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I~ <br /> <br /> 5. Beakers, 300 ml tall form. <br /> 6. Graduated cylinder, 25 ml. <br /> 7. Olaes fiber filter (Reeve Angel 934AH or equivalent). <br /> 8. Burets, 50 ml capacity. <br />- 9. Balance, cea be read to 0.01 g. <br /> <br /> 10. pH Meter (Corning Model 12 or equivalent) with cambiaetioa electrode. <br />i~ 3.2.11.5 Procedure (modified and updated from Smith et al., 197x4)- <br /> 1. Sleigh 2.00 grams of lees they 60 mesh sample. <br /> NOTE: If the Semple contains no carbonated sad no eulfatee, sad the paste <br /> pN is lads than 5.5, then steps 2 through 5 can be eliminated and procedure <br /> can be continued at step 6. <br /> 2. Place sample into a f~mael fitted with filter paper sad leach with 200 ml <br /> of 2:3 HC1 in funnel-full increments. <br /> <br /> 3. Leach sample with distilled water (ia funnel-full increments) until <br /> effluent is free from chloride.sa detected by lOx silver nitrate. Note: Add <br /> three drops of silver nitrate. I! a white precipitate forms, chlorides are <br /> present. <br /> k, Air dry rilter sad sample overnight, or place is 50°C forced air oven <br />until dry <br /> . <br /> 5, Carefully scrape dried sample from filter surface end mix sample. <br /> <br /> 6. Plsce sample is a 300 ml tall form beaker. <br /> 7. Add 24 ml of 30~ H202 and heat beaker on hotplste until solution is <br /> approximately 40°C. Remove beaker from hotplate and allow renetion to go to <br /> completion se dhovn when bubbling ceases. NOTE: Three bleats for each <br /> batch of ammplea should be handled is the same manner. CAUTION: Initial <br />reaction ma <br />be <br />uite turbulent whe <br />sam <br />l <br />co <br />t <br />i <br />th <br />O <br />lx <br />lfur <br /> y <br />q <br />p <br />es <br />n <br />a <br />n more <br />an <br />. <br />su <br />. <br />n <br /> 8. Add as additional 12 ml of H202 (30x) to beaker end allow reaction to <br /> go to completion as shave when bubbling ceased. <br />• 9. Place beaker on hotplate sad hest to approximately 90 to 95°T, solution <br /> temperature, until any unreacted H202 left in beaker is destroyed ae shown <br /> when bubbling ceases. Do not allow to go to dryness. <br />10. Wash dawn the sides of the beaker with distilled water and make the <br />volume of the solution to approximately 100 ml. <br />71 <br />r <br />