Polycyclic aromatic hydrocarbons (PAHs) and organochlorines (OCs) in bottom sediments of the Guba Pechenga, Barents Sea, Russia

The Science of the Total Environment 306(2003) 39–56

0048-9697/03/$ - see front matter� 2002 Elsevier Science B.V. All rights reserved.PII: S0048-9697Ž02.00483-7

Polycyclic aromatic hydrocarbons(PAHs) and organochlorines(OCs) in bottom sediments of the Guba Pechenga, Barents Sea,

Russia

Vladimir M. Savinov *, Tatiana N. Savinova , Gennady G. Matishov , Salve Dahle ,a,b, a,b a b

Kristoffer Næsc

Murmansk Marine Biological Institute, 17, Vladimirskaya St., Murmansk, 183010 Russiaa

Akvaplan-niva AS, Polar Environmental Centre, N-9296 Tromsø, Norwayb

Norwegian Institute of Water Research Southern Branch, Televn 3, N-4879 Grimstad, Norwayc

Received 12 April 2002; accepted 22 May 2002

Abstract

Surface sediment samples from the Guba Pechenga and adjacent areas: Varangerfjord, Guba Malaya Volokovayaand Guba Bol’shaya Volokovaya(south-western Barents Sea) collected in March–April 1997 were analysed forpolycyclic aromatic hydrocarbons(PAHs), polychlorinated biphenyls(PCBs), chlorinated pesticides:p,p9-DDT, p,p9-DDE, p,p9-DDD, a- andg-HCH, and hexachlorobenzene(HCB). Mean8PAH (sum of the two- to six-ring PAHs)concentration in sediments from the Guba Pechenga(1481 ngyg dry wt.) was significantly higher than in sedimentsfrom adjacent areas(252 ngyg dry wt.), where PAH contamination levels were similar to reported for unpollutedsediments of the northern Norway fjords and open parts of the Barents Sea. Differences between HCB levels as wellas8HCH (sum ofa- andg-HCH) levels found in Guba Pechenga sediments and adjacent area sediments were notsignificant. Concentrations of these contaminants varied in ranges 0.28–1.76 and 0.05–0.68 ngyg dry wt., respectively,and were consistent with literature data on PAH levels in sediments from the northern Norway harbours, Kola Bay(Russia) and south-eastern part of the Barents Sea. Average total DDT concentration in Guba Pechenga sediments(10.5 ngyg dry wt.) was one and 2–3 orders higher than those found in sediments from the Pechora Sea and fromthe seas of eastern Arctic, respectively, however, it was comparable with DDT levels reported for harbours of northernNorway and Kola Bay. Significant difference between total DDT levels in Guba Pechenga and in the adjacent areas(mean 1.8 ngyg) was found. Among compounds of DDT family,p,p9-DDT isomer prevailed in all sediment samplesindicating a possible local ‘fresh’ DDT source. Mean8PCB (sum of PCB-28, 31, 52, 101, 118, 105, 153, 138, 156,180, 209) concentration in the Guba Pechenga sediments(12.8 ngyg dry wt.) was significantly higher than insediments of adjacent areas(2.1 ngyg dry wt.), but it was lower in comparison with8PCB levels reported for thenorthern Norway harbours and Kola Bay sediments. The highest levels of contaminants were found in sediments

*Corresponding author. Tel.:q47-777-50347; fax:q47-777-50301.E-mail address: [email protected](V.M. Savinov).

40 V.M. Savinov et al. / The Science of the Total Environment 306 (2003) 39–56

collected close to the Liinakhamari harbour. The origin of both PAHs and OCs in the Guba Pechenga sediments is acombination of local sources and long-range transport from lower latitudes.� 2002 Elsevier Science B.V. All rights reserved.

Keywords: PAHs; OCs; Bottom sediments; The south-western Barents Sea

1. Introduction

The Barents Sea supports rich and unique eco-systems, and marine resources of several speciesof fish, shellfish and marine mammals are exploit-ed. The coastal areas are important spawning andfeeding grounds for commercially important fishspecies as well as habitats for large colonies ofmarine mammals and marine birds.

The most heavily industrialised and populatedarea in the Barents Sea region is the coastal areanear the Norwegian–Russian border. There areseveral big metallurgical smelters(Kirkenes, Nick-el and Zapolyarnyi). The smelters in Nickel andZapolyarnyi, run by the ‘Pechenganickel’ compa-ny, are the main pollution sources emitting sulfurdioxide, dust, polycyclic aromatic hydrocarbons(PAHs), heavy metals and other contaminants tothe atmosphere and surroundings. The total emis-sion of pollutants from metallurgic enterprises inMurmansk region was estimated to be 312 100tons in 1998(MREC, 1999). For several decades,untreated effluents from the metallurgic smelterscontaining a broad range of organic and inorganiccontaminants have been discharged via the smallrivers into the Barents Sea. In 1998 alone, the‘Pechenganickel’ discharged more than 12 millionm of wastes, 33% without treatment(MREC,3

1999).In addition to local sources, the region is sub-

jected to long-range transported pollutants fromindustrialised areas further south in Europe, boththrough the atmosphere and through the oceancurrents. Anthropogenic contamination of remoteregions of the world, such as the Arctic, by PAHsand persistent organochlorine compounds(OCs)has been recognised for several decades(AMAP,1998). Temperature-dependent physicochemicalproperties of semivolatile organic compounds arebelieved to make them more prone to long-rangeatmospheric transport and accumulation in Arcticwaters(Wania and Mackay, 1993).

Contaminant concentrations in bottom marinesediments represent a critical measure of healthfor any coastal ecosystem. The sediments are asignificant reservoir for hydrophobic contaminantsand reflect the input of them to the ecosystem.

The purpose of the present investigations wasto determine PAH and OC contamination levelsand distribution patterns in the bottom sedimentsfrom the south-western coastal area of the BarentsSea and to compare with those from the adjacentareas. An attempt to evaluate the toxicity ofconcentrations measured has also been made.

