ll. t. Ch . 24 (
THE ART OF DISTILLATION AND THE DAWN OF THE HYDROCARBON SOCIETY
M rt n . S ltz n, r v d n C ll
Of ll th t hn pl d n th l b r t r n n n b h lf f th S n O l C p n . h ll f r t h h n n nt l n th t f d t ll t n. h pr d d r d l n A t 2 , 8 , nd th th l f r t f d t ll t n r hr d d n nt t , b t nd tr b n n t t d . Id rb ll h rt nl b th M ddl A b d f l t r t r x r tt n, h v r ( : t d d r b n v r p t f th t hn . h ... h d v l p nt f th A r n l nd tr d En l p d f n d r t ( 84 , h h p n t b n, nl d, th th d v r p r d n v nt n v l fr 2, nt n f l n A t, 8 , n r t v ll , nn lv n xt n v ntr n d t ll t n th n r f r n n . t n d v r , l d t n th b nn n f t v r tr t n th bj t. . . rb h pr r r r v l t n, n f h t r t d d p rh p th t d f n t v t d f th bj t l d n h rt t . v r l r nd r v fr nt t thr h th n n t nth nt r n h b l t n h v l n b r nd . A Short History of h r t f th the Art of Distilla- l nd tr n tion ( . b tr d b t th f rth n h pr d t t r .C. n th th t t d M ddl E t. In t l t nd M p t , th t t d p tr l pr d th d t ll t n t r v l l h l. v r, bl fr b t n th r pr d t, p n p , l tr l , h h d f r pr n , nd l r t r n b r n r . n f r r t n t . h b nn n d b th f th h dr rb n S r n , t (2 ll A r n , nd t d th th b l n n ll dr ll d t l n f r t v ll , nn l th r b t , rr v n , b Ed n . t n t , r ( 8 880 St C rt f t f th S n O l C p n 54 Bull. Hist. Chem. 24 (1999)
t th d t ll t n f r d l f nd n th r t n f n Al h ( 0 0 , S r n h t r n nd n f l tt r (4): Many types of naft are water white by nature and so volatile that they cannot be stored in open vessels. Others are obtained from a kind of pitch in a turbid and dark condition, but by further treatment they can be made clear and white by distilling them like rose water. h r r n r p rt n th Ar b l t r t r f th d n l v l f n ft r t v f r v r lln . Cr d l nt n ll r f n d n th M ddl E t, p rt l rl n th r n rr nd n th t f n pr nt d Az rb j n fr th v nth nt r A n rd. tr l p n th Un t d St t h d b n d v r d rl 62 n t rn Y r n r th pr nt t n f C b . h b t t r f nd n t rn nn lv n l n tr ppr pr t l n d O l Cr , n r th t n f t v ll . h l p r d v r d b M r v n n r , v d b r r, n 68. h S n h d b n n r d l f r d n l p rp , nd t n b n t Edwin L. Drake f tr d th th E r p n ttl r . h n r t n l nd n n br . h E pt n d b t n n pr r b d r d l n th f r t p rt f th n n t nth th r f t n pr d r . h t r l b nt r r:: f r v r t f lln . t n d fr th d S h r h b ll p r d ll h r r t j r pr bl n th f p r t th rf . h E pt n tr d ntr ll d tr l f r l ht n nd h t n . r t, th r n t n b Ar b h v th Ar b n "n ft" t th pr d ff nt b rn r f r th t r l nd nd, ppl t, fr h h d r v d th d rn t r n phth . f r f n d pr d t n t v l bl t cost p t ft b f r p n n th r n l f th t v th th th r f l v l bl . In 80 r n z nt n nd M l r nd n v , h h r rr A Ar nd ( 0 80 nv nt d b rn r th t nt nd n f r d n n n th r n n th th n pr d d n nt n t f l ht th t h d n v r b n p t r . It b l v d th t th p n h h b n n bl b f r ( . h Ar nd b rn r t xp n v th "Gr r " h v b n d t ll t r th r t pr d f r th r t, b t th d v l p nt n th n r d l. h p n d th r t ff t th rl 8 0 n A tr f b rn r th fl t b th z nt n t th ttl f K z n 680 C n h h h h p r t pr d lv d th f r t h h th M l fl t ff r d n r lt pr bl . h fl t b th t nd rd n r fr b rn n . n l p nd l nt rn fr th t t n rd nd h f r t r rd d r f r n t d t ll t n f r d t ll pr d d t d n h th . l pp r n th r t n f M h d l z In 8 0 n h d th h f v r t f l d ( 4 2 0 , r n ph n nd h t, n h f l f v r n l ht n b l t nd pr . h b t was Book of Secrets. h pr d r b d nv lv th d p r l, b t th A r n h l n nd tr h d v ll d n l b , h h h b n tr n l t r t d d t d th p r h l p p l t n th t th t f nt En l h l b . h l b b t n th pr d t b pr h b t v f r th n r l p p l d rd p f pp r t thr h t th M ddl E t nd t n. n l, b rn n fl d, nd ph n th n b E r p f r pl d t ll t n ( . 2 . h d t ll t l th pr n p l f l . C ph n , xt r f p r z d r b d t r bl r n , th t fr f d t rp nt n nd l h l, was very popular v n t n f r d l d f r h t n nd l ht n nd th th h t p rt l rl d n r b f th v l p t f r dr ll n th f r t l ll. A l t r r f r n t l t f t p n nt nd r r d p l b rn r. A ll. t. Ch . 24 (
