With a basal injector, loblolly pines were treated with 5% paraquat cation (weight weight basis) and harvested after 18 months. The resin acid, turpentine, moisture content (MC), and energy value were measured in three bolts of the stem. In bolt 1, the first 152 cm above the injection site, the increase in resin acids was 392% and in turpentine, 564%. Within the whole stem (the first two 152-cm bolts and the third bolt to a 7.6-cm inside-bark diameter), resin acids and turpentine increased 203 and 296%, respectively. Moisture content was reduced 9%, 8%, and 8% in bolts 1, 2, and 3, respectively. Turpentine from treated and untreated trees had an average heating value of 19,369 cal/g. When weighted for volume, net energy content was 7.8% greater for treated than control trees because of the increase in resin, including turpentine and the lowered MC

Huffman, Jacob B.

Kossuth, Susan V.

Roberts, Donald R.

Wang, Shih-Chi

English

Wood and Fiber Science (E-Journal)

ENERGY VALUE OF PARAQUAT-TREATED AND RESIN-SOAKED LOBLOLLY PINE' Susan V. Kossuth Supervisory Research Plant GeneticisWPhysiologist USDA Forest Service, Southeastern Forest Experiment Station, Gainesville, n 3261 1 Donald R. Roberts Research Plant Physiologist. Retired IJSDA Forest Service, Southeastern Forest Experiment Station, Olustee, FL 32072 Jacob B. Huffman Associate Professor of Forest Products and Shih-Chi Wang Assistant Research Scientist in Wood Science School of Forest Resources and Conservation. University of Florida, Gainesville. FL 326 1 I (Received March 1983) ABSTRACT With a basal injector, loblolly pines were treated with 5% paraquat cation (weightlweight basis) and harvested after 18 months. The resin acid, turpentine, moisture content (MC), and energy value were measured in three bolts of the stem. In bolt 1, the first 152 cm above the injection site, the increase in resin acids was 392% and in turpentine, 564%. Within the whole stem (the first two 152-cm bolts and the third bolt to a 7.6-cm inside-bark diameter), resin acids and turpentine increased 203 and 296%. respectively. Moisture content was reduced 9% R%, and 8 %  in bolts I, 2, and 3, respectively. Turpentine from treated and untreated trees had an average heating value of 19.369 callg. When weighted for volume, net energy content was 7.8% greater for treated than control trees because of the increase in resin, including turpentine and the lowered MC. Keywordr Oleoresin. resin soaking, turpentine, resin acids, paraquat. energy As energy prices soar and supplies become limited, the interest in growing trees for fuel has increased (Bente 1979; McAlpine et al. 1966; S7ego et al. 1972; Young 1972). Considerable research has been conducted to study Increases in resin of pines after treatment with paraquat (LRCC 1974-1979). However, no studies have been made to measure the caloric content of resin-soaked pine. The tre- mendous increase in resin, especially in the first 3 m of the stem above the treatment site, should result in large increases in the caloric value of treated trees. The objectives of this study were to measure resin acid, moisture, turpentine, and caloric content of stem wood of paraquat-treated loblolly pine (Pinus tarda L.). ' Appreciation is extended to John Munson, Junior Broomfield, Gary Holmes, Kimberly Horgan, Southeastern Forest Experiment Station, Olustee, FL 32072, and Lyn Brown, School of Forest Rc- sources and Conservation, University of Florida, Gainesville. FL 3261 1 for tcchnical assistance. This publication repons research involving pesticides. It does not contain recommcndations for their use, nor does it imply that the uses discussed here have been registered. All uses of pesticides must be registered by appropriate state andlor federal agencies before thcy can be recommended. W w d  and Fiber Science. 1601, 1984. pp. 398402 o 1984 by the Society of Wood Sciencc and Technology Kossulh n a/.