2. Material and methods

2.1. Field sampling procedures

Surface sediment samples were collected in theGuba Pechenga and adjacent areas: Varangerfjord,Guba Malaya Volokovaya and Guba Bol’shayaVolokovaya during the expedition of the Mur-mansk Marine Biological Institute of RussianAcademy of Sciences(MMBI ) onboard RyV Dal-niye Zelentsy in March–April 1997(Fig. 1). Thesampling covered 10 stations, seven of them werelocated in Guba Pechenga and the others were inadjacent areas(Table 1). Sediments were retrievedby a 0.1-m van Veen grab. Sub-samples of the2

0–1 cm layer were collected from the grab sampleswith a stainless steel spoon for PAH, OCs andgrain size analysis. All samples were stored inspecially cleaned glass jars and frozen aty20 8C.

2.2. Grain size determinations

Grain size distribution was determined for eachsample gravimetrically after wet sieving. Sedimentwater content was determined after drying a sam-ple to constant weight(for 4 days at 508C). Theanalyses were carried out by GeoGruppen AS(Tromsø, Norway) and MMBI.

41V.M. Savinov et al. / The Science of the Total Environment 306 (2003) 39–56

Fig. 1. Map showing the sampling locations, March–April 1997.

Table 1Sampling sites and grain size composition of bottom sediments, March–April 1997

Station Latitude Longitude Location* Depth Grain size composition(%)(N) (E) (m)

Gravel Sand Siltqclay)1 mm 1–0.063 mm -0.063 mm

2 69837.89 31822.79 GP 55 50.0 39.7 13.64 69838.59 31822.59 GP 82 2.7 42.3 55.05 69838.69 31824.49 GP 100 0.5 8.1 89.46 69838.79 31826.09 GP 100 5.6 35.6 58.87 69839.59 31826.39 GP 120 1.4 41.8 83.88 69840.459 31827.29 GP 140 0.9 48.6 50.59 69841.549 31828.059 GP 80 0.8 48.6 50.6

11 69852.09 31851.09 GBV 79 0.4 33.6 66.015 69841.69 31841.39 GMV 85–90 0.4 78.0 21.616 69844.19 31831.29 VF 180–220 0.1 15.6 84.3

GP, Guba Pechenga; GBV, Guba Bol’shaya Volokovaya; GMV, Guba Malaya Volokovaya; VF, Varangerfjord.*


2.3. Polycyclic aromatic hydrocarbon analysis

The procedure used for the analysis of PAHs isbased on the International Oceanographic Com-mission guidelines(IOC, 1982) with minor mod-ifications. Individual sediment samples(25–110g) were homogenised, treated with methanol andKOH, and refluxed for 1.5 h together with a 1.0ml solution of seven deuterated PAHs. This solu-tion included the following PAHs, obtained fromthe Cambridge Isotope Laboratories, Inc.(CIL):naphthalene-d (CIL, DLM-365), biphenyl-d8 10

(CIL, DLM-494), anthracene-d (CIL, DLM-10

102), phenanthrene-d (CIL, DLM-371), pyrene-10

d (CIL, DLM-155), chrysene-d (CIL,10 12

DLM-261), and perylene-d (CIL, DLM-366).12

The solid fraction was removed by filtration andthe elute containing PAHs was extracted withpentane. The extracts were purified by columnchromatography using Varian Bond Elute solidphase extraction cartridges containing 500 mgsilica (Varian LRC, A1211-3036) and eluted withpentane and dichloromethane. The final extractwas analysed by capillary column gas chromatog-raphy with mass spectrometric detection(Hewlett–Packard MS 5971, HP 5890 Gas Chromatographequipped with a splitysplitless injector and a 25m=0.20 mm ID HP Ultra 1 column, and HP G1034 B software for MS ChemStation). Detectionlimits were determined based on procedural blanks(blind samples) and for each of the aromaticcompound varied from 0.005–0.20 ngyg dry wt.

2.4. Organochlorine compound analysis

The method involved freeze drying of samples(‘HETO DRYWINNER’, Model DW3, Denmark),extraction with acetone–cyclohexane mixture(15:20 by volume) by high-energy ultrasonic dis-integration(475 W), and repetition of the extrac-tion. The sediment extracts were purified with gelpermeation chromatography followed by sulfuricacid treatment to remove sulfur and other interfer-ing compounds.

The individual PCB congeners and pesticideswere determined by gas chromatography(HP5890) against the corresponding individual stan-

dards obtained from: Promochem, Sweden(PCBs,chemical purity)99%) and Supelco(pesticides,chemical purity 99%, Bellefonte, PA, USA). PCB-53 (Dr Ehrenstorfer, GmbH) has been used asInternal standard. GC parameters were: injectortemperature 2808C; detector temperature 3008C;carrier gas H , 2.5 mlymin; make-up gas N , 502 2

mlymin; split 1:30; splitless time 60 s; and injec-tion temperature 908C in 2 min, 30 8Cyminincrease to 1808C, 2.5 8Cymin increase to 2698C, in 10 min increase to 2758C. The capillarycolumn(HP35) was 60 m, 0.25 mm i.d., and 0.25mm film thickness. For extra checking of the 5CBcompounds, the HP5 column has been used.

A HP chromatography work station connectedto the gas chromatograph was used for identifyingchlorinated compounds. The analytes were: 19polychlorinated biphenyl(PCB) congeners, 28, 31,52, 101, 118, 153, 105, 138, 156, 180 and 209;hexachlorobenzene(HCB); the DDT group(pp9

DDT, and DDE); and the HCH group(a- andg-). The detection limit was 0.05 ngyg for eachcompound determined.

2.5. Quality assurance

Both PAH and OC analyses were performed atUnilab Analyse AS, Tromsø, Norway. The labor-atory is accredited for hydrocarbon analysesaccording to the European standards of NS-EN45001 and ISOyIEC Guide 25. Since 1996, thelaboratory has participated successfully in theQuality Assurance Laboratory Performance Stud-ies for Environmental Measurements in MarineSamples(QUASIMEME).