much better fuel was needed; and this was produced by mercial success (Fig.4). Having an excess of crude oil Abraham Gesner ( I 797-1864), a Canadian physician by in his possession, Kier turned his attention to its use as training but also a geologist, chemist, and inventor (6). an illuminant. Crude oil itself was unsatisfactory be- Sometime in 1845 Gesner began experiments to pro- cause of its odor and the smoke it produced when burned. duce a better fuel by dry distillation from a black min- Kier sought the advice of James C. Booth (1810-1888), eral named albertite found in New Brunswick. He ob- a consulting chemist in Philadelphia, who suggested he tained a liquid whose use as a fuel for lighting he dem- distill the crude. A small-scale refinery was built in Pitts- onstrated as early as 1846 in public lectures on Prince burgh in 1850; and Kier's product, which he named "car- Édward Island. bon oil," was a local success. That prompted this pio- A similar material could be obtained by dis- tillation of pitch found on the island of Trinidad (Fig. 3) and also of certain types of English fuel called can- nel coal. In 1853 Gesner moved to New York to su- perintend the construction of the first commercial plant to produce this new hydrocarbon fuel, generi- cally named rock oil. Gesner's patent (US Patent 70525, Jan. 29,1850) cov- ered a process to produce a volatile fraction to which he gave the name keroselain, C r l r U d b K r t Adv rt tr l M d n from the Greek kerns for wax and elain for oil. For public relations reasons the n r oil refiner to build a larger scale plant outside Pitts- name was changed to kerosene so that it resembled the burgh. The major drawback to the use of Kier's product name camphene. Kerosene was shown to be a much was a disagreeable odor, but yet 1,183 barrels (each 31 better value for money than any other of its competi- 1/2 gallons) were sold at very high prices. Demand ex- tors. This even included coal gas, both in terms of the ceeded supply, but every attempt to produce more oil cost and the resulting brilliance of the illumination. by drilling additional salt wells proved a failure. The Kerosene became an instant success; by 1859 between value of hydrocarbon fuels for lighting and heating had fifty and sixty plants, representing an investment of four been well established; the major problems were still the million dollars, had been built. These were based on supply and the cost. The solution to this dilemma be- Gesner's process as well as a similar one that had been gan in the fall of 1853. invented and patented by the Scotsman James Young (1811-1883) in Britain and the United States (US Patent Francis B. Brewer (1820-1881), a physician and 8833, March 21, 1852) (7). No one, however, at this graduate of Dartmouth College, had moved to Titusville time was producing kerosene in any significant quanti- in 1851 to join the firm of Brewer, Watson, and Com- ties because of the lack of a supply of crude oil. pany, which had been established by Brewer's father Ebenezer in 1844 to produce lumber from a large tract In parts of Pennsylvania wells had been drilled for of land he owned on Oil Creek. After having completed some time which produced salt water as a source of salt. his medical studies at Jefferson Medical School in Phila- In many of these wells besides the salt water quantities delphia, Brewer began the practice of medicine in Barnet, of crude oil came to the surface. In 1849 Samuel Kier Vermont. He had used petroleum oil in his medical prac- (1813-1874) conceived the idea of selling oil from the tice beginning in 1848. In 1850 Brewer decided to give salt wells for medicinal purposes; but "Kier's Petroleum up the practice of medicine and become an active part- or Rock Oil," put up in half-pint bottles, was not a corn- 6 ll. t. Ch . 24 (
