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._.. .. ~ ....__.,. ,~. ..•.~..~n ~.... ~w :d. L~b< 9:1=:d", Y.P. <br />5.2.~ Reagent water for volatile extractions may also be prepared <br />by boiling water for ]5 minutes. Subsequently, while maintaining the <br />water temperature at 90 ± 5 degrees C, bubble a contaminant-free in?rt gas <br />(e.g. nitrogen) through the water for 1 hour. ;lhile still hot, transfer <br />the water to a narrow mouth screw-cap bottle under zero-heap!space and seal <br />with a Tefinn-lined septum and cap. <br />5.3 Sulfuric acid/nitric acid (60/40 wciyht percent mixture) HzSO;/HNOJ. <br />Cautiously mix 60 g of concentrated sulfuric acid with 40 g of concentrated <br />nitric acid. <br />5.4 Extraction fluids. <br />5.4.1 Extraction fluid N1: This fluid is made by adding the <br />60/40 weight percent mixture of sulfuric and nitric acids to reagent water <br />(Step 5.2) until the pH is 4.20 ± 0.05. The fluid is used to determine <br />the leachability of soil from a site that is east of the Mississippi <br />River, and the leachability of wastes and wastewaters. <br />NOTE: Solutions are unbuffered and exact pH may not be attained. - .- - <br />5.4.2 Extraction fluid y2: This fluid is made by adding the <br />60/40 weight percent mixture of sulfuric and nitric acids to reagent water <br />(Step 5.2) until the pH is 5.00 ± 0.05. The fluid is used to determine <br />the leachability of soil from a site that is west of the Mississippi <br />River. <br />5.4.3• Extraction fluid X3: This fluid is reagent water (Step <br />S..J and is used to determine cyanide and volatiles leachability. <br />NOTE: These extraction fluids should be monitored frequently for impurities. <br />The pH should be checked prior to use to ensure that these fluids are made <br />up accurately. If impurities are found ar the pH is not within the above <br />specifications, the fluid shall be discarded and fresh extraction fluid <br />prepared. <br />5.5 Analytical standards shall be prepared according to the appropriate <br />analytical method. <br />b.0 SAMPLE COLlECT10N, PRESERVATION, AND HANDLING <br />6.1 All samples shall be collected using an appropriate sampling plan. <br />6.2 There may be requirements on the minimal size of the field sample <br />depending upon the physical state or states of the waste and the analytes of, _ <br />concern. An aliquot is needed for the preliminary evaluations of the percent <br />solids and the partfcle size. An aliquot may he needed to conduct the <br />nonvolatile analyte extraction procedure (see Step 1.4 concerning the use of this <br />extract for volatile organics). If volatile organics are of concern, another <br />aliquot may be needed. Quality control measures may require additional aliquots. <br />Further, it is always wise to collect more sample just 1n case something goes <br />wrong with the initial attempt to conduct the test. <br />1312 - 5 Revision 0 <br />November 1992 <br />