Quality assurance and control protocols aredescribed in the Unilab Quality Assurance Hand-book (UNILAB, 1998). Laboratory quality controlprocedures include analyses of sample blanks,reference material and spiked samples. The refer-ence material used for quality control was HS4(National Research Council of Canada) for PAHsand SRM 1941a(National Institute of Standardsand Technology, Gaithersburg, MD, USA) forPCBs and OCs. Instrument stability and responsewas checked using NIST standard solutions.


2.6. Statistical methods

Significance of differences between levels oforganic pollutants found in different areas wastested with the help of the Median test(P-0.05).

Principal component analysis(PCA) was usedtwice to study the relationships between relativePAHs concentrations(in terms of percentage of8PAH), and between log-transformed concentra-tions of PAHs and OCs compounds recalculatedon weight unit of pelites. Principal componentsare calculated by linear combinations of the orig-inal variables taken as orthogonal to one another.The first principal component accounts for themaximum amount of variance and subsequentprincipal components explain successively smallerquantities of the original variance. Principal com-ponents with eigenvalues greater than 1 were onlyretained for interpretation of the analysis results(Kaiser, 1960).

Cluster analysis(K means clustering method)was used for grouping of stations by relativecontents of PCB congeners in the sediment sam-ples. All statistical procedures were performedusingSTATISTICA version 4.5, StatSoft, Inc.

3. Results

3.1. Sediment characteristics

Sediment samples were classified as pelite(siltqclay) (-0.063 mm), sand(0.063–1 mm)and gravel()1 mm). Pelite predominated()50%) in bottom sediments collected at all stationsexcept stations 2(14%) and 15(22%) (Table 1).The maximum pelite contents were found at sta-tions 5(89%) and 7(84%).

3.2. Total PAH concentrations

Concentrations of8PAH (sum of the two- tosix-ring PAHs) in the Guba Pechenga bottomsediments varied from 428 to 3257 ngyg dry wt.(Table 2). Maximum PAH levels were found insediments close to Liinakhamari harbour(3257ngyg, station 4), and at stations 7(2053 ngyg)and 2(1594 ngyg) northward and southward from

the harbour, respectively. Almost all PAH com-pounds investigated had their maximum values atstation 4; exceptions were C3-naphthalene, C2-phenanthreneyanthracene, and benzowghixperylene(maximum concentrations were found at station2), and naphthalene, anthracene, C1-phenan-threneyanthracene and C1-dibenzothiophene(maximum concentrations were found at station7). It should be emphasised that the granulometryof the sediments varied between the stations. Thepelite content in the sediments from station 2 was4 and 6.5 times lower than in sediments fromstations 7 and 4, respectively. It is known thatPAH concentrations correlate with the pelite con-tent (Boehm et al., 1998; Sanger et al., 1999).

Concentrations ofSPAH in sediments from theadjacent areas varied from 151(station 16) to 442ngyg dry wt. (station 11) (Table 2), which aresignificantly lower compared with the concentra-tions found in Guba Pechenga sediments.

3.3. Total concentration of CPAH and toxicity ofbottom sediments

Several PAHs, and especially their metabolicproducts, are known to be carcinogenic(Conney,1982; Connel et al., 1997). Total concentrations ofpotentially carcinogenic PAHs(CPAH) (sum ofbenzowaxanthracene, benzofluoranthenes, ben-zowaxpyrene, indenow1,2,3-cdxpyrene and diben-zowa,hxanthracene) varied from 63 to 864 ngygdry wt., and accounted for 11–27% ofSPAH insediments from Guba Pechenga. Both absolute andrelative CPAH contents were highest in sedimentfrom station 4(Fig. 2).

CPAH concentrations in sediments from adja-cent areas(stations 11, 15 and 16) varied from 39to 115 ngyg dry wt. (22–30% ofSPAH). CPAHlevel found at these stations was significantlylower than in samples from Guba Pechenga(Table2).

Among all known potentially carcinogenicPAHs, benzowaxpyrene is the only PAH for whichtoxicological data are sufficient for derivation of acarcinogenic potency factor(Peters et al., 1999).Data are available, however, to quantify the tox-icities of other PAHs relative to benzowaxpyrene,


Table 2Polycyclic aromatic hydrocarbons(ngyg dry wt.), some ratios between PAH compounds and organochlorines(ngyg dry wt.) inbottom sediments from the Guba Pechenga(stations 2, 4, 5, 6, 7, 8 and 9) and adjacent areas: Guba Bol’shaya Volokovaya(station11), Guba Malaya Volokovaya(station 15), and Varangerfjord(station 16); data show range, arithmetic mean and standard deviation(S.D.)

Compounds, Guba Pechenga Adjacent areasabbreviations

n Range Mean"S.D. n Range Mean"S.D.