r l nd G n r l l n n nt n r l . Ev r n th l t f r pr f t bl v nt r , ll n d x Cr b n Alb rt t t t v ll n th r f 8 4 t bt n f r t h nd nf r t n nd t v l t th l pr n . h n r Cr b pr d b h t h , nd ll nd Ev l th b n pl n t t bl h j nt t p n t p r h th l b r n pr p rt n t v ll nd t br n th pr d t t r t. In S pt b r, 8 4 th nn lv n O l C p n f nd d th f f t 46 r d n th . Appl t n nd C p n b ld n n Y r . r r, t n n b h lf f h p rtn r , t Y r n th f ll f 8 4 t n th p p r t th ff f ll nd Ev l th nd th p n ff ll n rp r t d n Y r n b r 0, 8 4. In nv r t n th r r t b v d nt th t Cr b h d x r t d r tl th nt t f l pr nt. ll nd Ev l th b h t pt l nd h t nt b t pr d n . v r, r n . r r r r pr p d n ff r t l nd Ev l th th ld n t r f . E th r ll r Ev l th ld p r n r n th f l b n . r r, W t n, nd C n ll n p t th pr p rt , nd f th r n t t p n d th r d l ll t d fr tr n h b th f d, th r nt ld b n l d nd r r, l br nt nd f r l ht n n th ll. r. r r W t n nd C p n ld p ll th xp n f r f n t d b th pr p t f th r l v l n rr d. f r th r f th ld t t v ll , f l nd p r d d h p rtn r t tr t d v l p th l tt r rr v d fr v n. An n Sh ld n, r pr d t. t r d n t r h h d h rd b t th n v nt r , t d th t ll nd Ev l th h ld v t In th f ll f 8 r r v t d h l t r v n, th r r p rt h ht b nt r t d n th pl f th r l th t h d b n ll t d fr th l pr n n th r r pr p rt . h h n t r. x Cr b f th M d l S h l nd r f r O. . bb rd, h tr pr f r, nd l ft f r th r v l t n. bb rd b l v d th t r l t b p t nt ll v r v l bl , b t th l t d ppl d t pr p t d . S n th l ld t b t pr d ht n ll n p r d fr th r r l nd . h r n d n n th f ll f 8 , f ft r r r v t t rt th, G r nr ll ( 82 884 ( . , n t v f n v r nd n 84 r d t f rt th, h pp n d t b v t n h b rth pl . ll h d b n r ntl d tt d t th b r n Y r ft r v r d r r h h n l d d rv n p r nt nd nt f p bl h l n Orl n b f r b n l r. ll nd h l p rtn r n th n G. Ev l th r t v pr t r f r th l f th h r n n l f r d p n . l b h n h pp n d t th b ttl f r l n Cr b ff nd d b t t. Cr b r l t d t ll th t h h d d n f pl xp r nt nd n v n d th t r l ld b p r r ll n nt. ll r n z d th nn t n b t n r r G r M. ll ll. t. Ch . 24 (
nv t n n th r p n . On f th M. Sh ld n r p t b th l v nt r . S ll n r t n nd, pr d nt f th C t S v n n . t Ev l th nd ll n b r 2 , 8 4 th f l n nd nd h p rtn r , h v r, p f d t n l n , h h r l d t r n r r ( : d t n b f r n h r ld b b ht: v t t I v r h nt r t d n th r r h nd th n th pr p rt b r pr nt t v f th r r p, nd I n pr th t th r lt ll t r x nt f n l t d t r n th r l v l p t t n f th v l f th t r l f r n t f p tr l . h th r t n l f r n f th t f l p rp . h l h h I h v f r b p rt nt l nd r n l b d t ll t n b t. t n d r p rf tl fl d...A t th nt t I h v n r h n f r th nt rpr , th r At d bt n d h v ll b n d t ll d n l fr n r f t n nd nj n S ll n, r., f Y l C ll . n l ht d nt t , nd th ht f th v r l On v b r 4, 8 4 Ev l th nd ll r t t r n pr d t h v b n r f ll n t d. h t p r t n h n d fr 2 t nd t ll n pr r r th f ll n (8 : . r. At d f t n n l z n th l, nd t n S ll n r p rt d f rth r pr r h h p d n th h nd f r f. S ll n f Y l C ll . W h ll h v t n l z d b v r l f th b t h t n b Ev l th nd ll t r r ( : th ntr , nd h ll f th r n l nd S n th b v l tt r r tt n fr h h th t f r b t t rn n t x n nd t xtr t h b n t n, th n l h b n xt nd d t t f t f t th r . nd x d ff r nt l pr d d, n n ll th t h th r At d ( 826 868 p rtn r th h th f r b n bt n d 0 p r nt...th r f r f th p n n th t th ld ll b t l t r 80 br th r W ll nd