SAMPLE PREP CARTRIDGES FOR THE EXTRACTION OF ACIDIC, BASIC, AND NEUTRAL SEMI-VOLATILE ORGANIC COMPOUNDS IN WATER UCT ENVIRO ENVIRO-CLEAN METHOD 8270

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1 ENVIRO UCT SAMPLE PREP CARTRIDGES FOR THE EXTRACTION OF ACIDIC, BASIC, AND NEUTRAL SEMI-VOLATILE ORGANIC COMPOUNDS IN WATER ENVIRO-CLEAN METHOD 8270

2 ENVIRO-CLEAN METHOD 8270 UCT, Inc now offers a unique, 2 cartridge solid phase extraction (SPE) system and procedure for EPA Method The method is shown to be reliable, efficient, and cost-effective. The tandem cartridge system uses UCT s proprietary 8270 cartridge material in-line with our activated carbon cartridges. High throughput can be achieved by extracting multiple samples simultaneously using a multi-port SPE manifold a set of 24 samples should be able to be extracted within 5 to 6 hours. UCT s SPE procedure offers several advantages over traditional liquid/liquid extractions. The liquid/liquid extraction requires the use of large amounts of organic solvents, typically anywhere from ml. The extraction also requires the analyst to extract materials at two different ph s. Finally, as with many liquid/liquid extractions, there is potential for the formation of emulsions during the process. SPE overcomes all these drawbacks; it uses less organic solvent, extracts at a single ph, and there is no threat of emulsions forming. In addition to offering advantages over traditional liquid/liquid extraction, UCT s proprietary 8270 cartridge and activated carbon procedure has been tested against the widest range of semi-volatile organic compounds of any solid phase extraction material currently on the market. A wide range of 137 target analytes and 6 surrogates have been successfully analyzed using this method. The UCT 8270 cartridge retains many target analytes including acids, bases, and neutrals; meanwhile the carbon cartridge, connected downstream from the 8270 cartridge, captures several very polar compounds, such as n-nitrosodimethylamine, n-nitrosomethylethylamine, methyl methanesulfonate, ethylmethanesulfonate, and 1-nitrosopyrrolidine. Product Benefits Cost-effective Reduced usage of organic solvents Simple and fast: only one sample pass is needed o 5-6 hrs for a batch of 24 samples No emulsion generated Shorter solvent evaporation time Shorter sample turnaround time High sample throughput Excellent recovery and reproducibility Cartridge body manufactured from special, proprietary polypropylene minimizing a potential source of interferences Packaged in Mylar to maintain cleanliness Cleaner extracts and chromatograms Sold as a complete kit containing 8270 cartridges, carbon cartridges, and adaptors

3 Table of Compounds Tested Compound For fied reagent blank MDL ( μg/l) Recovery% RSD% (n=4) (n=7) 1,2,4,5-Tetrachlorobenzene ,2,4-Trichlorobenzene ,2-Dichlorobenzene ,3,5-Trinitrobenzne ,3-Dichlorobenzene ,4-Dichlorobenzene ,4-Naphthalenedione Methyl fluorene Methyl phenanthrene Naphthalenamine Nitroso pyrrolidine Nitrosopiperidine ,3,4,6-Tetrachlorophenol ,3-Dichloroaniline ,4,5-Trichlorophenol ,4,6-Trichlorophenol ,4-Dichlorophenol ,4-Dimethylphenol ,4-Dinitrophenol ,4-Dinitrotulene ,6-Dichlorophenol ,6-Dinitrotoluene Acetylamino fluorene Chloro naphthalene Chlorophenol Isopropyl naphthalene Methyl naphthalene Methylphenol Naphthalenamine Nitroaniline Nitrophenol Picoline ,3'-Dichlorobenzidine ,3'-Dimethyl benzidine ,6-Dimethyl phenanthrene /4-Methylphenol Methylcholanthrene Nitroaniline ,4'-DDD ,4'-DDE ,4'-DDT ,6-Dinitro-2-methylphenol Aminobiphenyl Chloro-3-methylphenol Chloroaniline Chlorophenylphenylether Nitroaniline Nitrophenol Nitro-o-toluidine ,12-Dimethyl benz[a]anthracene Acenaphthene Acenaphthylene Acetophenone Aldrin alpha lindane Aniline Anthracene Azobenzene Benz[a]anthracene Benzidine Benzo[a]pyrene Benzo[b]fluoranthene Benzo[ghi]perylene Benzo[k]fluoranthene Benzoic acid Benzyl Alcohol Benzyl butyl phthalate beta lindane Bis(2-ethylhexyl) phthalate Bis[2-chloroethoxy]methane Bis[2-chloroethyl]ether Bis[2-chloroisopropyl]ether Compound For fied reagent blank MDL ( μg/l) Recovery% RSD% (n=4) (n=7) Bromophenoxy benzene Carbazole Chlorobenzilate Chrysene delta lindane Diallate (cis & trans) Dibenz[ah]anthracene Dibenzofuran Dibutyl phthalate Dieldrin Diethyl phthalate Dimethoate Dimethyl phthalate Di-n-octyl phthalate Diphenylamine Disulfoton Endosulfan I Endosulfan II Endosulfan sulfate Endrin Endrin aldehyde Ethyl methanesulfonate Famphur Fluoranthene Fluorene gamma lindane Heptachlor Heptachlor epoxide Hexachlorobenzene Hexachlorobutadiene Hexachlorocyclopentadiene Hexachloroethane Hexachloropropene Indeno[123-cd]pyrene Isodrin Isophorone Isosafrole (cis & trans) Kepone Methyl methanesulfonate Methyl parathion Naphthalene Nitrobenzene N-nitro-di-n-propyl amine N-nitroso di-n-butyl amine N-nitrosodiethylamine N-nitrosodimethylamine N-nitrosomethylethylamine o,o,o-triethylphosphorothioate o-toluidine Parathion p-dimethylamino azobenzene Pentachlorobenzene Pentachloroethane Pentachloronitrobenzene Pentachlorophenol Phenace n Phenanthrene Phenol Phorate Pronamide Pyrene Pyridine Safrole Sulfotep Thionazin Surrogates 2-Fluorophenol (S) Phenol d6 (S) MDL not Nitrobenzene d5 (S) determined 2-Fluorobiphenyl (S) for surrogates 2,4,6-Tribromophenol (S) p-terphenyl d14 (S)

