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Title 22 l ronmental Health Standards-Hazardouselte §66261.126 <br /> Bilge water(X) 2.0 Summary of Method. <br /> Boiler cleaning waste(X,C) 2.1 Organolead is separated from the sample matrix by extraction with <br /> Bunker Oil(X,I) xylene.The organolead in the extract is reacted with Aliquat 336 and io- <br /> Catalyst(X,I,C) dine and the solution is made up to volume with MIBK.Lead contained <br /> Caustic sludge(C) in this mixture is determined by flame atomic absorption spectrometry <br /> Caustic wastewater(C) (FAAS).If the original sample is completely soluble in xylene,the ex- <br /> Cleaning solvents(I) traction step is omitted. <br /> Corrosion inhibitor(X,C) 3.0 Safety. <br /> Data processing fluid(I) 3.1 Some organic lead compounds are volatile and toxic. Therefore, <br /> Drilling fluids(X,C) samples must be processed in a well-ventilated hood. Antiknock lead <br /> Drilling mud(X) compounds are particularly poisonous and must not be inhaled or in- <br /> Dyes(X) gested or come into contact with the skin. Antiknock lead compounds <br /> Etching acid liquid or solvent(C,I) should never be exposed to elevated temperatures (above 50°C) or to <br /> Fly ash(X,C) acids and oxidizing agents.Whenever organic lead compounds are han- <br /> Fuel waste(X,I) dled outside of a well-ventilated hood,protective respiratory equipment, <br /> Insecticides(X) protective clothing and rubber gloves must be wom.The material safety <br /> Laboratory waste(X,C,R,I) data sheets(MSDS)for organolead standards must be read. <br /> Lime and sulfur sludge(C) 3.2 The solvents used in this method are flammable. Proper precau- <br /> Lime and water(C) tions must be taken to prevent contact with sparks or open flames(other <br /> Lime sludge(C) than the AAS flame). <br /> Lime wastewater(C) 4.0 Interferences. <br /> Liquid cement(I) 4.1 To reduce loss of organic lead compounds which are very volatile <br /> Mine tailings(X,R) and sensitive to oxygen,samples must not be exposed to elevated temper- <br /> Obsolete explosives(R) atures or to air for extended periods of time.Such losses shall be mini- <br /> Oil and water(X) mized by adhering to the sample collection, preservation and handling <br /> Oil Ash(X,C) procedures in subdivisions 7.2-7.4 and 8.1.1 of this appendix. <br /> Paint(or varnish)remover or stripper(I) 4.2 If the samples are moist,there may be poor wettability with xylene. <br /> Paint thinner(X,I) 5.0 Apparatus and Materials. <br /> Paint waste(or slops)(X,I) 5.1 flame atomic absorption spectrometer(FAA spectrometer) with <br /> Pickling liquor(C) background corrector and recorder or integrator; <br /> Pigments(X) 5.2 lead hollow cathode lamp or electrodeless discharge lamp; <br /> Plating waste(X,C) 5.3 nebulizer with impact bead;the standard rubber gasket in the nebu- <br /> Printing Ink(X) lizer must be replaced with a cork gasket because the organic solvents <br /> Retrograde explosives(R) used in this method attack rubber; <br /> Sludge acid(C) 5.4 air,acetylene and appropriate AAS burner head; <br /> Soda ash(C) 5.5 erlenmeyer flasks,250 ml and 100 ml,with ground glass stoppers; <br /> Solvents(I) 5.6 mechanical shaker; <br /> Spent acid(C) 5.7 glass filter funnel and filter paper(Whatman#40,#42 or equiva- <br /> Spent caustic(C) lent); <br /> Spent(or waste)cyanide solutions(X,C) 5.8 separatory funnels,250 ml capacity; <br /> Spent mixed acid(C) 5.9 volumetric flasks,250 ml, 100 ml,and 50 ml. <br /> Spent plating solution(X,C) 6.0 Reagents. <br /> Spent sulfuric acid(C) All solvents and reagents must be at least analytical reagent grade,if <br /> Stripping solution(X,I) available. <br /> Sulfonation oil(I) 6.1 xylene(use p-xylene if available); <br /> Tank bottom sediment(X) 6.2 methyl isobutyl ketone(MIBK,4-methyl-2-pentanone); <br /> Tanning sludges(X) 6.3 iodine solution:dissolve 3.0 g of elemental iodine in toluene and <br /> Toxic chemical toilet wastes(X) make up to 100 ml with the same solvent.Store in a brown bottle in a re- <br /> Unrinsed pesticide containers(X) frigerator; <br /> Unwanted or waste pesticides-an unusable portion of active ingredi- 6.4 Aliquat 336 (Tri-capryl methyl ammonium chloride), available <br /> ent or undiluted formulation(X) from Aldrich, Milwaukee, WI, or from McKesson Co., Minneapolis, <br /> Waste epoxides(X,I) MN. Aliquat is a registered trademark of Henkel Corporation. Prepare <br /> Waste(or slop)oil(X) two solutions, one containing 10 percent weight to volume ratio (w/v) <br /> Weed Killer(X) and one containing 1 percent(w/v)in MIBK.Store in a refrigerator; <br /> NOTE:Authority cited:Sections 208,25140 and 25141,Health and Safety Code. 6.5 anhydrous sodium sulfate,granular; <br /> Reference:Sections 25115,25117,25140 and 25141,Health and Safety Code. 6.6 lead chloride,crystals.Dry at 105°C for 3 hours before use. <br /> HISTORY 6.6.1 Prepare a stock solution containing 1000 mg/1 of lead(Pb)by dis- <br /> t.New section filed 5-24-91;effective 7-1-91(Register 91,No.22). solving 0.3356 g of lead chloride in 10 percent Aliquat 336 in MIBK and <br /> Appendix XI dilute to 250 ml.Store in a brown bottle in a refrigerator. <br /> Organic Lead Test Method 6.6.2 Prepare an intermediate Pb standard by pipetting 10 ml of the <br /> 1.0 Scope and Application. stock standard into a volumetric flask and diluting to 100 ml with a 40 <br /> 1.1 This method is used to determine the sum of organic lead com- percent volume to volume ratio(v/v)solution of xylene in MIBK.Store <br /> pounds ("organolead")in liquids,solids or sludges.The method detec- in a brown bottle in a refrigerator; <br /> tion limit for a 50 g sample is 0.5 µg/g(as lead);the method detection 6.7 sodium chloride(NaCl). <br /> limit for 200 ml water samples is 0.1 mg/1(as lead). 7.0 Sample Collection,Preservation,and Handling. <br /> Page 689 Register 91,No.22;5-31-91 <br />