Partner; Democritus University of Thrace (UTHR.DEE.APL) Workpackage; WP 4 and WP 1
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1 First report on Project Assessment of the selected POPs(PCBs,PCDDs/PsPOCPs) in the atmosphere and water ecosystems from the waste generated by warfare in the area of formal Yugoslavia Contract ICA2-CT Introduction Period 1 st from 01 Sep to 31 Aug Partner; Democritus University of Thrace (UTHR.DEE.APL) Workpackage; WP 4 and WP 1 This first report of the project Apopsbal is presenting some of the results from our sampling campaign in Serbia. Our main task is to investigate the level of PCBs in the atmosphere of some areas that have been destroyed from war activities. The results from the first and the last day of sampling as well as the results from qc exchange filters and pufs are presented in this report. Methodology Three high volume samplers used to sample air in Zastava factory in Kravugevac from to and in Pancevo industrial zone from to In Zastava factory two samplers have been placed inside the factory one at energetic building and other at FNP building (point K1 and K2 respectively). The third sampler used as background sampler located at the University of Kragujevac Department of Chemistry (point K3). All the samplers have been placed on the ground. Exact points can be seen on maps in Annex 1. In the Pancevo industrial zone one sampler have been placed inside the HNC refinery and other inside the Petrochemika Factory (point P1 and P2 respectively). Both samplers were placed on the ground. The roof of an eight floor building (Pancevo City Hall) have been used as the location of the third background sampler (point P3). One sampler was a GV2360 Thermoandersen TSP sampler used in the background sites. Other two samplers were made of stainless steel boxes equipped with 8X10 inches filter holder and 9cm-diameter puf holder 30 cm long. Air was drown using a 1200 watt motor controlled by an inverter (Hitachi L NPE) and flow was measured by a Sierra 620 fast flo insertion mass flow meter. The average total air sampled was 1200 cubic meters per day. One glass fiber 8X10 inches filter (Whatman grade G653) and three puf filters with density of 0,02 gr/cm 3, 9 cm diameter and 5 cm long were used for sampling. Sample analysis Glass fiber filters were burned in 400 C for 5 hrs and pufs filters were soxlet extracted by 1:1 acetone/hexane (Merk suprasolv) by a Foss Tecator Soxtec 1045 HT-2 apparatus for 4 hrs to 120 C, prior the sampling campaign. s and pufs have been placed in a zipped plastic bag after have been wrapped with aluminum foil. After sampling, filters (half of the filters were used) and pufs were extracted as described above. Methodology for clean up of samples is described in M. Mandalakis et al The extract was concentrated in a rotary evaporator and loaded onto a 1,5 g. silica gel column ( mesh, activated at 150 C for 4 h) and eluted with 12 ml of n-hexane (1,4 ml/min). the eluted fraction was reduced to 4 ml by a rotary evaporator and treated twice with 2 ml of concentrated sulfuric acid. Then the h-hexane phase was loaded onto a disposable Paster pipete with the following components: 1 cm of dehydrated NaSO 4, 1 cm of H 2 SO 4 impregnated silica, 1 cm of KOH impregnated silica and 1 cm of deactivated silica in seriers. This colum have been eluted with 6 ml of hexane. The extract was reduced by a rotary evaporator and further evaporated under a gentle nitrogen stream. An HP 5890 Series II chromatography instrument equipped with a Trio 1000 Mass spectrometer as detector have been used to analyze samples. The chromatography column was DB 5MS from J&W Scientific 60m long, 0,25 I.D. and 0,1m film. The GC oven operation conditions was Ramp 1; 40 o C hold 4 min, Ramp 2; 10 o C /min to 180 o C hold 2 min, Ramp 3; 4 o C/min to 300 o C hold 10 min, Injector temp 280 o C. The MS was manually tuned operated at 69 ev. The GC injector was operated splitless. Flow was set to 16 psi head pressure.
