GC WITH ATOMIC EMISSION DETECTION IN ENVIRONMENTAL ANALYSIS
Gas Chromatography with
Atomic Emission Detection
in Environmental Analysis
Stig Pedersen-Bjergaard
University of Oslo, Oslo, Norway
1 Introduction
2 Selectivity and Sensitivity Considerations
3 Compound Independent Calibration for
Quantitative Analysis
4 Estimation of Molecular Formulas
5 Environmental Applications
5.1 Tin-containing Compounds
5.2 Lead-containing Compounds
5.3 Mercury-containing Compounds
5.4 Pesticides
5.5 Chlorinated Biphenyls and Phenols
5.6 Other Compounds Containing
Nonmetallic Elements
6 Current Status and Future Directions
Abbreviations and Acronyms
Related Articles
References
When capillary gas chromatography (GC) is coupled with
atomic emission detection (AED), mixtures of volatile and
semivolatile organic compounds are first separated based
on different retention in a capillary GC column, where-
after the separated compounds are introduced directly into
a helium (or argon) plasma. The high temperature of
this plasma results in atomization of the separated com-
pounds followed by excitation of the constituent atoms.
From the excited states, the atoms emit light of char-
acteristic wavelengths which are monitored continuously
during the chromatographic separation by an optical spec-
trometer. This results in element-selective chromatograms,
where all elements from the periodic table (except helium
or argon) may be monitored selectively with a sim-
ple change of wavelength on the spectrometer. With the
use of multichannel spectrometers, several elements may
be monitored simultaneously resulting in multielemen-
tal detection. Both nonmetallic and metallic elements are
detected with a very high selectivity. This enables environ-
mental contaminants containing heteroatoms to be deter-
mined in dirty extracts without extensive sample cleanup.
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1
However, since detection limits (DLs) in GC/AED range
from 1 – 100 pg s 1 , extensive analyte enrichment is often
required prior to environmental analysis. Because the sep-
arated compounds are atomized within the plasma, only
minor structural variations are observed for the detector
responses. This, in combination with the multielemental
capability, enables estimation of empirical formulas for
each of the separated compounds, which may be utilized
to support identification of environmental micropollutants.
In addition, the structure-independent detector responses
enable simplified calibration for quantitative purposes
1 because different compounds may be quantified based
2 on a single elemental calibration curve.
4
5
1 INTRODUCTION
7
When capillary GC is coupled with AED, high separation
7
9 power and simultaneous multielemental detectability
9 are combined into an attractive (hyphenated) analytical
10 technique GC/AED. Volatile and semivolatile organic
11 compounds present in complex mixtures are separated
in the GC and subsequently introduced into a small
12 helium (or argon) plasma placed in continuation of
the GC column (Figure 1). The high temperature of
12 this discharge (3000 – 10 000 K) results in atomization of
12 each of the separated compounds followed by excitation
13 of the constituent atoms to higher electronic states.
Light of wavelengths characteristic of the elements
13
introduced are emitted by the excited atoms as they
undergo transitions to lower energy levels. With an optical
spectrometer, emission light for the elements of interest is
selected and measured continuously resulting in element-
selective chromatograms. Since atomic lines are narrow
and often intense, GC/AED provides high elemental
selectivity and acceptable sensitivity. Theoretically, every
element from the periodic table (except helium or argon)
may be detected by a simple change of wavelength.
Since all emission lines are present in the plasma
simultaneously, either single- or multichannel detection is
possible. Compared with the array of selective detectors
responding to one or two elements (e.g. flame photometric
detection (FPD), nitrogen – phosphorus detection (NPD),
sulfur chemiluminescence detection (SCD), oxygen-
flame ionization detection (O-FID)), this multielemental
capability represents a major improvement in terms of
versatility.
The attractive features of GC/AED were reported
for the first time in 1965 by McCormick et al. with an
atmospheric pressure argon microwave induced plasma
(MIP) coupled to packed column GC..1/ Although the
period 1965 – 1975 also saw research into direct current
discharges,.2/ most GC/AED research was carried out
2 ENVIRONMENT: WATER AND WASTE
Injector
Plasma
generator
GC
column
* 837.6 nm
Gas chromatograph
Plasma
Helium
Figure 1 Principle of AED in capillary GC.
with systems utilizing argon MIPs or reduced-pressure
helium MIPs. Unfortunately, the excitation potential
of the argon plasmas was insufficient for the detection
of several nonmetallic elements, and the evacuation
equipment required to produce low-pressure helium
plasmas was complex. Therefore, the introduction of
the TM010 cavity by Beenakker in 1976 represented a
distinct technical improvement in the field of GC/AED
because this permitted helium MIPs to be sustained at
atmospheric pressure..3/ Implementation of the TM010
cavity by other workers was reported from 1978 – 1980,
which almost terminated the interest for reduced-pressure
MIP systems.
Although most effort has been focused on MIP
systems, after 1980, successful GC detection was accom-
plished with several alternative discharges, including
a 25 kHz helium after-glow device,.4/ a 350 kHz radio
frequency helium plasma,.5,6/ a 60 Hz alternating cur-
rent helium plasma,.7/ a 27.18 MHz capacitively coupled
helium plasma,.8/ and a 27.12 MHz stabilized capacitively
coupled helium plasma..9/ In addition, with argon at
atmospheric pressure, direct current plasmas (DCPs).10/
and inductively coupled plasmas (ICPs).11/ have been
evaluated, but both plasma systems suffered from poor
excitation characteristics for several important nonmetal-
lic elements and from a large consumption of high-purity
argon.
GC/AED was carried out solely with laboratory-
built instrumentation until the late 1970s, when the
first commercial atomic emission detector for GC was
introduced by Applied Chromatography Systems. This
equipment was based on a reduced-pressure helium
MIP and a Rowland circle spectrometer with 12 fixed
channels for simultaneous multielement detection..12/
However, the popularity was low, and even a modified
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Emission intensity
C
940.5 nm
Spectrometer
Cl
S
921.3 nm
Retention time
version based on an atmospheric-pressure helium MIP
sustained in a TM010 cavity was implemented only in
a limited number of research laboratories. In 1989,
a second attempt was made by Hewlett-Packard to
commercialize an atomic emission detector for GC. A
totally automated benchtop system was introduced, which
utilized an atmospheric-pressure helium MIP for analyte
excitation and a photodiode array for the monitoring
of atomic emission..13,14/ The photodiode array, which
covered the wavelength range from 160 – 800 nm in
25 nm portions, provided simultaneous multielement
detection, multipoint spectral background correction,
and elemental confirmation by atomic emission spectra.
From the same company, an improved version of
this atomic emission detector was recently introduced
as a less expensive second-generation instrument with
enhanced sensitivity. The two commercially available
GC/AED systems from Hewlett-Packard have increased
the interest for the technique substantially, and several
environmental applications of GC/AED have emerged
in recent years. Below, advantages and limitations of
GC/AED for environmental analysis are discussed and
some of the most interesting environmental applications
are reviewed. Principal attention is focused on results
obtained with the commercial system, while only a
few data from home-built systems are included owing
to the difficulties of reproducing this type of complex
instrumentation.
2 SELECTIVITY AND SENSITIVITY
CONSIDERATIONS
Environmental samples are typically very complex with
a large number of matrix components, among which
GC WITH ATOMIC EMISSION DETECTION IN ENVIRONMENTAL ANALYSIS 3

