Forest Products Laboratory (U.S.)

Schorger, A. W. (Arlie William), 1884-1972

Undetermined

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822(.41	ib 64U. S. Department of Agriculture, Forest ServiceFOREST PRODUCTS LABORATORYIn cooperation with the University of WisconsinMADISON, WISCONSINTHE CONIFER LEAF OIL INDUSTRYBy A. W. SCHORGERChemist in Forest ProductsPublished inAMERICAN LUMBERMANApril 29, 1916THE CONIFER LEAF OIL INDUSTRY-ByA . W . Schorge rChemist in Forest Product sThe production of oils from the leaves or needle sof various conifers is a small but fairly old industry i nthe United States . According to the best estimates obtainabl ethe value of the oils produced annually from this sourc eamounts to approximately $50,000 . The leaves of only a fe wspecies of conifers are regularly distilled for their oils ,since it is only for these oils that a steady demand ha sbeen created . The principal species employed are the blac kspruce (Picea mariana, Hill .), white spruce (Picea canadensis ,Mill .), eastern hemlock (Tsuga canadensis, Linn .), red junipe r(Juniperus virginiana, Linn .), and arborvitae (Thuj aoccidentalis, Linn .) . The oils of white spruce, black spruce ,and hemlock are very similar in composition . No attemp tappears to be made to keep the leaves of the latter specie sseparate, and for practical purposes a distinction betwee nthem seems unnecessary . The annual consumption of spruc eand hemlock oil is estimated at 40,000 to 50,000 pounds .It is quoted at 45 to 60 cents a pound . The leaf oil of thered juniper is used largely in insecticides, the annual con-sumption being 15,000 to 20,000 pounds . The prices of theoils from the various native conifers are approximately th esane as that given above . The oil of Pinus picea importedfrom Europe is sold at about $4 per pound but the annua ldemand is below 50 pounds .Yields of Oil from Various Specie sThe oil is found in longitudinal ducts runnin gthrough the needles . The number and size of the oil duct svary greatly with the different species, and on these factor sthe yield of oil is largely dependent . The number of oi lducts may vary from one to ten . Naturally the species con-taining numerous ducts of large size will give the larges t-Published in American Lumberman, April 29, 1916 .R272	-1-yield of oil . This assumption has been verified in the var-ious species examined . The longleaf pine needle containsfive large oil ducts, the average yield of oil being 0 .42per cent, while the lodgepole pine needle contains two oi lducts, the average yield of oil being only 0 .16 per cent .In all cases the yields are given in per cent of the weigh tof the green leaves .The approximate yields and principal constituent sof the various species are given in the table presented o nthe following page .Properties, Composition and Use sAs a general rule, the oils have a pleasant odo rresembling the fragrance of coniferous forests . Occasionallythe freshly distilled oils have a disagreeable odor tha tfrequently improves with age .The oils are composed mainly of terpenes, terpen ealcohols and their esters, and sesquiterpenes . (See table . )Among the terpenes pinene and limonene are ordinarily present .The attractive odor of the oils is due mainly to borneol an dits acetic ester . In general, the more highly prized oil scontain large amounts of borneol, both free and combined .Spruce and hemlock oil contain 35 to 50 per cent of thes econstituents . The popular Siberian needle oil, of whic h5,000 to 10,000 pounds are imported, contains from 29 t o39 per cent bornyl acetate . Among the sesquiterpenes