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In oration with tho Univorsite of Wisconsin

Library --Forest Research LaboratoryCollege of ForestryOregon State UniversityCorvallis, Oregon 97331

STUDIES OF THE METHODOLOGY

OF SOIL-140CE TESTING

FOREST RESEARCH CENTERLIBRARY

FOREST RESEARCH CENTERTABLE OF CONTENTS LIBRARY

Page

Toluene as a diluent for testing oil-type preservatives bythe soil-block method....

3

Effect of species of wood on preservative threshold valuesobtained in the soil-block test. 25

Effect of different soils on preservative threshold valuesin the soil-block test 41

Effect of aeration through modified bottle lids on decay inthe soil-block test 69

Representativeness of the preservative tolerance of standardisolates of Lentinus lepideus, Lenzites trabea, and Poriamonticola . • • 74

Development of a weathering phase for the soil-block test ... 84

Differences among test fungi in their tolerance of preserva-tives when appraised by the soil-block method 108

Miscellaneous data.... 122

Literature cited. 125

STUDIES OF THE METHODOLOGY OF SOIL-BLOCK TESTING

By

CATHERINE G. DUNCAN, Pathologist

Forest Products Laboratory, 1 Forest ServiceU. S. Department of Agriculture

Introduction

During the period 1950 through 1956, numerous studies were directed at thestandardization of the soil-block method as a laboratory tool for acceleratedtesting of wood preservatives. These studies were aimed at simplifying themethod, improving its reproducibility, establishing the validity of variousphases of the procedure, and developing a reasonably suitable weatheringschedule. Much of the data obtained served as a background for, "TentativeMethod of Testing Wood Preservatives by Laboratory Soil-Block Cultures, "American Society for Testing Materials Designation: D1413-56T.

It is recognized that modifications in the soil-block method as now standard-ized probably will evolve in time. In fact, an eventual laboratory methodthat differs drastically in some respects from the present one is not unlikely.Regardless of the method, however, some of the data obtained from studiesreported herein will prove helpful in its development. These data also havea broader significance and value that extend into the fields of fungus physi-ology and the behavior, effectiveness, and factors influencing common pre-servatives.

The present report is of special interest to members of the Association forStandardizing Laboratory Evaluation of Wood Preservatives. This Associa-tion was formed by about 20 producers, processors, and users of commer-cial preservative materials to cooperate with the Forest Products Laboratoryin furthering the development of accelerated laboratory methods of testingpreservatives. Much of the data presented in the report was made possible

1—Maintained at Madison, Wis. , in cooperation with the University of Wis-

consin.

Rept. No. 2114 -1-

through a substantial contribution of funds by the Association over a 4-yearperiod (July 1952 to July 1956). To make the results more widely available,all of the data eventually will be published.

In presenting the data, all tests pertaining to certain specific aspects of thesoil-block method are grouped together. Each test is described briefly asto purposes and methods, and the results and conclusions are supported. bysummarized tabular data. Some data already published or from other sourceshave been included to strengthen the evidence for accepting or rejecting cer-tain procedures as part of a standard test.

If not otherwise specified, the blocks were 3/4-inch southern pine cubes,conditioning was done in a room controlled at 70 percent relative humidityand 80° F. for 2 weeks, weathering was in the laboratory and each figurein the tables represents the average of a minimum of 4 and usually 5 repli-cates.

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TOLUENE AS A DILUENT FOR TESTING OIL-TYPE

PRESERVATIVES BY THE SOIL-BLOCK METHOD

The dilution of oil-type preservatives with toluene as a means of obtaininguniform preservative distribution over a range of retentions in test blockshas been questioned from several standpoints. The primary questions andthe tests or studies that were directed toward answering them were:

Can toluene or any other diluent be advantageously eliminated in the treat-ment of blocks with oil-type preservatives? (Studies 1 and 2).

Do the treated blocks contain a toluene residual which, because of its toxicityto fungi, affects weight loss or threshold values? (Studies 3, 4, and 5).

Is the preservative unevenly distributed (such as at the surfaces of the testblocks) or changed in type in the course of toluene evaporation (Studies 6 and7).

Each study is presented separately as to purpose, method, results, and con-clusions.

1. and 2. Comparisons of the Empty Cell With the Toluene-Dilution or Full-Cell Method of Treatment

For maximum significance the threshold, as determined by the soil-blockmethod, should be based on an essentially uniform distribution of the pre-servative in the test block. The primary purpose of tests 1 and 2 was todetermine whether the preservative at threshold retentions is as uniformlydistributed by the empty-cell method as by the toluene-dilution or full-cellmethod of treatment.

Test 1

Methods. --The 3/4-inch southern pine blocks for this test were treated witha creosote by either the toluene-dilution or the empty-cell process, by W.H. Henry of the Koppers Company. After determining absorptions the treatedblocks were wrapped in foil and allowed to stand for approximately 4 months.They were then sent to the Forest Products Laboratory for testing. Onarrival, some of the blocks were removed from the foil and placed in thedecay test without prior conditioning, while others were first conditioned for

Rept. No. 2114 -3-

3 weeks and weighed. A part of each group was tested as the original cubes;those remaining were cut in half across the grain before testing, thus expos-ing the central zone of the blocks. Lentinus lepideus (Madison 534) was usedas the test fungus for all blocks.

Results. --The absorptions obtained by the two methods of treatment and therelationship of the absorptions obtained to the basic weight of the untreatedblocks are shown, respectively, in table 1 and figure 1. The amount of mois-ture represented in the untreated weight was not known but was assumed tobe the same in all blocks for purposes of determining specific gravity of theblocks. It is evident that a considerably greater variation in retention ofcreosote was obtained by the empty-cell process than by the toluene-dilutionmethod.

The results of the decay phase are shown in table 2. These indicate thatwithout conditioning, no visible decay occurred in the blocks treated eitherby the empty-cell method or to similar retentions by the toluene-dilutionmethod. After conditioning, all blocks treated by the toluene-dilution methodwere definitely decayed, with somewhat more weight loss in those that werecut in half before testing. Consistent decay in the empty-cell-treated blocksoccurred, however, in only those that had been cut in half, exposing the in-side of the block. Decay appeared fairly uniform throughout each half of thetoluene-treated blocks treated by the toluene-dilution method but took placeonly in the inner core of the blocks treated by the empty-cell method.

Test 2

Methods. --Southern pine blocks for this test were of the same specific gravityand treated with a low residue coal-tar creosote at the Forest Products Lab-oratory. The retentions in one group of blocks were obtained by treating theblocks to refusal with different concentrations of creosote in toluene, in ac-cordance with the standard procedure in the soil-block method. The othergroup of blocks was treated by the empty-cell process in an experimentalcylinder. The latter treatments were made 60 days prior to the toluene-dilution treatments, after which the blocks were wrapped in foil and placedin air-tight jars. These blocks were finally unwrapped and placed in theconditioning room together with those just treated by the toluene-dilutionprocess.

Part of the blocks were tested after the conditioning period and the remainderafter additional exposure to laboratory weathering. One half of each of theconditioned and weathered blocks were cut in half across the grain just beforetesting. The fungus used in the decay tests was Lentinus lepideus (Madison534).

Rept. No. 2114 -4-

Results. --A summary of the retentions obtained by the empty-cell and toluene-dilution treatments is shown in table 1. The individual block retentions ob-tained by the two methods of treatment are shown in figure 2. Since initialspecific gravities of the treated blocks were the same, retentions in the re-spective charges or treating solutions were not affected by this factor. Figure2 shows that retentions were closely similar in given charges of the toluene-dilution treatments, but that retention differences as large as 2 to 3 poundsper cubic foot resulted in the two empty-cell charges.

The percentage losses of creosote during conditioning and weathering and theresults of the decay test are shown in table 3. During conditioning the lossof creosote was greater from the blocks treated by toluene-dilution than fromthose treated by the empty-cell method, except for blocks of retentions higherthan six pounds per cubic foot. After both conditioning and weathering therewas little difference in loss from blocks treated by the two methods, exceptwhen the retentions were greater than about eight pounds per cubic foot. Thegreater loss from blocks treated with more than eight pounds by the empty-cell process was not due entirely to losses during conditioning or weathering.Bleeding from these blocks was evident when they were removed from the foilwrappers, but the exact amount of such loss could not be determined by weight.

In the blocks treated by the toluene-dilution method and conditioned only, therewas decay in the 4-pound blocks but not in the blocks with higher retentions,whether they were tested as cubes or halves of cubes. In conditioned blockstreated by the empty-cell method, decay was absent in 4-pound blocks testedas cubes, but occurred in the halves of cubes treated with as much as 8 pounds.In the weathered blocks, there was decay in the cubes or the halves from cubestreated with 4 and 6 pounds by the toluene-dilution method, but not in those inthe 8-pound group. In the groups treated by the empty-cell method, decay didnot occur in blocks with retentions from about 4.5 to 8.6 pounds when they weretested whole. When the cubes were halved there was decay in all groups upto the approximate retention of eight pounds. Such decay was always presenton the inner face of the block regardless of whether it was next to or awayfrom the fungus mat.

Conclusions for Tests 1 and 2

The marked variation in block retentions despite control of specific gravity,the occurrence of bleeding, and decay of block interior when exterior remainedsound, indicated that the preservative was not uniformly distributed by theempty-cell method of treatment. Such uneven distribution would precludeany chance of obtaining the consistent retentions that are needed in blocksfor reproducible threshold determinations.

Rept. No. 2114 -5-

Differences in preservative penetration appeared to be minor or absent withtreatment by the toluene-dilution method.

Unequal distribution of preservative in the blocks was primarily responsiblefor threshold differences for the two methods of treatment.

3. Comparison of Rates of Decay Between Untreated Blocks andBlocks Treated with Toluene

The primary aim of this test was to determine, without the complication ofpreservatives, whether the rate of decay in blocks treated, with toluene aloneis affected by residual toluene.

Methods

Forty-five southern pine blocks were treated to refusal with 100 percenttoluene. Absorptions of toluene were approximately 30 pounds per cubic foot.An equal number of blocks, with comparable specific gravities, were left un-treated.

The test fungi were Lentinus lepideus (Madison 534), Lenzites trabea (Madison617), and Poria monticola (Madison 698). Five of the toluene-treated and un-treated blocks being tested against each fungus were removed at the end of 4,8, and 12 weeks of incubation. The weight losses due to decay were thendetermined.

Results and Conclusions

The average percent weight losses produced by the three fungi in the toluene-treated and untreated blocks are shown in table 4. These losses indicate thatthe rates of decay in toluene-treated and untreated test blocks were essentiallythe same for the several periods of incubation.

It was concluded that any toluene remaining in the blocks after a 2-week con-ditioning period had no significant effect on the rate of decay.

Rept. No. 2114 -6-

4. Comparison of Blocks Treated with the PreservativeDiluted in Either Toluene or Acetone

The purpose of this test was to determine whether decay losses and thresholdvalues vary when acetone and toluene are compared as diluents for oil-typepreservatives. According to the agar-flask toxicity test, toluene is toxicwhile acetone is nontoxic to decay fungi.

Methods

The oil-type preservatives tested were a coal-tar creosote and 5 percent byweight of pentachlorophenol in a petroleum. One series of retentions was ob-tained by diluting the preservatives with toluene; a second similar series wasmade by diluting the preservatives with acetone. Five blocks with similaramounts of each preservative were tested against each of the fungi, Lentinus lepideus (Madison 534), Lenzites trabea (Madison 617), and Poria monticola (Madison 698).

Results and Conclusions

Average weight losses due to decay in the treated blocks are shown in table5. These data show that there was little difference in the decay of blocks withsimilar retentions of a given preservative.

The losses of creosote or pentachlorophenol solution also were similar whethertoluene or acetone was the diluent.

There was no evidence in these tests that residual toluene in the treated blocksaffected threshold determinations. It seemed unlikely that significant residu-als of either toluene or acetone were present after the standard 2 weeks of con-ditioning. The indications also were that toluene and acetone are similar inany effect they might have on the distribution and amount of, preservative re-maining in the blocks after conditioning.