Naphthalene NAP 7 1.9–58 24"23 3 0.2–3.5 1.3"1.9C1-naphthalene C1N 7 10–69 30"21 3 1.7–17 7.1"8.9C2-naphthalene C2N 7 12–89 40"28 3 3.1–26 11"13C3-naphthalene C3N 7 10–82 38"30 3 1.3–26 10"14Phenanthrene PHE 7 28–362 169"132 3 8.2–22 16"6.8Anthracene ANT 7 13–236 117"87 3 2.4–11 7.0"4.2C1-phenantreneyanthracene C1P 7 27–124 68"40 3 3.5–19 10"8.0C2-phenantreneyanthracene C2P 7 24–86 57"28 3 4.4–28 13"13C3-phenantreneyanthracene C3P 7 10–64 41"23 3 3.0–31 13"16Dibenzothiophene DBT 7 1.7–21 6.6"6.8 3 0.2–1.2 0.9"0.6C1-dibenzothiophene C1D 7 4.5–24 15"8 3 1.6–8.5 4.0"3.9C2-dibenzothiophene C2D 7 6.6–70 26"21 3 2–20 8.8"10C3-dibenzothiophene C3D 7 3.9–40 21"14 3 1.9–17 7.2"8.4Acenaphthylene ACL 7 0.6–3.1 1.7"1.0 3 0.2–0.8 0.5"0.3Acenaphthene ACN 7 2.7–47 20"17 3 0.4–1.9 1.4"0.9Fluorene FLN 7 2.0–139 52"45 3 0.1–8.9 5.8"5.0Fluoranthene FLT 7 43–399 176"117 3 18–26 22"3.7Pyrene PYR 7 28–236 110"68 3 8.6–17 13"4.0Benzwaxanthracene BAA 7 18–180 73"51 3 4.7–12 8.6"3.5Chrysene CHR 7 27–160 82"43 3 9.0–17 13"4.1Benzowb,kxfluoranthene BKF 7 19–389 109"126 3 19–74 38"32Benzowexpyrene BEP 7 18–67 38"17 3 4.3–12 7.0"4.2Benzowaxpyrene BAP 7 13–207 64"64 3 7.9–19 12"5.9Perylene PER 7 8.9–35 21"10 3 2.9–9.3 6.0"3.2Benzowghixperylene BP 7 4.7–75 44"29 3 3.6–19 12"7.8Indenow1,2,3-cdxpyrene IND 7 4.0–57 29"20 3 2.1–11 6.9"4.5Dibenzowa,hxanthracene DBA 7 0.0–30 6.7"11 3 0.0–2.5 1.1"1.3Total PAH 8PAH 7 428–3257 1481"954 3 151–442 255"162Total carcinogenic PAHa CPAH 7 63–864 282"263 3 39–115 67"42PHEyANT 7 0.84–2.24 1.60"0.49 3 2.05–3.45 2.54"0.78FLTyPYR 7 1.41–1.71 1.58"0.12 3 1.55–2.14 1.80"0.30Fossil fuel pollution index FFPI 7 18.9–39.6 29.1"7.2 3 17.4–44.4 28.8"14.0(FLTqPYR)y(C2PqC3P) 7 1.1–6.2 3.3"1.8 3 0.7–3.6 2.5"1.6HCB 7 0.28–1.76 1.08"0.57 3 0.74–1.33 1.05"0.30a-HCH 7 0.04–0.23 0.13"0.08 3 0.02–0.54 0.20"0.29g-HCH 7 0.04–0.45 0.17"0.14 3 0.00–0.05 0.03"0.03SHCHb 7 0.08–0.68 0.31"0.21 3 0.05–0.54 0.23"0.27p,p9-DDE 7 0.09–1.34 0.52"0.54 3 0.06–0.29 0.15"0.13p,p9-DDD 7 0.08–10.1 3.07"3.41 3 0.13–0.46 0.25"0.19p,p9-DDT 7 0.10–31.3 6.87"11.1 3 0.05–2.97 1.39"1.47SDDTc 7 0.27–36.7 10.5"12.5 3 0.27–3.72 1.79"1.76SPCBd 7 1.11–37.9 12.8"12.4 3 1.06–4.10 2.14"1.70

CPAH is a sum of benzwaxanthracene, benzowaxpyrene, benzowb,kxfluoranthene, indenow1,2,3-cdxpyrene anda

dibenzowa,hxanthracene.8HCHssum ofa- andg-HCH.b

8DDTsp,p9-DDE, p,p9-DDD, andp,p9-DDE.c

8PCBssum of congeners 31, 28, 52, 101, 118, 105, 153, 138, 156, 180 and 209.d


Fig. 2. Total benzwaxpyrene-equivalent toxicities and relative contents of toxic benzowaxpyrene doses of potentially carcinogenicPAHs in bottom sediments from Guba Pechenga and adjacent areas.

expressed as toxic equivalency factors(TEFs).These are used to estimate benzowaxpyrene-equiv-alent doses(BaP dose). For a PAH compoundieq

BaP dosesTEF=dose (IARC, 1987).eq i i i

According to the US Environmental ProtectionAgency (US EPA, 1993), TEFs for benzwaxanthracene, benzowaxpyrene, benzowbxfluoranthene,benzowkxfluoranthene, indenow1,2,3-cdxpyrene anddibenzowa,hxanthracene are 0.1, 1, 0.1, 0.01, 0.1and 1, respectively. Total toxic benzowaxpyrene-equivalent(TEQ) of all these PAHs is

Total TEQs BaP doseeq i8i

Total TEQ calculated for all samples investigat-ed varied from 11 to 300 ngTEQyg dry wt. (Fig.2). The maximum value of Total TEQ was foundat station 4 situated right outside the harbourindicating a local source of contamination. Averagevalues of relative contents BaP doses in Totaleq

TEQ decreased in the order: BAP(69.5%), BKF(13.3%), BAA (7.9%), DBA (5.2%) and IND(4.2%) (Fig. 2).

3.4. Toxicity of bottom sediments from differentfjords in the south-western Barents Sea

The results obtained in Guba Pechenga andadjacent areas were compared with literature dataon PAH levels in bottom sediments from thedifferent fjords of south-western part of the BarentsSea(Fig. 1): Varangerfjord(coasts of Vardø andVadsø harbours), Korsfjord (close to Kirkenes),Jarfjord(Konieczny, 1996) and Kola Bay(Iljin etal., 1997). Since concentrations of alkylated hom-ologues of naphthalene, phenanthrene and diben-zothiophene were not presented in data reportedby Konieczny(1996), the sum of parent PAHs ofmolecular mass 128–278(SParent PAH) as wellas levels of CPAH and Total TEQ have been usedfor comparison.

The average levels ofSParent PAH, CPAH, andTotal TEQ found in bottom sediments from GubaPechenga were lower than in sediments from Vardøharbour (Norway) and Kola Bay (Russia), butwere higher than in Jarfjord, Korsfjord and Vadsøharbour (Norway). PAH contamination level in


Table 3Level of PAH (ngyg dry wt.), and total toxic benzowaxpyrene-equivalent(total TEQ, ngTEQyg dry wt.) in bottom sediments fromdifferent fjords of the Barents Sea; data show range and mean"S.D.