cadineneoccurs most commonly . Thujone .is a characteristic constituentof thuja oil from Thuja plicata and Thuja occidentalis .It is difficult to obtain direct information on th epurposes for which the various oils are employed . A largeamount of correspondence addressed to manufacturers purporte dto use these oils in their products afforded very little in-formation . Information on the uses to which the oils are putwas obtained mainly from dealers and distillers of the oil .The spruce and hemlock oils are extensively employe das a perfume in greases and shoe blackenings . They are als oused in considerable quantities in liniments and othe rmedicinal preparations .R272	-2-a)	ci	ci a) a)	a)	F+	C ] a)	P4P.1	'	H	W	0rl a) H	O	0 0	a) 'd F-t•H E	~`' Q) Q) a) a) cl fi o ci 'd	o	o	cd cd ci c	ci a). . . .	.	• (J)l~ a) lM'o C) ~'	6 wa	PI MIU 1 Q ) p a) O a) a) ci 0 a ] a) a) H a) a) a) o a )I~: I	o •H a) -H g 0 0	id +	. . d e--I r-f	r" g	g O ~-~ •r•IH I	H >~ 'd 4 rJ •H •H Fi •H r-I r-i •H F4 •H H U) '." .̂ '+•,-1 •r-i •rl O •rip •H ''d •HFi I	p, cd P-i cd p p, o	ri rl P., o P., o	P, Pi n, • r-) a • P+ cdP4 I	I	O	o I	1 ,0 I a) a) I ,0 I A F-i Fa F-I 1	1	i	r-i I U 1H0a)I~Fi0a)0 H Hci '- O Q)Oa )o a) a) a)s co a)+)+'ci F-4H a)a) , A cd cd ci o O cdcdacia)o4-) Oa)a) a) F Cd cd a) a) a) cdci 0 a) •H ci ci 0a) cd +' rl rt H O a) a) H•H rl	- ^ 0 ci O a) O O .1~PiIa)	a) FI	Fi	t~	F+I~' •P -P O O a) a) • H Q) 0cd	HH ,0O	4-3	H	a)a)	a )a)	O	a) ci	ci •r1 •H ci0	+3 a)	a)	p, a)ci a)	d) cis~ a)Ocirl a)q F-lN 'dte a )H. ~l~ciq HHI	a1	0150	N- 01 0 0	0 0	0 1 4 1d1	I` r1 ~f)	ti lfl LO Oti O O EllMq 1 50 50 5o N- Lfl ti r--- H H N N O N f- O▪ +~ ! 50 t50 50 50 50 5o so rr1 5o o	4-i •H I	• +' 4-	4' +) 01+' • 01•H 1 O O O O O O O cd cd cd cd • cd oU cd I I 1 1 I I I O I O	a) F-1 1	N 01 Imo- t50	f~- 0 LC10I f'-- 01 z " O 50 H I Lcl Lf1	I	P, bD I	H N Imo- H I`- H 01\O N N Pal l- i-4 50 t50 Lcl0 LCl t`U)	1	0 tO '60 f`\O LC\lD \O ti f` LcI N N N 50 H 1Y1~D 5001150 l5q 60 60 t50 )50 50 t50 t50	01010101150 010150 '60000 00 O . 00 00 O. 00 00 00 00 00 00 00 00 00 00 00 00 00 0	00 00 00 00,00 00 00 0 0ri E c tom-r4 •H Ia) O 1 0000 N- 5001 O N\LC l rl•H	I r-irirlZ N OO ONri H4-1	I	•	.	.	.	.	.	.q 1 00Hto500000 •00M 0 LflN HHR272w o p.	.1-4	H	Q) (D 5a,	'2	Q)ciPi Q,cda 0 Pi•H	a)	F-1a H• O-P	Cdd +) cda) .HO• 0P4 PA	0	cf.)	*	*	* *q-4.HPCcdr•, i • ^ 4-DCd' Fi, .	F-1cd, O Oc .-p o rl-H ~; .•i . . O0 (A U C•H O •r.4 c; -4-)cd • $D O 'dCQ p. Cd	,- a	a)	dD	(D	a) 14'4	p ,Ha) p, O	F-i	•c	• H•HH a) -A--04r	F-1	4-1 v	o F-1 4-1	cAFi a •H	CdQ) a) CH a)	,- I~~- cia•H O	Oa) ,raIZ	f=l* * * * *cd▪• . . r ..l ^ cd • ci• • <-- r-i O -p cd• CA ••H•H cd .~ •H▪ .H o co•r• ita Cd •H c •H• cd ci • - +) H a) iiO• cia) cdciP4F-i N( -HH ai co '0 Cd cvcdcd	o	a)	COU d Cdo o ,.gEH	F-1• a) U RAcd p acd U o rd Cci r~ F1 •H	• Ha) •H -H O o	cd ,..-IU 1=4 P,	• rl .i ''a	iH .._.~ Cd ,Oo F4- , U 0 c	- 'd b•HO	•H 'd H O P+Pi	a)F-1 a ,	o t~ .a)	Fr'to rte, a) O Cd a) a)U+)H CY]4-'4~ a)• cd .  zi(D r-l .s; ; a) Cd•Ha) S~	a)ar~xm	Fi x*• F.a s a)• vv ci9HIDf +fCedar oil from Juniperus virginiana is' employe dmainly in insecticides . Thuja oil from Thuja occidentali sis used in insecticides and liniments . Various native andforeign oils are employed medicinally as inhalations fo rlung diseases, and as additions to baths and ointments i nrheumatic afflictions . Various perfumes contain certai namounts of needle oils whose value consists in having aso-called "ozonizing" effect . The oil of Pinus montanatamed with chloroform is used in quantity as an eibrocation .Tnt'Europe, especially, the finer neet1B 611 --grit ised .tensively as perfumes in soaps ." tThe great	,	lli'4 ' r-small farriers in Ne	ngland duringthe farm work is slac-	In 1912 a cw4v eng od in the di	')*ton of tcata) oij an~~I,~q	>' "' The,r -	deli* r '` n Seattle in bundle of1ki	nt, ct price of	50 to $5 .50 per tort ,or). t'	oil content . The material was packed i n'tom	E and 0 tilled with steam at a pressure of 40 t o90, pCAi	, for 3 - . 