4 ENVIRO-CLEAN METHOD 8270 EPA Method 8270 Extraction of Acidic, Basic, and Neutral Semi-Volatile Organic Compounds in Water Using Solid Phase Extraction Apparatus and reagents SPE manifold: 16-port or 24-port vacuum manifold (UCT part#: VMF016GL or VMF024GL), or 6-station universal manifold (UCT part#: ECUCTVAC6) SPE cartridges and adaptors: 8270 Kit (UCT part#: EC8270-KIT) these pieces are only sold as a kit - Please order using the kit part number 1. UCT8270 cartridge: 1000 mg 8270 sorbent in 15 ml cartridge (UCT part#: EC82701M15) 2. Carbon cartridge: 2000 mg activated carbon in 6 ml cartridge (UCT part#: EU52112M6) 3. Cartridge adaptor: Connects cartridge of any size onto a 1, 3, 6, 10 or 15 ml cartridge (UCT part#: AD0000AS) Other apparatus needed: ph meter, large sample delivery tubes, 15 ml empty fritted polypropylene reservoirs (UCT part#: RFV1F15P), nitrogen evaporator, glass vials and other commonly used labware. Reagents: HPLC grade Methanol (MeOH) ACS grade Ammonium hydroxide (28-30%) Pesticide grade Acetone 6N Hydrochloric acid (HCl) Pesticide grade Dichloromethane (DCM) Reagent grade Sodium thiosulfate Pesticide grade Ethyl acetate (EtOAc) ACS grade anhydrous sodium sulfate (Na 2 ) (UCT part#: ECSS05K) SPE Procedure Sample pretreatment 1. Transfer 500 ml of water sample to a 1-L amber glass bottle; add mg of sodium thiosulfate if free chlorine is present. 2. Adjust sample ph to less than 2 using 6N HCl. 3. Spike with surrogates, and target analytes for fortified samples. Note: A carbon cartridge is NOT needed if very polar analytes are not being analyzed (e.g. n-nitrosodimethylamine, n-nitrosomethylethylamine, methyl methanesulfonate, ethyl methanesulfonate, and 1-Nitrosopyrrolidine)

5 SPE system setup 1. Connect the carbon cartridge (EU52112M6) to the bottom of the 8270 cartridge (EC82701M15) using cartridge adaptor (AD0000AS). 2. Insert a loose plug of deactivated glass wool into the 8270 cartridge. This will minimize sorbent clogging caused by samples high in particulates. 3. Attach the connected SPE cartridges to the SPE manifold. UCT SPE System for EPA Method Cartridge Cartridge Adaptor Activated Carbon Cartridge

