Document ba8LGL3YvevXNk9womGwOpr71

INTER-OFFICE ORflESPONDCNCE Et h y l Ga s o l in e Co r p o r a t io n Re s e a e c h La b o r a t o r ie s 723 Ea s t Mil w a u k e e Av e n u b De t r o it , Mic h ig a n September 12, 1938* Dr, fill lard F, Machie College of Medicine University of Cincinnati Cincinnati, Ohio Dear Bill: I am sending you herewith a copy of our report LTD $38-46 covering the steam distillation of some of your sludges, I will be interested to bear from you how our results compare with yours on these same samples. Vie are continuing our systematic studies on the stability of lead compounds, concentrating at present on PbEtgOH and PbEtgCOH^, I am looking forward to your promised visit to discuss some of these matters. GC:AMC LEAD OOaEST OF SLUDGES AND WATER BOTSQI-iS FliOM SLEilDIW AND STORAGE TASKS USED -FOR ETHYL GuSOLIEE LTD #38-48 277.AP.1,2,4,5,6,7, 8,9 and 10. F. J. Bykstra Sept. 7, 1938. FUHFOSE To determine the lead content of sludges read water bottom sample a from blending and stareg tanks used for Ethyl Gasoline, particular emphasis vt&s placed upon the volatile lead, i.e., the FbEt^ already present or f`or3d by steaming of the sludge. CQECLU5IQKS - The tan water bottom samples from both blending and storage tanks 'were with two exceptions, free of soluble lead compounds. The two sample)a with lead each had only 7 mg. pb per 100 cc. of solution. 2. The eight sludges fraa both blending and storage tanks had with two exceptions only small amounts (l/j-3#) of load in them, and only a small part of that could be removed by steaming. 3. Sludges with high lead content, but with or without volatile lead are possible. One sludge contained on water-free basis, approximately 20,'i load, of which about could be removed by nine hours of steaming. Another sludge contained 07; lead, of which only a trace was volatile lead. The water bottom camples were simply filtered and analysed for lead. The sludges usually containing gasoline, water, rust and solid matter were placed in a distilling flask and enough water added to bring the liquid volume to approximately 300 co. iho lighter gasoline fractions wore first taken off from the side tube of the distilling flask and condensed in ice. The side tube was then dosed and all of the vapors refluxed using a water oondenser to return the condensate to an ice-cooled trap which separated the water from the oil layer, and returned the water only to the boiler flask* The portion of the trap vjhero the oil layer collected was graduated, enabling readings to be taken. If more than one fraction of oil was dosired, the refluxing was stopped long enough to pipette out the oil layer already formed. After equilibrium was established, the system with a C'Og cooled condenser and a gas burette in the line was closed. Atmospheric pressure in the system was maintained and the gas, non-condensable in CO2 ice was .measured in the burette. The refluxing was continued until no wore oil or ?bEt^ layer was formed. This tine varied from throe to nine hours, but ivas usually about six hours. 0022269 N22448.01 The products then submitted for load analysis were the? following 1st - hater-white gasoline fraction, fad - Yellow oil layer. 3rd - filtered "ator solution from the? boiler ilask. 4th - The solid residue, dried over activated aluzainum until moderately dry. ISSCRIPTIOU 0? SAMPLES USED 277-SP-l - Jampie 37A-2S5S. Bottom sludge from Esso storage Tank, -$9 Standard Oil ox' H.J ., Rookaway, li .J. Sulk Plant. Storage only, never previously deemed. March 11, 1337* 277-XP-2 - Sample 37A - 3064. Bottom sludge from the Texas Go., Claymont, Del. Tank -<1362 ('Blending Tank). 