S l h lbr n 8 4 n th p r nt f p r l. US M n f t r n C p n n W lth , M h tt n 8 4 ( . h p n h d b n r n z d t x On br r , 8 Ev l th r p rt d t r r ( : pl t p t nt f th r At d t l br nt f r S ll n pr r n th th n l , h v h n r b th d t ll t n f th l t r r d pr b n bl d t t ll n pp r t f r h , th d d b r (US t nt ,6 0 M r h 2 , 8 . h d n xpl n, b t h p t h v th r p rt n. At d n 8 6 t bl h d th l l b n n h f ll d n Apr l 0, 8 b l tt r fr t n nd d d Abr h G n r h f h An n Sh ld n t r r th f rth r n f S ll n t f th K r n C p n n Y r . At d r ( : t h v v n th r r l pl f rl r r f r S ll n h n t t pl t d h ph t r x n t n nd pr n n d t t h v p t nt l tr l x n t n f th O l n p r n n ll n nt. th th r b rn n fl d , b t ll pr b bl nd p h n l n ll th .... h v l f th l nj n S ll n, r. ( 8 6 88 th n f d p nd tl n t pr p rt b rn n fl d. nj n S ll n ( 864 , pr f r f h In th r p t th n l nd t r lt , h [ ] tr t Y l C ll ( 0 . S ll n, r. h d t d d th b n h hl t f t r . h f th r t Y l , h r h r v d h nd r r d t On Apr l 2 , 8 Ev l th r t t r r ( : d r n 8 nd n MA n 840. Aft r h rt p r d v r d. r f. S ll n p rt. ll $ 26.08. p nt n t n th th h t Ch rl . n, W h d p d t f r th r th n f r h , v r $ 00. S ll n r t rn d t v n nd t d l b r C ld n t h v th r p rt t ll p d f r....It n n t r n tr t r f r h f th r dv n d t d nt . In th h nd f th r nt r. W ll b r d f r ddl f 846 th Y l C rp r t n r t d pr f r h p n n xt ....It r t r p rt. ppl d h tr t h h S ll n r. pp nt d. An n Sh ld n r t t r r b t th r p rt n Apr l th p t n h d n l r tt h d t t, S ll n 2 , 8 ( : f r d t l v Y l nd nt t th Un v r t f v ll . In 8 4, th th r t r nt f h f th r, h S ll n p rt n n h nd , nd f v r bl t r nt rpr , b t ll nd Ev l th h d d th l tt r p t n nd t n th r h f l d t t th r f r h n pl n $ 00 ppr h d t n l z th l pl pr v d d b t h r d t n th n f Y r ...h pl d th r r. It d l l t th v n nv t r p rt n th h nd f fr nd n Y r th th t h t f S ll n t t r h ld n l z th n tr t n n t t d l v r t p nt l t f t r r l. v r th r h n l nd t h r n nt r d f r th p nt f h b ll r p rt, d t d Apr l 6, 8 , th t th n tt n h h nt , ( n l d n th xp n f h pp 58 Bull. Hist. Chem. 24 (1999)
ratus employed in the analysis), to the round sum of narrow range over 43% of the crude oil distilled. The $526.08 about $75 had been previously paid....making temperature was raised again, this time to above 360° the whole expense exceed $600.This sum may at first C, and another 31% of the crude distilled. This frac- appear exorbitant, but when we take into account the tion, after treatment by boiling with water, was used as time consumed, the nature of the experiments, and the material for the illumination tests. h l t the value of the Report, I think those concerned will be satisfied....Several gentlemen here of known abil- 75% of the crude oil was separable into distillates by ity have assured me that they should take some stock, using external temperatures ranging from 280-360" C. if Silliman's Report should be favorable to the oil. Further distillation at even higher temperature in the end That point is settled, the Report is more favorable, led to a recovery close to 90%. Silliman concluded (12): even, than I had dared to hope. Anson Sheldon reported to Frank Brewer on May 11, 1855 that "Prof. Silliman pro- poses to take some stock (11)." The report, printed in New Haven, amounted to twenty 5" x 8" pages. How did Silliman do this most impor- tant analysis? His own words provide the answer (12): To determine what products might be ob- tained in the oil, a portion was submitted to fractional distillation.*..