Extraction Adviser

for Environmental
Samples
Perfecting solvent extraction for optimized
environmental analysis

1
Abstract following advisor will showcase process parameters
and final data in the extraction of oil and grease in waste
Solvent extraction is an essential part of sample prepa- water, PAH and PCBs in sediments and atmospheric
ration for the analysis of environmental contaminants PCDD/F levels using the BUCHI UniversalExtractor
and residues. BUCHI’s UniversalExtractor E-800 offers E-800.
automated fast and reliable Soxhlet extraction for a wide
range of environmental samples. In this advisor, studies An extraction is usually part of the analytical procedure
with the determination of oil and grease in waste water, for the determination of organic pollutants in solid and
dioxin determination on air filters, as well as the deter- semi-solid matrices. The quality of the extraction influenc-
mination of PCBs and PAHs from sediment samples are es the accuracy of the results and the sample through-
presented. All results were in accordance with the ex- put as it is often the bottleneck of the entire procedure.
pected values. Thus, efficient and reliable extractions are a prerequisite
for successful determinations of environmental contam-
inants. Soxhlet, as the accepted standard method for
extraction, is widely used in the field of environmental
1. Introduction analysis.

The issue of environmental sustainability has steadily In the past two decades, modern extraction methods,
gained relevance for both the scientific community and such as pressurized solvent extraction, sonication and
the general public. The importance of protecting the en- microwave extraction have also found their way into en-
vironment and human health from pollutants has never vironmental analysis and official standard methods [1, 2].
been more obvious. The main advantages of these modern extraction meth-
ods over traditional Soxhlet are shorter extraction times
and higher sample throughput. This paper focuses on
the classic solvent extraction of environmental samples
using Soxhlet only. Determinations of environmental con-
taminants with high speed and throughput using pres-
surized solvent extraction using BUCHI’s SpeedExtractor
E-914 / E-916 are described elsewhere [3-5].

All modern extraction methods are always compared

and validated against Soxhlet. Numerous publications
compare these different extraction techniques, eg. [6-8].
The mostly cited disadvantages of the traditional Soxhlet
Figure 1: A safe, clean environment is a pre-requisite for good health method are the long extraction times and the large sol-
and a high quality of life.
vent consumption. Investing in an extraction unit that can
To efficiently prevent or clean-up contamination, pro- alleviate these issues without compromising quality can
cesses and methods used for environmental analysis help achieve optimized environmental anlaysis.
need to be robust, versatile and deliver dependable data.
BUCHI supports environmental protection initiatives by Automated Soxhlet, as provided by BUCHI’s powerful
providing market-leading solutions for reliable sample UniversalExtractor E-800, can substantially decrease the
preparation and analysis to companies, environmental extraction times and solvent consumption per sample
testing labs and government authorities. Our solutions compared to traditional Soxhlet set-ups with glassware.
comprise sample preparation and testing of air, soil, sed- The all-in-one universal extraction chamber of the Uni-
iment, sewage sludge, waste and waste water. versalExtractor E-800 supports five different extraction
methods. This unique multitasking feature enables indi-
Determining pollutants in environmental and food matri- vidual control and simultaneous operation of six indepen-
ces requires efficient sample preparation. Optimizing the dent extraction methods for fast method development
sample preparation step for a particular sample type is and high sample throughput.
key to achieving accurate environmental analysis. The
2
 ‘‘Oil and grease’’ is defined as any material recovered
such as a substance soluble in the solvent. It includes
other material extracted by the solvent from an acidified
sample (such as sulfur compounds, certain organic dyes,
and chlorophyll) and not volatilized during the test [15].
Oil and grease can be determined as a sum parameter
gravimetrically or by infrared absorption after solvent ex-
traction. Unlike infrared and gravimetric methods, the use
of GC-FID offers the potential to obtain details of the dif-
ferent types of hydrocarbons in the oil fraction [14].

