Hello! This is the first of the “new” 1998 incarnation of the ISPAC newsletter. I am now serving as the sole editor of this newsletter, after almost 4 years as co-editor. First I have one obligation which would be to thank Art Greenberg for our 3+ years of collaboration as co-editors of the newsletter in its previous conformations. I will generally follow the style and layout of those past newsletters that Art was so key in creating. This, in turn, relied some on the initial work that Doug Lane did when ISPAC was still the informal network known as the International Committee on
Polycyclic Aromatic Compounds and his ICPAC newsletter. I hope to build on both of their hard work.
In the past, Art and I ended up putting out a newsletter about once a year. I know I can also speak for Art in first offering our apologies for that infrequency. We both have some of the usual excuses. First, we were both busy, and second, it was much more difficult trying to coordinate when
Art was first in New Jersey and then in North
Carolina and I was clear across the United States in
California.
I hope to streamline the process of gathering the items and composing the text, and thus (hopefully) getting more newsletters out. My initial goal will be to have the newsletter issued semi-annually, but I hope that it will grow into a quarterly schedule. From past experiences this could be both ambitious and daunting.
The content of the newsletter is open, so I am asking each of you to send me any info items or news in the fields of polycyclic aromatic compounds research. This would include sources of compounds, references from lesser-known publications, or anything else that you think would be of interest. This newsletter can be a good vehicle for the sorts of info that we regularly spread through our own individual networking.
Also, if perchance one of you gets ambitious too, please volunteer to write the research synopsis/main feature. It has been brief, 1-3 pages
(but possibly more) that are aimed at letting other researchers who are working in others areas of polycyclics know about your field. Past topics have included PAH spectra and astrophysics, the Martian meteorite findings, and others. At times I will be personally soliciting these articles from those of you who I think have a good story to tell.
Items can be sent to John Fetzer, Chevron
Research and Technology Company, P.O. Box
1627, Richmond, CA 94802 USA, e-mailed to jcfe@chevron.com
, or faxed to 510-242-1792.
Also, please send any address changes or additions of colleagues who might be interested in receiving a copy of the newsletter or becoming a member of ISPAC. I am putting together an
“address book” database, and especially would like e-mail addresses for people (hopefully in the nottoo-distant future we will electronically send out information to the bulk of the members).
FOCUSED MICROWAVE-ASSISTED
EXTRACTION OF POLYCYCLIC
AROMATIC HYDROCARBONS
M. Letellier, H. Budzinski, and P. Garrigues
LPTC
UPRESA 5472 CNRS
University of Bordeaux I
33404 Talence, France
ABSTRACT
Focused microwave assisted extraction
(FMW) was used to extract Polycyclic Aromatic
Hydrocarbons (PAHs) from environmental matrices. The procedure was validated on a marine

sediment, the Standard Reference Material SRM
1941a (NIST, Gaithersburg, MD, USA). The concentrations obtained by the FMW method are in agreement with the certified values and the concentrations obtained by Soxhlet. The average recoveries of individual compounds are 89% compared to certified values and 96% compared to
Soxhlet. The coefficients of variation are lower or equal than those obtained by Soxhlet (<10%). This method allows a reduction of time (10 minutes) and a reduction of solvent volume (30 mL). The results show that the FMW extraction at atmospheric pressure is an interesting alternative to Soxhlet extraction for PAH analysis.
Keywords: Microwave, PAHs, extraction.
INTRODUCTION
Organic contaminant analyses in environment require complex procedures with several steps such as extraction, purification, and quantification. The extraction is often performed by reflux of organic solvent. This method is long
(several hours) and solvent consuming (several hundreds of milliliters). Some new techniques have been developed in the last few years [Supercritical fluid extraction (SFE), Accelerated solvent extraction (ASE), Microwave-assisted extraction
(MAE)] to replace classical extraction techniques.
Microwave digestor, often used for mineralization in trace element analysis (1), represents an interesting alternative method in the case of organic contaminant extraction. Different apparatus have been investigated. Some studies (2-
6), using closed vessels, showed that microwave assisted extraction under pressure of organic contaminants can substitute conventional extraction techniques like Soxhlet extraction. Other studies
(7-9) showed the efficiency of Focused microwaveassisted extraction (FMW) at atmospheric pressure of contaminants in environmental matrices.
This study describes the principles and the advantages of FMW method. This method has been validated for the extraction of Polycyclic Aromatic
Hydrocarbons (PAHs) using a certified matrix, the
"Standard Reference Material, SRM 1941a" (a marine sediment distributed by NIST, Gaithersburg,
Maryland, USA). The possible improvement of the extraction recovery and the application to other classes of compounds are discussed.