the analytes of interest are present at low concen-
tration levels. Therefore, both selectivity and DLs
are important parameters for the successful determi-
nation of most environmental micropollutants. In this
section, attention will be focused on both of these
parameters in order to understand the advantages
and the limitations of GC/AED for environmental
analysis.
As atomic emission lines are very narrow, overlap from
different elements is normally not a problem in GC/AED.
However, emission spectra from helium plasmas utilized
for GC/AED normally also contain molecular bands
(originating from incomplete atomization or from atomic
recombinations) which are generally relatively broad.
Unfortunately, these may interfere with the atomic lines
of interest causing false positive signals (interferences)
or negative baseline excursions. Therefore, in order
to realize the full potential of the narrow atomic
emission lines and to ensure high elemental selectivity,
spectral background correction is of great importance
in GC/AED..15/ With commercial instrumentation, this
is accomplished utilizing a photodiode array for the
optical measurements, where continuous multipoint data
correction results in very high selectivity for the most
important elements found in GC amenable compounds.
This is illustrated in Table 1, where the selectivity for
several metallic and nonmetallic elements has been
determined relative to carbon. With chlorine as an
example (selectivity value of 27 000), 27 000 ng carbon
(from a hydrocarbon) is required to produce the same
signal on the chlorine channel as obtained from 1 ng of
chlorine. For practical work with environmental samples,
the high elemental selectivities obtained by GC/AED is
Table 1 Selectivities and DLs for the second generation of the
commercial GC/AED system from Hewlett-Packard.16/
Element Wavelength (nm) Selectivitya
(pg s 1 )b
C 193 – 0.6
H 656 – 0.2
F 690 166 000
Cl 837 27 000
Br 827 15 000
N 174 7 000
O 171 18 000
S 181 37 000
P 186 14 000
Sn 326 3 300 000
Hg 254 258 000
Pb 406 286 000
a Selectivities were defined as the ratio of the response per nanogram
of element to the response per nanogram of carbon.
b DLs were defined as the amount of element required to produce a
peak twice the noise level, divided by the full width at half-height of
the peak in seconds.
obviously a major advantage. Organic micropollutants
containing heteroatoms (such as Cl, Br, S, Sn, and Hg)
may be selectively detected even in very complicated
extracts where the resolving power of GC is insufficient.
This is illustrated in Figure 2, where GC/AED was utilized
for the detection of polychlorinated biphenyls (PCBs) in
a highly contaminated marine sediment..17/ In spite of
the high background from a crude oil matrix, the PCBs
emerged as distinct peaks in the highly selective chlorine
trace. Thus, the PCBs were easily located in the chlorine
trace and quantitative analysis was rapidly performed
because no interferences distorted the peak areas. The
highly contaminated sediment sample was also exposed
to analysis by GC/MS,.17/ but this technique suffered from
serious interference when operated both in the low- and
high-resolution modes (Figure 2). Thus, although selected
ion monitoring was utilized, localization and quantitation
of the PCBs were almost impossible based on the GC/MS
results.
In addition to selectivity considerations, DLs of
GC/AED are of great importance in evaluating the poten-
tial for environmental analysis. As illustrated in Table 1
for the commercial system, DLs of GC/AED are gener-
ally at the low picograms per second level. Unfortunately,
values for the different elements vary by a factor of 200
depending on several factors such as atomic line inten-
sity, excitation potential, and natural background in the
plasma. For oxygen, an important element in environmen-
tal micropollutants, the DL is relatively high and therefore
the practical utility of O-selective detection by GC/AED
is strongly limited for environmental applications. DLs
for chlorine and bromine, which are important elements
within environmental monitoring, were relatively high for
the first generation of the Hewlett-Packard GC/AED, but
significantly lower values have been reported especially
for chlorine with the new version..17/ Thus, especially
with the second generation of GC/AED, the technique
DL may be an alternative for the determination of pesti-
cides and polyhalogenated compounds such as PCBs
(discussed in detail in sections 5.4 and 5.5). For sulfur,
phosphorus, and most of the metallic elements, DLs
10.7 are at the low picograms per second level supporting
13.0 the idea that compounds containing these elements may
15.3
be monitored at relatively low concentration levels by
4.6
43.4 GC/AED.
0.6 From the discussion above, high elemental selectivity
0.5 is the major advantage of GC/AED for environmental
0.4 analysis. Thus, organic micropollutants containing het-
0.6
eroatoms may be selectively detected in complicated sam-
0.2
ples without serious interference, and time-consuming
sample cleanup may be reduced. However, for some
elements DLs are relatively high, which may limit the
applicability of the technique or which may call for
extensive analyte preconcentration in order to match