5. Comparison of Blocks Treated with the Preservative Carried inToluene Alone, Petroleums Alone, or in Petroleum

Solutions Diluted with Toluene

These tests compared threshold values when blocks were treated with penta-chlorophenol or copper naphthenate carried in toluene, straight petroleum,

Rept. No. 2114 -7

or petroleum diluted with toluene. Similar retentions of preservative wereobtained by varying concentrations of the preservative in the solutions usedto treat the blocks to refusal.

Methods

The stock preservative solutions were pentachlorophenol (5 percent by weight)and copper naphthenate (0.5 percent copper metal) carried in toluene or ineach of three petroleums (A, B, and C) used as carriers alone or diluted withtoluene. Varying percentages of the pentachlorophenol or copper were obtainedin the treating solutions by diluting each stock solution with toluene or thepetroleum carrier. The treating solutions thus prepared gave approximatelythe same retentions of either pentachlorophenol or copper metal in the blocks.Retentions of the petroleum carriers varied greatly depending upon the dilutionmethod used.

Part of the blocks were tested after a conditioning period and the remainderafter conditioning and laboratory weathering. Poria monticola (Madison 698)was used in all tests of blocks containing copper; Lenzites trabea (Madison617) was used for the blocks treated with pentachlorophenol.

Results

Losses in weight of the treated blocks during conditioning and weathering arean indication of the loss of the toluene or petroleum carriers, but cannot beused to calculate the loss of pentachlorophenol or copper naphthenate. Suchlosses indicated that practically no toluene remained when it was used aloneas a carrier. However, 5, 70, and 98 percent of carriers A, B, and C, re-spectively, remained in the blocks after conditioning. After weathering,carrier A largely had been lost, but 36 percent of carrier B, and 90 percentof carrier C remained in the blocks. The percentage loss of these petroleumcarriers appeared to be similar whether the preservative solution was dilutedwith toluene or the petroleum carrier itself.

The weight losses due to decay and the estimated threshold values for blockstreated with the different pentachlorophenol solutions are shown in table 6.Similar data for the blocks treated with the copper naphthenate solutions areshown in table 7.

The thresholds for pentachlorophenol in toluene or petroleum A, regardlessof dilution method, were similar after conditioning or weathering; those forcopper in the same carriers were indeterminate because considerable decay

Rept. No. 2114 -8-

occurred in all blocks. There was no evidence from either threshold valuesor decay losses that the use of this petroleum carrier without toluene dilutionhad depressed the rate of decay. It was indicated, by weight, that little orno toluene or petroleum A remained in the blocks at the time of the decay tests.

The respective thresholds for pentachlorophenol or copper naphthenate inpetroleum B and C carriers were higher when the preservative solutions werediluted with toluene rather than the carrier itself, even though weathering hadreduced the amount of petroleum in the blocks. Although the percentage lossof petroleum was similar in both types of dilutions, the amount of petroleumremaining in the blocks was considerably greater when the petroleum was theonly diluent. For example, a block treated with 0.5 pound of pentachlorophenolabsorbed approximately 10 pounds of petroleum B when diluted with toluene ascompared to 30 pounds when diluted with the carrier. During conditioning andweathering, approximately 64 percent of petroleum B was lost. Therefore,the blocks treated with 10 pounds contained only 3 to 4 pounds of petroleum Bwhen placed in the decay test, while those treated with 30 pounds still containedmore than 10 pounds of the petroleum.

Previous soil-block tests (9) 2— in which different preservative-petroleum solu-tions were diluted with toluene have shown that the less volatile petroleumcarriers tend to give lower threshold values for these preservatives. There-fore, lower thresholds were not unexpected when the amount of petroleum re-maining in the blocks was much greater than that resulting from toluene-dilution. Previous tests also showed that a variety of straight petroleumsmay inhibit but not prevent decay. Table 8 illustrates the effect that differ-ent amounts of petroleum B, without any preservative, had on weight lossescaused by the test fungi. These results indicate that weight losses decreaseas the amount of petroleum B increases in the blocks. Such retardation ofdecay is conceivably great enough to affect the threshold when considerablepetroleum remains.

Conclusions

The threshold of a preservative may be somewhat lower when the petroleumcarrier rather than toluene is used as the diluent in the treating solution.Such differences seem to be related, at least in part, to the volatility of thepetroleum carrier and how much of it remains in the block at the time of thedecay test.

2—Numbers in parentheses refer to Literature Cited at the end of this report.

Rept. No. 2114 -9-

Regardless of differences in threshold, the order of effectiveness of the penta-chlorophenol or copper naphthenate solutions in the present tests was thesame whether toluene or the petroleum carrier was used as the diluent for thedifferent preservative solutions.

The type of petroleum carrier apparently may influence the preservative ef-fectiveness of pentachlorophenol and copper naphthenate, and this effect doesnot seem to be obscured by the toluene-dilution method.

6. Toluene Dilution as Affecting Preservative Distributionin Blocks of Different Types

These tests were directed at determining whether there were indications ofappreciable movement of preservative from the interior to the surface ofblocks of different types in the course of toluene evaporation.

Methods

Southern pine blocks, 3/4-inch cubes and 3/4 by 3/4 by 2-1/4 (along the grain)inches, were treated to refusal with a low-residue coal-tar creosote or a 5-percent pentachlorophenol-petroleum solution, both diluted with toluene. Allblocks were of similar specific gravity. The larger blocks, which had 3 timesthe volume of the cubes absorbed 3 times more treating solution so that theretentions in pounds per cubic foot of penta-petroleum or creosote were simi-lar in both types of blocks.

All the blocks were weathered in a circulating-air oven at 140° F. , withouta leaching phase. The cubes were weathered 9 days, conditioned, weighed,and the loss of creosote or pentachlordphenol solution determined. The lar-ger blocks were weathered 19 days at which time the percent losses of pre-servative were indicated to be similar to those from the smaller blocks (seetable 9).

Some of the treated and weathered cubes were tested whole, others were cutin half across the grain before testing. The treated and weathered largerblocks were tested after being cut in half lengthwise or into thirds or sixthsacross the grain. All blocks were cut at their conditioned weight, and eachportion of the block was weighed immediately after cutting. The blocks werethen placed in the decay test without further conditioning.

The usual culture technique was used except for the larger blocks which hadNbeen cut lengthwise. The soil substrate for these was placed in bottles in

Rept. No. 2114 -10-

in the horizontal position, and a 1/4- by 1- by 2-1/2-inch feeder was used.Each bottle contained either a 3/4-inch cube or both its halves, or one 1-third, two 1-sixths, or one lengthwise half of a 3/4- by 3/4- by 2-1/4-inchblock. All the creosote blocks were tested with Lentinus lepideus (Madison534) and the pentachlorophenol-petroleum blocks with Lenzites trabea (Madi-son 617).

Results

The average percent weight losses due to decay in the creosote-treated blocksare shown in table 10 and those for the penta-petroleum blocks in table 11.

The weight losses show that the cubes tested whole or halved decayed simi-larly, indicating that the amounts of creosote or pentachlorophenol in the outerand inner parts of the block were not significantly different. However, theweight losses for the 3/4- by 3/4- by 2-1/2-inch blocks indicated that therewas less pentachlorophenol or creosote in the outer than in the inner portionsof the blocks. For example:

(a) Large blocks treated with creosote and cut into sixths showed: similardecay in the all parts of the 4-pound treatments, only one-half as much decayin the 2 center as the 2 outer sixths of 6 - pound treatments, no decay in the 2center sixths, but decay in the 4 outer sixths of 8-pound treatments, and nodecay in any parts of the blocks treated with 10 pounds.

(b) Likewise, large blocks treated with pentachlorophenol-petroleum and cutinto sixths showed: similar decay in all parts of the 2.6-pound treatments,only one-third as much decay in the 4 inner sixths as the 2 outer sixths of 4-pound treatments, no decay in the 4 inner sixths but about 7 percent weightloss in the 2 outer sixths of 6-pound treatments, and no decay in any parts ofthe blocks treated with 8 pounds.

(c) Large blocks treated with creosote or pentachlorophenol-petroleum andcut into thirds also indicated that there was less decay in the inner third thanin the outer portion of the blocks.

(d) Large blocks treated with both preservatives and cut in half lengthwise,definitely indicated that most of the weight loss due to decay had occurred inthe block ends.

The thresholds for the 3/4-inch cubes treated with both preservatives weresimilar to those for the outer thirds or sixths of the larger blocks.

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Conclusions

For blocks of two sizes and subjected to one type of weathering, there was noevidence of appreciable movement of creosote or pentachlorophenol from theinterior to the surface due to toluene evaporation. Instead, there was evidencethat the preservatives were present in lower amounts near the surface thantoward the interior of the blocks. However, differences were apparent onlyin the blocks larger than the 3/4-inch cubes.

7. Results Reported by Other Laboratories on the Use of Toluene-Dilution in Soil-Block Testing

Radioactivity Measurements by Bell Telephone Laboratories

L. R. Snoke of the Bell Telephone Laboratories reported data on radioactivitymeasurements in 3/4-inch cube blocks to determine depletion of toluene resid-uals. The data were presented at the meeting of ASTM Subcommittee XIII,"Durability and Exposure" in Chicago, March 12, 13, 1956. Eight blockswere treated to refusal with toluene 1-C 14 alone and 16 with 32 percent creo-

sote in toluene 1-C 14. Radioactivity measurements were made at intervalsafter treatments.

The results of these measurements are shown in figure 3, a reproduction ofthe graph distributed to committee members. The data indicate that at theend of 1 day no toluene remained in the blocks treated with toluene alone. Theloss of toluene from blocks treated with creosote-toluene was slower butnone remained at the end of 7 days. Since a conditioning or weathering periodof at least 2 weeks precedes the decay test in the soil-block method, tolueneresiduals that might affect weight losses due to decay and threshold valuesseemed unlikely.

Colley, R. H. The evaluation of wood preservatives.Bell Telephone System Monograph 2118 (page 90) 1953.

Blocks treated with 6 pounds of creosote were weathered outdoors for 60 daysand cut through the cross-sectional face into three equal parts. On tolueneextraction, the creosote remaining in the inner and outer thirds of the blockswas approximately the same.

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H. L. Stasse. Experiments on the distribution of creosote in wood after full-cell treatments withsolutions of creosote in acetone or toluene. Report of Committee P-6, Methods for the evaluation of wood preservatives. American Wood-Preservers'Association Proceedings 51: 121-128. 1955.

Southern pine sapwood blocks were impregnated with acetone and toluenesolutions of creosote by the full-cell process, strung on wire, and exposed

in the laboratory. At the end of 6 hours, 2 days, 7 days, and 30 days, theblocks were cut so that the outer surface layers were equal in volume to theinner core of remaining wood. The creosote was then extracted from theinner cores and outer faces. The results indicated that there was no signifi-cant difference in the amount of creosote in the outer layers and inner coreof the block, either shortly after impregnation or after 30 days conditioningat room temperature.

L. R. Snoke. Specific studies on the soil-block procedure for bioassay of wood preservatives.Bell Telephone Monograph 2577 or Applied Microbiology 4:21-31. 1956.

Blocks were treated with a creosote and weathered. Thresholds determinedon the whole block, on 1/8-inch pieces cut from the cross section; on theradial or tangential faces, or from the center of the block were essentiallythe same. The conclusions were that the total amount of the various com-ponents responsible for the effectiveness of the creosote were not distributederratically due to toluene dilution.

Rept. No. 2114 -13-

Table 1.--Summary of retentions of creosote obtained by empty-celland toluene-dilution treatments. (Tests 1 and 2)

Treatment method :Number of: Creosote : Retentions obtainedblocks :concentration:

: treated : : Range : Average

Percent : Lb. per : Lb. per: cu. ft. : cu. ft.