2 Analysis have been performed by using SIM Mode external standard. Calibration standard PESTI mix 13 was used from Dr. Ehrenstorfer laboratories. Area based calibration has been done from 0,01 ppm, to 10 ppm using 2l injections of calibration standard Compounds that have been calibrated are presented in the following table 1. Table 1. Calibrated compounds. ORDER OF Compound RT IONs used ELUTION MIN 1 A-HCH 24,05 181,183,219 2 HEXACHROROBENZENE 24,11 282,284,286 3 B-HCH 25,04 181,183,219 4 G-HCH 25,19 181,183,219 5 D-HCH 26,28 181,183,219 6 E-HCH 26,50 181,183, ,4,4 TRICHROROBIPHENYL 27,38 186,256,258 8 HEPTACHROR 28,11 272,274,337 29,00 220,290, ALDRIN R 29,41 263,265, ISODRIN 30,57 193,263, HEPTACHROR EPOXIDE 31,27 351,353, CHORDANE 31,27 375, HEPTACHROR EPOXIDE 31,40 351,353, CIS CHORDANE 32,27 375, ,4 DDE 32,35 246,248,318 (PCB 101) 32,46 254,326, ENDOSULFAN I 33,03 241,265, TRANS CHORDANE 33,03 375, ,4 DDE 34,03 246,248, DIELDRIN 34,16 263,277, ,4 DDD 34,22 165,235, ENDRIN 35,12 263,281, ENDOSULFAN BETA 35,45 241,265, ,4 DDD 35,59 165,235, ,4 DDT 36,04 165,235,237 36,30 290,360, ,4 DDT 37,14 165, 235,237 37,44 290,360, METHOXYCHLOR 40,20 152,227,228 40,45 324,394, MIREX 42,29 272,237,274 Quality control Reference material BCR 481 have been used to examine recovery and clean up methodology.. Exchange of 3 filters and pufs from campaigns between the laboratory of RECETOX and UTHR.DEE.APL have been performed to investigate convergence of air measurements. Results Average recovery found to be 75 % for pcb 101, 153 and180 From Recetox campaign exchanged filters and pufs results are presented in table 2. Table 2. Exchanged filters and pufs results in ng per cubic meter Compound
3 135 GF 1,2, 135 PUF 1,1, 139 GF 5,2, 139 PUF 5,1, 137 GF 3,2, 137 PUF 3,1, 2 HEXACHROROBENZENE nd nd 3 B-HCH nd nd nd nd 4 G-HCH nd nd nd nd nd nd 5 D-HCH nd nd nd nd nd nd 6 E-HCH nd nd nd nd nd nd 7 2,4,4 TRICHROROBIPHENYL nd bdl bdl nd bdl bdl bdl bdl bdl nd bdl bdl 11 ISODRIN nd bdl nd nd bdl nd (PCB 101) nd nd nd nd 20 4,4 DDE nd nd nd nd nd nd 22 2,4 DDD nd nd nd nd ENDOSULFAN BETA nd nd nd nd nd nd 25 4,4 DDD nd nd nd nd nd nd 26 2,4 DDT nd nd nd nd nd nd nd ,4 DDT nd nd nd nd nd nd nd nd MIREX nd nd nd nd nd nd Table 3. Exchanged filters and pufs results in ng per cubic meter from (UTHR.DEE.APL) Compound 411 filter 1/2 411 puf 333 filter 333 puf 1,2,1 121 puf 1/2 1st 1/2 1st 1/2 1st 2 HEXACHROROBENZENE B-HCH nd nd nd 0 4 G-HCH nd nd nd 0 5 D-HCH nd nd nd nd nd 0
4 6 E-HCH nd nd nd nd nd 0 7 2,4,4 TRICHROROBIPHENYL bdl bdl nd nd bdl bdl bdl bdl bdl ISODRIN bdl nd nd nd nd nd nd nd nd (PCB 101) 20 4,4 DDE nd nd nd nd nd nd 22 2,4 DDD nd nd nd ENDOSULFAN BETA nd nd nd nd nd 25 4,4 DDD nd nd nd nd ,4 DDT nd nd nd nd nd ,4 DDT nd nd nd nd nd nd nd MIREX nd nd nd nd nd nd Results from Kragujevac sampling period to are presented in table 4 Table 4. Results from Kragujevac in ng per cubic meter Point K1 Point K2 Point K3 Compound 1,1,1 1,1,1 1,2,1 1,2,1 1,3,1 1,3,1 2 HEXACHROROBENZENE nd nd B-HCH nd nd nd nd G-HCH nd nd nd nd nd D-HCH nd nd nd nd nd nd 6 E-HCH nd nd nd nd nd nd 7 2,4,4 TRICHROROBIPHENYL nd nd Bdl bdl bdl bdl
5 11 ISODRIN nd nd nd nd nd nd (PCB 101) nd nd bdl 20 4,4 DDE nd nd nd nd nd ,4 DDD nd nd 24 ENDOSULFAN BETA nd nd nd nd nd 25 4,4 DDD nd nd nd 26 2,4 DDT nd nd ,4 DDT nd nd nd nd nd nd nd 32 MIREX nd nd nd nd nd Results from Pancevo sampling period to are presented in table 5 Table 5. Results from Pancevo in ng per cubic meter Point P1 Point P2 Point P3 Compound 6,1,3 6,1,3 6,2,2 6,2,2 6,3,3 6,3,3 2 HEXACHROROBENZENE B-HCH nd nd nd nd 4 G-HCH nd nd nd nd nd 5 D-HCH nd nd nd nd nd nd 6 E-HCH nd nd nd nd nd nd 7 2,4,4 nd nd nd TRICHROROBIPHENYL bdl bdl 11 ISODRIN nd bdl nd bdl nd nd nd nd nd nd nd
6 (PCB 101) 20 4,4 DDE nd nd nd nd nd nd 22 2,4 DDD nd nd bdl ENDOSULFAN BETA nd nd nd nd nd 25 4,4 DDD nd nd ,4 DDT nd nd nd nd nd ,4 DDT nd nd nd nd nd nd nd MIREX nd nd nd nd nd nd tations Nd; not detectable Bdl; below detection limit The above results are being verified by one external contractor and inter calibrated with the lab Recetox. Hence conclusions will follow the above verifications. Scientific coordinator notice Due to uncertainty of UTHR.DEE.APL results of analysis POPs in atmospheric samples collected during June 2003 in Serbia and analysed by UTHR.DEE.APL, scientific coordinator decided them do not include into the scientific part of the first year Report. They will be included into the Partner report but on exclusively responsibility of the contractor UTHR.DEE.APL.
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