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4 ENVIRONMENT: WATER AND WASTE

138
16

153

118

101

180
12
52

156

28

5
8

4
(a) 0 5 10 15 20 25 30 35 40 45 50 55 60 65 70 75 80 85 90 95 100 105 110 115 120 125 130

Figure 2 GC analysis of an extract of a highly contaminated marine sediment by (a) GC/AED in the Cl-selective mode and by
GC/MS in the (b) low- and (c) high-resolution modes (summarized ion selective chromatograms for molecular ions of PCBs)..16/
(Reproduced from Chromatographia, 43, 44 – 52, 1996, with permission from Vieweg.)

the low concentration levels typical for environmental
samples.
3 COMPOUND INDEPENDENT
CALIBRATION FOR QUANTITATIVE
ANALYSIS
During detection, the compounds separated by GC are
atomized within the AED and emission is measured
from excited atoms. Therefore, in theory, the detec-
tor response per element (area counts per nanogram
of element) should be independent of the molecular
structure from which it originated. For quantitative pur-
poses, this should enable universal calibration where
a large number of different compounds are quanti-
fied based on a single elemental calibration curve (e.g.
for chlorine) obtained for a randomly selected refer-
ence compound. Unfortunately, for practical work, this
type of universal calibration is somewhat complicated
by discrimination during GC injection and by chemi-
cal reactions/spectral interferences occurring within the
plasma. As illustrated in Table 2 for some PCBs, devi-
ations up to 10% occurred when the chlorine signal
from a standard solution of PCB no. 128 was uti-
lized for the quantitation of the other PCBs included
in Table 2..17/ Nevertheless, for the determination of
organic micropollutants, purchase of reference material
is expensive and in several cases, reference standards for
the compounds are not commercially available. Thus, for
applications where very high accuracy is not required,
analysis by GC/AED and universal calibration may be
a very fast and simple concept to obtain quantitative
data.