-ENERGY VALUE OF RESIN-SOAKED LOBLOLLY PINE 399 TAHLE I .  Analysis of chan~es  in moss ofloblolly pine stem components 18 monrhs qfier trearment wirh 5% oarayuor cation (weight/weighl basis)." Resin acids Turpcnlinc Waod Water Iln- I ln -  On- IJn. stem "orlion ~ r e r t e d  trerfcd lncrearc Treated lriated Increase Treated trealrd Treatsd mated ............ kg/mJ ............ IN, .......... kg/& ........... % .......... kg/m3 ........... . . . .  kg/m' ........... Bolt 1 V 4 . l V  13.8 392 17.5" 3.1 564 621. 621 444' 485 Bolt 2 27.4. 9.2 298 9.4' 1.5 626 611* 615 493' 539 Bolt3 11.8 11.3 4 2.9 2.4 I21 548 544 530 575 Wt. ave.' 23.4' 11.5 203 7.1* 2.4 296 574" 574 505* 518 D a t a  anallred by ScheQ's lest. *Bolt I = first 152 cm. Bolt 2 -second 152 cm above the treatment rile, and BoL 3 =the remaining merchantable stem to a 7.6- insidr-hnrk dinmner. ~ Wl.iahlcd rcrordingto vo1vmc of tach bolt. S~gnilicanlly dilPren! lrom control at 0.05 level. MATERIALS AND METHODS Plantation-grown loblolly pines, approximately 20 years old, near Aiken, South Carolina, were injected between April and July 1977, with 5% paraquat cation (weight/weight basis). This was done in a 3.8-cm-wide slash through the bark every 12.7 cm around the trees. Fifteen injected and fifteen similar but untreated trees randomly assigned as controls were harvested for analysis after 18 months. The trces were felled and crosscut into 3 bolts: bolt I was the first 152 cm (60 in.) above the injection site, bolt 2 the second 152 cm (60 in.), and bolt 3 the remaining merchantable stem to a 7.6-cm (3-in.) inside-bark diameter. A 2.5-cm (I-in.) stem disk was cut every 30.4 cm (12 in.) of the tree length, and the disks were combined on a bolt basis (i.e., 5 disks each from bolts I and 2, and a variable number of disks from bolt 3, depending on the total length of this bolt). The bark was peeled from each disk and the combined disks were first ground in a wood grinder to pass a 0.5-cm mesh screen for chemical analysis and then in a Wiley Mill to pass a 0.6-mm mesh screen for caloric determinations. Disks and chips were frozen to retard loss of volatiles between all stages of processing samples. Turpentine was determined by a modified procedure of Pulp Chemicals As- sociation (Kossuth and Munson 1980). An internal standard of 250 al n-tetra- decane was added to each 50-g sample of wood chips, which were digested in 0.5 N sodium hydroxide and refluxed for 90 min. The volatiles, including the internal standard, were condensed and analyzed by gas-liquid chromatography. Resin acids were determined by a modified method of Shepard (1975) employing xylene extraction and titration to determine free acid content. Analyses of variances and ScheWs test were used to test for differences among bolts. Heats of combustion were determined with an adiabatic oxygen bomb calorim- eter with automatic jacket controls, following the general procedures of Howard (1973). Two duplicate ground-wood samples, each approximately 0.5 g, were combusted. If the duplicates differed by 1%. additional samples were combusted until consistent values were obtained. Heat value of turpentine was measured for samples contained in closed capsules, which were weighed immediately before combustion. Specific gravity of the unextracted samples was obtained by volume displace- ment in water of a weighed sample of the chips used for resin acid and turpentine analysis. 400 WOOD AND FIBER SCIENCE. JULY 1984. V. 16(3) TABLE 2. Gross cnergv valur and distribution in stems oJIohlol!vpinc 18 months qncr injrction with 5% paraquat cation (wcight/wright hasisi: lot i l l  Resin acid p1ux wood (includes tur"cntine1 stem oonion Trcated unlriatcd 'rrcricd untreated Bolt I "  5,039' 4,698 5,173* 4,727 Bolt 2 3,823* 4,652 4,904* 4,666 Bolt 3 4,701 4,670 4.732 4.695 Wt. avgC 4.809* 4.663 4.875' 4.686 voiume,ric valued Rrrin acids plus wood Turpenllne Toinl Treated Untreated Dlf .  