Moldavian Journal of the Physical Sciences, Vol.

3, N2, 2004

PCBs DETERMINATION IN TRANSFORMER OIL BY SPE AND GAS

CHROMATOGRAPHY ANALYSIS

Bogdevich O.P.*, Cadocinicov O.P.

*
Institute of Geophysics and Geology, Laboratory of Geochemistry GEOLAB
Academiei str. 3, of. 133, Chisinau, MD2028, Moldova,
Tel: 373-22-739636; Fax: 373-22-739663; e-mail: bogdevicholeg@yahoo.com

Keywords: Gas Chromatography, Polychlorinated biphenyls (PCBs), Solid Phase Extraction

(SPE), transformer oil.

Summary
The aim of this work is the development of the PCBs determination method in the
transformer oil by the SPE and Gas Chromatograph analysis. The proposed method was used for
the cleanup of modeling solutions of transformer oil polluted by PCBs congeners and
Aroclor1254. PCB 209 was used as internal standard for quantitation purposes. Octadecyl bonded
silica phase AccuBOND C18 100mg/1ml cartridge was chosen for extraction performing. This
technology has shown a very good recovery (84 109 %) and accuracy for investigated samples.
The following advantages can be indicated for this method in comparison with others: a little
solvent amount, a short labor time, a low analysis cost, a good recovery and accuracy. By this
case this method can be recommended for PCBs determination in the complex oil matrix.

1. Introduction

Polychlorinated biphenyls (PCBs) are a subset of the synthetic organic chemicals known as
chlorinated hydrocarbons. PCBs have been produced in high volume by the chemical industry
and used as additives to oils in electrical equipment, hydraulic machinery, and other applications
where chemical stability has been required. These organic compounds can be transported for long
distances, and have been detected in the furthest corners of the globe, including places far from
where they were manufactured or used. Since PCBs exhibit a high degree of chemical and
biological stability and also lipid solubility, they tend to accumulate in the food chains and have
been detected in animal and human tissues [2,6,17]. Protection of human health and the
environment requires that PCBs be disposed of in such a way that they do not enter the
environment. The important step in the environmental management of PCBs is to identify their
sources and develop strategies for reducing or eliminating their release into the environment.

The chemical formula for PCBs is C12H(10-n)Cln, where n is a number of chlorine atoms within
the range of 1-10. Theoretically, a total of 209 possible PCBs congeners exist, but only about 130
of these are likely to occur in commercial products [4]. These compounds were widely used as
dielectric fluids: transformer oil, capacitors. The example of the total PCBs application is
characterized as follows [4]:
Germany dielectric fluids - 56 %; dissapative uses 28,7 %; hydraulic fluids 14,3 %.
Japan dielectric fluids 66 %; copying paper 18 %; heat transfer fluids 11 %; other 5
%.
USA dielectric fluids - 70 % of total application.

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 Moldavian Journal of the Physical Sciences, Vol.3, N2, 2004

From this data we can see that transformer oil is a principal pollution source of PCBs in the
environment.

The US Department of Health and Human Services as well as the International Agency for
Research on Cancer (IARC) consider PCBs to be probable carcinogens in humans (ATSDR
1997; IARC 1987). Many countries have developed classification for PCB-containing fluids and
materials. The benchmark level for PCBs is considered as 50 mg kg-1 (or 50 ppm) in many
countries [4].

The analytical determination is very important task for the control of PCBs concentration in
the environment. Some Screening Test and Gas Chromatography methods are used for the
determination of PCBs in different media [1,15,16]. Gas Chromatography with ECD detector is
more accurate for this purpose. The matrix impact is very strong for this determination by the
case of close chemical properties of oil and our interested substances (PCBs). Different methods
for sample preparation and cleanup exist [5, 7-14,19,20]. These methods are needed in the detail
development for the specific analyses.

This paper presents the procedure for determination of PCBs in the transformer oil with the
utilization of Solid Phase Extraction (SPE) for the sample preparation. With SPE, many of the
problems associated with liquid/liquid extraction can be prevented, such as incomplete phase
separations, less-than-quantitative recoveries, use of expensive, breakable specialty glassware,
and disposal of large quantities of organic solvents. SPE is more efficient than liquid/liquid
extraction, yields quantitative extractions that are easy to perform, is rapid, and can be automated.
Solvent use and laboratory time is reduced.