TEST 1

Toluene dilution : 29 15 : 3.2 - 3.8 : 3.5Do • 10 20 : 4.8 - 5.2 : 4.9

Empty-cell : 30 100 : 3.2 - 5.2 : 3.8

TEST 2

Toluene dilution : 16 13 : 3.9 - 4.1 : 4.0Do 16 : • 19 : 5.8 - 6.0 : 5.9Do 16 25 : 7.9 - 8.1 : 8.0Do 16 31 : 9.9 -10.1 : 10.0

Empty-cell: • •

Charge 1 : 40 100 : 3.8 - 6.0 : 4.6Charge 2 : 40 100 : 6.4 - 9.7 t 7.8

Table 2.--Decay in blocks treated with a creosote by the empty-cell and toluene-dilution methods (Test 1)

Toluene dilution (full-cell)

••

•• Empty-cell

Retention: Weight loss :Retention: Weight loss

:Whole blocks:Halved blocks: :Whole blocks:Halved blocks

Lb. per : Percent : Percent : Lb. per : Percent : Percent cu. ft. : : cu. ft. :

NO CONDITIONING1-

3.5 : No decay : No decay : 3.8 : No decay : No decay

4.9 • do

AFTER CONDITIONING

3.5 : 12 : 18 : 3.8 : 1 26

4.9 : 2

1Decay loss determined by visual inspection only, consequently Emailamounts of decay may not have been detected.

Decay confined to the inner cross-sectional face of block even thoughthe outer face was neat to the feeder strip. With the toluene-dilutionmethod, decay was more pronounced on face of block neat to feeder re-gardless of whether it represented inner or outer part of block.

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Table 5.--Loss of creosote durinic_conditioning and weathering and the amount of decay in empty-cell and toluene-dilution treated blocke (Test 2)

Toluene dilution (full cell) : Empty-cell

Retention:Loss of : Weight loss 1- :Retention:Loss of : Weight loss 1-(approx. :creosote: :(approx. :creosote:

k 0.2) : : Whole :Halved : ± 0.2) : : Whole :Halved

Lb. per :Percent :Percent:Percent: Lb. per :Percent :Percent:Percent

cu. ft. : . . : cu. ft. :

CONDITIONED ONLY

4.0 : 36 : 5.8 : 5.2 : 3.8 : 20 : (0.6) : 5.06.0 : 36 : (1.4) : (1.2) : 4.3 : 25 : ( .5) : 4.o8.o : 37 : ( .7) : ( .6) : 4.8 : ,25 : ( .4) : 3.7

10.0 : 32 : (1.6) : (1.7) : 6.9 : 38 : ( .6) : (1.o)

CONDITIONED AND WEATHERED

4.o : 51 : 9.9 : 7.8 : 4.2 : 48 : 1.o : 9.o• • 5.4 : 5o : (o) : 4.o

6.o : 52 : 5.2 : 5.7 : 6.o • 4.3

7.o : 53 : (0.2) : 3.3• • • 7.5 • 1.6

8.o : 52 : (1.0) : (1.3) 8.0 : 59 : ( .2) : ( .9)• 8.6 : 6o : ( .7) : (1.0)

10.0 51 : ( .7) : (1.4) • •

1-Weight losses in parentheses attributed to factors other than decay.

-Bleeding losses also involved.

Table 4.--Weight losses due to decay in untreated and toluene-treated blocks subjected to similar testing methodsi

. . :Test fungus : Duration : Blocks not : Blocks treated with

: of test : treated : toluene-

: Weeks : Percent : Percent • .

Lentinus lekideus : 4 •. 118 32

12 42

93344

Lenzites trabea

Feria monticola

4 128 34

12 52

12335o

4 20 188 42 40

12 56 54

•Each weight loss is an average for 5 blocks.

2Retentions approximately 30 pounds per cubic foot. At the time oftesting (2 weeks after treatment) conditioned weights indicatedthat all the toluene had been lost.

Rept. No. 2114 -1 5 -

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Rept . No. 2114 - 18-

Table 8.--Losses in blocks treated with different amounts of petroleumB without preservative, subjected to decay by 3 fungi

Petroleum B:Retention (approximate)in toluene : indicated fungus

At : At time of : -

: treatment : decay test : Lentinus : Lenzites : Poria: lepideus : trabea : monticola

Percent : Lb. per : Lb. per : Percent : Percent : Percent

cu. ft. : Cu. ft.

BLOCKS NOT WEATHERED

to o : o : 4o : 42 465 2 1+ : 34 32 45

15 : 5 3 : 29 : 27 263o : 10 7 : 26 16 206o : 20 : 14 : 24 : 10 16

100 35 : 24 : 19 8 5

BLOCKS WEATHERED

0 0 0 43 51 •. 525 : 2 : 1- : 44 49 5315 : 5 : 2 39 37 •. 49

30 : 10 : 4 32 : 31 •. 326o : 20 : 7 : 29 20 •. 17

100 : 35 13 : 24 15 15

1-Untreated control.

Table 9.--Loss of creosote or pentachlorophenol-petroleum solution (as indicated by weight) from blacks of two sizes treated bytoluene-dilution method

•Preservative1- :Retention: Block size

3/4 by 3/4 : 3/4 by 3/‘4by 3/4 in. . by 2-1 in.

: (Weathered 9 days) : (Weathered 19 days)

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: 6.o 49 49

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10.0 45 43

Weight loss caused by

-Creosote was a low residue type and petroleum a high boiling type.

Rept. No. 2114 -19-

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Rept. No. 2114 21 -

EFFECT OF SPECIES OF WOOD ON PRESERVATIVE THRESHOLD

VALUES OBTAINED IN THE SOIL-BLOCK TEST

This study was conducted to determine whether species of wood influencesthe threshold values of preservatives sufficiently to warrant strict limitationof species for standard testing.

Methods

The testing was performed in two parts and at different times. In part 1, acomparison was made of thresholds obtained with sapwood blocks of a soft-wood and a hardwood, namely, southern pine and sweetgum (Liquidambar styraciflua). In part 2, comparisons were made of the thresholds obtainedwith sapwood of three different pines: ponderosa (Pinus ponderosa), red (P.resinosa), and southern. The southern pine used in parts 1 and 2 was un-selected for species and might have included any or all of four species: short-leaf (P. echinata), longleaf (P. palustris), loblolly (P. taeda), or slash (P.elliottii).

The test blocks in all cases were 3/4-inch cubes. Those of sweetgum andponderosa pine were cut from single boards and those of red pine from nar-row strips of board supplied by H. P. Sedziak. The southern pine blockswere selected from a large stock in general use.

The initial values of specific gravity for the southern pine and sweetgumblocks used in part 1 of the testing were similar, as indicated by the condi-tioned weights, which were 3.9 to 4.1 grams for the pine and 3.8 to 4.2 gramsfor the sweetgum. In part 2, conditioned block weights were 3.0 to 3.3, 3.2to 3.5, and 3.7 grams, respectively, for the ponderosa pine, the red pine,and southern pine.

The test blocks were treated with four different preservatives: (1) low-residuecoal-tar creosote; (2) pentachlorophenol, 5 percent by weight, in petroleum;(3) copper naphthenate, 0.5 percent copper by weight in petroleum; and (4)copperized chromated zinc chloride. Treatments were made with 6 or 9 con-centrations of each of the 3 oil-type preservatives in toluene and of the saltmixture in distilled water. Blocks of the different woods to be compared forthreshold retentions obtained with them were treated together in the samecharge of preservative solution.

Rept. No. 2114 -25-

In both parts 1 and 2, representative blocks were placed in test after 3 weeksof conditioning in air at 80° F. and 70 percent relative humidity. In part 2,

a portion of the blocks also was subjected to simulated weathering in the lab-oratory prior to testing. Blocks of each kind of wood treated with a given con-centration of preservative, as well as untreated blocks, were exposed in quad-ruplicate to the test fungus.

The fungi used to test the various preservatives were: Lentinus lepideus (Madison 534), Lenzites trabea (Madison 617), Poria monticola (Madison698) and Polyporus versicolor (Madison 697).

The first three are brown-rot fungi of considerable importance in the decayof both hardwoods and softwoods, while the fourth, Poly. versicolor, is awhite-rot fungus that attacks mainly hardwoods. Poly. versicolor was omittedfrom part 2, since hardwood test blocks were not used.

The culture bottles for the tests were made up as previously described exceptthat gum-feeder strips were used for testing the gum blocks.

Results and Discussion

Threshold Differences Between Sweetgumand Southern Pine

Average weight losses in the southern pine and sweetgum blocks treated withthe different preservatives are shown in tables 12 to 15. The indicated thresh-old retentions or retention zones in which the thresholds were indicated to be,.are given in table 16.

The data indicate that the threshold retentions for the three brown-rot fungi,Lentinus lepideus, Lenzites trabea, and Poria monticola, were materiallygreater in the pine than in the sweetgum blocks when the preservative wascreosote. The reverse situation occurred, however, for at least two of thebrown-rot fungi when the preservative was copper naphthenate. With penta-chlorophenol and copperized chromated zinc chloride, thresholds for thebrown-rot fungi were for the most part essentially the same in the two kindsof woods.

The data also indicate that the threshold retentions for the white-rot fungus,Poly. versicolor, were considerably higher in the sweetgum than in the pineblocks treated with any of the four preservatives. The untreated sweetgumsapwood was much more susceptible to Poly. versicolor than pine sapwood,a fact that presumably accounts in some measure for these differences.

Rept. No. 2114 -26-

The differences in threshold brought about by changing from southern pine tosweetgum test blocks were accompanied by a change in the relative levels oftolerance of a particular fungus to the four preservatives. However, therewas no indication that these changes in relative tolerance had reversed theorder of thresholds. This is fortunate because if the white-rot fungus Poly. versicolor, is used, its tolerance for preservatives is more effectively deter-mined in sweetgum, which offers considerably less natural resistance to at-tack by this fungus than southern pine.

The variation between thresholds obtained with southern pine and sweetgumcannot be explained by any known differences in the physical characteristicsof the blocks, since the higher thresholds were not obtained consistently oneither wood. By the same token, differences in the initial absorptions of thetwo woods seemingly do not account for the variation, although they may beconnected in some way.

Although the differences in initial absorption offer no ready explanation forthe observed threshold differences, they are of some further interest. Sincethe southern pine and sweetgum were of similar specific gravity, it might beexpected that absorptions would be similar when treatments were made to re-fusal. As shown in table 17, however, absorptions of all oil-type preserva-tives were lower in the sweetgum than in the pine blocks. Absorptions weresimilar when the two woods were treated with the lower concentrations ofcopperized chromated zinc chloride, but were slightly greater in sweetgumthan in pine with the two higher concentrations. The differences in absorp-tion between the two woods apparently cannot be practically eliminated. Theabsorptions of the oil-type preservatives were near the maximum obtainablein the pine blocks, but the same amounts could not be obtained in sweetgumeven by greatly intensifying the treating procedure. For example, absorp-tion of the oils in the sweetgum did not increase materially when the blockswere allowed to stand in the treating solution for as long as 24 hours, norwhen pressure was applied.

Absorptions of the oil solutions were not only smaller, but more variable inthe sweetgum than in the pine. Thus, individual absorptions in the pine devi-ated less than 0.1 gram from the average shown in table 17, but those of thegum deviated as much as 0.5 gram. (Gum blocks which differed more or lessthan 0.1 gram from the averaged absorptions shown in table 17 were not usedin the decay test. )

Threshold Differences Among Pines

The average weight losses in sapwood of ponderosa, red, and southern pinetreated with the different preservatives are shown in tables 18 to 21. Thesummary of indicated threshold values is shown in table 22.

Rept. No. 2114 -27-

The principal general indications of the data are that (1) the threshold forcreosote as tested by Lentinus lepideus was higher in ponderosa pine blocksthan in blocks of the other two pines, and (2) the thresholds for the otherthree preservatives tested against Lenzites trabea or Poria monticola wereeither a little higher in the ponderosa pine blocks or differed comparativelylittle among the three pine species.

Weathering in all cases resulted in higher threshold values. Also, weather-ing increased somewhat the difference between the creosote thresholds inblocks of ponderosa and the other two pines. The possibility existed thatpreservative losses during conditioning and weathering that preceded the de-cay test differed among the several pines. Such a result would affect reportedthresholds, because they are based on initial retention at treatment and not onthe amount of preservative in the block when tested. Since the chief differ-ences in thresholds were obtained in the several pines treated with creosote,the losses of creosote by weight between the time of treating and testing wereexamined. These losses, shown in table 23, indicate that the losses fromponderosa and southern pine were similar but slightly lower than those fromred pine. Therefore, the losses of creosote from the different pines seem-ingly were not correlated with the differences in thresholds.

