Determination of polychlorinated biphenyls in waste oils by gas chromatography

Danes se za določanje polikloriranih bifenilov v vzorcih olj uporabljata evropski standardni metodi (EN 12766 in EN 61619). Za določitev vsebnosti polikloriranih bifenilov (PCB) v transformatorskih oljih, motornih rabljenih oljih, nerabljenih oljih in certificiranih referenčnih materialih (BCR-449 in BCR-420) smo uporabili plinsko kromatografijo z detektorjem na zajetje elektronov (GC-ECD). Postopek priprave vzorca je bila ekstrakcija iz olj s heksanom. Nepolarne matrične spojine se eluirajo iz adsorbenta skupaj s PCB-ji, nato jih injiciramo v analitski sistem. Njihova prisotnost pa onesnažuje injekcijski prostor detektorja in kolone in s tem se zmanjša občutljivost. Zaradi nezadostnega čiščenja pride do zakasnitve elucije PCB-jev iz kolone. Z uporabo sulfoksidne kolone se PCB-ji bolje ločijo od alifatskih ogljikovodikov. Uporabili smo plinski kromatograf Agilent Technologies (AT 6890N) z dvema kapilarnima kolonama različne polarnosti HP-5MS in DB-1701 v povezavi z ECD detektorjem. Rezultate vsebnosti polikloriranih bifernilov smo statistično ovrednotili glede na zahteve validacijskega postopka (linearnost, meja določanja LOQ, pravilnost, izkoristek metode, ponovljivost in obnovljivost). Iz rezultatov smo ugotovili, da so izkoristki pri certificiranih referenčnih materialih znotraj predpisanega kriterija. Izkoristki za transformatorska olja so nekoliko manjši vendar še vedno znotraj predpisanega kriterija. Z uporabo certificiranih referenčnih materialov smo dokazali, da je analizna metoda pravilna.Two European standard methods (EN 12766 and EN 61619) are currently used for the determination of PCBs in specific oil matrix. For determination PCBs in transformer oils, motor used and unused oils and certified reference materials (BCR-449 and BCR-420), gas chromatography with electron capture detector (GC-ECD) was used. Analytical procedure is based on extraction of oils with hexane. However, apolar matrix compounds (e.g. hydrocarbons) elute from the adsorbent together with the PCBs and are injected into the analytical system where their presence contaminates the inlet, detectors and columns and decreases system performances. Insufficient cleanup causes delay of elution of PCBs from GC columns. By using new sulfoxide-bonded silica, PCBs are better separated from aliphatic hydrocarbons because the specificity of the stationary phase for these compounds is much higher that that used in both standard methods. A gas chromatograph Agilent Technologies AT6890N with two capillary columns of different polarities (HP-5MS and DB-1701) coupled to two μECDs is used. Results were statistically evaluated according to validation requirements (linearity, limit of quantitation LOQ, accuracy, recovery, repeatability and reproducibility). From the results we can conclude that recoveries for certified reference materials are within permitted limits. Recoveries for transformer oils are lower, but still within permitted limits. Using certified reference materials it was confirmed that the analytical method for the determination of PCBs in specific oil matrix is accurate and reliable