2. Experimental
2.1 Chemicals
All solvents were GC-pure quality and were purchased from Supelco and Sigma-Aldrich
Inc. (Germany). A working stock solution was prepared from PCBs congener mix standard
(IUPAC Nos. 18, 29, 31, 52, 44, 101, 118, 138, 149, 180, 194) containing 10 g of each in 1 ml
of heptane, and from Aroclor 1254 1000 g in 1 ml of hexane. These standard solutions were
purchased from Supelco Inc. (Germany). PCB 209 was used as an internal standard.

Octadecyl bonded silica phase AccuBOND C18 100mg/1ml cartridge was chosen for
extraction performing. Reversed phase separations involve a polar or moderately polar sample
matrix (mobile phase) and a nonpolar stationary phase. C18 SPE cartridge has following
characteristics: surface area 546 m2 g-1; average pore size 60 ; Surface pH 7; carbon
loading 18,8%; surface coverage 1,6 mol m-2. Compounds are retained in C18 by nonpolar-
nonpolar interactions and van der Waals or dispersion forces. This cartridge is used usually for
reversed phase extraction of nonpolar to moderately polar compound [3].

2.2 Instrumentation
GC 6890 (Agilent, Germany) gas chromatograph equipped with ECD detector,
split/splitless injection system, and capillary columns HP-5MS. Parameters of the gas
chromatograph system are characterized in Table 1.

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Table 1. Experimental Conditions

Equipment and system
Method parameters
elements
Gas chromatograph: Agilent 6890
Split/splitless inlet; injection - Splitless 1 l, inlet
Injection ports:
temperature of 300C
HP-5MS 30 m Length, 0,25 mm I.D., 0,25 m Film; Part
Column
number
H2, 1,5 ml min-1, or Average Velocity 46 cm sec-1,
Carrier gas
Constant Flow
First ramp: 100C (hold 1 min) to 190C at 30C min-1
Oven
Second ramp: 190C to 280C (hold 1 min) at 6C/min
Detector ECD, 3200 C, N2 makeup, 60 ml min-1
Data collection ChemStation

GC was calibrated with five calibration standard solutions in the concentration range 0,05
0,70 g ml-1 for PCBs, and 0,5 7,0 g ml-1 for Aroclor1254. The calibration standards were
prepared on pure oil matrix passed through cartridges C18 for the removal of the matrix impact.
The quantitative calculation was based on the area count obtained for the merged peaks. The area
obtained for interested peaks in the chromatograms was compared to the standard and calibration
curve to quantify the PCBs concentration. The analysis control and quatitation were performed
by ChemStation software version C 00-01 (Agilent).

2.3 Study of the matrix removal by SPE cartridges

The pure transformer oil sample without PCBs was chosen for the preparation of
experimental modeling solutions. This sample was diluted in 10 times with hexane by EPA
method 3580. PCBs congener mix and Aroclor1254 were added to the diluted oil sample to final
concentrations of 0,2 and 0,5 g ml-1 for each compounds for PCBs and to the total
concentrations of 2,0 and 5,0 g ml-1 for Aroclor1254. Then an internal standard (PCB 209) was
added to samples. Samples were shaken for 10 min for the better dissolution. These
concentrations were considered by the reason of PCBs limit concentration of 50,0 mg kg-1 in
PCBs containing materials. Thereby four modeling samples were prepared for the experiment.

The extraction is performed in three steps. First is a disk cleaning by dichlormethane 5 ml

under vacuum near 50 kPa, and drying under vacuum 5 min. Second is a conditioning by hexane
10 ml (the functional groups of the sorbent bed are solvated in order to make them interact with
the sample). Third is a matrix removal. This step was started right after hexane conditioning by
the sample addition to the cartridge (1 ml) and the elution by 2 ml of hexane under vacuum.
PCBs were extracted in this eluate. The total time of extraction procedure was near 10 min. This
procedure was repeated three times for every concentration and for blank solution. The sample
volume was striped to 1 ml under Argon stream. Then 1 l aliquots of hexane extract is injected
into chromatographic column. The same procedure was used for the sample preparation of real
transformer oil samples. The vacuum was controlled by Supelco Vacuum Manifold, which has a
solvent resistant main vacuum gauge and valve used to monitor the vacuum and release the
vacuum during processing.