Conclusions

The tests indicated that thresholds for a given fungus are not always the samein different woods. Differences in this respect varied with the combinationsof preservative and test fungus. They occurred even among the different pines,but were most marked between southern pine and sweetgum. These resultsprobably are representative of what might be expected with other combinationsof preservative, test fungus, and wood. The present differences were greatenough in some cases, even among the pines, to warrant limitation or identifi-cation of the sapwood used in soil-block tests. The differences in thresholdsfor the same preservative were more marked and consistent with the white-rot fungus, Polyporus versicolor, than with the brown-rot test fungi; there-fore further consideration should be given to the choice of test fungi if hard-wood blocks are to be used.

Rept. No. 2114 -28-

Table 12.--Results of testing creosote-- in southern yellow pine and sweetgum sapwood conditioned blocks subjected to decayby brown-rot and white-rot fungi

Preservative Weight loss in test blockssubjected to indicated fungus-Con

centration:Retention: in toluene : : Lentinus : Lenzites : Poria : Polyporus

: lepideus : trabea : monticola : versicolor

Percent : Lb. per : Percent : Percent : Percent : Percent cu. ft. :

SOUTHERN YELLOW PINE

o 0 40.0 : 54.o : 54.o : 26.02 0.7 40.4 : 20.4 : 40.0 : (0.4)4 1.3 23.5 : 13.3 : 3.7 : (0.4)6 2.0 15.9 : 6.2 : (0.4) : (0.4)9 3.0 7.6 : (1.1) : (0.6) (0.7)

14 4.8 (1.4) : (1.4) : (1.4) (0.9)19 6.5 (1.6) : (1.7) : (1.8) (1.5)

SWEETGUM

0 0 •. 41.0 64.o : 58.0 : 59.02 o.6 30.6 30.1 55.3 : 51.34 1.1 : 17.0 : (0.6) (0.6) : 17.56 : 1.7 : 5.3 : (0.5) : (0..3) 8.99 : 2.6 : (0.8) : (0.9) : (0.7) (0.5)

14 : 4.1 (1.5) : (1.5) : (1.5) (1.6)19 : 5.5 : (2.o) : (1.7) : (1.8) (1.7)

• •

2Low residue coal-tar creosote.2-Each weight loss is an average result for 4 test blocks. Weight

losses in parentheses are attributed to factors other than decay.

Rept. No. 2114 -29-

Table 13.--Results of testing pentachlorophenol1- using southern yellow

pine and sweetgum sapwood conditioned blocks subjected to decay by brown-rot and white-rot fungi

Preservative Weight loss in test blocks 2subjected to indicated fungus-

Concentration:Retention: in toluene : : Lentinus : Lenzites : Poria : Polyporus

: lepideus : trabea : monticola versicolor

Percent : Lb. per : Percent : Percent : Percent : Percent cu. ft. :

SOUTHERN YELLOW PINE

0247

111520

0247

111520

:::::

00.71.32.23.54.86.4

00.61.12.03.14.15.6

: 40.0 :11.2 :(0.7) :(1.1) :(1.9)(2.6)(3.3)

SWEETGUM

41.012.6 :(0.6)(1.0)(1.4) :(2.4) :(2.6) :

54.022.920.29.1(2.2)(2.5)(3.4)

64.o53.548.224.07.5(2.3)(2.6)

::::::

:::::::

54.056.211.5(1.1)(2.1)(2.6)(3.3)

58.o64.o62.1(1.2)(1.6)(2.4)(2.5)

26.010.6(0.4)(1.1)(1.8)(2.4)(3.4)

59.056.o48.940.121.813.77.9

1Pentachlorophenol 5 percent by weight in petroleum 8278.

Each weight loss is an average result for 4 test blocks. Weightlosses in parentheses are attributed to factors other than decay.

Rept. No. 2114 -30-

Table 14.--Results of testing copper naphthenate using southern yellowpine and aweetgum conditioned blocks subjected to decay bybrown-rot and white-rot fungi

Preservative Weight loss in test blocks 2subjected to indicated fungus-

Concentration:Retention: in toluene : : Lentinus : Lenzites : Poria Polyporus

: lepideus : trabea monticola : versicolor

Percent : Lb. per : Percent : Percent : Percent : Percentcu. ft.

SOUTHERN YELLOW PINE

0 0 : 40.0 : 54.o : 54.o : 26.o3 : 0.9 : 36.3 : 49.9 : 55.o : 5.47 : 2.2 27.9 : 31.4 : 50.8 : (1.5)

13 : 4.1 : 21.3 : 25.8 : 38.8 : (2.2)19 : 6.o : 14.2 : 15.9 : 33.7 : (3.3)25 : 7.7 : 7.9 : 11.0 : 28.3 : (4.3)32 : 10.0 : (5.1) : (5.2) : 24.2 : (5.2)

SWEETGUM

o : o : 41.o : 64.o 58.o : 59.o3 : 0.8 : 39.9 : 60.0 . 62.7 : 50.27 : 1.9 : 35.o : 56.6 : 61.5 : 35.3

13 : 3.5 : 28.2 : 49.8 : 57.6 : 22.119 : 5.o : 25.4 : 38.o : 54.o : 14.925 : 6.6 : 17.2 : 31.0 : 19.0 : 5.432 8.4 : 10.2 : 20.0 : 10.3 : (4.8)

-Copper naphthenate in petroleum 8278 (0.5 percent copper).2Each weight loss is an average result for 4 test blocks. Weight

losses in parentheses are attributed to factors other than decay.

Rept. No. 2114 -31-

Table 15.--Results of testing CCZC 1- using southern yellow_pine andsweetgum conditioned blocks exposed to decay by brown-rot and white-rot fungi

Preservative Weight loss in test blocks 2subjected to indicated fungus-

Concentration:Retention:

in distilled: : Lentinus : Lenzites : Poria : Polyporus water . : lepideus : trabea : monticola : versicolor

Percent : Lb. per : Percent : Percent : Percent : Percent cu. ft. : :

SOUTHERN YELLOW PINE

o : o 40.0 : 54.o : 54.o 26.00.1 0.04 29.8 : 41.3 : 56.6 8.4

.3 .13 13.1 17.1 : 56.1 (0.5)

.5 .21 4.5 : 6.3 : 46.2 (1.0)

.8 : .34 (1.1) : (1.0) : 30.0 (1.0)1.2 : .46 (1.6) : (1.7) : 2.0 (1.6)1.8 : .75 (2.1) : (2.0) : (2.1) (2.2)

SWEETGUM

o 0 41.o : 64.o 58.o : 59.o0.1 : 0.04 35.2 : 54.5 61.6 38.2

.3 .13 18.o : 39.9 59.o : 3.1

.5 .21 5.2 : 19.0 56.6 : (1.2)

.8 .34 (1.0) : 2.2 9.6 (1.1)1.2 : .52 (1.6) : (1.6) : 2.1 : (1.5)1.8 : .8o (2.1) : (1.9) : (2.2) (2.1)

•

1-Copperized chromated zinc chloride.

?Each weight loss is an average result for 4 test blocks. Weightlosses in parentheses are attributed to factors other than decay.

Rept. No. 2114 -32-

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Rept . No. 2114 —33—

Table 17.--Relationship of absorption to weight- of untreated, conditioned southernyellow pine and sweetgum sapwood blocks

Preservative :Concentra-:Southern yellow pine sapwood: Sweetgum sapwood: tion of :preserva- :Weight: Absorption :Weight: Absorption: tive in : of : : of :

toluene :blocks:Treating:Preservative:blocks:Treating:Preservative:solution: :solution:

: Percent : Gm. Gm. : Lb. per : Gm. : Gm. : Lb. percu. ft. : cu. ft.

•

Creosote low- 2 : 3.9 : 3.66 : 0.66 3.8 : 3.13 o.56residue coal- 4 : 3.9 : 3.70 : 1.34 : 3.8 : 3.11 1.12tar 6 : 3.9 : 3.70 : 2.00 : 3.8 : 3.14 : 1.70

9 : 3.9 : 3.7o : 3.01 : 3.8 : 3.17 : 2.5814 : 3.9 : 3.79 : 4.79 : 3.9 : 3.23 : 4.0819 : 4.o : 3.8o : 6.52 : 3.9 : 3.23 : 5.54

• • •

Pentachloro- 2 : 4.0 3.59 .65 : 3.9 : 3.06 : .55phenol, 5 4 : 4.o : 3.54 1.28 : 3.9 : 3.08 : 1.11percent by 7 : 4.0 3.52 2.22 : 3.9 : 3.08 1.97weight in 11 : 4.0 : 3.55 3.53 : 3.9 : 3.10 3.08petroleum 15 : 4.0 3.53 : 4.78 : 3.9 : 3.06 4.14

20 : 4.0 : 3.54 : 6.39 : 3.9 : 3.10 : 5.6o•

Copper naphth-: 3 : 4.1 : 3.46 •94 : 4.1 : 2. 97 : .81enate in • 7 : 4.1 : 3.50 2.21 : 4.1 : 3.00 : 1.90petroleum (0.5: 13 : 4.1 : 3.50 4.11 : 4.2 : 2.94 : 3.45percent copper 19 : 4.1 : 3.47 5.95 : 4.2 : 2.94 : 5.04

25 : 4.1 : 3.42 : 7.72 4.2 : 2.93 : 6.6232 : 4.1 : 3.46 : 10.00 4.2 : 2.92 8.44

Copperized 0.1 : 4.1 : 4.65 .042 4.o : 4.68 .042chromated zinc: .3 : 4.1 : 4.67 : .127 4.o : 4.66 .126chloride .5 : 4.1 : 4.63 : .209 : 4.0 : 4.70 .212

.8 : 4.1 : 4.68 : .338 : 4.o : 4.78 .3451.2 : 4.1 : 4.61 .463 : 4.o : 4.8o .52o1.8 : 4.1 : 4.63 : .753 : 4.o : 4.90 .796

2Weight in this case is a measure of relative specific gravity as the blocks wereof virtually the same size and moisture co

2-Each value is the average absorption for 20

ntent.

test blocks.

Rept. No. 2114 -34-

Table 18.--Weight losses in sapwood test blocks of different pine species treated with creosote- and exposed to Lentinus lepideus

Preservative : Weight loss2- in test blocks of the in-

, dicated type of pine sapwoodConcentration: Retentions : in toluene : : Ponderosa : Red :Southern yellow

Percent : Lb. per : Percent : Percent : Percent cu. ft. :

BLOCKS CONDITIONED

o o : 52.o 53.9 : 40.55 : 1.6 - 1.8 : 20.4 21.3 : 13.o8 : 2.7 - 2.9 : 19.o 12.9 : 8.6

11 : 3.8 - 4.1 : 13.5 6.1 : 4.314 : 4.7 - 5.2 : 7.1 (1.9) : (1.8)17 : 5.9 - 6.4 : (2.2) (2.3) (2.2)20 : 7.0 - 7.5 • (3.3) (3.2) (2.9)

BLOCKS WEATHERED

0 0 : 56.4 56.o 43.911 : 3.7 - 4.0 : 20.4 : 19.0 12.114 4.8 - 5.1 : 18.4 17.0 7.817 5.9 - 6.3 : 15.1 •. 10.8 7.220 7.o - 7.4 : 13.9 9.1 3.123 8.o - 8.6 : 11.5 4.6 (1.5)26 : 9.o - 9.8 : 7.8 (2.3) (1.8)29 : 10.4 -11.1 : 4.7 : (2.3) (2.0)

2Lower figure represents approximate retention in southern yellow

pine; the higher that in red pine. Retention in ponderosa pinewas between that in southern yellow and red pine.

1-Low residue coal-tar creosote.

Each weight loss is the average result for 4 blocks. Weightlosses in parentheses are attributed to factors other than decay.