MATERIALS AND METHODS
Standards, Solvents, and Reagents
The studied PAHs range from triaromatics to hexaaromatics: Phenanthrene (P), Anthracene
(A), Fluoranthene (Fluo), Pyrene (Pyr),
Benz[ a ]anthracene (BaA), Chrysene coeluting with
Triphenylene (Chr + Trip), Benzo[ b ]fluoranthene coeluting with Benzo[ k ]fluoranthene
Benzo[ j ]fluoran-thene (BF), Benzo[ e ]pyrene (BeP),
Benzo[ a ]pyrene (BaP), Perylene (Per),
Indeno[ 1,2,3 -cd]pyrene (IP), Benzo[ g,h,i ]-perylene
(BP), Dibenz[ a,h ]anthracene coeluting with
Dibenz[ a,c ]anthracene (DaA).
The compounds used as internal standards were perdeuterated PAHs. Phenanthrene-d
10
,
Fluoranthene-d
10
, Pyrene-d
10
, Chrysene-d
12
,
Benzo[ a ]pyrene-d
12
and Benzo[ g,h,i ]perylene-d
12
.
Solvents (pestinorm or HPLC grade), standards and reageants are the same as described in
Reference 9.
Matrix
Standard Reference Material, SRM 1941a,
"Organics in Marine Sediment," was provided by the National Institute of Standards and Technology
(NIST, Gaithersburg, Maryland, USA). It is a marine sediment collected from Chesapeake Bay at the mouth of Baltimore Harbor. The sediment is freeze-dried, sieved (150-250 µm particles), homogenized, and sterilized (10).
Extraction Procedure
Microwave Apparatus
Focused Microwave (FMW) assisted extractions in open cells were performed at a frequency of 2450 MHz using a Soxwave 100 apparatus (Prolabo, Fontenay-sous-Bois, France) with a programmable heating power (from 30 watts to 300 watts). The Soxwave proceeds at atmospheric pressure. Its schematic diagram is presented in Figure 1.
Procedure
The FMW and Soxhlet extractions were performed using 1 g of freeze-dried sediment. A solution containing the perdeuterated PAHs used for the quantification was added to the matrix prior

Figure 1: Microwave Apparatus (SOXWAVE 100,
Prolabo, France) to the extraction. The FMW extraction was performed at 30 watts during 10 minutes with 30 mL of dichloromethane. The FMW extract was filtered. Soxhlet extractions with dichloromethane
(2 x 250 mL) lasted for 48 hours. Blank experiments were performed and used for correcting the concentration if needed.
FMW and Soxhlet extracts were reduced to a small volume (a few milliliters) using a rotary evaporator. The organic extract was desulfurized on activated copper. Then it was purified on a micro-column of alumina and on a micro-column of silica (11). The purified aromatic fraction was finally reconcentrated to few microliters in isooctane and analyzed by Gas Chromatography coupled to Mass Spectrometry (GC/MS) operated under single ion monitoring (9).
RESULTS AND
DISCUSSION
Principle of Extraction Under Microwave
The principle is the heating of the solvent and the matrix by interactions of wave/matter (1).
The microwave energy is converted into heating by two mechanisms, the dipole rotation and the ionic conductance. The heating is selective. Only polar or moderately polar compounds can be heated.
The dichloromethane is chosen for its polarity; it is able to absorb and transmit the energy of microwave beam. Moreover this solvent is a good solvent for aromatic compounds.
Advantages of FMW Method
The use of Soxwave apparatus allows homogeneous and reproducible treatment of the sample owing to the focusing of the microwave on the medium. The heating at the boiling temperature is very rapid (less than 1 minute at 30 watts). There is no inertia.
This method is secure, because the extraction is performed at atmospheric pressure.
There is no risk of explosion. The temperature of extraction is the boiling point of the solvent. There is no problem of compound degradation by high temperature. It does not need cooling after the extraction.
This method is not time consuming. Only
10 minutes are required (7). Only 30 milliliters are necessary for the extraction of 1 gram of contaminated matrix. This apparatus allows the treatment of large amount of matrix up to 30 grams.
Extraction of PAHs From SRM 1941a
Efficiency of FMW to extract contaminants has been tested on a certified matrix, the SRM
1941a, which is a natural marine sediment.
Three Soxhlet and three FMW extractions have been performed. The comparison of certified values with concentrations obtained by Soxhlet and
FMW extraction of dry matrix is shown in Figure 2.
Figure 2: Comparison of concentrations (ng/g) of
PAHs in SRM 1941a obtained by Soxhlet and
Focused microwave-assisted extraction (FMW) with and without 30% of moisture with certified values.

The FMW recoveries compared to Soxhlet extraction vary between 71% to 97%. The average recoveries of individual compounds are 80% compared to certified values and 87% compared to
Soxhlet. The coefficients of variation are in the same order of magnitude than those obtained by
Soxhlet (<10%). There is no selectivity of extraction between the different compounds.