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 Moldavian Journal of the Physical Sciences, Vol.3, N2, 2004

Results and discussion

Chromatograms of PCBs mix standard solutions with the concentration of 0,5 g ml-1 and
Aroclor1254 with the concentration of 5,0 g ml-1 are presented in Fig. 1. Column HP-5MS
showed a good chromatographic separation, resolution and reproducibility. The calibration
database of Gas Chromatography System was created for 12 PCB congeners and 45 compounds
for Aroclor1254. The correlation coefficient for all calibration compounds was in the interval of
0,990 to 1,000.

Table 2 Results of PCBs determination in modeling solutions of 0,2 g ml-1

IUPAC Repetitions Recovery
Nr Average St. dev.
No 1 2 3 %
1) PCB 31 0,222 0,185 0,194 0,2003 0,01937 100,13
2) PCB 29 0,221 0,183 0,192 0,1986 0,02023 99,30
3) PCB 18 0,218 0,184 0,193 0,1983 0,01740 99,14
4) PCB 52 0,197 0,191 0,188 0,1920 0,00469 95,99
5) PCB 44 0,211 0,177 0,186 0,1914 0,01780 95,70
6) PCB 101 0,214 0,181 0,188 0,1943 0,01759 97,15
7) PCB 149 0,212 0,180 0,187 0,1932 0,01688 96,58
8) PCB 118 0,209 0,177 0,184 0,1902 0,01665 95,10
9) PCB 167 0,211 0,180 0,186 0,1926 0,01666 96,30
10) PCB 138 0,209 0,179 0,185 0,1909 0,01622 95,46
11) PCB 180 0,210 0,180 0,186 0,1922 0,01580 96,11
12) PCB 194 0,215 0,185 0,190 0,1963 0,01606 98,15
Integration result for IS
IS PCB 209 48110207 47467063 46632829 47403366 740745,7 94,14

Table 3 Results of PCBs determination in modeling solutions of 0,5 g ml-1

IUPAC Repetitions Recovery
Nr Average St. dev.
No 1 2 3 %
1) PCB 31 0,495 0,469 0,475 0,4799 0,01371 95,97
2) PCB 29 0,501 0,469 0,482 0,4843 0,01613 96,86
3) PCB 18 0,495 0,474 0,484 0,4843 0,01037 96,87
4) PCB 52 0,498 0,501 0,497 0,4988 0,00192 99,77
5) PCB 44 0,487 0,462 0,474 0,4741 0,01281 94,83
6) PCB 101 0,483 0,460 0,476 0,4731 0,01171 94,63
7) PCB 149 0,479 0,458 0,473 0,4702 0,01089 94,04
8) PCB 118 0,484 0,462 0,473 0,4730 0,01094 94,59
9) PCB 167 0,478 0,458 0,471 0,4690 0,00985 93,81
10) PCB 138 0,480 0,460 0,473 0,4710 0,01000 94,20
11) PCB 180 0 479 0 461 0 475 0 4719 0 00933 94 38

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Table 4 Results of Aroclor1254 determination in modeling solutions of 2,0 g ml-1