Area 8Parent PAHa CPAH Total TEQ Reference

Vardø harbour 2 4611; 8898 870; 1412 472; 733 Konieczny(1996)6755"3031 1141"383 602"184

Vadsø harbour 2 373; 881 68; 124 40; 66 Konieczny(1996)627"359 96"40 53"18

Jarfjord 6 166–383 30–70 19–35 Konieczny(1996)282"83 50"13 27"5

Korsfjord 2 126; 526 30; 134 18; 60 Konieczny(1996)326"283 82"74 39"30

Kola Bay 5 1246–6239 240–1211 71–583 Iljin et al.(1997)3453"2141 622"369 244"208

Guba Pechengab 7 263–2672 63–864 18–300 Present data1143"792 282"263 92"94

Adjacent areasc 3 127–250 39–115 12–31 Present data172"67 67"42 19"11

Sum of parent PAHs of molecular mass 128–278.a

Stations 2, 4, 5, 6, 7, 8 and 9.b

Stations 11, 15 and 16.c

adjacent areas of Guba Pechenga was similar tothose found in unpolluted sediments of Jarfjord(Table 3) and open parts of the Barents Sea(Yunker et al., 1996).

3.5. Composition and genesis of PAH

Similarities and differences between the com-position of the PAH components can be used aschemical fingerprints to identify potential sources(Kennicutt and Comet, 1992; Bence et al., 1996;Page et al., 1999).

Fluoranthene and phenanthrene were predomi-nant in sediments from all stations from the GubaPechenga(Fig. 3). Each of these compoundsaccounted approximately for 10–16% ofSPAH.The exception was the sample from station 5,where anthracene dominated. In addition, benzo-fluoranthenes were among dominant compoundsin sediments from station 4 and 6, and high-alkylated homologues of phenanthrene dominatedthe unsubstituted compound at station 8. Ben-zowb,kxfluoranthene (11–17% of SPAH), andfluoranthene(up to 13%) were dominant in sedi-ments samples from the adjacent areas. Ben-

zowghixperylene, which accounted for 13% ofSPAH, and phenanthrene(12.4%) was also amongdominant PAH compounds at station 16 and 15,respectively(Fig. 3).

Fluoranthene is a universal product of combus-tion of organic matter and is present in fossil fuelproducts. Phenanthrene has petroleum, combus-tion, and diagenetic origin. Phenanthreneyanthra-cene and fluorantheneypyrene ratios have beenused in order to distinguish between PAHs ofdiverse origin(Gschwend and Hites, 1981; Colom-bo et al., 1989; Budzinski et al., 1997). Thephenanthreneyanthracene ratio is temperature-dependent and is approximately 3 for the emissionsfrom combustion of various fuels(Gschwend andHites, 1981). Predominance of fluoranthene con-centration over pyrene is classically related pyro-lytic origin, namely coal combustion(Sicre et al.,1987). The phenanthreneyanthracene ratios calcu-lated for all samples from both Guba Pechengaand adjacent areas were not higher than 3.5, andfluorantheneypyrene ratios were not lower than1.4 (Table 2), which indicate the pyrolytic originof the predominant PAH compounds. However,the presence of the more highly alkylated homo-


Fig. 3. PAH fingerprints of sediments from the Guba Pechenga and adjacent area. Station 11 is not shown on the map.

logues of phenanthrene with concentrations higherthan the parent compounds is usually indicative ofpetroleum source(Steinhauer and Boehm, 1992).Unsubstituted parent phenanthrene was less abun-dant than the alkylated homologues(C2- and C3-phananthrenes) in samples not only from the GubaPechenga(station 8), but also from adjacent area(station 11).

Concentrations of perylene, which can have bothterrigenous (terrigenous plant residues, peatydeposits) and marine(diatoms, bacterial degrada-

tion of organic matter in anoxic sediments) origin(Venkatesan, 1988; Yunker et al., 1993; Loring etal., 1995; Page et al., 1999), varied from 3 to 35ngyg dry wt. and was not more than 3.8% ofSPAH.

The analysis of composition and genesis of PAHwas further investigated using PCA. The PCAmatrix was loaded with data on relative concentra-tions of the PAHs, relative contents of PAH inatmospheric dust(NIST SRM-1649, Burns et al.,1997) and two indices: Fossil Fuel Pollution Index


Table 4Loading matrix for PAH in bottom sediments from the Guba Pechenga and adjacent areas

Compounds Abbreviation Principal components

PC 1 PC 2 PC 3 PC 4 PC 5

Naphthalene NAP 0.585* 0.580*

C1-naphthalene C1N y0.781C2-naphthalene C2N y0.866C3-naphthalene C3N y0.814Phenanthrene PHE 0.703Anthracene ANT 0.736C1-phenantreneyanthracene C1P y0.484* 0.616* y0.462*

C2-phenantreneyanthracene C2P y0.871C3-phenantreneyanthracene C3P y0.921Dibenzothiophene DBT 0.616* 0.522*

C1-dibenzothiophene C1D y0.933C2-dibenzothiophene C2D y0.791C3-dibenzothiophene C3D y0.893Acenaphthylene ACL y0.830Acenaphthene ACN 0.748Fluorene FLN 0.534* 0.649*

Fluoranthene FLT 0.920Pyrene PYR 0.788Benzwaxanthracene BAA 0.633* 0.497*

Chrysene CHR y0.453* y0.546*

Benzowb,kxfluoranthene BKF y0.682Benzowaxpyrene BAP y0.586* 0.488*

Benzowghixperylene BP y0.836Indenow1,2,3-cdxpyre IND y0.856Dibenzowa,hxanthracene DBA 0.665* 0.455*

(FLTqPYR)y(C2PqC3P) 0.932Fossil Fuel Pollution Index FFPI y0.895

Percent of total variance 41.3 24.0 12.8 5.9 4.8Eigenvalues 11.1 6.5 3.5 1.6 1.3

-no significance.*

(FFPI) and the ratio of the sum of fluorantheneand pyrene(FLTqPYR) to the sum of the C2 andC3 alkyl phenanthrenes(C2PqC3P) (Table 2).The FFPI is a diagnostic ratio designed to deter-mine the approximate percentage of fossil PAHsrelative to the total PAH in a sample(Boehm andFarrington, 1984). In contrast, the(FLTqPYR)y(C2PqC3P) ratio reflects the relative amount ofpyrogenic PAH in the sample and increases withincreasing pyrogenic character(Page et al., 1999).Perylene and benzowexpyrene were not included inPCA due to absence of them in NIST SRM-1649.