Treated Llnfrcated DiIC Treamd llnfrcated Dlf. . . .  kcal X loJ .............. 9h ......... kcal X 10' . . . .  '% . . .  kcal X 10' .............. % Bolt 1 135,062* 118.009 14 7,195* 1,275 565 142,257. 119,373 19 Bolt 2 100,298' 94,573 6 3,177' 507 627 103,475. 95,080 9 Bolt 3 304,512 299,804 2 3.477 2,787 21 307.989 302.681 2 Stem totalc 539.872' 512,476 5 13,849' 4,659 297 553,721* 517.135 7 'I D a t a  analylrd by ScheRe's ten. B o l l  I - Lrri I52 cm. Boll 1 = wcond IS2 cm ahoverxscmcmritr, and Boll 3 - rcmain~ngrncrchrntahlcrlrm ton 7.6.crn inridc. bark dinmetcr. We~phwd according to !he volume "leach bolt. d calurlmettic mearvrcmcntr timer quantity olcornoonents per halt. Llntrerlcd volume? r'ljlluslcd In Ihc same as treated-Cree volurncs. s~enilicantly dirtrent from control at 0.05 levd. Percent resin acids, turpentine, and moisture on a weight basis were obtained in the extraction processes. The quantities of resin acid and turpentine in the wood samples were obtained by using the unextracted specific gravities of 0.64. 0.63, and 0.56 for treated bolts 1, 2, and 3: and 0.69, 0.65, and 0.56 for control bolts. Bolt volume was calculated as a frustrum of a cone from measurements of height and diameter inside bark at harvest. Gross energy yield (kilocalories) per bolt was obtained by multiplying the kcal/ m' for each component by the bolt volume. Quantitative determinations of resin acids and turpentine, and caloric value for control tree yield, were adjusted to reflect the same volume as treated trees. The energy loss resulting from combustion in a commercial process was de- termined by values from Saeman (1977). Reduction of heat value due to the presence of moisture was 0.28% for every percent green weight moisture content (MC). Heat lost due to evaporation of water formed by hydrogen combustion and flue gasses was 7.67 and 8.02%. respectively. RESULTS In bolts I and 2, resin acid content showed a 392 and 298% increase over control bolts and a 564 and 626% increase in turpentine over controls (Table 1). Caloric content of extracted turpentine fractions was similar in all bolts, av- eraging 19,369 cal/g from 25 determinations. Treated tree energy values of dry wood (resin acids plus wood) obtained from bolts 1 and 2 were significantly greater (0.05 level) than those of the controls (Table 2). Bolt 3 of the treated trees also Kosrulh a aL-ENERGY VALUE OF RESIN-SOAKED LOBLOLLY PINE 40 1 TABLE 3. Net energy yield and di,stribulion on a green-weigh1 basis of whole stem components of 1ohlolt.v pine 18 months afier treatment with 5% paraquar carion (weixhhl/weight basis). Nel eneny yielda Sicm panion Treated Control" D>Rcrcnce ............................................ kcat x 10' .... % Bolt I<  104,398 86,208 I 2  Bolt 2 74,720 67,836 10 Bolt 3 217,841 214,095 2 Total 396,959 368,138 8 calorimetric measurements times quantity of romwnen~r per bull. bCnmrul volumes adjusted to he the some as lrealcd-wee volumes. 'Boll I - first 152 cm. Boll 2 - second I52 cm above treatment sire, and Bolt 3 = tho remaining mmhanlablc a c m  to a 7.6- inside-bark diameter. had higher energy values, but they were not significantly greater than those of the controls. On a whole stem basis, the gross energy value of the treated trees was 7% higher than for control trees. Net energy yield (effective heating value) ofwhole stems of treated trees was 8% greater than for control trees (Table 3). This was due to the large increases in resin and a decrease in MC in bolts 1 and 2 of the treated trees. DISCUSSION AND CONCLUSIONS The combined effect of lower MC coupled with higher resin yields (Table I) significantly increased the net energy value of treated loblolly pines, especially in bolts I and 2. Desiccation is listed on the marketing label