Document v62qKG4BeLY6q3dx0MR1L4raE

E. I. du P o n t de Nemours 5 Company ( I n e . ) A n a l y t i c a l and P h y s i c a l Measurements S e r v i c e E x p e r i m e n t a l S t a t i o n - B l d g . 269 W i l m i n g t o n , D e l a w a r e 19 898 P h o n e : (302) 772-2821 Mr. D. H. Wilkins General Electric Company Bldg. K-l Schenectady, New York 12301 O O OJ bo 4^ A N A L Y T I C A L OR P H Y S I C A L MEASUREMENTS S E R V I C E REP ORT Customer's Reference: P.O. #002-129982 Du P o n t No. 774-81 Date Received 6/1/77 CHLORODIBENZQFURANS IN POLYCHLORINATED BIPHENYLS A sample of polychlorinated biphenyl (PCB) with General Electric Company's designation A.R. No. 88118, Sample 8111453, was sent to us for. analysis of chlorinated benzofuran (CDBF) con tent. We agreed to attempt to perchlorinate the mixture and look for octachlorodibenzofuran in the presence of decachlorobiphenyl. We have made two attempts to (1) separate the chlorinated dibenzofurans from the PCB's by liquid chromatography, (2) form the octachlorodibenzofuran derivative by perchlorination of the residue from the liquid chromatography fraction and (3) detect the presence of the octachlorodibenzofuran in the perchlorination mixture. However, from the data available we have not been able to determine if the perchlorinated dibenzofuran exists in the reactior mixture. The procedure used for separation, perchlorination and detection was based on information in References 1, 2 and 3. One gram of the PCB mixture was taken up in hexane and added to a 1.2 cm liquid chromatographic column containing 20 grams of preactivated This report has been issued, subject to the Terms and Conditions on the reverse side of the DU PONT Request for Analytical or Physical Measurements Service form. 783135 Dahl Senior SuDervisor Signed 12/ 9/77 Lace Continued on Page 2 Du Pont Report No. 774-81 Page 2 Florisil. The column was washed with 200 mL of hexane, 50 mL of hexane/acetone (95/5) and finally with 100 m L of acetone. The acetone fraction presumably held any chlorinated dibenzofurans as well as any other chlorinated oxygen containing organic compounds which were present in the original PCB mixture. The P C B 's should have been removed from the column by the hexane. The acetone column wash was reduced to 0.5-1.0 mL with a Kudema-Danish evaporator. Low steam heat and slow nitrogen gas flush were used for the evaporation. The concentrated acetone fraction was transferred to a Carius tube. The acetone was removed with a slow nitrogen purge through a narrow tube inserted in the Carius tube. No heat was applied to the tube. The residue was perchlorinated with antimony pentachloride according to the pro cedure in Reference 1. Hexane instead of ben z e n e was used in the final work up of the reaction mixture. The hexane solution of the perchlorination reaction was analyzed by gas chromatography with an electron capture detector. The GC column was a stainless steel tube, 180 cm x 3 mm, packed with 3% OV-17 on 60-80 m e s h Gas Chrom Q. The column temperature was 200C; the h elium carrier gas flow was 30 mL/minute. Two control experiments were run. Dibenzofuran was p e r chlorinated and dibenzofuran was added to a portion of the PC3 mixture before liquid chromatography separation.| Also, acetone was added to a Carius tube and evaporated; then a perchlorination reaction was run on the acetone residue. The reaction products from the perchlorination of the acetone solvent residue were very similar to the products from the per chlorination of dibenzofuran and the LC fraction from the PCB mixture However, examination of the GC charts reveals several GC peaks which are not attributed to reaction products from the residue of acetone. The peak areas and retention times of these components are shown in the attached table. The chromatograms are also attached. At the request of Don Wilkins the final reaction product mixture from the dibenzofuran and the acetone LC fraction of the PCB mixture are being sent to General Electric. , md Q tn 783136 o o to bo Du Pont Report No. 774-81 taction ixture Code )-6-2A )-6-4A J-12-3A )-12-2A GC PEAK AREAS AND RETENTION TIMES FOR COMPONENTS FROM PERCHLORINATION REACTIONS (Area units are arbitrary integrator units divided by 106) Starting Material Dibenzofuran LC Fraction of PCB Mix Dibenzofuran LC Fraction of PCB Mix Spiked with Dibenzofuran 0.41-0.45 - Retention Times (Minutes) 0.42-0.47 3.16-3.17 3.23-31 8.25-8.49 - - 0.4 - 8.73-8.88 0.04 - 12.5 - 12.5 - 35.6 6.4 10.5 0.5 0.5 0.4 0.3 19.2 20.5 1.6 1.7 0.7 0.7 oC" sOoi CO "v l 9Z{01odbiao