According to the Standard AWWA 5520 part D Soxhlet

[15], the acifidied waste water sample is filtred on a muslin
cloth and paper filter disk. The dried filters are then ex-
Figure 2: UniversalExtractor E-800 tracted using hexane. The residue in the hexane extract
is then determined gravimetrically and corresponds to the
Examples of the use of BUCHI’s automated Soxhlet oil and grease content of the waste water sample.
extraction units in literature include PAH determination in
soil [9], determination of atmospheric PBDE levels [10], A sample was spiked with certified reference material
extraction of dioxin-like and endocrine disruptive com- (sunflower oil) which was equivalent to a pollution of 100
pounds from sediments [11], PCB, PAH and OCP deter- ppm. This sample was filtered, extracted and the recov-
mination in sediments [12] and obtaining the contamina- ery was determined. The extraction time was 4 h, as re-
tion profile of DDT by measurement of bioaccumulation in quired by the standard method [15]. Results are shown
Greenland sharks [13]. in Table 1.

Table 1: Determined blanks and recoveries of oil and grease

Some of the studies carried out on the UniversalExtractor
determination (mean values, n=3, rsd % in brackets)
E-800 by BUCHI in collaboration with universities and
service laboratories are presented below.
Blank 4.6 mg (11.3%)

Recovery 102.4% (2.5%)

2. Oil and grease in waste water
Oil is one of the most common types and highly visible
forms of water pollution. As oil can easily spread, even 3. Dioxins in air filters
small quantities can potentially cause harm to the aquatic
environment [14]. The amount of oil and grease in surface Air quality is an emerging concern for the human popu-
or groundwater is regulated by law in most countries. lations’ health, especially in urban areas where anthro-
pogenic activities and pollution sources coexist. Special
attention is devoted to airborne particulate matter (PM), a
mixture of microscopic particles and liquid droplets pres-
ent in the air that once inhaled could get into the lungs
and bloodstream. Dioxines are halogenated aromatic hy-
drocarbons formed as by-products of thermal processes
that may be unintentionally released into the environment
and attach to PM.

Air is sampled on PUF filters or Quarz fiber filters. The

Soxhlet extraction of the contaminated filters, as prepa-
ration for the analysis, is described in the EPA compen-

Figure 3: Waste water

3
dium TO-9 [16] and the determination of dioxins in EPA
1613 [17]. PUF filters were pre-extracted with Soxhlet as
a cleaning step. The spiked filters were then extracted
with Soxhlet warm using toluene as solvent for approx.
13 h, whereas the QFF were extracted with Soxhlet using
dichloromethane as solvent for 12 h. The concentrated
extracts were analyzed with GC-MS. The determined
recoveries were all within the 50-150% range (see table
2) as required by EPA 1613 [17]. Figure 4: Formula of Polychlorinated Biphenyles

Table 2: Determined recoveries [%] of dioxins on spiked PUF filters, n=

PCBs are toxic, persistent, they bioaccumulate in terres-
4. No analyte could be quanfitied in the blank sample.
trial and aquatic biosystems and are ubiquitous in the
Recovery, (rsd%) environment. Production and use is nowadays banned
nearly worldwide. A round-robin SETOC sediment sam-
13
C 2,3,7,8 TCDF 94.6 (16.7%) ple [18] was extracted according to EPA 3541 [19] us-
ing the Soxhlet warm mode. Hexane:Acetone 1:1 was
13
C 2,3,7,8 TCDD 115 (14.7%) used as solvent. The extracts were concentrated to a
final volume of 1 mL using BUCHI’s Syncore® Analyst.
13
C 2,3,4,7,8 PeCDF 88.1 (7.00%) An extraction time of 3 h is sufficient for the extraction
of PCBs from a sediment sample. The dermined values
13
C 1,2,3,7,8 PeCDD 60.0 (28.3%) were in accordance with the consensus values. A longer
extraction time did not result in higher recoveries (see
13
C 1,2,3,4,7,8 HxCDF 60.4 (10.3%) Figure 5).
PCB content [μg/kg]
13
C 1,2,3,6,7,8 HxCDF 55.1 (8.47%)