277-XP-4 - Sample 37A - 1713. Bottom sludge from standard Oil oiE.J*, ilockBsmy, H.J. Bulk Plant. Tank #4. Sssolene (storage only). 277-XP-5 - Sample 37A - 3678. Dry sludge from Atlantic Refining Co,, Franklin, ?&., Tank #340. 277-XP-S - Sample 37A - 3001. Bottom sludge from Richfield Oil Corp. of H.Y., Bayonne, H.J. torainal. Blending Tank #2. 277-XI-7 - Sample 37A - 3681. Bottom sludge Texas Co., Mobile, da. Tank #7038. 277-XP-8 - Sample 37A - 3100. Texas Co., port Arthur, Texas Refinery. Tank #1086. 277-XF-9 - Sample 37A - 3014. Side l all 3calo from Standard Oil, hew Jersey, Paterson, li.J. Bulk Plant. Used for storage only. Tank #1. 277-XP-1G - Water bottom samples: ,1 - Bradford Oil Refining Co., Bradford, ?a. Tank #77, Kov. 12, 1936. #2 - Sinclair Refining Co., Houston, Texas, Tank (424, Bov. 25, 1936. ,?'S - Standard Oil Co. of R.J., Canton rbf., Baltimore, Md. Tank #225. Seven blends since tank cleaned. 5,248 lbs. T.B.L. "Q.'* Blend, Oct. 26, 1936. (4 - Cities Service Ref. Co., East Braintree, Mass. Tank . 23, Bov. 12, 1936 #5 - Humble Oil & Kef. Co., Baytown, Tex. Blending Tank #716, 1,'ov. 25, 1936. #6 - Cocony-Vacuua Oil Co., Portland, Maine, Tank #32, Hov. 20, 19S6. ,7 - The Texas Co., Terminal Baltimore, Md. Tank #7094. Seven "<4n Blonds, 4,443 lbs. T.B.L., Oct. 28, 1936. - 2 Hi 0022270 #6 - Continental Oil Co., Kef. Baltimore, Ad., Tank #154, 58 Blends, 100,650 los, X.S.L. Oct. 28, 1936. #9 - Mid-Continent Pet. Corp., West Tulsa, Okla. Tank >313, Hov. 17, 1936. 10 - Oolonial Beacon Oil co., Everett, Mass. Tank ,118, Bov. 18, 1336. STEAMING C)F TAI.iK SLUI&-.ES Experiment 277-XB- Sludge (Dry basis) Appr. Gr. Gasoline Gas 17ol. Pb :Evolved frontont cc. CO . -JS?-.... 1 45 70 9 0.756 2 15 7 7 0.066 4 29 10 5 0.004. > 01 49 nil 8 3 5 4 0.002 V1 12 68 0.46 NJ 42 10 32 trace 9 36 13 nil Oil water Vol. Fb Pb Content v: Content CO. gr. a . gr. G, 5 1 1.3 drop J m& 1.2 2.2 drop 0,933 S f A' 0.233 0.092 ' 0.061 0.002 0.027 0.0003 nil ' 0.023 0.08 ; .0.012 trace 0.044 yj. 0.019 277-XP-10 Analysis of VJater IP>ttom Samples (lOO cca.) fl Blank Pb 2 $i El -n , /' s ' < t <' ,, ' o a ti .. . . /"' 1 ^ , . A it r r it it ' G V 11 /` V ;t ?! ( h O 0.0067 g . Pb/lOQ cc 9 Blank Pb z S/ C 10 0.0075 c . Fb/100 CO. ,'A 'A " BI3CUS8I0N or RESULTS .... - ' -V-. X i Aasiduo Pb Content . .... . ....... 18.5 . 0.3 3.1 3.1 2.8 O ,0 67.3 3.2 Gas evolution, which usually accompanies tils steaming of the pure load alkyl halides was not an infallible indication of these compounds. Experiment 277-XP-5 with no volatilo lead and hardly any water soluble* lead gave a large amount of gas* At least volatilo lead and water soluble 2sad compounds wore not farmed by the changes which produced the gas evolution. The 67# Pb residue of 277-XP-8 was black, suggesting strongly precipitated PbS. Alien some of this residua was dropped in dilhta 14SO4, HgS gas was evolved, a tost duplicated on pure FbS. '..lis type of sludge or water bottom sample produced is likely dependant upon the cleaning history of the tank. For instance, the storage tank mioh had the volatile load producing sludge of 277-XP-l1had never been cleaned, and one of the . water bottom samples, 277-AP-1G #8 with soluble load had come from a tank in which 68 blonds using 100,650 lbs. of T.A.L. had been made. HS 0022271 Ilia tank records of the water bottom and sludges tested are very incomplete, but designated blending tanks did not pro due o sludges with, high lead content, or orator bottoms with more than a snail amount of soluble 3sad in i.lion 1'he storage tank appears to be a jaost likely source of dangerous lead containing sludges. iC HZ 0022272 mm