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GC WITH ATOMIC EMISSION DETECTION IN ENVIRONMENTAL ANALYSIS 5
100%
m/z 188 + 222 + 256 + 290 + 324 + 358 + 392 + 426 + 460 + 494
95
90

85

80
75

70

65
60

55

50
45

40
35
30

25
20

15

10
5
0
(b) 4:17 8:34 12:50 17:07 21:23 25:40 29:56 34:13 38:29 42:46 47:03 51:19

Figure 2 (Continued)

4 ESTIMATION OF MOLECULAR the molecular formula for several halogenated alkylben-

FORMULAS
With GC/AED operated in the multielement selective
mode, where several different elements are monitored
simultaneously, the resulting element-selective chro-
matograms directly give qualitative information about
the constituent elements for each of the separated com-
pounds. With peak no. 5 in Figure 3 as an example, where
halogenated alkylbenzenes were detected in nickel indus-
try wastewater, the element-selective chromatograms
proved that C, H, and Cl were all present in the compound,
while Br was not a constituent of this particular com-
pound. In addition to this, since elemental responses
are almost independent of molecular structures (as dis-
cussed in section 3), the element-selective chromatograms
also contain quantitative information about the elemental
composition for each of the separated compounds. Thus,
based on simple calibration and multielemental detec-
tion, empirical/molecular formulas may be calculated
based on GC/AED. This is illustrated in Table 3, where
zenes present in nickel refinery wastewater (Figure 3)
was calculated based on dichlorobenzene as reference..18/
Although deviations up to 30% from correct values
were observed in some cases, the approximate empirical
formulas were utilized to support rapid analyte identi-
fication. For target compound analysis, where analyte
identification principally is based on retention time data
obtained with standard solutions of the components of
interest, empirical formulas calculated by GC/AED may
significantly improve the reliability of analyte identifica-
tions. For nontarget purposes, however, where retention
time information normally is not available, identification
based solely on GC/AED is unreliable and should be
based principally on GC with mass spectrometric or
infrared detection..19,20/ Although identification is based
on GC/MS, results from GC/AED may be of great interest
to complement mass spectral data. This is illustrated in
Figure 4, where chromatograms from both GC/MS and
GC/AED analysis of an extract of a pulp mill effluent are
shown..19/ The compound corresponding to peak no. 4
was identified as tetrachlorothiophene (C4 Cl4 S) based on

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6 ENVIRONMENT: WATER AND WASTE

m/z 188.0393 + 222.0003 +

255.9613 + 289.9224 + 323.8834

138

m/z 357.8444 + 391.8055 +

425.7665 + 459.7275 + 493.6885

156
153

209

180

(c) 4:41 9:22 14:03 18:43 23:24 28:05 32:46 37:27

Figure 2 (Continued)

library search on the GC/MS system. This conclusion was
supported by the GC/AED results proving that C, Cl,
and S were present in the compound while H and O
were absent. For peak no. 5, no library mass spectrum
was available and manual interpretation was necessary.
The mass spectrum (Figure 4) revealed the presence of
three chlorine atoms and a molecular mass of 216. Unfor-
tunately, the mass spectrum also contained fragments
from co-eluting compounds, and further interpretation
was therefore difficult. However, the GC/AED results

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GC WITH ATOMIC EMISSION DETECTION IN ENVIRONMENTAL ANALYSIS 7

Table 2 Normalized chlorine response factors (area

counts per nanogram) for selected PCB congeners 5

Congener No. of chlorine Normalized chlorine

number atoms response factora C 247.9 nm
(2nd order)
31 3 0.974
53 4 1.049
105 5 1.000
128 6 0.966 12
185 7 1.018 4 6
194 8 1.050
3
209 10 1.059
a Chlorine response factors normalized against congener no. 105.
5

demonstrated that C, H, S, Cl, and O were all present in H 486.1 nm

the compound. Based on this additional information, and
assuming also that peak no. 5 was a thiophene, the com-
pound contained one S atom, three Cl atoms, and at least
four C atoms (C4 Cl3 S corresponds to 185 mass units). 2
The remaining mass difference up to 216 was 31, and for 1 4 6
this part of the molecule, the GC/AED results proved
3
the presence of a single O atom. The 31 mass units
probably corresponded to a methoxy group ( OCH3 ),
and the compound was suspected to be an isomer of 5
trichloromethoxythiophene.

