Ie Me DOWELL INDUSTRIAL SERVICE LABORATORY PROCEDURES MANUAL DAILY ROUTINE PROCEDURES: A.” Receive sample by stamping with the date. B. Assign sample identification number. C. Write up the work sheet (see attached work sheet). 0. Perform wet analysis. E. Perform solubility testing (Every morning. Samples should be on at least by 10:00 a.m.) F. Finalize work sheet for computer printode hen solubilities are complete. Na MISCELLANEOUS: & yy A. Wash glassware when needed 8. Make up solutions. SY a C. General housekeeping. &My SANPLE ANALYSIS PROCEDURES MAXIMUM POSSIBLE SOLUBILITY IN HCI (MPS) and GAS EVOLUTION A. Grind up a portion of loose scale with a mortar and pestle. If the ~ sampte is a tube section, cut a 1 inch ring off, remove the scale mechanically (i.e., use an electric engraver), and determine the scale distribution (grams per square foot). (See information sheet for scale distribution formula). Weigh out one gram of scale, if possible, A minimum of 0.4 grams are required for reliable results, C. Place the sample in a 125 mL. reflux flask. Add 50 mL. of 1:1 HCI (one part concentrated HC] plus one part 0.1. water). Observe any gas evolution. The evolution of gas will generally be CO, or HS, although it is possible that HCN or SO, maybe evolved. D. Determine the presence of Hs by plactng-a wet strip of lead ace- tate paper ever the edge of the flasks, \f metallic dark brown color indicates sulfide. Express the amqunt of sulfide as heavy, mod- erate, light or nil (determined ty. the rate of bubble formation) aN If cyanide ts suspected (as {mn Seales from petroleum plants) wet a strip of picric acid paper with 10% NaC9, . Hold the paper over the edge of the flask. QA .bJood red colo® will develop if cyanide is present. S ON F. Place the flask on@ hot plate and boil for one hour using a reflux condensor. Atfow ‘the flask to cool. Filter the contents with a Buchner funne]\Using ashless filter paper (i.e., Fisher or Whatman brand}, and (water aspirator to provide a vacuum, G. Dilute the filtrate with D.I. water using a 100 ml. volumetric flask. Be sure to rinse the filter funnel and flask, adding the rinse to the 100 ml. volumetric flask. Add enough D.I. water to reach the 100 mL. mark and save for metals analysis. H. Ory and weigh the residue: weight lost (grams dissolved) %MPS = x 100% initial sample weight Record the data on the work sheet. LOSS ON IGNITION A. Place the filter paper containing the residue from the MPS test into a weighed porcelain crucible and heat for at least one hour over a Meeker burner (the crucible should get hot enough to glow.)mm. WW. B. Cool the crucible and reweigh. The percent of material burned off indicates the amount of organic or carbonaceous material present. weight loss (grams burned off) % LOI = x 100% initial sample weight + If the LOI is greater that 10% an extraction using organic solvents (i.e.; toluene, perchloroethylene, etc.) should be performed. Place one gram’ of the sample into a weighed extraction thimble. Place the thimble into an extraction flask containing 50 ml of solvent and reflux for 2 hours. Dry and reweigh the thimble, weight oss % extractable = ——————--___ x 100% initial sample weight SILICA CONTENT Y Place the residue from the LOI test sae platinum crucible. wh fluoric acid (see attached iid he With extreme caution add a few drops of information sheet about HF hazards Sai at_on a hotplate to dry- ness. Then heat the crucible es feeker burner for ten minutes. Reweigh the crucible. WY weight e 1 S10 = < initial aphe jeight 38% to 100% of eS je should be accounted for after tests A, B, and Cc. If 5% to 10 the initial sample remains after the silica test, try to dissolve the material in 1:1 HCl. If this residue does not dissolve note the percent insoluble residue on the analysis report, however, if the residue in the crucible is soluble in 1:1 HC] dilute the sample to 100 ml, re-run the metals analysis and note the amounts obtained on the analysis report, x 100% PHOSPHATE AND SULFATE QUALITATIVE TESTS A. Pour 10 ml of the filtrate (from the MPS test) into a test tube. Add 10 mL of 12% barium chloride solution. Place the test tube in a beaker of boiling water for 2 minutes. The presence of a white Suspension indicates sulfate. Express the amount as heavy, mod- erate, 1ight or nil. B. Into a second tube pour 10 ml of the filtrate and add 1:1 annonium hydroxide until a metal hydroxide forms. Redissolve the hydroxide with 1:1 nitric acid, Pour 5 ml of this solution into a third test tube containing 10 mL of 7% ammoniun molybdate, solution (see Preparation instructions). The formation of a bright yellow pre-