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' SOP TO-14A/15 <br /> Rev 4 <br /> December 2007 <br /> ' Zero grade air,Nitrogen or helium is used for preparation of standards and for preparation of laboratory <br /> blanks. Primary standards for analytes, surrogates and internal standards are normally purchased from <br /> ' commercial vendors and are diluted for use. As of 11/10/04 there is only one manufacturer of gas standards <br /> for TO-14/15, Spectra Gases, Branchburg,N.J., although they sell the gases through other supply houses <br /> (e.g., Restek) All purchased standards are shipped with certification attesting to their purity and authenticity. <br /> ' Each mobile lab and the fixed-based lab performing TO-14/15 shall have notebooks to record standards. <br /> Refer to H&Ps SOP manual or the individual notebook for nomenclature of standards. <br /> ' All standards are prepared in 6L or greater Summa canisters and stored at room temperature. <br /> ' 7.2.1 Standard Preparation <br /> Three standards are required to be prepared for Method TO14A/15. The first contains <br /> ' the internal standards(Bromochloromethane, chlorobenzene-d5, 1,4-difluorobenzene) <br /> and surrogate compounds (Toluene-d8, 1,2-dichloroethane-4, 4- <br /> bromofluorobenzene). The second two contain the target analytes. Commercial <br /> ' mixes are used to prepare these. <br /> 7.2.1.1 Using the Entech can cleaner, clean three six liter summa canisters. Refer to the <br /> ' Entech literature for guidance. In general ten cycles of evacuation down to 1000 <br /> millitorr and filling with zero grade gas will be sufficient. Evacuate the cylinder to <br /> at least 1000 millitorr at the end of the cleaning. Allow cans to completely cool <br /> ' before proceeding. <br /> 7.2.1.2 Introduce about 20 ul of reagent grade water into the quick connects on each of the <br /> three summa canisters to be used. <br /> ' 7.2.1.3 Using a gas-tight 100 mL syringe introduce 300 mL of internal standard/surrogate <br /> mix @ 1.0 ppmv into one of the 6-L summa canisters. Then attach summa to <br /> helium or zero air source and pressurize to a stable 14.7 psi (2 ATM). This will <br /> yield a vapor standard containing 25 ppbv of internal standard and surrogate.(Note <br /> that there is one atmosphere of pressure in the cylinder, thus roughly two <br /> atmospheres of diluent has been added to the standard.) <br /> ' 7.2.1.4 Into the second clean humidified evacuated canister, introduce 120 mL of each of <br /> the 1 ppmv standard mixes to be used. Then attach summa to helium or zero air <br /> source and pressurize to a stable 14.7 psi (2 ATM).This will result in a standard at <br /> ' 10 ppbv containing the target analytes. <br /> 7.2.1.5 Prepare a second source standard as described in 7.2.1.4 using second source gas <br /> standards. <br /> 7.2.1.6 Allow 2 hours for equilibration <br /> 7.2.2 Standard Expiration <br /> ' The primary purchased have been given an expiration date by the manufacturer of one <br /> year. <br /> ' Page 6 of 24 <br />