of paraquat as one of the effects of this contact herbicide, and in this study, moisture loss approximated the increase in resin. The desiccation greatly increased the net energy of the stem wood because less energy was lost in the combustion process because of moisture in the raw material. Because paraquat is a highly toxic herbicide, some reduction in volume growth due to death of the cambium might be expected in treated trees. An earlier study (Nix 1979) showed volume growth reduction of 3 1 and 2 1% in the first and second years after loblolly pines were treated using one-half-tree circumference by 2.54- cm bark streak sprayed to runoff with 4% paraquat. This was similar to findings in slash pine (Squillace and Moyer 1976). Further studies are needed to clarify expected volume growth loss with various kinds of treatment and concentrations of the chemical so that per acre yields of wood and potential energy values can be calculated. In this study we found a 12% higher net energy value in paraquat-treated 20- year-old loblolly pines than controls in bolt 1, and somewhat lesser values in bolts 2 and 3. When optimum treatment procedures are known, growth reductions may be low enough that this high energy per unit volume in the first 3 m could be of value for fuel. For example, small wood-fueled gasifiers could utilize the first 300 cm and would then need to be refueled less often. REFERENCES BENTE, P. F., ed. 1979. Bio-energy directory. Bio-Energy Council. Washington. DC. 533 pp. HOWARD, E. T .  1973. Heat of combustion of various southern pine materials. Wood Sci. 5:194- 197. 402 WOOD AND FlBER SCIENCE. JULY 1984. V. 16(3) KOSSIJTH, S. V., AND J .  W. MIINSON. 1980. Automated terpene analysis with an internal standard. Tappi 64(3):174-175. L~GHTWOOD RESEARCH COORUlNKIING COUNCII.. 1974-1979. Sponsored by Pulp Chemicals Asso- ciation in cooperation with USDA Forest Service, Southeastern Forest Experiment Station, Ashe- ville, NC. 6 vol. MCALPINF., R. G., C. L. BROWN, A.M. HERRICK, A N D  H. E. RUARK. 1966. "Silage" sycamore. Forest Farmer 26(1):6-7, 16. NIX, L. E. 1979. The effects of paraquat treatment on height growth, branch extension, and cambial activity of loblolly pine. Pages 21-27 in  Mary H. Esser, comp./ed. Sixth Annual Lightwood Research Conference Proceedings. Pulp Chemical Association in cooperation with USDA Forest Service, Southeastern Forest Experiment Station, Asheville, NC. SAEMAN, J. F. 1977. Energy and materials from the forest biomass. Pages 153-158 in .I. W. White and W. McGrew, eds. Symposium Papers, Clean Fuels from Biomass and Wastes, January 25- 28. Institute of Gas Technology, Orlando, FL. SHEPHARD, C. 1975. Analytical procedure for determining the extractions of paraquat treated trees. Pages 78-83 in Robert N. Stone, ed. Lightwood Research Coordinating Council Proceedings, January 22-23, Jacksonville, FL. Chevron Chemical Co., Box 160. Ocoee, FL. S Q ~ J I L L A ~ E ,  . ., AND E. MOYER. 1976. Genetic and environmental variation of induced resin soaking in slash pine-Second-year results. Pages 93-101 in Mary H. Esser, comp./ed. Second Annual Lightwood Research Conference Proceedings. Pulp Chemicals Association in cooperation with USDA Forest SCN~CC, Southeastern Forest Experiment Station. Asheville, NC. SLEGO, G. C., J. A. Fox, AND D. R. EATON. 1972. The energy plantation. Interscience Energy Conversion Engineering Conference, Seventh Conference, Proc. Paper 729168. San Diego, CA. 210 pp. YOIJNG, H. E. 1972. Woody fiber farming: An ecologically sound and productive use of right-of- ways. University of Maine, School of Forest Resources. Orono, ME. 19 pp. 

Energy Value of Paraquat-Treated and Resin-Soaked Loblolly Pine

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Energy Value of Paraquat-Treated and Resin-Soaked Loblolly Pine

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