Principal component analyses revealed that thefirst principal component(PC1) accounts for41.3% of the total variance(Table 4, Fig. 4a).This component has significant negative loadings

on alkylated homologues of naphthalene, phenan-threne and dibenzothiophene and FFPI, and signif-icant positive loading on fluoranthene, pyrene and(FLTqPYR)y(C2PqC3P) ratio. Thus, PC1 givesa differentiation between the main genesis types(pyrogenic and petrogenic) of the PAH com-pounds. The second principal component(PC2,24.0% of total variance) has significant positiveloadings on PAH compounds with low molecularmass: phenanthrene, anthracene, and acenaphtheneand significant negative loadings on PAH com-pounds with high molecular mass: benzofluoran-thenes, benzowghixperylene, and indenowa,hxanthracene and also acenaphthylene. All thesecompounds have pyrolytic genesis, but variousorigins. For example, phenanthrene is mainly


Fig. 4. Results of principal component analysis of PAH composition in sediments from the Guba Pechenga and adjacent areaspresented in the form of loading(a) and score plots(b). Only significant factor loadings are shown.

derived from combustion of coal and fossil fuels(Bresson et al., 1984), while benzowghixperyleneand indenopyrene come mainly from combustionof gasoline in vehicles(Nikolaou et al., 1984).Therefore, PC2 apparently, carries informationabout the pyrogenic sources of the PAH contami-nation. None of the others principal componentsinvestigated(PC3-PC5) added any further infor-mation(Table 4).

The distribution of the data points onto a factorscore plot(Fig. 4b), using coordinates of the firsttwo principal components representing 65.3% ofthe total variance, shows that the samples formedthree distinct groups. The first group unites thedata points located in the left-hand side of thebiplot (stations 11, 8, 2 and 5) which are charac-terised by relative high abundance of petrogenicPAH. The values of FFPI, calculated for thesestations, varied from 44.4 to 31.6% and decreasedin the order shown above. Recognising that thesestations are widely geographically distributed, theexistence of only one source of petrogenic PAHcontamination is unlikely. Due to the absence ofhuman settlements close to station 11 and 8, itmay be assumed that the petrogenic PAH contam-ination in sediments from these two stations isconnected to shipping activity. Stations 2 and 5are close to the harbour of Liinakhamari, and thesestations may also be influenced by the PechengaRiver run-off and by activities in the harbour itself,

which may account for the high relative concen-trations of petrogenic PAHs in sediments fromthese two stations.

All other stations are located at the right-handside of the score plot, characterised by high levelsof pyrogenic PAH. These stations may be dividedinto two groups. In the lower part of the biplot,bottom sediments sample from station 16 in theVarangerfjord are found together with the sampleof atmospheric dust, probably connected with long-range transport of PAH. In the upper part of thebiplot, bottom sediments samples from the stations4, 6, 7, 9 and 15 form a heterogeneous group,most likely reflecting various local sources ofpyrogenic PAH contamination.

3.6. Organochlorine residue levels

OC concentrations in bottom sediments fromthe Guba Pechenga and adjacent areas are sum-marised in Table 2. Comparison of main OCresidue levels in various stations is shown in Fig.5.

HCB is a widespread contaminant that hasentered the environment through its past manufac-ture and use as a pesticide and its formation as aby-product during the production of a variety ofchlorinated compounds. In aquatic systems, HCBis persistent in sediments and tends to accumulatein the tissues of organisms. HCB concentrations


Fig. 5. Residue levels of HCB(a), 8HCH (b), 8DDT (c) and 8PCB (d) in surface sediments from the Guba Pechenga andadjacent areas and PCB profiles in sediment samples(e) from the stations combined to cluster I(stations 2, 4, 5 and 6), cluster II(stations 7, 8, 9, 11 and 15), and cluster III(station 16).

in all samples investigated were found to be in therange of 0.28–1.76 ngyg dry wt. (Table 2). Max-imum HCB concentration was found at station 6(Fig. 5a). HCB residue levels in bottom sedimentsof the eastern Arctic seas(Bering and Chukchi

Seas and Gulf of Alaska), varied from 0.035 to0.079 ngyg dry wt. (Iwata et al., 1994). HCBlevels found in Guba Pechenga sediments werehigher that might appear at first glance to be theresult of local contamination. However, lack of


difference between HCB levels in Guba Pechengasediments and sediments from adjacent areas(Table 2) did not support such conclusion. It isknown that in surface sediments from coastal areasof Western Europe, the HCB concentrations canamount to 4 ngyg dry wt. (Northern Sea, NSTF,1993) and up to 6.7 ngyg dry wt., in harbours ofnorthern Norway(Dahle et al., 2000). Though, itshould be noted, differences between HCB residuelevels in Guba Pechenga sediments and sedimentsfrom the northern Norway harbours were notsignificant (Dahle et al., 2000). Elevated HCBlevels in bottom sediments from Guba Pechengaand adjacent areas are the result of long-rangeatmospheric transport andyor widespread regionalcontamination. More detailed survey with coresampling is required in order to find out the sourceof contamination.

Hexachlorocyclohexane(HCH) consists of mix-ture of four major isomers. The proportion of HCHisomers(a-, b-, g- andd-isomers) in the technicalmixture varies (Metcalf, 1955; Jantunen et al.,2000). Pure insecticidal isomer,g-HCH, is calledlindane. Lindane was used in Norway in the 1980sas an insecticide(Skaare et al., 1985). In theSoviet Union, lindane(90% g-HCH) was usedinstead of technical HCH(IRPTC, 1983). Theformer Soviet Union banned technical HCH in1990(Li et al., 1998).