Rept. No. 2114 -35-

Table 19.--Weight losses in sapwood test blocks of different pine species treated with pentachlorophenoll and exposed

to Lenzites trabea

Preservative : Weight loss2- in test blocks of the in-

x dicated type of pine sapwoodConcentration: Retention : in toluene : : Ponderosa : Red :Southern yellow

: : : •Percent : Lb. per : Percent : Percent Percent

: cu. ft.

BLOCKS CONDITIONED

0 0 : 57.9 • 60.5 : 54.64 1.3 - 1.4 : 49.6 . 36.2 •. 23.4

7 : 2.3 - 2.5 : 9.6 8.4 : 8.olo 3.4 - 3.6 : 4.o : (2.2) : (1.8)13 : 4.5 - 4.7 : (2.o) • (3.0) - (2.2)

16 : 5.5 - 5.7 : (2.4) (3.0) (2.4)19 : 6.6 - 6.9 : (2.8) •• (3.5) : (2.9)

BLOCKS WEATHERED

0 0 : 68.3 64.5 61.410 3.4 - 3.6 : 10.1 9.2 5.613 4.5 - 4.7 : 3.9 2.9 1.616 5.5 - 5.7 : (2.o) (1.7) (1.o)19 6.6 - 6.9 : (2.o) (1.4) (1.2)22 7.5 - 8.1 : (1.7) (1.5) (1.3)26 8.8 - 9.6 : (2.2) (2.o) (1.5)3o 9.8 -11.o : (2.4) (2.1) (1.6)

1-Pentachlorophenol 5 percent by weight in petroleum 7936.

Each weight loss is an average result for 4 blocks. Weight lossesin parentheses are attributed to factors other than decay.

2Lower value represents approximate retention in southern yellowpine; the higher that in red pine. The retention in ponderosapine was between that in southern yellow and red pine.

Rept. No. 2114 -36-

Table 20.--Weight losses in sapwood of different pine species treated with copper naphthenatel and exposed to Poriamonticola

Preservative : Weight loss? in test blocks of theindicated type of pine sapwood

Concentration: Retention3- : in toluene : : Ponderosa : Red :Southern yellow

Percent Lb. per : Percent : Percent : Percentcu. ft. :

BLOCKS CONDITIONED

0 0 : 57.1 •. 59.7 49.64 1.3 - 1.4 : 60.1 -. 59.1 45.37 2.3 - 2.5 : 41.2 •. 50.2 31.1

10 3.4 - 3.6 : 6.8 7.3 2.513 4.4 - 4.6 : (2.8) (2.7) . (2.1)16 5.2 - 5.8 : (2.8) (2.8) (1.7)19 6.3 - 6.9 : (3.2) (2.9) : (1.9)

BLOCKS WEATHERED

0 0 : 57.4 56.9 : 53.9lo : 3.4 - 3.6 : 58.5 56.2 •. 45.313 : 4.4 - 4.6 : 57.7 55.o : 43.716 . 5.2 - 5.8 : 51.7 33.8 33.019 : 6.3 - 6.9 : 27.4 : 16.4 • 16.522 : 7.3 - 7.9 : 15.4 : 8.2 : 10.426 : 8.3 - 9.4 : 4.1 : (1.6) : 2.93o : 10.1 -10.8 : (1.9) (1.5) (1.4)

Copper naphthenate in petroleum (0.5 percent copper) 7936.2-Each weight loss is an average of 4 blocks. Weight losses in

parentheses are attributed to factors other than decay.

-Lower value represents approximate retention in southern yellowpine; the higher that in red pine. Retention in ponderosapine was between that in southern yellow and red pine.

Rept. No. 2114 -37-

Table 21.--Weight losses in sapwood of different pine species treated with connerized chramated zinc chloride and exposed to Poria monticola

Preservative : Weight losa1- in test blocks of the

0 • indicated type of pine sapwoodConcentration: Retention :--

in water : : Ponderosa : Red :Southern yellow

Percent : Lb. per : Percent : Percent : Percent cu. ft. : .

BLOCKS CONDITIONED3-

o o : 35.5 36.9 28.50.2 :0.086 - .093: 22.8 19.3 15.3.6 : .27 - .29 : 3.8 3.3 2.9

1.2 : .52 - .58 : (1.4) : (1.2) (1.0)2.0 : .87 - .97 • (2.3) • ( 1 .9) (1.7)3.0 :1.3 -1.5 : (3.6) : (3.1) (2.6)4.o :1.8 -2.0 : (4.7) : (4.1) (3.4)

BLOCKS WEATHERED

o o •. 57.4 : 56.9 53.91.2 : .52 - .58 : 52.1 53.4 40.82.0 : .87 - .97 : 38.6 : 30.9 24.83.0 :1.3 -1.5 : (0.7) : (0.1) (0.3)4.o :1.8 -2.0 : (1.0) : (0.7) (0.6)5.0 :2.3 -2.5 : (1.0) : (1.2.) (1.2)6.0 :2.7 -3.0 : (1.3) : (1.8) (1.2)7.0 :3.2 -3.6 : (2.2) : (2.5) (2.4)

1-Each weight loss is the average of 4 blocks. Weight losses in

parentheses are attributed to factors other than decay.2Lower value represents approximate retention in southern yellow

pine; the higher that in red pine. Retention in ponderosapine was between that in southern yellow and red.

Weight losses after only 4-week decay test.

Rept. No. 2114 -38-

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Table 25.--Losses of creosote from the ponderosa, red, and southernyellow pine blocks during conditioning and weathering

of creosote : pine species species-in toluene :

:Southern:Ponderosa: Red :Southern:Ponderosa: Red: yellow : • : yellow :

Percent :Lb. per ::

Lb. per : Lb. per :Percent : Percent : Percent:cu. ft. cu. ft. : cu. ft. :

DURING CONDITIONING

5 1.6 : 1.7 : 1.8 : 48 48 : 548 2.7 : 2.8 : 2.9 : 46 46 : 51

11 3.8 : 3.8 : 4.1 : 44 44 : 4914 4.7 : 5.o : 5.2 . 42 42 : 4517 5.9 • 6.1 • 6.4 : 40 • 39 : 4220 7.o 7.3 : 7.5 : 39 37 : 4o

DURING WEATHERING

11 3.7 3.8 : 4.o 56 : 57 6o14 4.8 5.o : 5.1 55 : 55 : 5917 5.9 6.1 6.3 54 : 55 : 5820 7.o : 7.3 7.4 54 53 : 5823 8.o : 8.4 8.6 53 52 : 5626 : 9.o : 9.5 9.8 52 52 : 5629 : 10.4 : 10.7 11.1 51 52 55

1-Each loss figure is the average result for 12 blocks.

Concentration: Retention in indicated : Loss in indicated pine

Rept. No. 2114 -40-

EFFECT OF DIFFERENT SOILS ON PRESERVATIVE THRESHOLD

VALUES IN THE SOIL-BLOCK TEST

General

The preservative threshold obtained in the soil-block test has been found tobe a reproducible value so long as the soil and other conditions are keptessentially the same. Since it would be impracticable for different labora-tories to use the same soil, a series of tests were made to determine whatvariation in soil character and constituency might be tolerated without seri-ously affecting the threshold. Factors particularly considered were texture,organic content, pH, specific gravity, moisture holding capacity, and mois-ture content.

Moisture content was stressed in these tests because it was considered to bethe only constituent that could be altered without changing the natural char-acter of the soil. The primary aim in testing soil moisture was to find anamount, measured in terms of some constant volume or proportion of soilweight or moisture-holding capacity, that would permit maximum latitude inchoice of soils.

Test Series I

The purpose of the first series of tests (Series I) was to determine the varia-tion in decay and in preservative threshold values when using soils of differ-ent texture but with the same volume of water added to each test bottle ofsoil. A wide range of textures was provided by soils that were chosen es-pecially for differences in proportion of sand and organic content.

Method

Four soils classified by their texture as silt loam, sandy loam, loamy sand,and sand were used. A partial analysis of the soils (table 24) showed thatthe loamy sand and sandy loam contained, respectively, only 1/4 and 1/2 asmuch organic matter as the silt loam. The sand, which was washed and ig-nited, contained no organic matter.

The test bottles were about half filled (4-ounce volume) with a uniform volumeof the air-dry soils, after first putting 40 cubic centimeters of distilled water

Rept. No. 2114 -41-

in each bottle. This amount of water saturated the sand. Based on the oven-dry weights of the soils, the percentage of moisture varied from 21 percentin the sand to 40 percent in the silt loam (table 24).

Two southern pine sapwood feeder strips were placed on the surface of thesoil, and the loosely capped bottles were sterilized. Sterilization causedan increase in the volume of the sand, thereby creating air spaces whichwere not filled with water.

The test blocks were 3/4-inch cubes of southern yellow pine sapwood with a1/8-inch hole drilled through the center of a tangential face. The blocks weretreated to refusal with five concentrations (toluene used as diluent) of fourpreservatives containing creosote or pentachlorophenol:-3

(a) Coal-tar creosote (M)(b) Coal-tar creosote (X)(c) Pentachlorophenol, 5 percent by weight, in petroleum (Y)(d) Pentachlorophenol, 5.48 percent by weight, in petroleum (Z)

Before testing, all blocks were weathered outdoors for 60 days.

Lentinus lepedius (Madison 534) was used in tests with the creosote-treatedblocks and Lenzites trabea (Madison 617) with the pentachlorophenol-treatedblocks.

Five replicate blocks treated with each concentration of preservative, aswell as four untreated blocks, were tested on each soil type. Three culturebottles, containing either one or two blocks, were used for each group offour untreated or five treated blocks.

In addition to the blocks subjected to fungus attack, duplicate blocks fromeach treatment group, including untreated controls, were placed in uninocu-lated test bottles.

Results

Threshold differences in the different soils. --The weight losses occurringin the test blocks when using the four soils and two fungi are shown in tables25 and 26. These indicate that the preservative threshold was considerably

3Treatment and weathering of blocks containing the "X" creosote and the 5.48percent pentachlorophenol in petroleum "Z" were done at the Bell Tele-phone Laboratories. The specific gravity of these blocks was lower thanthat of blocks treated with the other two preservatives.

Rept. No. 2114 -42-

higher in three of the four test groups than when using loamy sand. A num-

ber of differential factors associated with the several soils were examinedfor a possible explanation of these threshold differences.

Behavior of the test fungi in the soils and feeder strips. --The growth of thetest fungi into the soils and feeder strips was considered. Three weeks afterinoculating the soil, the mycelium of both fungi had completely covered thefeeder strips and had penetrated to at least one-half the depth of the soil sub-strate. On sand the penetration was not as deep and growth was less abundant

than on the other soils. In the sand cultures, few or no abortive fruitingstructures were formed, while such structures developed on the other soilsbefore the end of the test period.

An abundance of rounded, slightly brown protuberances were formed byLentinus lepideus on the sandy loam and loamy sand; these were distinctivebut were not correlated with a higher or lower threshold.

The feeder strips were more heavily covered when using sand but were lessdecayed by the end of the test period than when using the other soils. Decayof feeder strips was rated as 70 percent or more on the silt loam, about 60percent on sandy loam, 40 percent on loamy sand, and 20 percent on sand.With sand the decay was confined almost entirely to the springwood part ofthe strips.

While the amount of decay in the feeder strips was directly correlated withthe organic content of the soils, it was inversely correlated with the amountof water absorbed from the soil. In uninoculated bottles, for example, thefeeder strips on the different soils contained the following average percent-ages of moisture: on silt loam -- 30, on sandy loam -- 38, on loamy sand-- 56, and on sand -- 134.

Thus, it appeared that high threshold values were associated with low organiccontent and moisture-holding capacity of the soil and with small amounts ofdecay in the feeder strips. Also, the percentage of moisture in the feederstrips was large when the thresholds were high. This suggested that varia-tions in wood moisture resulting from differences in soil texture were mostdirectly responsible for the observed differences in the preservative thresh-

olds. Attention was next directed, therefore, to the moisture content of thetest blocks themselves.

Rept. No. 2114 -43-

Moisture Conditions in the Test Blocks

The percentage of moisture in blocks subjected to decay by Lent. lepideusand L. trabea and in blocks placed in uninoculated bottles is shown in tables27 and 28. The percentages indicate that the moisture content of undecayedblocks over the silt and sandy loam y tended to be near the fiber saturationvalue (about 28 percent for pine). Over loamy sand, block moisture wasonly slightly above fiber saturation. Over sand, the amount of moistureusually was several points above the fiber saturation value and also showedthe greatest variation among the blocks of any group.