5 ENVIRONMENTAL APPLICATIONS Cl 479.5 nm

Based on the discussion in sections 2, 3, and 4, the

1
major limitation of GC/AED is related to relatively 6
high DLs for some of the nonmetallic elements, while
the major advantages are related to the high selectivity,
the multielemental capability, and the possibilities of
performing universal calibration (quantitative analysis) 2 4
as well as estimating empirical/molecular formulas.
Based on these characteristics, important environmental Br 478.6 nm
applications will be reviewed in this section (section 5).

3
5.1 Tin-containing Compounds
Substantial research has been reported on the GC/AED
determination of organotin compounds originally used
as antifouling paints on ships, slimicides, pesticides,
and as stabilizers in polyvinyl chloride. Thus, organotin 12 14 16 18 20
compounds have been determined in sediments,.21 – 27/
Time (min)
soil,.23/ water,.22,26 – 31/ and biological samples.21,24,25/
by GC/AED. An example is illustrated in Figure 5, Figure 3 GC/AED analysis of an extract of nickel industry
where tin-organic compounds were detected in mussel wastewater in the C-, H-, Cl-, and Br-selective modes..18/
tissue..24/ Excellent selectivity has been reported for (Reproduced by permission of ‘MicroSeparations. Molecular
GC/AED operated in the Sn-selective mode. For complex Formula Determination of Halogenated Compound in Environ-
mental Samples Using GC and AED’, S. Pedersen-Bjergaard,
environmental samples, the selectivity of GC/AED T.N. Asp, J. Vedde, T. Greibrokk, J. Microcolumn. Sep.
significantly exceeded both GC/MS.26/ and GC/FPD..21/ Copyright. Reprinted by permission of John Wiley & Sons,
In addition to the high selectivity, the presence of Inc.)

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8 ENVIRONMENT: WATER AND WASTE

Table 3 Molecular formulas determined by GC/AED
for six halogenated alkylbenzenes present in nickel
refinery waste water.18/
Peak no. Correct formula
1 C9 H9 Cl3
2 C9 H10 Br2
3 C9 H10 Br2
4 C9 H10 Br2
5 C9 H9 Cl3
6 C9 H9 Cl3
tin was confirmed in the case of GC/AED utilizing
atomic emission spectra obtained by the photodiode
array and stored during each GC analysis..21/ The DL
of the commercial GC/AED has been reported to
be comparable with GC/FPD,.27/ which is the most
popular detector for Sn-selective detection. GC with
Formula determined atomic absorption spectrometry has also been utilized
by GC/AED for Sn-selective detection, but this technique was 1 – 2
orders of magnitude less sensitive than GC/AED..24,27/
C8.8 H8.3 Cl3
C11.3 H13.2 Br2 When operated in the selected ion monitoring mode,
C8.1 H7.9 Br2 GC/MS was found to provide only slightly better DLs
C7.3 H7.2 Br2 than GC/AED.26/ supporting the idea that GC/AED
C9.0 H8.6 Cl3 is highly attractive for Sn-selective detection. With
C8.2 H7.9 Cl3
GC/AED, organotin compounds have been detected
down to the 0.1-ng L 1 level in water samples.28 – 31/
and to the 0.2-ng g 1 level in sediments..23,25/ While
quantification by GC/MS required references for each of
the compounds of interest, several tin-organic compounds

Total ion current chromatogram

2 5 7
3 4 6

100 200 300 400 500 600

3:25 6:47 10:10 13:33 16:55 28:18

Mass spectrum of peak no. 5 201

100

80 79

60
210

175
40

87 103
47
20
52 68 95
56 110 124 147 153 150 178
73 130 162168 181 191
0
60 80 100 120 140 160 180 200 220
(a) Time (min)

Figure 4 GC analysis of an extract of a pulp mill effluent by (a) GC/MS and by (b) GC/AED in the C-, H-, Cl-, S-, and O-selective
modes..19/ (Reproduced from Chromatographia, 35, 193 – 198, 1993, with permission from Vieweg.)