Peak Ret. Repetitions 2,0 g ml-1 St
Average Recovery %
No time 1 2 3 deviation
1 8,02 0,0693 0,0307 0,0685 0,0562 0,02208 98,8
2 8,11 0,0161 0,0158 0,0168 0,0162 0,00052 99,2
3 8,43 0,0332 0,0311 0,0338 0,0327 0,00140 95,0
4 8,50 0,0032 0,0030 0,0031 0,0031 0,00010 90,1
5 8,68 0,0135 0,0131 0,0138 0,0135 0,00034 84,0
6 8,84 0,0031 0,0031 0,0032 0,0031 0,00008 102,1
7 9,15 0,0139 0,0134 0,0143 0,0139 0,00044 94,9
8 9,24 0,0439 0,0416 0,0486 0,0447 0,00357 84,9
9 9,31 0,1033 0,1004 0,1059 0,1032 0,00275 94,9
10 9,45 0,0168 0,0161 0,0171 0,0167 0,00053 94,3
11 9,67 0,0352 0,0348 0,0367 0,0356 0,00103 96,1
12 9,80 0,1501 0,1469 0,1548 0,1506 0,00395 94,8
13 9,92 0,0509 0,0495 0,0523 0,0509 0,00145 94,0
14 10,17 0,0089 0,0088 0,0092 0,0089 0,00021 93,7
15 10,29 0,0463 0,0452 0,0477 0,0464 0,00121 94,6
16 10,40 0,0951 0,0928 0,0980 0,0953 0,00258 94,6
17 10,51 0,0302 0,0298 0,0312 0,0304 0,00077 91,1
18 10,57 0,0132 0,0132 0,0137 0,0134 0,00030 95,0
19 10,63 0,1694 0,1660 0,1747 0,1700 0,00438 96,6
20 10,91 0,0394 0,0384 0,0406 0,0395 0,00112 95,5
21 11,02 0,0291 0,0285 0,0298 0,0291 0,00067 99,0
22 11,19 0,0143 0,0138 0,0147 0,0143 0,00041 97,0
23 11,19 0,0596 0,0577 0,0614 0,0596 0,00187 87,5
24 11,24 0,1256 0,1218 0,1297 0,1257 0,00391 95,4
25 11,45 0,0115 0,0110 0,0123 0,0116 0,00065 87,8
26 11,51 0,0048 0,0045 0,0048 0,0047 0,00017 81,6
27 11,56 0,0055 0,0053 0,0057 0,0055 0,00019 91,3
28 11,63 0,0178 0,0172 0,0184 0,0178 0,00059 94,6
29 11,78 0,0798 0,0774 0,0823 0,0798 0,00244 92,3
30 11,88 0,0733 0,1265 0,1341 0,1113 0,03318 83,8
31 12,09 0,0260 0,0269 0,0287 0,0272 0,00136 89,2
32 12,26 0,0150 0,0142 0,0155 0,0149 0,00066 88,9
33 12,32 0,0154 0,0148 0,0159 0,0154 0,00058 93,4
34 12,46 0,1628 0,1579 0,1682 0,1630 0,00518 94,1
35 12,52 0,0286 0,0278 0,0295 0,0286 0,00086 92,9
36 13,01 0,0165 0,0161 0,0168 0,0165 0,00039 91,2
37 12,88 0,0073 0,0101 0,0108 0,0094 0,00187 81,9
38 13,01 0,0075 0,0073 0,0077 0,0075 0,00018 92,5
39 13,15 0,0563 0,0544 0,0585 0,0564 0,00207 93,2
40 13,47 0,0123 0,0117 0,0127 0,0122 0,00052 89,5
41 13,61 0,0074 0,0070 0,0078 0,0074 0,00042 90,0
42 13,75 0,0377 0,0362 0,0389 0,0376 0,00133 93,7
43 13,89 0,0080 0,0077 0,0083 0,0080 0,00031 90,6
44 14,18 0,0257 0,0249 0,0270 0,0259 0,00105 92,5
45 14 94 0 0274 0 0267 0 0293 0 0278 0 00132 91 6

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Table 5 Results of Aroclor1254 determination in modeling solutions of 5,0 g ml-1