*(Fractional distil- lation is a process intended to separate vari- ous products in a mixture, and having un- like boiling points, by keeping the mixture contained in an alembic at regulated suc- cessive stages of temperature as long as there is any distillate at v n p nt, nd th n r n th h t t n th r d r , t . . From a sample of 304 grams of crude, Silliman was able to distill 160 grams into several different fractions (12): We infer from them (boiling points) that the Rock Oil is a mixture of numerous com- pounds, all having the same chemical con- stitution, but differing in density and boil- ing points, and capable of separation from each other, by well-regulated heat. Silliman performed various chemical tests such as elemental analysis, tests for acidity and corrosive action on copper, inertness to hydrochloric, chromic, and acetic acid, as well as the action of metal oxides. Lack of reaction with calcium chloride, potash, sodium carbonate, and calcium oxide was The Drake Well in 1866. also observed. Reaction with bleaching Peter Wilson and E. . Drake are shown standing in the foreground. powder produced a product resembling in character that of chloroform. The oil was slightly soluble It is safe to add that, by the original distillation about in alcohol but easily soluble in ether. Silliman did a 50 per cent of the crude oil is obtained in a state fit second distillation of the crude oil, this time on a much for use as an illuminant without further preparation larger scale and with a copper still. The temperature than simple clarification by boiling a short time with fair water. was raised to 280°C initially and then to 300° C. In this Bull. Hist. Chem. 24 (1999) 59
The report concluded with a discussion of the naphtha traded his shares for cigars, which he gave out freely to as an illuminant and photometric studies. Silliman stated young men in Titusville. What a mistake he had made that the fraction from the high-temperature distillation, became very evident on the weekend ofAugust 27, 1859, that which boiled below 360°C, burned without smok- when the first oil came in. Although Drake is usually ing and gave light which was (12): given most of the credit for the dawn of the hydrocar- .....p r nd h t th t d r. It r t f n p bon society, would it have started in 1859 if not for Ben- t n n h lf f th f t l h jamin Silliman, Jr. and his application of the art of dis- ph n h h n n . I h v b tt d tillation? th l p b rn n tr l t th n p t n f th t xp r n d l p t h r bl t ACK OW E GME , nd th r t t n , th t l p b rn n th fl d v h l ht n h h th h d n, I would like to thank the Drake Well Museum and the th t th l p nt r n ll , nd th n f r t f l ht r t r th n n ph n . Pennsylvania Historical and Museum Commission for assistance in obtaining copies of the Brewer papers. A To test the intensity of the light Silliman constructed a special n t f appreciation goes to my colleague Mario photometer. The standard used was Judd's Patent Sixes DiNunzio of the History Department of Providence Col- Sperm Candles which were assigned a value of 1. Com- lege for his help in preparing this paper. pared to coal gas light, sperm oil, and camphene, the Rock Oil produced the highest value for the light inten- sity and possibly the best value for cost. At this time it was difficult to fix a value for the Rock Oil because it E E E CES A O ES was not yet in commercial production. Silliman noted that preliminary results indicated the oil was also a good . . . rb , A Sh rt t r f t ll t n, E. . r ll, lubricant (12): d n, ll nd, 0. 2. h t r h dr rb n t h b n d b n l In n l n, ntl n, t pp r t th t th r Y r n n h b h r z , h Ep Q t f r O l, h r nd f r n r nt n th b l f th t M n & , h t n , Y r , . r C p n h v n th r p n r t . I. rb ll, n th ntr d t n t P.H. Giddens, h rth r l fr h h, b pl nd n t xp n v pr f th O l Ind tr , M ll n, Y r , 8. , th n f t r v r v l bl pr d t . 