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F;=CM:IML ~OZS""pN TO~KCNIC~ FAX ~ ~LG :_ _._ ~:~ •-~~ _~'?.E <br />• <br />6.3 Preservatives shall not be added to samples before extraction. <br />r <br />6.4 Samples may be refrigerated unless refrigeration r=_suits in <br />irreversible physical chance to 'NZSte. if precipitation occurs, the entire <br />sample (including precipitate}"uld be extracted. <br />6.5 41hen the same~.~,,ee is to be evaluated for vc'a_ile zna'ytes, care <br />shall be taRen to minimize tf2~loss of volatiles. Samples shall be collected and <br />stored in a manner intended to prevent the loss of volatile analytes (o.Q „ <br />samples should be collected in Teflon-lined septum capped vials and stored at <br />4'C. Samples should be opened only immediately prior to extraction). <br />6.6 1312 extracts should be prepared for analysis and znalyzed as soon <br />as possible following extraction. Extracts or portions of extracts for metallic <br />analyte determinations must be acidiffed with nitric acid to a pH < 2, un]ess <br />precipitation occurs (see Step 7.2.]4 if precipitation occurs). Extracts should <br />be preserved for other analytes according to the guidance given in the individual <br />analysis methods. Extracts or portions of extracts for organic analyte <br />determinations shall not be allowed to ccme into contact with the atmosphere <br />(ire., no headspace) to prevent lasses. See Section 8.0 (Quality Control) for <br />acceptable sample and extract holding times. <br />7.0 PROCEDURE <br />1.1 Preliminary Evaluations <br />Perform preliminary 1312 evaluations on a minimum 100 gram aliquot of <br />sample, This aliquot may nat actually andergo 1312 extraction. These <br />preliminary evaluations include: (1) determination of the percent solids (Step <br />7.1.1); (2) determination of whether the waste contains insignificant solids and <br />is, therefore, its own extract after filtration (Step 7.1.2); and (3) <br />determination of whether the solid portion of the waste requires particle size ~ <br />reduction (section 7.1.3). <br />1.1.1 Preliminary determination of percent solids: Percent <br />solids is defined as that fraction of a waste sample (as a percentage of <br />the total sample) from which no liquid may be forced out by an applied <br />pressure, as described below. <br />7.1.1.1 [f the sample will obviously yield no free <br />liquid when subSected to pressure filtration (i_e?., is 100; <br />solids), weigh out a representative subsample (100 g minimum) and <br />proceed to Step 7.1.3. <br />7.1.1.2 If the sample is liquid or multiphasic, <br />liquid/solid separation to make a preliminary determination of <br />percent solids is required. This involves [he filtration device <br />discussed in Step 4.3.2, and is outlined in Steps 7.1.1.3 through <br />7.1.1.9. <br />7.1.1.3 Pre-weigh the filter and the container that will <br />receive the filtrate. <br />1312 - 6 Revision 0 <br />November 1992 ~ <br />