5-• ours, the distillation being discon-tinued when the amount of oil coming over did not excel10 cubic 'centimeters in 5 minutes .	-'The average yield of oil was about 1 per cerit '--th-o weight of the green material . Young trees containe dlargest a lount Qf oil, and the haves= were richest in. .-	' : •January, , f ebru_a fir, , and , ag.rch . , T .,	a market value of . .4+0	its a pi)	, buf' t*	arcely suffici. _it to cove rths cost of p	tion .	ri'f the oil was	v .	+o 'ITtsu31B.c' e' is	insel44de ca	-'Mothine . " VIM, art . iday '	cont	about 35 pc*,	of cedar &I' -End45 por	t . of	1 ~~ . . bent made .	ating the fine .gstbund Che1ls of peac 4 pits .. i: ,tempts:-'hac,n mad®•4 i''OrItious times to utilil epine fiz	• .fstiori .of fiber after the oil :-been removed by distillation . The most ambitious attempin this direction were made by C . A . and O . C . Terrell ,Grant's Pass, Oreg ., who obtained patents Nos . 675,206 a _758,874, Rovering methods and apparatus . The plant, des Zbecby Erown, utilized leaves systematically picked from Ong2-Scien. Amer . 84, 344 (1901) .8272rill ed i*'onths when . 'at t l~e , ?'~a 1	of red ,l tbranches,, 3A4 inch-4-trees of the western yellow pine . The stills consisted o fwooden tanks with steam connections, and had a daily capacit yof 2,000 pounds from which 10 pounds of oil were obtained .After suitable treatment the spent needles produced a long . ,tough fiber that could be woven into fabrics or made int omattresses when mixed with hair .Forest Service Investigation sThe large amount of lumber cut from coniferou swoods renders available large quantities of needles and twig sthat at the present time are not only a sheer waste but ar efrequently the cause of destructive forest fires . If a suf-ficient market could be created for the oils a great economi cadvance in management would be effected . At present, however ,the demand and price for oils of this type do not warran ttheir manufacture on a large scale .The leaves of a number of the most important wester nand southern conifers were distilled to determine the yiel dand chemical composition of the oil . Samples of these oil swere sent to various manufacturers for practical tests . Themost promising oils, judged from odor, were those of the long -leaf pine and western yellow pine . Unfortunately in nearl yall the oils and ester content was low and their odors di dnot surpass those of the already firmly established spruc eand hemlock oils . There appears to be an increasing utiliza-tion of conifer leaf oils, and the creation of a demand fo rnew oils, as well as the extension of markets for the commo nones, may be anticipated . It is frequently difficult, however ,to introduce a new oil on the market, even though it may hav edecided merit .Principles of DistillationThe oil is removed from the leaves by the familia rmethod of steam distillation, usually at atmospheric pressure .As the steam passes upward through the needles the oil vola-tilizes and the mixed vapors pass together into a coolin gapparatus where condensation takes place y. The condensationproducts soon separate into a layer of oil and water, owingto their immiscibility and difference in specific gravity .'S' :rig' distillation under pressure is more rapi dand produces_iwot& *41 