13
C 2,3,4,6,7,8 HxCDF 119 (8.65%)

13
C 1,2,3,4,7,8 HxCDD 99.6 (4.19%)

13
C 1,2,3,6,7,8 HxCDD 99.6 (7.13%)

13
C 1,2,3,4,6,7,8 HpCDF 95.7 (3.89%)

13
C 1,2,3,4,6,7,8 HpCDD 88.9 (3.62%)

13
C OCDF 80.2 (3.30%)

13
C OCDD 92.0 (4.86%)

2h 3h 4h SETOC 777

4. PCBs in sediment samples

Figure 5: Recovery of PCBs after 2h, 3h and 4 h of extraction, the
Polychlorinated biphenyls (PCBs) are a class of organic error bars indicate the accepted range (+/- standard deviation) of
the concensus value of the SETOC sample.
compounds based on biphenyl substituted with 1-10
chlorine atoms. There are 209 different congeners. To
simplify the description, they are usually specified with a
number from 1 to 209.

4
5. PAHs in sediment samples 6. Conclusion

PAHs occur in oil, coal and tar produced by carbon- BUCHI’s UniversalExtractor E-800 provides a powerful
ization of coal. They can also be found in grilled meat, solvent extraction solution designed specifically for chal-
cigarette smoke and automobile exhaust. PAH are per- lenging environmental samples. The extraction unit offers
sistent, ubiquitous and some of them have carcinogenic, ultimate time-savings through its smart design and true
mutagenic and teratogenic properties. There are more multitasking capabilities, which allow multiple indepen-
than 100 different PAH, but usually only the 16 PAH dent runs to be carried out simultaneously. More power
defined by the United States Environmental Protection through high speed heaters, intelligent level-sensors and
Agency (EPA) are analyzed. A round-robin SETOC sedi- magnetic valve design, sophisticated process control
ment sample [18] was extracted according to EPA 3541 and optimized glass parts lead to fast and efficient ex-
[19] using the Soxhlet warm mode. Hexane:Acetone 1:1 tractions even for high boiling solvents such as toluene.
was used as solvent and the overall extraction time was The flexibility of the all-in-one extraction chamber allows
3 h. The final results were within the indicated consensus users to choose the optimal method, ideal extraction
values of the SETOC sample (see Figure 6). temperature and sample-solvent interaction for any ap-
PAH content [μg/kg] plication, resulting in high recovery rates and low results
variation.
1000 1500 2000 2500

In this guide, we have demonstrated that the Universal

Extractor E-800 offers fully automated Soxhlet extraction
for fast and reliable extraction as a sample preparation
step for the determination of environmental pollutants.
Oil and grease from waste water, dioxins from air filters
and PCBs and PAHs from sediment samples were suc-
cessfully extracted. The recoveries and the determined
values were in accordance with the expected or certified
values.

Acknowledgements
We greatly acknowledge Dr. Francesco Saliu and Profes-
sor Marina Lasagni from the University of Milano Bicocca
for their support in the development of the study on the
air filters.

We greatly acknowledge Labor Veritas Zürich, Mr. Pascal

Leupin and Mr. Oleg Altergott for the analytics and their
UniversalExtractor E-800 SETOC support in the study of the PAHs and the PCBs in sedi-
ment samples.
Figure 6: Results of the PAH determination of a sediment sample us-
ing the UniversalExtractor E-800. The error bars indicate the accepted
range (+/- standard deviation) of the concensus value of the SETOC
sample.