The FMW technique gives satisfactory results in only 10 minutes and with a low quantity of solvent.
Improvement of Extraction
For some matrices, the extraction recoveries can be improved with optimization of parameters. Percentage of moisture of the matrix has been found the most important parameter
(8,12). The addition of about 30% of moisture (g of water per g of sediment) can improve the extraction depending on the nature of the matrix. In these conditions, the average recoveries of individual compounds for SRM 1941a are 89% compared to certified values and 96% compared to Soxhlet
(Figure 2). Nature of solvent and power can also be optimized (12).
Applications
This method can be applied to the extraction of other classes of compounds (nalkanes, pesticides, PCBs...) and other matrices
(soil, atmospheric particulate, source rocks, biological tissues...) (8,9,13,14) with good extraction recoveries and reproducibilities and the same advantages of reduction of solvent and time.
CONCLUSIONS
Focused microwave assisted extraction of organic contaminants allows a considerable time saving and a notable reduction of solvent volume.
The recoveries and reproducibilities are good and comparable to those obtained by conventional techniques (resp. >80 and <10%). The longest step in the procedure of preparation and analysis of
PAHs becomes the step of analysis.
ACKNOWLEDGMENTS
PROLABO (France) is acknowledged for financial support and the loan of the microwave system. S.Wise (NIST, USA) is acknowledged for
Standard Reference Material supply.
REFERENCES
1.
Zlotorzynski A (1995) Critical Reviews in
Analytical Chemistry 25:43.
2.
Lopez-Avila V, Young R, Beckert WF
(1994) Anal Chem 66 : 1097.
3.
4.
Onuska FI and Terry KA (1993)
Chromatographia 36:191.
Paré JRJ, Belanger JMR (1994) Trends
5.
6.
Anal Chem 13:176.
Ganzler K, Salgo A and Valco K (1986) J
Chromatogr 371:299.
Barnabas IJ, Dean JR, Fowlis IA, Owen SP
7.
8.
9.
(1995) Analyst 120 : 189.
Budzinski H, Papineau A, Baumard P,
Garrigues P (1995) C R Acad Sci Paris t.321
Serie II b:69.
Budzinski H, Baumard P, Papineau A,
Wise S, Garrigues P, (1996) PAC Journal
9:225.
Letellier M, Budzinski H, Garrigues P,
Wise S (1997) Spectroscopy 13:71-80.
10.
National Institute of Standards and
Technology, USA (1994) Certificate of analysis for Standard Reference Material
1941a, Organics in Marine Sediment.
11.
Behar F, Leblond C, Saint-Paul C (1989)
Rev Inst Français du Pét 44:387.
12.
Letellier M, Budzinski H, Charrier L,
Capes S, Dorthe AM (submitted to
Frenesius’ Journal of Analytical
Chemistry).
13.
Letellier M, Budzinski H, LeMenach K,
Garriques P, Focused microwave assisted extration of Polycyclic Aromatic
Hydrocarbons from standard reference materials and natural matrices, 16th
Annual Symposium on Polycyclic
Aromatic Compounds, Charlotte, USA,
November 4-8, 1997.
14.
Letellier M, Budzinski H, Le Menach K,
Garrigues P, Focused Microwave assisted extraction of organic contaminants (PAHs,
PCBs, Pesticides, alkanes) from environmental matrices, presented at 8th
Annual Meeting of SETAC-Europe,
Bordeaux, France, April 14-18, 1998.

ISPAC WEB PAGE
By Douglas A. Lane
At the recent ISPAC conference, Stan
Townsend and Douglas Lane volunteered to set up a web page for the society. The basic structure of the page has been established and created. We hope to have the page up and running soon. The server on which it will exist is yet to be determined but I anticipate that it will be on one of the Environment
Canada servers and that it will be placed there at no charge to the society.
We intend to place information on the following areas of interest on the web page:
ISPAC Executive and Board of Directors :
This will include a list of all executive and board of directors showing the terms of office, affiliation and e-mail addresses. In addition, there will be photographs and short biographies of each of the executive.
How to Become a Member of ISPAC :
This will detail the steps one takes to become a member. We should have a blank application form which can be downloaded and sent in electronically to our membership chairman.
History of ISPAC : This is being compiled and will include the history of the International
Symposium on PAH, the International Committee on PAC, the merger of the two organization, the awards presented by the society, the recipients of the awards, the locations of the past conferences, society presidents from the merger on, and how to find the proceedings of all conferences.
Subcommittees : When subcommittees have been established, the chairman, contact information, mandate, and subcommittee members will be found here.
Conference 1997 : A summary of the conference will appear here. We have not yet established the content of this section.
Conference 1999 : On this page, we will, as information becomes available, indicate the location of the conference, registration information, information links for the particular area, and registration forms if possible. Also, the call for papers will appear here.