than distillation at ordinary pressure .Then, steam dt dt.inospheWIPkessure is employed a greate ryield; is obtained if tine n-d*d..es are cut into small pieces .In this .may the oil ducts are more exposed to the action o fthe steam and more materi-a'l tan be placed in the still .Experiments have shown that a still will hold 25 to 50 pe rcent more material when it is finely cut .The largest yields are obtained from young trees .In New England c- Oar oil is distilled almost entirely fromsmall tr,e•es growing- in. aid pas'Gur-es and abandoned fields .All trrees growing ifs the open contain more oil than thos ein a normal forest stand . The season of the year also ap-pears to have a considerable effect, the data availabl eessentially agrAeti g irvVhat the most oil is obtained dur-ing the winter amd spring months . The leaves of the wester nred cedar (Thu12:plica ) were richest in January, February ,and March ; the leaves oif •incense cedar vvexe r _~ e ice,	February and November than during tie 'llervening summeft -, 4 -months .TheStill and :_Tts 0a01j.onThM . exp,e-rimentaJ, - ,s : • .ll used by the., Forest	~~ c et.	4 =	onstructL i nn~	Sri•+bed	f the - till for holdingheight by 2 feet 3 inche ss	B	G . copper . The ends were'1-3/4 inches wide ,he heating vessel	ty fla	h rings . The cove r`1 1 fast :	, linden with malleable iro n~ F -	-~	usl in the joints . I nbase of the cylinde rremovable frameThe exteriored	ss►er .	of asbestos i n- . .	yeti• .~r~	~_	rr,► -~	{	nsation of th e	- { '	r was 3 fee tconstructed of1. 1et 6 inmade of 1 6and the . **	and	ded w/2-in hstop fo r,' --	- - - e d1-1/2 feet internal diameter, placed in a galvanized iro ntank 2 feet in diameter by 2-1/2 feet deep . The condenserwas connected to the still with an 8-foot copper pipe, i ntwo sections 2 inches in diameter . A 2-gallon aspirato rbottle, having a brass syphon, served as a receiver .The material to be distilled was first passed throug ha feed cutter, the needles and twigs being cut into lengths o f1/2 to 1 inch. When the chopped material was well packed int othe still the charge varied from 350 to 500 pounds, dependin gupon the species . By filling the cylinder ahead of the risin gcolumn of steam, the needles are decidedly more compressible .The distillation was continued at the rate of 2-1/2 gallon sper hour . At the end of 7 to 8 hours the quantity of oil fel lto 5 to 6 cubic centimeters per hour, and the distillatio nwas then considered complete . The oils are dried and filtere dthrough cotton batting or fine muslin, and are then ready fo rmarket. Sometimes they are subsequently rectified by dealers .The small distillers usually employ apparatus con-structed partly of wood. The leaves are placed in rectangularcr cylindrical wooden tanks while steam is introduced from aseparate generator . The simple apparatus used by a Ne wEngland distiller of cedar leaf oil will serve as a type ofthe stills frequently employed . His description is thefollowing :A steam-tight box, 3 feet by 4 feet and 3-1/2 fee tdeep, with a boiler plate bottom is set on a rock fur-nace . Inside of this box is a grating 4 inches abov ethe bottom to hold the cedar up to the top of the grat -ing ; a pipe from the top of the box 10 feet long carrie soff the steam . This steam pipe runs nearly its entir elength through a trough of water kept cold by runnin gwater . The condensed steam drops into a glass ja rcovered with cloth for a strainer .c

The conifer leaf oil industry

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The conifer leaf oil industry

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