6 ENVIRO-CLEAN METHOD 8270 Cartridge conditioning 1. Wash the cartridges with 10 ml of DCM, allow them to soak for 1 min, and then apply full vacuum for 1 min. 2. Condition with 10 ml of methanol. Do not let cartridges go dry from this step until instructed to do so at the cartridge drying step. 3. Equilibrate with 10 ml of reagent water and 10 ml of 0.05N HCl. Sample extraction 1. Attach the large sample delivery tube to the 8270 cartridge, and insert the stainless steel end of the tube into the sample bottle. 2. Turn on the vacuum to the manifold and adjust it for a fast, dropwise sample flow (about 10 ml/min). Draw the entire sample through the dual cartridge system. Washing and drying 1. Rinse the sample bottle with 10 ml of reagent water, and draw the rinsate to the cartridges using the sample delivery tube. 2. Disassemble the tube and separate the connected SPE cartridges. Dry the 8270 cartridge under full vacuum for 10 min and the carbon cartridge for 15 min. Note: Remove as much water as possible, wet sorbent results in low analyte recovery. Analyte elution 1. Insert glass containers into the manifold to collect eluate. 2. The 8270 and Activated Carbon Cartridges are eluted separately. Apply the elution solvents described below to the respective SPE cartridges; draw 1/3 through, allow the solvent to soak for 1 min., and draw the remaining through in a slow dropwise fashion. a cartridge elution: Add about 2 cm of anhydrous Na 2 to the 8270 cartridge. Elute with: 2 * 2.5 ml of acetone; followed by 5 ml of DCM; then 1 ml of ammonium hydroxide (28-30%); and lastly 2 * 5 ml of DCM. b. Activated Carbon Cartridge elution: Elute with: 3 * 5 ml of DCM. Eluate drying 1. Dry the eluate using a blank cartridge (RFV1F15P) (or a glass funnel stopped with glass wool) holding about 20 g of anhydrous Na 2, pre-rinse the Na 2 with 5 ml of DCM. 2. Insert a 50-mL glass vial into the manifold to collect the dried eluate. 3. Pass the eluate from both the 8270 cartridge and the activated carbon cartridge through the Na 2 bed. 4. Rinse the sample bottle with 5 ml of DCM, transfer the bottle rinse to the eluate vial, cap and shake before passing the rinsate through the Na Repeat Step 4) with 5 ml of EtOAc. Note: Bottle rinse is critical for good recovery of PAHs, which can be adsorbed onto the glass wall. If the Na 2 appears greenish, rinse with additional solvent until it turns white.

7 Concentration 4. Concentrate the dried eluent to about 1 ml under a gentle stream of N 2 at 40 ºC. 5. Transfer the concentrated extract to a 2-mL autosampler vial, adjust the final volume to 1 ml with EtOAc. 6. Add IS and mix well. The samples are ready for GC/MS analysis. GC/MS parameters GC/MS: An Agilent 6890N GC coupled with a 5975C MSD and a 7683 autosampler Liner: 4 mm splitless gooseneck liner packed with deactivated glass wool (UCT part#: GCLGN4MMGW) Injector: 1 μl splitless injection at 250 ºC, with a split vent of 30 ml/min at 1 min GC capillary column: Restek Rxi -5sil MS, 30m*0.25mm*0.25μm, with 10 m integrated guard column Temperature program: Initial oven temperature of 40 ºC, hold for 3 min; ramp at 15 ºC/min to 240 ºC; ramp at 6 ºC/min to a final temperature of 310 ºC, hold for 2 min. Carrier gas: Ultra high purity Helium at a constant flow of 1.5 ml/min. MSD condition: Aux temperature: 280 ºC; MS Source: 230 ºC; MS Quad: 150 ºC Tune: dftpp.u Full scan: amu Chromatogram of a Laboratory Fortified Blank at 40 μg/l Abundance TIC: LFB40.D\data.ms Time-->

8 ENVIRO-CLEAN METHOD 8270 PRICES AND TERMS Our prices are subject to change without notice. The price in effect when we receive your order will apply. All prices are in US Dollars and are F.O.B. Lewistown, PA Terms of payment are net 30 days. MINIMUM ORDERS We welcome all orders, therefore, we do not have a minimum order requirement. When ordering, please include your purchase order number, complete Ship To and Bill To address, catalog number, quantity, and description of product(s). Also include your name and a phone number where you can be reached should we have any questions concerning your order. SHIPMENTS Normal processing is within 24 hours after receipt of an order. Unless special shipping requests have been made, our trained staff will send all orders by UPS Ground service. The appropriate shipping charges (freight & insurance costs) will be added to the invoice, unless otherwise instructed by the customer. SPECIAL PRICING We offer special pricing for volume purchases and standing orders. These discounts apply to bonded phase extraction column purchases only. Please call a sales representative for more information on special pricing qualifications. RETURN POLICY Our Quality Manager will handle all returns. Before returning merchandise, please call to obtain a return authorization number from the quality manager. We will need to know the reason for the return, date of purchase, purchase order number and invoice number in order to issue a return authorization number. Return merchandise must be received before a credit can be issued. Returns will not be accepted after 90 days. A restocking fee of 25% of the price paid, or a minimum of $25.00 (whichever is greater) will be charged on all returns. WARRANTY All products manufactured by UCT are guaranteed against defects in materials and workmanship for a period of 90 days after shipment. UCT will replace any items that prove to be defective during this time period. The exclusive remedy requires the end user to first advise UCT of the defective product by phone or in writing. Secondly, the defective product must be returned within 30 days after proper approval from our Quality Manager. All returns must indicate the purchase order number, the lot number and the shipping date. UCT s total liability is limited to the replacement cost of UCT products. This warranty does not apply to damage resulting from misuse. Contact Us Phone: Fax: UCT, Inc Bartram Rd. Bristol, PA info@unitedchem.com Web: DCN UCT ENVIRO

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