The greater moisture content of the blocks over sand, especially since itwas just above the critical fiber saturation level, presumably was responsiblein some way for the higher threshold value for blocks tested over sand.

A peculiarity of near-threshold decay obtained over sand was that the fungusattack seemed to be strictly limited to the surface of the blocks. Visual ob-servations indicated that such attack was confined entirely to the tangentialand radial block surfaces, which were not in contact with the feeder strip.Microscopical sections confirmed that the fungus had not penetrated thecross-sectional face next to the feeder strip as it customarily has done inprevious soil-block tests. This abnormal situation raises a question of therepresentativeness of a threshold obtained over sand, or over any other soil,that leads to block moisture contents much above the fiber-saturation level.

Another feature of the sand, as already noted, was the greater variation inthreshold values obtained with it. This probably is due to a poorer relation-ship between weight loss due to decay and moisture content in blocks oversand than in those tested over the other soils (fig. 4). Except for blocksover sand, the decay fungus seems to have been responsible for increasingthe moisture in the blocks above fiber saturation.

Conclusions

Soil texture and organic content do not tend to cause serious variations inthreshold values unless extreme differences are involved, such as betweenloam and sand. The factor mainly responsible for differences in thresholdseems to be the amount of water transmitted from the soil to the test block,independently of fungus action. Where this amount does not appreciablyexceed the fiber-saturation level, thresholds appear to be reasonably uni-form regardless of the soil type. However, if the blocks tend to exceedfiber saturation in moisture content, as in the case of sand, threshold valuesmay be both higher and more variable than otherwise. Obviously, extremes

Rept. No. 2114 -44-

of soil character are to be avoided if similar thresholds are to be obtained bythe soil-block test. Consequently, it seemed desirable to consider soils ofone texture in the next test series.

Test Series II

Series II was conducted to ascertain the variation in decay and preservativethreshold when using different soils with a uniform moisture content basedon both the water-holding capacity and the dry weight of each soil. Most ofthe soils were of a silt loam texture. Silt loam was chosen as the texture tobe emphasized because of its widespread availability and generally good water-holding capacity. Also, the soil moistures in this series were equalizedchiefly on the basis of moisture-holding capacity because this method of regu-lating water in the soil seemed to provide the most practical system of obtain-ing uniform wetting of the test block.

Methods

Nineteen soils were used. Their source, texture, pH, organic content, andwater-holding capacity4 varied as shown in table 29.

:1–The term, "water-holding capacity," as used here denotes a laboratory esti-mate of the field moisture capacity of a soil. Practically speaking, it isthe maximum percentage of water (based on the ovendry weight) that a well-drained soil can hold except for short periods of infiltration following rainor irrigation. The estimate can be made in several ways. However, themethod of Bouyoucos, with modifications suggested by E. B. Tanner of theUniversity of Wisconsin Soils Department, was used since it gave easilyreproducible results and required only simple laboratory equipment.The procedure is as follows: A short-stemmed Buchner funnel, approxi-mately 5 centimeters in diameter and 2.5 centimeters in depth and fittedwith a No. 613 "E and D" filter paper, is filled to somewhat more thancapacity with air-dry soil that has been passed through a 2-millimetersieve. The soil is then compacted by dropping the funnel 3 times througha height of 1 centimeter onto a wooden table top, and the surface is leveledwith a spatula. Then the filled funnel is placed in a 400-milliliter beakerand held in an upright position by wedges at the sides of the funnel. Wateris added to the beaker to a depth slightly beyond the top of the filter paper.The soil then is wetted from below by capillarity, and this reduces thedanger of entrapping air within the column. When the upper soil surfaceshows signs of wetting, more water is added to the beaker until the waterlevel approximates the top of the funnel. A cover is next placed over the

Rept. No. 2114 -45-

Three moisture groups were used for each soil: the moisture content waseither equal to the water-holding capacity (M1), to the water-holding capacityplus 7 percent of the dry soil weight (M2), or to the water-holding capacityplus 14 percent of the dry soil weight (M3). The corresponding soil moisturesin terms of the percent of the water-holding capacity or of the percent of theovendry weight of the soil are shown in table 30.

A weighed amount of the sifted air-dry soil, sufficient to give a 4-ouncevolume (test bottle half-filled) was added to each bottle, which already con-tained a predetermined amount of water needed for the desired soil moisture.Two pine feeder strips were placed on the surface of the soil. The bottleswere then loosely capped and sterilized at 15 pounds pressure for 30 minutes.

The test blocks initially contained approximately 3.2 or 5.5 pounds of a low-residue creosote, 3.1 or 5.2 pounds of 5 percent pentachlorophenol in a highboiling petroleum, or were untreated. The treated blocks were conditionedbut not weathered before placing them in test.

The testing was limited by the small amounts of individual soils that wereavailable. It was possible to test duplicate blocks representing each creosotetreatment, soil, and soil-moisture group. However, the pentachlorophenol-treated blocks could not be included in all test categories, as will be apparentin the tabulation of results. To conserve soil, an untreated block was placedwith a treated block in each bottle.

As in Series I, soil bottles which were to hold creosote-treated blocks wereinoculated with Lent. lepideus (Madison 534) and those intended for penta-chlorophenol-treated blocks were inoculated with L. trabea (Madison 617).

Results

Weight losses in the blocks subjected to decay by Lent. lepideus and L. trabeain bottles with different soils and soil moisture contents are shown in tables31 and 32.

4 (continued)beaker and the soil is allowed to soak for 12 hours or overnight. Thefunnel is then placed in a suction flask connected to a water aspirator orvacuum pump, and full suction is applied for 15 minutes. To prevent ex-cessive drying of the soil during suctioning, the funnel is covered with amoist cloth on which an inverted cup is placed. After 15 minutes thesoil is transferred from the funnel to a weighed receptacle and its mois-ture content determined, based on ovendry weight.

Rept. No. 2114 -46-

Considering the creosoted blocks and their controls (table 31), it may benoted that all blocks treated with 32 pounds of creosote were decayed butmost blocks treated with 5.5 pounds of creosote were not visibly decayed.The threshold for Lent. lepideus indicated by about three fourths of the 57combinations of soil and soil-moisture lay between 32 and 5.5 pounds. More-over, most thresholds probably occurred within a range that was substantiallynarrower than 32 to 5.5 pounds. This is indicated by the few exceptions inwhich marked differences appeared in weight losses in the blocks with the3.2-pound treatments, or just below the threshold retention zones.

The soils and moisture contents that led to decay of blocks with the 5.5-poundtreatment, and so placed the thresholds outside the 32 to 5.5 range, had oneor more of these distinguishing characteristics:

(1) Three of the soils were not silt loam (Nos. 17, 18, and 19).

(2) All the soils had less than 2 percent organic matter (Nos. 1, 3, 10, 11,14, 17, 18, and 19).

(3) The moisture contents in 9 of the 11 cases exceeded 150 percent of thewater-holding capacity of the soil (table 30); the two exceptions occurred withsoil No. 11 for which the organic content (0.4 percent) was second lowest tothat of the sand (No. 19).

(4) The weight of a 4-ounce volume of 6 of the 8 unfavorable soils was in ex-cess of 130 grams, a weight greater than that of any of the other soils.

No conclusions are possible on the pentachlorophenol-treated blocks sub-jected to L. trabea (table 32) because none of the treated blocks except thosetested on sand were attacked, and none of those on sand were entirely withoutdecay. However, the sand was consistent in again producing thresholds ex-ceeding those obtained on loam soils (see Test Series I).

The pH of the soil (range in the tests: 4.7 to 7.9) had no discernible effect onthe decay of either the treated or the untreated blocks. Of particular inter-est in this connection was the normal decay of blocks on the single alkalinesoil (No. 4--pH 7.9). It is unlikely that this would have occurred had the pHof the test block been alkaline also, since decay fungi are generally intolerantof an alkaline substrate.

Conclusions

The tests in this series, as in Series I, indicate that excessive variations inthreshold values are associated primarily with soil moistures that are con-

Rept. No. 2114 -47-

siderably in excess of the moisture-holding capacity of the soil. Within thetested limits, the pH of the soil apparently has little influence on the thresh-old. A low organic content of the soil apparently may sometimes lead to highthreshold values and for reasons that are not entirely confined to high moist-ure contents.

In choosing soils and moisture contents for uniform soil-block testing, theresults indicate that: (1) A majority of silt loan's would be suitable. (2) Thesoil should have an organic content of at least 2 percent. (3) The soil shouldweigh not over 130 grams per 4 ounces of volume. (4) The moisture contentof the soil should not exceed 150 percent of its water-holding capacity.

The most appropriate soil moisture content for general testing cannot be as-certained from the data but it appears that there might be considerable toler-ance in this respect, provided the foregoing restrictions were imposed.

Test Series III

The tests in Series III were intended to (1) ascertain the variation in preserva-tive threshold associated with different percentages of moisture in a singlesilt loam soil with a water-holding capacity of 34 percent, and (2) observe theeffect of differences in soil moisture on a larger number of test fungi than thetwo species used in Series I and II.

The study was essentially a critical appraisal of the effect of soil moisture onpreservative thresholds when uncomplicated by other factors. It was expectedto provide data on the optimum level of initial moisture for the kind of soilused, and also on the variation in moisture that might be tolerated in prepar-ing the soil.

Methods

A silt loam soil with a water-holding capacity of 34 percent (sample 13,Series II) was used.

The moisture contents of the soil in the test bottles were made up to 130, 150,and 170 percent of water-holding capacity, or 44, 51, and 58 percent of theovendry weight of the soil.

The high soil moistures in some test bottles made precautions necessary tominimize the tendency of the soil to become excessively wet on the surface.

Rept. No. 2114 -48-

The soil was first sifted through a No. 6 mesh screen before it was placedin the bottles. At this time the soil contained approximately 20 percent mois-ture which made it easy to handle and measure. Except for a gentle tap onthe bottle to level the surface, the soil was not compacted. Even with thistechnique, the feeder strips became partially covered with soil and saturatedwith water during sterilization when the water placed in the bottles provideda moisture content of 170 percent of the water-holding capacity of the soil.This complication did not occur when the soil with lower moisture contentswas sterilized, so long as care was taken to minimize compacting of the soil.It was noted that with moisture contents at 150 percent of the water-holdingcapacity, the soil was made muddy by greater compacting than occurred fromthe above procedure.

The test blocks of southern pine sapwood were treated with one of three pre-servatives: a low residue coal-tar creosote, 5 percent pentachlorophenol ina high boiling petroleum, and copperized chromated zinc chloride. The vari-ous treating dilutions of the oil-borne preservatives were made with toluene.The blocks were conditioned but not weathered after treating.

The test fungi were: Lentinus lepideus (Madison 534), Lenzites trabea (Madison 617), Poria monticola (Madison 698), and Polyporus versicolor(Madison 697). The first three fungi produce brown rot. Poly. versicolor,a white-rot fungus, had previously been found to decay pine slowly and toshow less tolerance of preservatives in pine than in sweetgum. It was in-cluded in these tests to determine whether certain of the higher soil moist-ures might yield results that differed from the earlier ones.

Results

The results for the different preservatives, fungi, and soil moisture contentsare shown in tables 33, 34, and 35.

The data show that in conditioned blocks treated with any of the preservatives,decay by the three brown rot fungi, especially P. monticola and L. trabea,generally tended to be less when the soil moisture content was 170 comparedto 130 or 150 percent of the water-holding capacity. There was no similartendency in the case of the white-rot fungus, Poly. versicolor.

More significantly from the practical standpoint, the preservative thresholdsfor most of the fungi did not differ materially with the several levels of soilmoisture. The only exceptions for each preservative involved fungi that wereparticularly tolerant. In these cases, the thresholds obtained with a soilmoisture content of 150 percent of the water-holding capacity tended to besomewhat higher than those obtained with the soil at the other moisture levels.

