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1 <br />t 7.3.12 The following steps detail how to add the appropriate <br />amount of extraction fluid to the solid material within the ZHE and <br />agitation of the ZHE vessel. Extraction fluid #3 is used in all cases <br />1 (see Step 5.7). <br />7.3.12.1 With the ZHE in the vertical position, attach a <br />line from the extraction fluid reservoir to the liquid inlet/outlet <br />' valve. The line used shall contain fresh extraction fluid and <br />should be preflushed with fluid to eliminate any air pockets in the <br />line. Release gas pressure on the ZHE piston (from the gas <br />' inlet/outlet valve), open the liquid inlet/outlet valve, and begin <br />transferring extraction fluid (by pumping or similar means) into <br />the ZHE. Continue pumping extraction fluid into the ZHE until the <br />' appropriate amount of fluid has been introduced into the device. <br /> 7.3.12.2 After the extraction fluid has been added, <br /> immediately close the liquid inlet/outlet valve and disconnect the <br />' extraction fluid line. Check the ZHE to ensure that all valves are <br /> in their closed positions. Manually rotate the device in an <br /> end-over-end fashion 2 or 3 times. Reposition the ZHE in the <br /> vertical position with the liquid inlet/outlet valvfa on top. <br />' Pressurize the ZHE to 5-10 psi (if necessary) and slowly open the <br /> liquid inlet/outlet valve to bleed out any headspace (into a hood) <br /> that may have. been introduced due to the addition of extraction <br />' fluid. This bleeding shall be done quickly and shall be stopped <br /> at the first appearance of liquid from the valve. Re-pressurize <br />_ <br />"~~ <br />~ the ZHE with 5-10 psi and check all ZHE fittings to ensure that <br />~- they are closed. <br />7.3.12.3 Place the ZHE in the rotary-extractor apparatus <br />' (if it is not already there) and rotate at 30 ± 2 rpm 'For 18 ± 2 <br /> hours. Ambient temperature (i_e., temperature of room in which <br /> extraction occurs) shall be maintained at, 23 ± 2•C during <br />' agitation. <br /> 7.3.13 Following the 18 + 2 hour agitation period, check the <br /> pressure behind the ZHE piston by quickly opening and closing the gas <br />' inlet/outlet valve and noting the escape of gas. If the pressure has not <br /> been maintained (i_e.; no gas release observed), the ZHE i~~ leaking. <br /> Check the ZHE for leaking as specified in Step 4.2.1, and perform the <br />' extraction again with a new sample of waste. If the pressure within the <br /> device has been maintained, the material in the extractor vessel is once <br /> again separated into its component liquid and solid phases. If the waste <br /> contained an initial liquid phase, the liquid may be siltere~i directly <br />' into the same filtrate collection container (i.e., TEDLAR bag) holding the <br /> initial liquid phase of the waste. A separate filtrate collection <br /> container must be used if combining would create multiple phase<, or there <br />' is not enough volume left within the filtrate collection container. <br /> filter through the glass fiber filter, using the ZHE device as discussed <br /> in Step 1.3.9. All extracts shall be filtered and collected if 1:he TEDLAR <br /> bag is used, if the extract is multiphasic, or if the waste contained an <br /> initial liquid phase (see Steps 4.6 and 1.3.1). <br />r <br /> 1312 - 17 Revision 0 <br />November 1990 <br />