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GC WITH ATOMIC EMISSION DETECTION IN ENVIRONMENTAL ANALYSIS 9

Cl 479.5 nm
8

3
4
5
6
2 7

8
1 3

C 247.9 nm
(2nd order) 4
5 8
6
S 180.7 nm
2 7

2
3 5
6 7
4

8
O 777.2 nm
H 486.1 nm

3 5
3 5
7 6 7
2 6 8

0 5 10 15 20
(b) Time (min)

Figure 4 (Continued)

have been quantified by GC/AED utilizing universal
calibration..26,28/ In addition, tin-organic compounds have
been identified based on empirical formulas calculated
from GC/AED results..22/
5.2 Lead-containing Compounds
In addition to tin-organic compounds, GC/AED has
been successfully applied for the determination of lead-
containing compounds in water,.32 – 34/ road dust,.34/ and
snow..35/ With emphasis on organolead compounds used
as antiknock additives in gasoline, GC/AED was found
to be substantially more sensitive than GC coupled
with atomic absorption spectrometry,.32/ the latter of
which has been the most popular technique for Pb-
selective detection in capillary GC. Thus, with GC/AED,
organolead compounds were detected at the 0.1 – 2-ng L 1
level in water.32,33/ and down to the femtogram per gram
level in snow..35/ As for tin, GC/AED is very attractive
also for lead compounds because of excellent selectivity
and sensitivity.
5.3 Mercury-containing Compounds
Organomercury compounds have been utilized in paints,
wood preservatives, paper, and pesticides, and this class of

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10 ENVIRONMENT: WATER AND WASTE

Bu3Sn+
32 58 HgII
Emission intensity

30 57
MeHg+
28 56
Bu2Sn2+ Ph2Sn+
26
54 Hg 254
BuSn3+
24
53
22
52

6 8 10 12 32 Me3Sn+
Retention time (min)

Emission units
30

Figure 5 GC/AED analysis of an extract of mussel tissue in 28

the Sn-selective mode..24/ (Reproduced by permission LC – GC
International, Advanstar Communications Inc.)
compounds is of great importance within environmental
monitoring. GC/AED operated in the Hg-selective mode
has been used for the determination of organomercury
compounds present in biological samples.36,37/ and in
water..38/ Compared with gas chromatography/electron
capture detection (GC/ECD), which is in frequent use
for the detection of organomercurals, the selectivity
was superior utilizing GC/AED while DLs of the two
detectors were comparable..36/ Thus, with GC/AED,
organomercury compounds were detected down to the
low nanogram per liter level in water..38/
Owing to the simultaneous multielement capability
of GC/AED, several reports have emerged where tin,
lead, and mercury compounds have been determined
simultaneously in biological material,.39/ soil,.40/ and
water..41/ An example of this is illustrated in Figure 6,
where both organotin and organolead compounds were
found in river water..41/ This, in addition to excellent
selectivity and sensitivity, suggests that GC/AED is
a very attractive technique for the determination of
organometallic compounds in environmental samples.
5.4 Pesticides
Several publications have focused on the GC/AED
determination of pesticides in environmental and agri-
cultural samples. This broad class of compounds, which
are produced industrially as agricultural chemicals,
are particularly good candidates for GC/AED analy-
sis since they are rich in heteroatoms such as chlo-
rine, bromine, fluorine, phosphorus, sulfur, nitrogen,
and oxygen. Thus, pesticides have been detected in
different vegetables,.42 – 46/ soil,.47,48/ and water.48 – 53/ uti-
lizing GC/AED. An example is illustrated in Figure 7,
where several pesticides were detected in an onion
sample by GC/AED..43/ Excellent selectivity has been
reported in the chlorine-selective mode for different
26
Me2Sn2+
24 MeSn3+
Sn 271
22
7
6
5
4
Pb 261
3
1.5 2.0 2.5 3.0
Retention time (min)
Figure 6 GC/AED analysis of an extract of river water in
the Hg-, Sn-, and Pb-selective modes..41/ (Reproduced by
permission of The Royal Society of Chemistry.)
pesticides present in agricultural products, while the
established ECD (electron capture detection) and elec-
trolytic conductivity detection (ELCD) devices suffered
from matrix-related interferences..42,43/ Thus, a GC/AED
screening method has been tentatively approved by the
US Environmental Protection Agency for inclusion in
the Update IV of the SW-846 methods..48/ In addition,
GC/AED was found to provide accurate quantitation
based on a single chlorine calibration curve (univer-
sal calibration). Unfortunately, the pesticide DL in the
chlorine-selective mode of the first generation of the
commercial GC/AED system was found to be a factor
of 102 – 104 higher than for GC/ECD..54/ Thus, exten-
sive analyte preconcentration was required to detect
organochlorine pesticides by GC/AED at the 0.01 ppm
level in agricultural matrices..43/ With the second gener-
ation of the commercial GC/AED system, the sensitivity