Rept . No. 2114 -49-

Conclusions

Considering all results, a soil moisture content of 130 percent of the water-holding capacity apparently would provide adequate test severity without thehazard of creating a saturated soil condition. With most test fungi, somelatitude apparently can be tolerated in the amounts of soil moisture amongindividual test bottles; therefore, ordinary precautions to maintain uniformsoil moisture contents should be acceptable in standard testing. However,when testing with a fungus of relatively high tolerance to a particular preserva-tive, the range of moisture should be held to a minimum.

Test Series IV

The previous tests indicated that (1) adequate uniformity of results is possiblewith a variety of soils, provided a few easily manageable restrictions areplaced on the soils; (2) most silt loams will fulfill the soil requirements; and(3) when using a silt loam soil a moisture content of about 130 percent of thewater-holding capacity will provide good test conditions. However, it seemedadvisable to confirm the general suitability of a soil moisture level of 130 per-cent of the water-holding capacity and in doing so, to use soils having water-holding capacities within the range of 20 to 40 percent, which would be com-mon among silt loams.

The specific purpose of Series IV was to determine the variation in preserva-tive thresholds when using four soils with water-holding capacities rangingbetween 20 and 40 percent and with a moisture content equal to 130 percentof the water-holding capacity of each soil.

Methods

A considerable number of soils in the area of. Madison, Wis. , were sampledto determine their water-holding capacity. When four were found with water-holding capacities within the range of 20 to 40 percent, approximately 1 cubicfoot of each was brought into the laboratory. The textures of the four soilswere not ascertained.

Since the preparation of the soil may influence the results obtained with it,the manner of handling and preparing the soil is briefly described. Each ofthe soils was dry enough so that when thoroughly mixed and sifted through aNo. 6 sieve, the particles remained separated. These sifted soils were thenplaced in covered containers and a final check was made on each soil of the

Rept. No. 2 114 -50-

water-holding capacity, moisture content, and the weight in grams requiredto half fill a culture bottle. All determinations were made on an ovendry basis.The water-holding capacity, pH, and organic matter of each soil, and the per-centages of moisture provided for the testing are shown in table 36.

In preparing the soil-block bottles, the essential procedures described previ-ously were followed. As in Series III, there was no compacting of the soil ex-cept as resulted when the surface of the soil was leveled by gently tapping thebottle. A single southern pine feeder strip, 0.3 by 2.9 by 4.1 centimeters,used for the first time in this series, was placed on the soil surface with noattempt to push it into the soil.

The test blocks again were 3/4-inch cubes of southern yellow pine. Those tobe treated with preservative were treated with seven concentrations of a low-residue coal-tar creosote, 5 percent pentachlorophenol in a high boiling petro-leum, or copperized chromated zinc chloride. The blocks were conditionedfor 3 weeks but were not weathered.

Four untreated blocks and four blocks with replicate preservative treatmentwere tested on each soil and against each of the three test fungi.

The test fungi were Lentinus lepideus (Madison 534), Lenzites trabea (Madi-son 617), and Poria monticola (Madison 698).

Results

The block weight losses and preservative thresholds as determined on thefour different soils are shown in tables 37, 38, and 39.

Although the weight losses produced by a given fungus in similarly treatedblocks varied somewhat on the different soils, decay was prevented at thesame level of preservative retention in all cases. Therefore, any variationsin the preservative thresholds determined on the four soils could not haveexceeded approximately 1 pound per cubic foot of creosote or the pentachloro-phenol solution, or 02 pounds of copperized chromated zinc chloride (thetested retentions encompassing a threshold were no larger than these values).Actually, there were no material differences among thresholds whereverthese could be estimated by the line-intersection method.

Conclusions

The results indicate that threshold values will be similar when tests are madeon soils having a water-holding capacity within the range of about 20 to 40 per-cent and when the moisture content used for such soils is 130 percent of thiscapacity. A water-holding capacity greater than 40 percent might be toleratedbut this would have to be ascertained by further testing.

Rept. No. 2114 -51-

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Table 25.--Weight losses in weathered, creosote-treated and controlblocks subjected to decay by Lent. lepideus when usingsoils of four different textures but uniform volumes ofsoil and water in the test bottles

Preservative: Weight loss1- in test blocks when us- :Relative thresholds

retention : ing the indicated soils : indicated with the different soils

:Silt loam:Sandy loam:Loamy sand: Sand :A : B : C D

Lb. per : Percent : Percent : Percent : Percent:cu. ft.

CREOSOTE (M)

0 : 35.4 : 38.3 : 32.0 : 22.7 : A and C similar;4.2 .. 10.7 : 8.7 : 9.1 : 6.6 ; B lower and D6.1 5.5 : 2.9 : 7.0 : 4.3 : higher than A8.1 3.5 : (1.7) : 2.6 : 2.7 : and C.

10.2 , (1.9) : (1.8) : (1.7) : 2.4 :12.4 (2.0) : (1.9) : (1.7) : (1.7) :

CREOSOTE (x)

0 : 39.1 i 37.7 : 33.6 : 23.1 : A and B similar;3.9 : 11.2 : 8.3 : 9.6 : 8.4 : C and D similar5.9 : 4.8 : 2.1 : 7.8 : 7.6 : but higher than8.1 : (1.5) .: (1.3) : 3.5 : 5.1 : A and B.

10.1 : (1.3) : (1.3) : 2.1 : 3.2 :12.4 : (1.5) : (1.4) : (1.3) : (1.4) :

: .

2Each weight loss is an average result of 4 untreated or 5 treated blocks.Weight losses in parentheses are attributed to factors other than decay.

Rept. No. 2114 -53-

Table 26.--Weight losses in weathered pentachloruhenol-treated and con-trol blocks subjected to decay by Lenzites trabea when usingsoils of four different textures but uniform volumes of soiland water in the test bottles

Preservative: Weight losu1- in test blocks when :Relative thresholds

retention : using the indicated soils : indicated with the different soils

:Silt loam:Sandy loam:Loamy sand: Sand: A : B : C D

Lb. per : Percent : Percent : Percent :Percent :cu. ft.

PENTACHLOROPHENOL, 5 PERCENT, IN PETROLEUM Y

0 : 37.2 : 43.9 : 54.4 : 22.5 : Similar in A, B,2.2 : 15.7 : 7.6 : 8.1 : 6.7 : and C but higher4.o : 3.7 : 2.4 : 2.3 : 3.4 : in D.6.4 : (1.7) : (2.0) : (1.5) : 2.9 :8.3 : (1.9) (1.8) : (1.7) : (2.o) :

10.6 : (2.2) : (2.0) : (2.3) : (2.2) :

PENTACHLOROPHENOL, 5.48 PERCENT, IN PETROLEUM Z

0 : 39.2 : 51.8 : 55.0 : 32.4 : Similar in A, B,1.7 : 13.5 : 4.2 : 2.5 : 6.4 : and C but higher3.5 : (1.0) : (1.1) : (0.9) : 1.6 : in D.5.2 : (1.1) : (1.1) : (1.1) : (1.3) :7.3 : (1.1) : (1.2) : (1.0) : (1.3) :9.0 : (1.3) : (1.3) : (1.1) : (1.2) :

=Each weight loss is an average result of 4 untreated or 5 treated blocks.Weight losses in parentheses are attributed to factors other thandecay.

Rept. No. 2114 -54-

1

Table 27.--Moisture content- of creosote-treated and control blocks after12 weeks in test bottles containing the 4 different soils--uninoculated, or inoculated with Lentinus lepideus

Preservative: Moisture content in blocks using the

retentions : indicated soil-fungus combinations

Soil inoculated Soil uninoculated(Lentinus lepideus)

: Silt : Sandy : Loamy :Washed : Silt : Sandy : Loamy :Washed: loam : loam : sand : sand : loam : loam : sand : sand

Lb. per :Percent :Percent :Percent :Percent :Percent :Percent :Percent :Percentcu. ft. • •

CREOSOTE (M)

0 : 41 : 45 : 50 : 53 : 26 : 26 27 : 754.2 : 33 : 32 : 42 : 83 : 26 : 26 : 27 : 1006.1 28 27___: 38 : 75 : 25 : 26 : 29 : 858.1

_

:__26___: 25 :___33__: 56 : 25 : 26 : 32 : 8110.2 : 25 25 : 29 :___5__: 25 : 26 : 29 : 6012.4 : 25 25 : 26 : 42 : 24 : 25 : 26 : 36

CREOSOTE (x)

0 : 41 : 45 : 49 : 47 : 27 30 33 : 893.9 : 33 : 32 : 37 : 61 : 26 27 29 • : 305.9 :__2/___:__27___: 36 : 56 26 : 25 26 : 298.1 : 25 24 :___11__:___50__: 25 : 25 29 34

10.1 : 24 25 : 32 : 40 : 25 : 29 27 3512.4 : 24 : 24 : 25 : 33 : 24 : 24 31 31

2The moisture content is based on the computed ovendry weight of the block.The weight of residual chemical was included in the computed weight of adry block, consequently moisture figures for the treated blocks areslightly lower than the true values. The difference, however, has nobearing on the use made of the data. Each figure is an average valueof 4 or 5 blocks from inoculated bottles and of 2 from the uninoculated.Values below the broken line are for blocks that did not decay.

Rept. No. 2114 -55-

Table 28.--Moisture content1- of pentachlorophenol-treated and control

blocks after 12 weeks in test bottles containing the 4 different soils--uninoculatedi or inoculated with Lenzites trabea

Preservative: Moisture content in blocks using the

retentions : indicated soil-fungus combinations

Soil inoculated Soil uninoculated(Lenzites trabea)

: Silt : Sandy : Loamy :Washed : Silt : Sandy : Loamy :Washed: loam : loam : sand : sand : loam : loam : sand : sand

Lb. per :Percent :Percent :Percent :Percent :Percent :Percent :Percent :Percent cu. ft.

PENTACHLOROPHENOL, 5 PERCENT, IN PETROLEUM T

: 39 : 42 : 6o : 61 : 26 : 26 : 28 :: 32 : 29 : 34 : 63 : 27 : 27 28 :

55 : 26 : 27 : 31 :: 26 : 27 : 27 : 44 : 26 : 27 : 31 :: 26 : 26 : 26 : 38 : 26 : 26 : 35 :: 25 : 27 : 27 : 29 : 24 : 26 : 34 :

PENTACHLOROPHKNOL, 5.48 PERCENT, IN PETROLEUM Z

: 38 : 53 : 6o : 6o 27 : 28 : 33 : 891.7 _ 28 _:__22__: 6o : 26 27 : 34 : 763.5 : 26 : : 28 : 40 : 26 : 26 : 28 : 595.2 : 25 : 26 : 27 : 30 : 26 : 26 : 29 : 397.3 : 25 : 29 27 : 3o : 27 : 27 : 32 : 399.o 25 : 27 26 : 26 • 24 : 26 : 36 : 35

•

1-The moisture content is based on the computed ovendry weight of the block.

The weight of residual chemical was included in the computed weight ofdry block, consequently moisture figures for the treated blocks areslightly lower than the true values. The difference, however, has nobearing on the use made of the data. Each figure is an average value of4 or 5 blocks from inoculated bottles and of 2 from the uninoculated.Values below the broken line are for blocks that did not decay.

2.24.06.48.3

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757755675132

Rept. No. 2114 -56-

Table 29.--Data relative to the 19 soils considered in Test Series II

Sample: Source Texture : - : Water-holdingNo. : : matter : capacity

• : Percent Percent1 : Arkansas : Silt loam : 6.3 : 0.5 18

2 : California do • 5.5 : 2.8 29

3 : Connecticut • do • 5.2 : 1.4 23

4 : Florida do • 7.9 : 4.8 66

5 : Iowa :....do • 6.5 : 4.8 32

6 : Mississippi • do. • 5.2 : 2.0 28

7 : New York do • 5.5 : 3.6 32

8 : Ohio :....do • 5.4 : 3.4 30

9 : Oregon :....do • 5.7 : 2.5 26

10 : Tennessee do • 6.0 : 1.6 23

11 : Texas :....do • 5.4 : .4 17

12 : Virginia :....do • 5.7 : 2.2 30

13 : Wisconsin do • 5.0 : 3.6 34

14 : Tennessee • do • 5.8 : 1.8 24

15 : Ontario • 4.8 : 4.0 31

16 : Ontario • 5.3 : 3.2 27

17 : New Jersey : Sandy loam : 5.2 : 1.8 • 19

18 : Mississippi : Loamy sand : 4.7 : .9 14

19 : Michigan : Sand : 6.7 : .1 3

1-Organic matter determinations were made by the Agriculture Extension

Service, University of Wisconsin. They were run by the chromicacid digestion method and the percentages were read colorimetri-cally by comparison with a standard color chart.