5
References [10]  Degrendele, C. et al. 2018. Are atmospheric PBDE
levels declining in central Europe? Examination of the
[1]  EPA 3545A Test Methods for Evaluating Solid Waste: seasonal and semi-long-term variations, gas–particle
SW-846. Pressurized Fluid Extraction partitioning and implications for long-range atmospheric
transport. Atmos. Chem. Phys., 18, 12877–12890
[2]  LeBlanc, G. 2001. A review on EPA sample prepara-
tion techniques for organic compound analysis of liquid [11] Macikova, P. et al. 2014. Longer-term and short-
and solid samples. LCGC 19(11), 1120-1130. term variability in pollution of fluvial sediments by diox-
in-like and endocrine disruptive compounds. Environ Sci
[3] BUCHI Labortechnik. 2008. Determination of PAHs Pollut Res 21, 5007–5022.
in soil. Best@BUCHI 51/2008.
Available for download at https://www.buchi.com/sites/ [12]  Mitra, S. et al. 2019. Characterization, source iden-
default/files/downloads/BestBuchi_51_PAH_low_0.pdf tification and risk associated with polyaromatic and chlo-
rinated organic contaminants (PAHs, PCBs, PCBzs and
[4] BUCHI Labortechnik. 2016. High throughput ex- OCPs) in the surface sediments of Hooghly estuary, In-
traction for dioxin determination. Whitepaper dia, Chemosphere. 221, 154-165.
Available for download: https://www.buchi.com/sites/
default/files/downloads/20160524_Dioxin_in_different_ [13] Cotronell, S. et al. 2018. Contamination Profile
matrices.pdf of DDTs in the Shark Somniosus microcephalus from
Greenland Seawaters. Bulletin of Environmental Con-
[5]  BUCHI Labortechnik. 2015. Improved workflow in di- tamination and Toxicology. 101, 7–13.
oxin and PCB analysis. Whitepaper
Available for download: https://www.buchi.com/sites/ [14]  Ming, Y. 2016. Oil in water analysis, AWE Interna-
default/files/downloads/Whitepaper_Dioxin_and_PCB_ tional, published 6th Sept. 2016
in_foodstuff.pdf
[15]  AWWA (American Water Works Association) Stan-
[6] Sporring, S. et al. 2005. Comprehensive compari- dard method 5520, Part D Soxhlet.
son of classic Soxhlet extraction with Soxtec extraction,
ultrasonication extraction, supercritical fluid extraction, [16] EPA Compendium TO-9A. 1999. Compendium of
microwave assisted extraction and accelerated solvent Methods for the Determination of Toxic Organic Com-
extraction for the determination of polychlorinated biphe- pounds in Ambient Air.
nyls in soil Journal of Chromatography A, 1090, 1-9.
[17] EPA 1613 1994. Tetra-through Octa-Chlorinated
[7] Camel, V. 2001. Recent extraction techniques for Dioxins and Furans by Isotope Dilution HRGC/HRMS
solid matrices-supercritical fluid extraction, pressurized
fluid extraction and microwave-assisted extraction: their [18]  SETOC Round Robin, sample 777
potential and pitfalls. Analyst, 126, 1182–1193 http://www.wepal.nl/website/products/SEToc.htm

[8]  Itoh, N. et al. 2008. Comparison of low-level polycy- [19]  EPA 3541 Test Methods for Evaluating Solid Waste:
clic aromatic hydrocarbons in sediment revealed by Sox- SW-846. Automated Soxhlet
hlet extraction, microwave-assisted extraction, and pres-
surized liquid extraction. Anal. Chim. Acta. 612, 44–52.

[9]  Khan, Z.; Troquet J., and Vachelard, C. 2005. Sam-

ple preparation and analytical techniques for determina-
tion of polyaromatic hydrocarbons in soils-review paper.
Int. J. Environm., 2(3), 275-286.

6
Further reading

BÜCHI Labortechnik AG. Application note 374 / 2019 Oil

and grease in waste water,
Available for download: https://www.buchi.com/sites/
default/files/AN_374_2019_Oil_and_grease_in_waste_
water.pdf

BÜCHI Labortechnik AG. Application note 360 / 2019

Dioxin determination in ambient air,
Available for download: https://www.buchi.com/sites/
default/files/AN_360_2019_Dioxin_determination_in_
air_0.pdf

BÜCHI Labortechnik AG. Application note 359 / 2019

PCBs in sediment,
Available for download: https://www.buchi.com/sites/
default/files/AN_359_2019_PCB_determination_in_sed-
iment_0.pdf

BUCHI Labortechnik AG. Application note 358 / 2019

PAHs in sediment,
Available for download: https://www.buchi.com/sites/
default/files/AN_358_2019_PAH_determination_in_sed-
iment_0.pdf

7
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