4. f. , p . It rth f n t th t xp r nt pr v th t . h d f n t v t d f th Ar nd l p n b f nd n n rl th h l f th r pr d t b n M. S hr d r, h Ar nd rn r: It Or n nd f t r d th t t , nd th l l b ll d v l p nt n r n nd En l nd, 80 800, Od n r t d pr h h n pr t , n f th t Un v r t r , Od n , n r , 6 . S l M. pl f ll h l pr . . S ltz n, " r n rr A Ar nd: t h r The report created considerable interest in New York ht," ll. t. Ch ., 1999, 24, 48. and New Haven, and two-thirds of the shares were sold 6. r d f n t v t d f Abr h G n r, K. t n, reasonably quickly. For legal reasons the Pennsylvania " r. G n r K r n : h St rt f A r n O l Rock Oil Company of New York was reincorporated in f n n ," n t. v., 1955, 2 , 28 . . r f rth r nf r t n b t Y n , . tt, Connecticut on June 25, 1855, with offices in New Ha- " nd f th C l O l Ind tr ( 84 64 ," Expl r ven and Benjamin Silliman (13)) as president. t n n Entr pr n r l t r , 1964, 2, 6 0. All did not go smoothly with the attempts to obtain 8. tt r bt n d fr th r r Ar h v t th r oil in commercial quantities. The method of surface col- W ll M , t v ll , A. . r r b t th r At d, t n l C l p lection was abandoned in favor of the novel approach d f A r n r ph , . Wh t , Y r , of drilling a well. Edward Drake (14) was hired in De- 06, l. . cember, 1857 by the New Haven group to act as super- 0. r b r ph th r f r n f r f th r r d n , intendent at the Oil Creek site and to begin the drilling. . G. Gr n, " nj n S ll n," n t n r f S Various delays postponed drilling until May, 1859; and nt f r ph , Ch rl S r bn r S n , Y r , there was little confidence that drilling for oil in solid 0, l. 2, 4 2 4. rock would ever amount to anything. The shareholders . r r Ar h v , r W ll M . became increasingly disenchanted, and the money raised 2. . S ll n, r.. p rt n th O l, r tr l by the stock offering was running out. Frank Brewer fr nt n ( C ., nn lv n , . ., nh St r r , v n, C , 8 (I ld l th n 60 ll. t. Ch . 24 (
Dr. F. L. Holmes for his assistance in obtaining a copy drilling operations near Syracuse and Pittsburgh on his of this report.) trip and became convinced that this was the best way to 13. For a study of the work of Stlllman as a consultant, see extract the petroleum. His persistence in drilling led to G.E. Webb, "The Chemist as Consultant," Bull. Hist. the birth of the oil industry in Pennsylvania. Although Chem., 1994, 15/16, 9-14. not trained as an engineer, Drake was the inventor of the 14. Edward L Drake was by trade a railroad conductor on idea of using pipe to prevent the filling of the hole driven the New York & New Haven Railroad. Forced by ill in the bed rock by sand and clay., health to retire, he retained a pass for free travel. For this reason he was hired by Eveleth and Bissell in 1857 to go to Titusville to obtain some legal papers. He was ABOUT THE AUTHOR introduced as "Colonel" to impress the locals and for- ever has been known as such. He studied the salt well r. M rt n . S ltz n r f r f t r l S n t r v d n C ll , r v d n , I 02 8.
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1999 DEXTER AWARD
The Dexter Prize Committee of HIST has selected Dr. Mary Jo Nye, the Thomas Hart and Mary Jones Homing Professor of the Humanities and Professor of History at Oregon State University, as
recipient of the 1999 Dexter Award for , Outstanding Achievement in the History of Chemistry. Professor Nye is the author of tour books and more than three dozen articles on the history of chemistry and its interactions with physics. For 25 years she participated actively in the formation of leading undergraduate and graduate programs in history of science at the University of Okla- homa, and she served for three years as President of the History of Science Society. The award will be presented at a luncheon at the conclusion of the Dexter Award Symposium at the 219th National American Chemical Society meeting in the spring, 2000, in San Francisco.