potential to be used for
sampling of VOCs in indoor and ambient air. It
is very sensitive, small, flexible as to the selec-
tion of sampling time and relatively inexpensive.
While SPME cannot replace some conventional
methods, it can provide a powerful alternative
or validation technique, particularly in research
settings. Quantification models exist and are
applicable to several types of coatings and
groups of VOCs. Some coating-quality issues
affect SPME performance and therefore its
wide acceptance by air-pollution practitioners.
There remain several unknowns in the use of
SPME for air sampling and analysis, and there
are many opportunities for research, including:
(1) the development of quantification models and their
comparison/validation with conventional methods
for a wide range of VOCs;
(2) determination of sensitivity to air temperature,
pressure, relative humidity, air or wind velocity, and
other environmental variables;
(3) comprehensive evaluation of sample-preservation
techniques for both commercial and prototype
SPME devices; and,
(4) standardization and dissemination of protocols for
SPME-based methods.
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Jacek Koziel is an assistant professor at the Texas Agricultural
Experiment Station, Texas A&M University in Amarillo, Texas,
USA. He uses SPME for characterization and assessment of
abatement strategies for odorous gases. Inman Novak is a senior-
year student at the Amarillo Area Center for Advanced Learning.
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trends in analytical chemistry, vol. 21, no. 12, 2002