Differences between HCH levels measured inGuba Pechenga sediments and adjacent area sedi-ments were not significant. The sum ofa- andg-HCH in all sediment samples investigated rangedfrom 0.05 to 0.68 ngyg dry wt. These levels werecomparable with those in south-eastern part of theBarents Sea(Pechora Sea) 0.2–1.0 ngyg dry wt.(Loring et al., 1995), in Kola Bay samples 0.10–0.40 ngyg dry wt. (a-HCH only) (Savinov et al.,1997), and Tromsø harbour(Norwegian Sea)0.04–0.79 ngyg dry wt. (Dahle et al., 2000)surface sediments. While in surface sediment sam-ples from the Chukchi Sea, Bering Sea and theGulf of Alaska HCH levels were lower and rangedfrom 0.04 to 0.21 ngyg dry wt. (Iwata et al.,1994). In sediments from the Norwegian harboursHarstad and Honningsvag, the HCH concentrations˚were found to be higher: 2.1 and 3.8 ngyg drywt., respectively(Dahle et al., 2000).

Concentrations ofSDDT (sum of p,p9-DDD,p,p9-DDE andp,p9-DDT) varied much(0.27–36.7ngyg dry wt.) with the highest values close toLiinakhamari (Fig. 5c). Maximum SDDT wasfound in sediments from the station 4 and highSDDT residue levels were detected at the neigh-bour stations 2 and 5(10.7 and 13.8 ngyg dry wt.,respectively). The averageSDDT concentrationcalculated for Guba Pechenga sediments was,respectively, one and 2–3 orders higher than thosefound in surface sediment from Pechora Sea(Lor-ing et al., 1995), and from the seas of easternArctic (Iwata et al., 1994). However,SDDT levelsin Guba Pechenga sediments were comparablewith those in harbour sediments of northern Nor-way (Dahle et al., 2000) and Kola Bay(Savinovet al., 1997).

Residues ofp,p9-DDT prevailed in all sedimentsamples with the exception of station 11. Thep,p9-DDTyp,p9-DDE ratio (DDTyDDE) can be used toknow whether DDT input occurs recently or in thepast. Sincep,p9-DDE is a dehydrochlorinationproduct ofp,p9-DDT resulting from the biologicaland photochemical transformation of thep,p9-DDT(Wedemeyer, 1967; Ware and Clifford, 1970) andnot included in the technical DDT, higher andlower DDTyDDE ratios denote the recent and pastusage of technical DDT, respectively(Chernyak etal., 1995; Iwata et al., 1995; McConnell et al.,1996). DDTyDDE is -1 in the atmosphere ofhigh latitudes, and biotic and abiotic componentsof Arctic marine ecosystems(Hargrave et al.,1992; Iwata et al., 1993, 1994; Chernyak et al.,1995). Although in snow from the Pechora Seaice, this ratio can be up to 10(Matishov et al.,1998).

DDTyDDE ratio was found to range from 0.09to 0.62 in surface sediments from the Bering Sea,Chukchi Sea and Gulf of Alaska(Iwata et al.,1994) while the ratio varied from 0.6 to 30.4 inGuba Pechenga and adjacent area sediments. Theratio was 23.4 at station 4 located near Liinakha-mari harbour, where a maximumSDDT concen-tration was found. Both a high SDDTconcentration and high DDTyDDE ratio indicatea possible local DDT source in this area.

Concentrations ofSPCB (sum of 11 congeners)in Guba Pechenga sediments had the same patterns


as SDDT concentrations(Fig. 5c,d). MaximumSPCB residue level(37.9 ngyg dry wt.) was foundin samples from station 4. TheSPCB concentra-tions were somewhat lower at neighbouring sta-tions 2 and 5 (10.7 and 13.8 ngyg dry wt.,respectively) and decreased to 1.1 ngyg in theouter bay at station 9. In the sediments from theadjacent area, the range of theSPCB levels were1.1–4.1 ngyg. The range ofSPCB (with theexception of station 4) was comparable with dataobtained in the North Sea(2.9–19 ngyg, Klamerand Fomsgaard, 1993). The averageSPCB con-centration in Guba Pechenga sediments was morethan one order higher than those found in surfacesediments of the east Arctic seas(Iwata et al.,1994), south-eastern(Loring et al., 1995), andcentral parts (Klungsøyr et al., 1995) of theBarents Sea. However, this value was significantlylower in comparison with those found in harboursof the northern Norway and Kola Bay(Dahle etal., 2000; Savinova et al., 2000.

The PCB composition in sediment samples fromthe stations investigated differed. Three clusterswere formed with the help of the K-means clus-tering method(Fig. 5e).

Cluster I is a group of stations located nearLiinakhamari harbour(stations 2, 4, 5 and 6).Stations located in the outer part of Guba Pechenga(7, 8 and 9) and two stations from the adjacentareas(11 and 15) were combined in cluster II.And finally, station 16 forms cluster III. Thegreatest difference was found between clusters Iand III. Low-chlorinated(tri-, tetra- and penta-)PCB congeners, accounted for 75% ofSPCB,were predominant in sediments from station 16.Whereas in cluster I along withpenta-chlorinatedPCBs, prevalent PCB homologues were high-chlo-rinated hexa- and hepta-PCBs (PCB-138, PCB-153 and PCB-180), accounted for more 50% ofSPCB. The PCB profile of cluster II showed anintermediate picture. It is worth noting that therewere significant differences(P-0.05) betweenabsolute concentrations ofpenta-, hexa- andhepta-chlorinated PCBs in sediments from Guba Pech-enga and from the adjacent area, but there wereinsignificant differences between concentrations oftri- and tetra-chlorinated PCBs found in thesesurvey locations.

It is apparent that predominance of low-chlori-nated PCB congeners in sediments from station 16probably indicates that the main source of PCBresidues is precipitation that is characteristic ofunpolluted regions of Arctic(Iwata et al., 1993;de March et al., 1998). Due to the higher vapourpressure of low-chlorinated PCBs, they are sub-jected to atmospheric transport to a greater extentthan higher-chlorinated PCBs(Dunnivant et al.,1992).

