Report on Global Monitoring Project Pesticide Research Laboratory ...

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Table 1 Installation date **August 26, 2010 Sampling Time Round Number PUF samples analysed by Spain PUF samples analysed by PRL 9:24 am 1 1, 2, 5 and 7 3, 4, 6, 8 and (the “reserve” was analysed by Bennin) October 1, 2010 12:20 pm – 12:57 pm 2 1, 2, 5 and 6 3, 4, 7, 8 and “reserve” January 3, 2011 5:26 pm – 6:02 pm 3 1, 2, 5 and 6 3, 4, 7, 8 and “reserve” April 8, 2011 3:45 pm – 4:30 pm 4 1, 2, 5 and 6 3, 4, 7, 8 and “reserve” ** Due to late arrival of the PUFs from Spain, the first exposure of the PUFs was not done as proposed. (The proposed date was July 1, 2010). So, the first round of samples was only exposed for one (1) month instead of three (3) months. The final round of PUF exposure ended on July 8, 2011 between 3:30 pm and 3:45 pm . Section 2 Standard Operating Procedure (SOP) for the extraction of PUF sample by the Soxhlet Method A pair of clean scissors was used to cut the PUF into small pieces (about 1 cm 2 ) which then placed into the Soxhlet Apparatus (no thimble was used) with the aid of a pair of tweezers and a glass stirring rod. About 200 mL of toluene were added to a 500 mL round bottom flask. (This amount of toluene was added so that when the extraction tube was filled to the siphon point, there was enough solvent left in the flask to prevent cracking due to heating). The extraction apparatus was assembled, the round bottom flask positioned in the heating mantle and the water flow started through the condenser. The apparatus was supported using a clamp and stand. The heat was adjusted for at least six cycles per hour. (The cycle is the filling of the extraction tube with solvent which evaporates from the flask and then condenses into the tube, followed by siphoning of solvent back into the flask). The sample was extracted for ten (10) hours. The extract was concentrated to about 1 mL using a rotary evaporator. The 1 mL of evaporated sample extract was transferred to a florisil column which was prepared as follows: 25 cm x 1 cm glass column (with a Teflon stopcock and 250 mL reservoir) was plugged with 2 cm glass wool, filled with
hexane and then, 6 g of activated florisil was poured into the column (Florisil 60-100 mesh from FISCHER, activated overnight at 130C). A gentle shaking of the column was necessary to settle the florisil inside the column. Two cm of sodium sulphate was then added on top. Hexane was poured into the column and when the hexane reaches the top of the filling, the stopcock was closed, a 250 mL round bottom flask was placed under the column and the evaporated sample extract was transferred to the top of the column using a Pasteur pipette. As the sample passes through the column, the sample container was rinsed with 3 x 2 mL portions of hexane (from a premeasured 50 mL of hexane) and rinses were also transferred to the column. The remaining hexane was poured into the reservoir of the column and the elution of fraction 1 was performed at a steady drip of 3 mL/min. When the hexane reached the top of the filling, the stopcock was turned off, the flask with fraction 1 was replaced with another 250 mL flask, the column was eluted with 50 mL of 15% DCM/Hexane (v/v) and fraction 2 was collected. The procedure was then repeated for fraction 3 using 150 mL of 60% DCM/Hexane (v/v). Each of the 3 fractions was separately rotary-evaporated (after adding 5 mL of iso-octane – Optima grade) to 1.0 mL. 1 uL of the extract was analysed by a Agilent 6890 GC-MS (scan mode) fitted with a HP 5MS column (0.25mm x 0.25 um x 30m), the appropriate reference standards and the Chem-Station Software. Analysis of Mirror Samples Fish and Cow‟s Milk samples were collected and each one was splitted to two –A and B. Fish sample A and Cow‟s Milk sample A were sent to Dr. Estaben‟s Laboratory in Spain. B-samples were analyzed at he Pesticide Research Laboratory. Mirror Samples: Results for UNEP Mirror Samples PCB Congeners Fish/(ng/kg) Cow’s Milk/(ng/kg) PCB18 38.5 nd PCB17 17 nd PCB31 110.8 nd
Page 1 and 2: Report on Global M
Page 3 and 4: Preamble: The titled project was in
Page 5 and 6: Methodology The survey included col
Page 7: Training Programme: All samples wer
Page 11 and 12: Aldrin 25.6 12.9 Endosulfan I 79.4
Page 13 and 14: UNEP Inter-calibration 2010-2011 (P
Page 15 and 16: Basic POPs Results Sample type: Hum
Page 17 and 18: PCDD/Fs Results Sample type: Human
Page 19 and 20: PCB Results (cont’d) Sample type:
Page 21 and 22: -HCH 0.009 0.053 -HCH 0.044 0.0004
Page 23 and 24: Upper-bound Please enter NDs with t
Page 25 and 26: 0.00001 PCB 167 52.05 51.16 0.0001
Page 27 and 28: 0.00001 PCB 167 52.05 51.16 0.0001
Page 29 and 30: 11:30 am - 12:00 noon: Presentation

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