Peak No Ret. Repetitions 5,0 g ml-1 St
time Average Recovery %
1 2 3 deviation
1 8,02 0,1591 0,1349 0,1654 0,1531 0,01608 109,2
2 8,11 0,0420 0,0356 0,0418 0,0398 0,00368 96,0
3 8,43 0,0847 0,0709 0,0835 0,0797 0,00761 94,1
4 8,50 0,0076 0,0076 0,0076 0,0076 0,00002 84,3
5 8,68 0,0377 0,0320 0,0410 0,0369 0,00452 90,4
6 8,84 0,0084 0,0069 0,0083 0,0079 0,00083 96,3
7 9,15 0,0370 0,0316 0,0365 0,0350 0,00299 95,8
8 9,24 0,1308 0,0949 0,1427 0,1228 0,02485 94,5
9 9,31 0,2704 0,2278 0,2668 0,2550 0,02360 93,5
10 9,45 0,0439 0,0374 0,0433 0,0415 0,00356 95,5
11 9,67 0,0920 0,0775 0,0910 0,0868 0,00808 95,7
12 9,80 0,4006 0,3360 0,3955 0,3774 0,03591 94,6
13 9,92 0,1329 0,1130 0,1320 0,1260 0,01125 95,3
14 10,17 0,0250 0,0208 0,0243 0,0234 0,00224 95,7
15 10,29 0,1205 0,1020 0,1189 0,1138 0,01023 95,7
16 10,40 0,2553 0,2142 0,2518 0,2404 0,02276 94,7
17 10,51 0,0812 0,0684 0,0801 0,0766 0,00710 95,6
18 10,57 0,0354 0,0303 0,0354 0,0337 0,00295 98,2
19 10,63 0,4585 0,3845 0,4531 0,4320 0,04121 95,0
20 10,91 0,1023 0,0865 0,1007 0,0965 0,00869 95,8
21 11,02 0,0738 0,0630 0,0730 0,0699 0,00602 98,8
22 11,19 0,0375 0,0320 0,0372 0,0356 0,00312 95,1
23 11,19 0,1654 0,1402 0,1642 0,1566 0,01423 94,6
24 11,24 0,3400 0,2851 0,3337 0,3196 0,03003 95,1
25 11,45 0,0336 0,0284 0,0331 0,0317 0,00283 97,7
26 11,51 0,0150 0,0119 0,0149 0,0140 0,00176 90,9
27 11,56 0,0157 0,0133 0,0153 0,0148 0,00126 95,4
28 11,63 0,0467 0,0403 0,0462 0,0444 0,00356 97,1
29 11,78 0,2126 0,1805 0,2091 0,2007 0,01759 95,5
30 11,88 0,3388 0,2888 0,2084 0,2787 0,06581 83,9
31 12,09 0,0786 0,0673 0,0777 0,0746 0,00628 100,4
32 12,26 0,0415 0,0348 0,0416 0,0393 0,00386 96,3
33 12,32 0,0412 0,0355 0,0408 0,0391 0,00320 96,3
34 12,46 0,4392 0,3720 0,4334 0,4149 0,03728 94,8
35 12,52 0,0749 0,0651 0,0748 0,0716 0,00562 96,8
36 13,01 0,0464 0,0390 0,0456 0,0437 0,00403 97,0
37 12,88 0,0278 0,0233 0,0274 0,0262 0,00248 91,4
38 13,01 0,0211 0,0178 0,0208 0,0199 0,00184 97,0
39 13,15 0,1488 0,1272 0,1465 0,1408 0,01184 95,8
40 13,47 0,0349 0,0296 0,0341 0,0329 0,00287 96,7
41 13,61 0,0214 0,0181 0,0209 0,0201 0,00176 96,4
42 13,75 0,0996 0,0858 0,0982 0,0945 0,00761 96,1
43 13,89 0,0233 0,0201 0,0230 0,0221 0,00179 97,2
44 14,18 0,0671 0,0576 0,0661 0,0636 0,00525 96,6

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 Moldavian Journal of the Physical Sciences, Vol.3, N2, 2004
Response_

Signal: PCB05.D\ECD1B.CH
PCB194
2.2e+07 PCB180
16.60
14.16
2e+07

1.8e+07 PCB138 a)
12.45
1.6e+07 PCB118
PCB18
PCB149
PCB167
1.4e+07 7.40
PCB44 PCB101 11.23
PCB29 11.76
8.41 11.18
1.2e+07 9.78
7.37
PCB52
1e+07
8.01
PCB31
8000000 6.64

6000000
IS DCB
4000000
18.37

2000000

7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00
Time

Response_

Signal: AR545.D\ECD1B.CH
19
1.4e+07
b)
1.2e+07 34
12
24
1e+07 9
16
8000000
29
23 30
1
6000000 8 13 39
15
3 11
4000000 17 20 31 35 42 44
45 IS DCB
2 21 28
5 7 10 32
33
14 18 2225 36 40
37
38 4143
2000000 4 6 26
27

8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00
Time

Fig. 1 Chromatograms of PCBs (a) and Aroclor1254 (b) standard solutions with
concentrations of 0,5 and 5,0 g ml-1 respectively

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 Moldavian Journal of the Physical Sciences, Vol.3, N2, 2004

Response_

Signal: PCBOIL51.D\ECD1B.CH
PCB194
2.2e+07 16.59

2e+07 PCB180
14.16
1.8e+07
PCB138
12.45
1.6e+07
PCB18
PCB118
1.4e+07 7.41 PCB167
PCB44 11.23
11.76
PCB29 PCB149
PCB101
1.2e+07 8.42
11.18
7.38 9.79
PCB52
1e+07
8.02
PCB31
8000000 6.64

6000000 9.23

IS DCB
7.95
4000000 7.89 18.37
7.64 17.22
14.86
2000000

6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00
Time
Response_

Signal: OIL545_1.D\ECD1B.CH

19
1.4e+07

1.3e+07

1.2e+07
34

1.1e+07 12

24
1e+07

9
9000000

16
8000000

8 29
7000000
30
1
23
6000000

13
5000000 39
15
3 IS DCB
4000000 11
17 20 31 42
35 44 45
3000000 2 21
10 28
5 7 18 32
33
22 40
14 25
37
38
36 4143
2000000 26
27
4 6