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DOI: 10.1002/9780470027318.a0824
GC WITH ATOMIC EMISSION DETECTION IN ENVIRONMENTAL ANALYSIS 11

C-496 nm

4
9 + 10 11 12
Cl-479 nm

Br-479 nm

"6" "9 + 10" "12"

"11"
S-181 nm

N-174 nm
9
6

P-178 nm

10 15 20 25 30 35
Minutes
Figure 7 GC/AED analysis of an extract of onion in the C-, Cl-, Br-, S-, N-, and P-selective modes..43/ 4 D g-HCH, 6 D parathion,
9 D bromophos ethyl, 10 D a-endosulfan,11 = b-endosulfan, and 12 D endosulfan sulfate. (Reproduced from the Journal of High
Resolution Chromatography, 16, 539 – 548, 1993, with permission from Hüthig-GmbH.)

problem is expected to decrease, and GC/AED pesticide
DLs (concentration units) have been improved by a fac-
tor of 100 compared with 1-ml injections by performing
large volume injections (100 ml) with a solvent vapor exit
in front of the analytical column..49,52/
In addition to chlorine-selective detection, GC/AED
in the bromine-, phosphorus-, sulfur-, and nitrogen-
selective modes has been reported for the determination
of pesticides. While bromine-selective detection is used
only occasionally, several papers have emerged utilizing
phosphorus-selective detection. The selectivity has been
reported to be excellent in different agricultural matri-
ces, and superior to results with both NPD and FPD
detection..42,43/ The phosphorus DL of GC/AED was
found to be comparable with FPD,.43/ but significantly
higher than for NPD..54/ Nevertheless, organophospho-
rus pesticides have been detected down to the 0.01-ppm
level in plant foodstuffs by GC/AED utilizing 1 ml
injections..42,43/ With 100 ml injections, even lower DLs
have been obtained in the phosphorus-selective mode
utilizing a solvent vapor exit in front of the analytical
column..51,52/ Quantitative results from GC/AED were in
excellent accord with data from NPD, and GC/AED was
also found to enable accurate quantitation based on uni-
versal calibration in the phosphorus-selective mode..48/
Some of the commercial pesticides also contain sulfur,
and these may be selectively detected by GC/AED
operated in the sulfur-selective mode. With the com-
mercial GC/AED system, which is relatively sensitive
towards sulfur (Table 1), DLs for sulfur-containing pes-
ticides were lower than with FPD,.43/ and the linearity
problems of the FPD were eliminated..55/ Some pesti-
cides also contain nitrogen and oxygen, but GC/AED
is relatively insensitive towards these elements owing to
atmospheric contamination of the plasma. Nevertheless,
pesticides have been detected by GC/AED in several
environmental samples utilizing nitrogen-selective detec-
tion. The method was limited to pesticides present above
the 1.5 – 25-ng level in the final extracts, and the GC/AED
DLs were found to be a factor of 103 – 104 higher than
for NPD..54/
5.5 Chlorinated Biphenyls and Phenols
Among the large number of polyhalogenated organic
micropollutants included in environmental monitoring

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12 ENVIRONMENT: WATER AND WASTE