High levels ofSPCB and the predominance ofhigher-chlorinated biphenyls in sediments fromstations located close to Liinakhamari harbourindicates possible local contamination source. Theimpact of this source is also reflected by the PCBprofile of sediments from the stations belonging tocluster II.

3.7. Probable sources of contamination

Two alternatives were examined for clarificationof probable sources of Guba Pechenga sedimentscontamination. The first source was defined as anemission from the ‘Pechenganickel’ smelter andthe second one was the existence of a local sourceof contamination in Liinakhamari harbour that isconnected with human settlement andyor withintensive navigation and shipping. PCA was usedfor the examination. The data analysed were: PAHsas the sum of unsubstituted parent compounds andtheir alkyl-substituted homologues: naphthalene(N ), phenanthrenes(P ), dibenzothiophenes(D )S S S

and molecular mass totals for fluoranthene andpyrene (M202); benzwaxanthracene and chrysene(M228); benzowb,kxfluoranthene, benzowexpyrene,and benzowaxpyrene (M252); indenow1,2,3-cdxpyrene and benzowghixperylene(M276), diben-zowa,hxanthracene(M278), perylene (PER), aswell as HCB,SHCH, SDDT, sum of tri-, tetra-,penta-, hexa-, hepta- anddeca-CBs, distance fromhead of Guba Pechenga to the stations(D ), andP

distance from the Liinakhamari harbour to thestations(D ). Because of the remoteness of StationL

11 from the other stations it was not included inPCA.

Before performing the PCA, the concentrationsof all compounds were recalculated on a peliteweight base, because organic contaminants in


Table 5Varimax normalized matrix of factor loadings for PAHs and OCs residues in bottom sediments from the Guba Pechenga and adjacentareas

Compounds and abbreviations Principal components

PC 1 PC 2 PC 3 PC 4

Naphthalenes NS 0.870Phenanthrenes PS 0.912Dibenzothiophenes DS 0.820Fluorantheneqpyrene M202 0.941Benzwaxanthraceneqchrysene M228 0.934Benzowb,kxfluorantheneqbenzopyrenes M252 0.855Indenow1,2,3-cdxpyreneqbenzowghixperylene M276 0.719Dibenzowa,hxanthracene M278 0.774Perylene PER 0.786HCB HCB 0.914SHCH SHCH 0.915SDDT SDDT 0.838Sum of tri-CBs Tri-PCB 0.928Sum of tetra-CBs Tetra-PCB 0.871Sum ofpenta-PCB Penta-PCB 0.870Sum ofhexa-PCB Hexa-PCB 0.780Sum ofhepta-PCB Hepta-PCB 0.782Sum ofdeca-PCB Deca-PCB 0.592* y0.439*

Distance from the head of Guba Pechenga DP y0.680 y0.617*

Distance from Liinakhamari harbour DL y0.539* y0.706Percent of total variance 41.2 34.7 7.8 7.6Eigenvalues 13.5 2.3 1.5 1.0

-not significant.*

marine sediments are correlated with pelite con-tents, and log-transformed. PCA results as varimaxnormalised matrix of factor loadings for four firstprincipal components, which explain 91.3% oftotal variance, are summarised in Table 5. Theremaining principal components had eigenvaluesless than 1.

The first principal component(PC1) accountedfor 41.2% of the total variance. It contained sig-nificant positive loadings on all the PAHs exam-ined with the exception of PAH compounds withmolecular mass 276 and it had negative loadingon D . Therefore, PC1 can be defined as the PAHP

factor, in which the accumulation of the PAHcompounds is controlled by the distance from thehead of Guba Pechenga, and probably associatedwith the flow of the Pechenga River. However, thepossible impact of Liinakhamari harbour must notbe excluded, as indicated by a high factor loadingon D (Table 5), and differences between PAHL

fingerprints in sediments from the stations 2 and4 (Fig. 3), such as the highest levels of the mostcarcinogenic PAHs (benzowaxpyrene and ben-zowb,kxfluoranthene) found at station 4. The secondprincipal component explaining 34.7% of totalvariance contained significant positive loadings onPAH compounds with a molecular mass of 276 aswell as all OCs examined, with the exception ofHCB, tri- anddeca-PCB, and a significant negativeloading on the distance from Liinakhamari harbourto the stations. PC2 is essentially the OCs factor,in which the levels of OCs are controlled by thedistance from Liinakhamari. This result substanti-ates our supposition about the existence of localOC contamination sources in the Liinakhamariarea.

The third and fourth principal componentsaccounting for 7.6 and 7.8% of total variancecontained significant loadings ontri-PCB andHCB, respectively. Both these components possi-


bly reflect long-range transport of the con-taminants.

4. Conclusions

The concentrations of PAHs and OCs in Pech-enga Bay sediments may be characterised as mod-erate, and comparable to the levels found inharbours of northern Norway. However, the levelsare significantly higher than in open parts of thesouth-eastern Barents Sea and other offshore areasof the Arctic. The highest levels of contaminantswere found close to the harbour of Liinakhamari,and there was no evidence that the contaminantshad so far been transported to the adjacent coastalwaters.

The origin of both PAHs and OCs in thePechenga Bay sediments is a combination of localsources and long-range transport from lowerlatitudes.

Acknowledgments

The collection samples for the data presentedwere made possible by a close co-operationbetween Murmansk Marine Biological Institute(MMBI ) of the Russian Academy of Sciences andAkvaplan-niva AS, Polar Environmental Center(Tromsø, Norway). The authors wish to thank thescientists of MMBI, as well as the officers andcrew of RV Dalniye Zelentsy. The authors wish tothank the technical staff of GeoGruppen AS andMMBI for granulometric analysis, as well as sci-entists of Unilab Analyse AS for PAH and OCresidue concentrations determinations.

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Polycyclic aromatic hydrocarbons (PAHs) and organochlorines (OCs) in bottom sediments of the Guba Pechenga, Barents Sea, Russia