8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00 18.00
Time

Fig. 2 Chromatograms of PCBs (a) and Aroclor1254 (b) modeling solutions with concentrations
of 0,5 and 5,0 g ml-1 respectively

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 Moldavian Journal of the Physical Sciences, Vol.3, N2, 2004

The PCBs determination in transformer oil by Gas Chromatography has a strong matrix
impact. Proposed SPE extraction method has a possibility to clean up investigated modeling
samples and reduces this impact very well. Cartridges C18 are a good solution for this matrix
impact elimination. After this cleanup 1 l of the obtained extract was injected in column HP-
5MS. Chromatograms of modeling solutions have a minimal retention time drift (0,02 min) and
the close base line in comparison with chromatograms of calibration solutions.

The quantitative result of extracted modeling samples of PCBs congeners is presented in

tables 2 and 3. The average value of modeling solutions with the concentration of 0,2 and 0,5 g
ml-1 are in intervals 0,1902 0,2003 and 0,4690 0,4988 by Standard Deviation 0,00469
0,0202 and 0,0019 0,0161 respectively. The recovery of congener PCBs for modeling samples
was assessed by standard solutions with the same concentration and by internal standard
PCB209. The recovery was indicated in the interval of 95,10 100,13 % for modeling solution
with the PCBs concentration of 0,2 g ml-1 and 94,04 99,77 % for modeling solution with the
PCBs concentration of 0,5 g ml-1. (table 2, 3). The better statistic parameters were indicated for
samples with higher concentration.

The same result was indicated for modeling solutions of Aroclor1254 with concentrations
of 2,0 and 5,0 g ml-1 (table 4, 5). The total concentration of every 45 component can be assessed
easy by ChemStation software for this mixture. Maximal 4 peaks with retention times 9,80,
10,63, 11,24, 12,46 min have a good recovery in intervals 94,1 96,6 % for 2,0 g ml-1 and 94,6
95,0 % for 5,0 g ml-1 internal standard. The recovery for total Aroclor1254 amount is 93,1 %
for 2,0 g ml-1 and 94,9 % for 5,0 g ml-1. The internal standard recovery is 94,1 and 93,0 %
respectively for the different concentration. These good parameters for every solution are
explained by two reasons: first is a good cleanup of modeling samples by SPE procedure on C18
cartridges, and second is a good separation, resolution and accuracy of Chromatographic System
by the proposed method.

Conclusion
The utilization of AccuBOND C18 100mg/1ml cartridges with Octadecyl bonded silica
phase showed a good result of the SPE cleanup and PCBs determination by Gas Chromatography
in the transformer oil. The proposed method has following principal advantages:
reducing a solvent amount, labor time, and so an analysis cost in comparison with other
technologies;
increasing a labor capacity and number of samples up to 10 times (from 30 40 per
month to 300 400 per month for one worker);
minimization of the matrix impact on the Gas Chromatography analysis;
good recovery and accuracy of PCBs determination in the complex oil matrix.
This method can be recommended for the implementation in analytical laboratories for the
investigation of the pollutant content in the complex oil matrix.

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 Moldavian Journal of the Physical Sciences, Vol.3, N2, 2004

Reference
[1] Chang I. L., Sanders W. J. The Analysis of Chlorinated Pesticides and PCBs Using the HP-
608 Capillary Column. Agilent Technologies, Application Note 228, (2000).
[2] Custer T.W., Custer C.M., Hines R.K. Dioxins and congener-specific polychlorinated
biphenyls in three avian species from the Wisconsin River, Wisconsin. Environmental
Pollution 119, 323, (2002).
[3] Guide to Solid Phase Extraction Sigma-Aldrich Co, Bulletin 910, (1998).
[4] Guidance for the identification of PCBs and materials containing PCBs. UNEP, first issue,
(1999).
[5] Hartonen K., Bwadt S., Dybdahl H.P., Nylund K., Sporring S., Lund H., Oreld F. Nordic
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soil. Journal of Chromatography A, 958, 239, (2002).
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[10] Method 3610B Alumina Cleanup. EPA (1996).
[11] Method 3620B Florisil Cleanup. EPA (1996).
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