programs, most attention has been focused on the micropollutants have been detected by GC/AED, includ-
GC/AED determination of PCBs. These compounds, ing polychlorinated dibenzodioxins (PCDDs), volatile
which were used as, for example, electrical insula- organochlorines, trichloroacetic acid, chlorinated by-
tors and flame retardants until the 1980s, have been products of humic and fulvic acids, chlorinated aromat-
detected by GC/AED in human blood,.56/ seal blubber,.56/ ics, polybrominated biphenyls (PBBs), polybrominated
beef tallow,.57/ fish oil,.57/ fish liver,.58/ and marine diphenylethers (PBDEs), iodated herbicides, volatile sul-
sediments..16,58/ In addition to PCBs, their methylsul- fur compounds, nitrosubstituted aromatics, and nitro
fonyl metabolites have also been detected in seal blubber musks. More information on these applications as well as
by GC/AED..56/ With GC/AED, excellent selectivity others can be found in a review article concerned with
has been reported for PCBs in the chlorine-selective environmental applications of GC/AED..61/
mode (Figure 2)..16/ Thus, GC/AED has been successfully
applied for the determination of PCBs in highly contami-
nated marine sediments, while the established techniques 6 CURRENT STATUS AND FUTURE
of electron capture and mass spectrometric detection suf- DIRECTIONS
fered from matrix interferences..16/ Additionally, quan-
tification was significantly simplified by GC/AED because
The literature reviewed in the present paper has demon-
responses were dependent solely on the moles of chlo-
strated the great potential of GC/AED for analysis of
rine present.16,57,58/ (see also Table 2). Thus, individual
organic micropollutants. Owing to the elemental capa-
PCB congeners and total PCB were quantified with a
bility, GC/AED enables rapid screening by elemental
single chlorine calibration curve (universal calibration).
content of environmental samples, provides important
Unfortunately, with the first generation of the commercial
structural information complementary to mass spectral
GC/AED instrument, individual PCBs were not detected
data, and enables simplified quantitation based on univer-
below the 250 – 400-pg level..16,57,58/ This was a factor of
sal calibration with a single elemental calibration curve.
104 higher than reported with ECD, and a factor of 102
Particularly for environmental analysis, which frequently
higher than with electron ionization mass spectrometric
is complicated by matrix constituents, the very high
detection in the selected ion monitoring mode. There-
elemental selectivity of GC/AED may reduce both inter-
fore, extensive analyte preconcentration was required to
ference and the demands of sample cleanup. However,
obtain DLs at the 0.15-ppm level for individual PCB
as pointed out above, DLs of GC/AED are relatively
congeners in fat..57/ Minor technical modifications of the
high for some elements and extensive analyte precon-
commercial GC/AED instrument have been found to
centration may be crucial. This, in combination with
improve PCB DLs by a factor of approximately 5,.56/ but
the lack of low-price commercially available instrumen-
even these values are relatively high for PCB applications.
tation, currently limits the propagation of GC/AED in
Thus, while GC/AED may be utilized for contaminated
environmental laboratories.
samples, the technique is currently not an alternative for
For the future, therefore, it is hoped that the number of
the monitoring of PCB background levels.
companies committed to producing GC/AED instrumen-
In addition to PCBs, some GC/AED interest has been
tation will increase to reduce the price level of this highly
focused on the determination of chlorophenols (CPs)
versatile technology. With some further effort to improve
which originate as industrial byproducts. With principal
DLs and to include the concept in standard procedures for
attention on water, GC/AED was found to provide
the monitoring of organic micropollutants, GC/AED may
excellent selectivity for CPs in the chlorine-selective
rapidly become a ‘‘work horse’’ in laboratories concerned
mode, and CPs were determined in water below the
with environmental chemistry.
0.5-ppb level..59,60/

5.6 Other Compounds Containing Nonmetallic

ABBREVIATIONS AND ACRONYMS
Elements
Above, attention was focused on organic micropollu- AED Atomic Emission Detection
tants containing metallic elements (Sn, Pb, Hg), pesti- CP Chlorophenol
cides, PCBs, and CPs. For all of these contaminants, DCP Direct Current Plasma
substantial research has been documented within the DL Detection Limit
literature utilizing the commercial GC/AED system, ECD Electron Capture Detection
and GC/AED has been demonstrated to be an attrac- ELCD Electrolytic Conductivity Detection
tive alternative to existing methods. In addition to the FPD Flame Photometric Detection
above mentioned components, several other organic GC Gas Chromatography

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DOI: 10.1002/9780470027318.a0824
GC WITH ATOMIC EMISSION DETECTION IN ENVIRONMENTAL ANALYSIS 13

GC/ECD Gas Chromatography/Electron Chromatographic Detector’, Spectrochim. Acta, Part B,

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NPD Nitrogen– Phosphorus Detection Chromatogr., 11, 75 – 81 (1988).
O-FID Oxygen-flame Ionization Detection 6. S. Pedersen-Bjergaard, T. Greibrokk, ‘On-column Bro-
PBBs Polybrominated Biphenyls mine- and Chlorine-selective Detection for Capillary
PBDEs Polybrominated Diphenylethers Gas Chromatography Using a Radio Frequency Plasma’,
Anal. Chem., 65, 1998 – 2002 (1993).
PCB Polychlorinated Biphenyl
7. R.B. Constanzo, E.F. Barry, ‘Alternating Current Plasma
PCDD Polychlorinated Dibenzodioxin
Detector for Selective Mercury Detection in Gas Chro-
SCD Sulfur Chemiluminescence Detection
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8. D. Huang, D.C. Liang, M.W. Blades, ‘Capacitively Cou-
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Environment: Water and Waste (Volume 3) ‘Element Specific GC-detection by Plasma Atomic Emis-
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Current Atmospheric Pressure Argon Plasma Emission
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