ISPAC News and Newsletters : Stay tuned for late breaking news from ISPAC and catch up on the ISPAC newsletters.
Polycyclic Aromatic Compounds - The
Journal : Information on submitting articles to the journal and hot-links to the publisher will appear here. As will any other important information regarding the journal.
Recommended Nomenclature for PAC :
The nomenclature breakfasts at previous ISPAC conferences were a big hit and demonstrated that we have a lot to learn about how to name and classify the PACs. Here, recommended nomenclature discussions and lists will appear.
Suppliers of Chemical Standards for
PACs : A list of commercial and non-commercial suppliers of common and rare PAH will be listed.
If e-mail addresses and/or web-page listings are available, they will be included. Of course, mailing addresses will appear. This list will include suppliers worldwide.
Links to Other Relevant Pages : If you have a favorite web page for PAC or can recommend a page, whether it be government, industry or private, please let me know.
If you can assist by supplying information on any of these topics, could help to create a section, or have other areas which you would like to see covered on the ISPAC web page, please send me an e-mail message at Douglas.Lane@ec.gc.ca.
16 th INTERNATIONAL SYMPOSIUM
The Sixteenth International Symposium on
Polycyclic Aromatic Compounds (ISPAC-16) was held November 4 th through 8 th in Charlotte, North
Carolina, USA. Approximately 170 scientists attended.
New Society officers and board members were elected as part of the meeting. The new president is Philippe Garrigues of the Universite Du
Bordeaux. The president-elect is Louise Ball of the
University of North Carolina at Chapel Hill. The treasurer is Debra Costa of the Us Environmental
Protection Agency in Chapel Hill, North Carolina; and the secretary is John Fetzer of Chevron
Research and Technology Company, Richmond,
California. Officers’ terms are 1997-1999, with the president-elect serving as president for the next term of 1999-2001.
The board members are split into two categories, 2-year term and 4-year term, to ensure some carry over and continuity. The 2-year members are Ron Harvey of the Ben May Institute in Chicago, Illinois; Frieke Ariese, Uwe Kirso;
Willie May of the National Institutes for Standards and Technology in Gaithersburg, Maryland; and
Steve Wise also of NIST. The 4-year members are

Bill Baird of Oregon State University, Corvallis,
Oregon; Doug Lane, Ontario, Canada; Brian
McCarry, Ontario, Canada; Tuan Vo-Dinh, Oak
Ridge National Lab, Oak Ridge, Tennessee; and
David Warshawsky.
The biennial award for research in polycyclic aromatic compounds was presented to
Roger Atkinson of the University of California at
Riverside. This was in recognition for his many contributions to the understanding of the fate of
PACs after their release into the atmosphere during combustion. The Society would like to thank Bill
Baird, chairman of the awards committee, and his fellow members for the work they put into the selection process and the presentation.
Brian McCreary of Ontario, Canada, gave a vivid and very entertaining description of the fire.
He and his students collected and analyzed samples collected from the emissions cloud.
SEVERAL LESSER-KNOWN SOURCES OF
PACs HAVE SENT NEWLY AVAILABLE
CATALOGUES
ASTEC offers many thiophenic PACs, including methyl and other alkyl derivatives. Their address is Nottulner Landweg 90, Muenster
D-48161 Germany. Phone: 2534-8001-80, Fax number: 2534-8001-87. Their website is at http://www.uni-muenster. de/chemie/AC/anders/astec/welcome.html.
Chiron offers a variety of PACs, including certain large PAHs, including dibenzo[cd,lm]perylene (peropyrene), benzo[a]coronene, tetrabenzo[a,cd,j,lm]perylene, and isoviolanthrene.
Their address is Prof. Brochs gt. 6, N-7030
Trondheim, Norway. Telephone: 47-73-54-02-33,
Fax number: 47-73-54-02-32.
AccuStandard offers a few hard to find
PAHs such as periflanthene, dibenzo[a,l]pentacene, and many methylated PAHs. Their address is 25
Science Park, Hartford CT 05511 USA. Telephone:
01-203-786-5290 (in the USA 800-442-5290), Fax number: 01-203-786-5287.
PACs on the Internet!
In addition to the ISPAC website described in great detail elsewhere in the newsletter, there are several very useful PAC related sites. Lane Sander and Steve Wise NIST have put together a structure database for PAHs. It is arranged by molecular weight, includes many alternant and non-alternant structures, and gives computed values for each of the three dimensions of the structure. It is located at “http://ois.nist.gov/pah”.
Kiyokatsu Jinno’s research group in Japan has compiled a collection of reversed-phase HPLC chromatograms and diode-array UV absorbance spectra for many PAHs, including several large ones. The URL is http://chrom.tutms.ac.jp/ jinno/database.html
. A mirror site of this is operated by Jasco.

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