• 'Organic

1: pH

Rept. No. 2114 -57-

Table 30.--Moisture contents provided in the 19 soils listed in table 29and data upon which they are based.

Soil : Water- :Ovendry: Moisture content relative:sample:holding : weight: to weight of dry soil :

:capacity: of : :4-ounce:Equal to:Equal to:Equal to::volume : water- : water- : water :

Moisture contentrelative to water-holding capacity

of the soil

: in :holding :holding :holding : (M1)

(M2) : (M3): bottle:capacity:capacity:capacity:

:Percent—:1 Gm.

: (M1) : plus 7 : plus 14:: (M2) : (M3) :

:Percent :Percent :Percent :Percent:Percent:Percent

1 18 146 : 18 25 32 : 100 : 139 : 178

2 29 125 : 29 36 43 : 100 : 121+ : 1483 23 : 120 23 3o 37 : 100 : 130 : 161

66 82 : 66 73 8o : 100 : 111 : 121

5 32 115 : 32 39 46 : 100 : 122 : 144

6 28 : 119 : 28 35 1+2 : 100 : 125 150

7 32 122 : 32 39 46 : 100 : 122 : 1448 3o : 117 : 3o : 37 1+1+ : 100 : 123 : 11+79 26 118 : 26 33 4o : 100 : 127 : 154

lo 23 : 11+2 : 23 3o 37 : 100 : 130 : 161•

11 17 142 : 17 214- 31 : 100 : 11+1 : 18212 30 117 : 3o . 37 44 : 100 123 : 11+713 34 : 114 : 34 41 48 : 100 121 : 11+114 21+ 133 : 24 31 38 : 100 : 129 : 15815 31 : 106 : 31 38 45 : 100 : 123 : 145

••

• ••

16 : 27 : 122 : 27 34 41 : 100 : 126 : 15217 : 19 : 125 : 19 26 33 : 100 : 137 : 171+18 ; 11+ : 134 : 14 21 • 28 : 100 : 150 20019 : 3 172 : — 3 10 •

• 17 : 2–100 : 333 567

=Based on ovendry weight of the soil.

?No tests were made with this particular moisture content in the sand,since it was not sufficient to keep the sand suitably wet throughoutthe test period.

Rept. No. 2111+ -58-

:12 :13 :14 :15 :

16 :1718 :19 •

23 : 2130 36 :38 : 38 :26 : 3243 : 48

38 : 5023 : 38 :12 : 24 :

• 25 •

in soil equal toin soil equal todry soil weight.in soil equal todry soil weight.

the water-holdingthe water-holding

the water-holding

Table 31.--Weight losses in conditioned, creosote-treated test blocks sub-jected to decay by Lentinus lepideus

Soil : Weight loss insample: untreated blocks when :

using the indicated2soil-moisture group- :

: M1 : M2 : M3

Weight loss inblocks treated with3.2 pounds per cubic

foot of creosote whenusing the indicated2soil-moisture group-

Weight loss in: blocks treated with

5.5 pounds per cubic: foot of creosote when

using the indicatedsoil-moisture group,

M1 : M2 : M3 : Ml : M2 : M3

:Percent :Percent :Percent :Percent :Percent :Percent :Fercent :Fercent :Percent

: : •

1 : 24 : 39 36 : 7 6 : 42 : 29 : 37 : 49 : 12 : 15 : 15

3 : 26 : 33 : 38 : 9 : 7 : 8

4 : 25 : 58 : 57 : 14 : 10 : 14

5 : 40 : 50 : 50 : 14 : 14 : 15

6 • 47 : 13 : 10 : 15

7 : 46 : 8 : 11 : 6

8 : 56 : 8 : 12 : 16

9 : 52 : 14 : 12 : 1510 : 58 5 : 7 : 4

28 : 19 : 21 : 2252 : 11 : 12 : 946 : 13 : 21 : 1248 : 11 : 11 : 1154 : 9 : 11 : 5

55 : 8 • 6 653 : 6 : 8 : 932 : 9 • 9 522 • • 10 • 5

37 : 3840 : 40 :40 : 40 :30 : 32

46 : 54 :

: (1.8) : (1.9) : 2.7: (1.7) : (1.8) : (1.9): (2.0) : (1.9) : 2.8: (1.0) : (1.1) : (1.0): (2.0) : (1.8) : (1.9)

: (2.0) : (1.6) : (2.0): (2.0) : (1.6) : (1.6): (1.8) : (1.8) : (1.4): (2.0) : (1.8) : (1.9): (1.3) : (1.7) : 2.6

: 12.0 : 8.6 : 13.2. (1.6) : (1.5) : (1.3): (2.0) : (1.6) : (2.0): (1.7) : (1.7) : 3.1: (1.7) : (1.5) : (1.3)

: (1.9) : (2.0) : (1.2): (1.3) : (2.0) : 2.8: (1.8) : (1.6) : 3.- • 3.0 : 2.9

1-Each weight loss is an average result for two blocks. No

in blocks where weight losses are bracketed.

=Ml -- percent moistureM2 -- percent moisture

percent of theM3 -- percent moisture

percent of the

decay was visible

capacity.capacity plus 7

capacity plus 14

Rept. No. 2114 -5 9 -

2.1) : (2.0) (2.0)2.0) : (2.0) (2.0)

•

Table 32.--Weight lossl in conditioned; pentachlorophenol-treated blocks subjected to deca' by Lenzites trabea

Soil : Weight loss insample: untreated blocks when

using the indicated: soil-moisture group2-

M1 M2 M3

: Weight loss in blocks:treated with 3.1 pounds: per cubic foot of a: pentachlorophenol: solution when using

the indicated 2: soil-moisture group-

: Weight loss in blocks:treated with 5.2 pounds

per cubic foot of a: pentachlorophenol

solution when usingthe indicated

2soil-moisture group-

: M1 : M2 : M3 : Ml : M2 : M3

:Percent :Percent :Percent :Percent :Percent :Percent :Percent :Percent :Percent •

1 : 18 : 25 : 50 : (1.1) : (1.6) : (1.8) : (2.0) : (1.8) : (1.6)

2 • 28 - • (1.5) • • (2.o) •

3 ' •

4 : 42 : 39 : 46 : (1.1)) : (1.6) : (1.8)

5 : 26 : 29 : 46 : (1.3) : (1.5) : 1.4)

6 • •

7 ' - 3o • • (1.6) - (2.1)

8 : 25 : 27 : 14-4 : (1.1) : (1.4) : 1.5) : (2.0) : (2.1) : (2.0)

9 : 26 : 25 : 1l5 : (1.2) : (1.3) : (1.7) : (2.1) : (2.0) : (2.0)lo • •

. :

11 • 33 • • (1.2) . • (2.0) •

12 • 28 • 50 (1.2) • (1.4) • • (1.9) : (2.0)13 : 23 : 27 : 40 : (1.4) : (1.6) : (1.7) : (2.1) : (2.2) : (2.2)

14 : 25 : 27 : 47 : (1.3) : (0.9) : (1.4) : (1.9) : (1.8) : (2.0)

15 : 27 : 33 : 43 : (0.8) : (1.6) : (1.6) : (2.o) : (1.9) : (2.o)

• 34 • • (1.4) • . • (2.1) •16 •

17 : 20 : 31 : 43 : (1.0) : (1.0) : (1.2) : (2.0) : (1.8) : (2.2)

18 : 22 : 31 : 36 : (0.6) : (1.4) : (1.0) : (2.0) . : (2.0) : (2,0)19 22 • 34 • • 2.4 • 6.0 • • 2.4 : 4.5

1-Each weight loss is an

blocks where weight

411 -- percent moistureM2 -- percent moisture

percent of theM3 -- percent moisture

percent of the

average result for 2 blocks. No decay was visible inlosses are shown in parentheses.

in soil equal to the water-holding capacity.in soil equal to the water-holding capacity plus 7dry soil weight.in soil equal to the water-holding capacity plus 14dry soil weight.

•

Rept. No. 2114 -60-

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Table 36.--Characterization of soil and moisture in the different samples used in Test Series IV

Item measured Soil sample

A B : C D

1 :Organic matter– percent: 0.4 : 5.0 : 2.2

pH 5.0 : 5.6 : 4.5 : 6.2

Water-holding capacity...percent: 20 : 38 : 25 : 34

Air-dry soil....volume in ounces: 4 : 4 : 4 : 4

Ovendry soil grams: 127 : 97 : 114 : 100

Soil moisture provided fortesting:

Percent of ovendry weight • 26.0 : 49.4 : 32.5 : 44.2

Percent of water-holdingcapacity 130 : 130 : 130 : 130

1–Organic matter determinations were run by the chromic acid

digestion method and the percentages read colorimetricallyby comparison with a standard color chart.

Rept. No. 2114 -64-

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EFFECT OF AERATION THROUGH MODIFIED BOTTLE

LIDS ON DECAY IN THE SOIL-BLOCK TEST

Wood-destroying fungi are aerobic, using oxygen and releasing carbon dioxidein their metabolism. Therefore, the products of fungus metabolism, and insome cases preservative vapors from the test blocks, need to be continuallyreplaced by fresh air in the soil culture bottle to provide optimum conditionsfor decay. Furthermore, to assure that aeration does not contribute to vari-able decay, the exchange of air should be uniform in all test bottles.

To provide for exchange of air in the standard test bottles, the metal lids areused without liners, and in screwing them down they are stopped 1/4 turn shortof the terminal position. Moreover, only such lids as will screw on the bottlessmoothly are used. This technique has invariably permitted rapid and uniformgrowth of the test fungi where there was little or no interference by a preserva-tive. It has been used in all the soil-block tests at Madison except for two con-ducted prior to 1946 (13, 10), when the advocated procedure was to use lidswith oiled liners and to screw them down firmly. In those earlier tests, itbecame evident that there might be poor to no growth in more than half thetest bottles, and that this condition was due to insufficient oxygen.

In addition, provision is made for circulation of air around the bottles and theincubation room is large enough, 6 by 9 by 12 feet, so -that it does not imposeany restriction on the air supply. To minimize drying in the bottles and toprovide a constant drying potential, the relative humidity of the room is main-tained at 70 percent.

In 1953 Eades and Roff (11) concluded that blocks decayed more uniformly ifthe bottles were vented by a short glass tube, 6 mm. in diameter, insertedin the lid at an angle of 45 degrees than they did in bottles sealed or with lidshaving oiled paper liners and either screwed down tightly or released one-half turn from the stopping position. The vented bottles while apparentlyallowing sufficient aeration for rapid decay of as many as three blocks to-gether in a bottle, also provided more constant moisture conditions in thetest block, an additional factor contributing to uniform decay.

Since the Eades and Roff aeration study did not include bottle lids combiningboth loose attachment and absence of liner, duplicating the procedure beingused at Madison, the present test was conducted. The specific objective wasto ascertain whether a vented lid or some other special means of venting thetest bottle would improve associated rates and uniformity of decay over theMadison provision for aeration.

Rept. No. 2114 -69-GPO 813057-8

Method

The soil bottles were prepared in the standard manner, and the standardbrown-rot test fungi, Lentinus lepideus (Madison 534), Lenzites trabea (Madi-son 617), and Poria monticola (Madison 698) were used. After the usual incu-bation period of 3 weeks, an untreated southern pine sapwood test block wasplaced in each bottle. The standard lids and lid attachment were kept on afourth of the bottles, but the lids on three fourths of the bottles were replacedby previously sterilized ones altered in three different ways to vary the aera-tion of the cultures during the decay test. Thus four types of closures werecompared:

Type A. Metal lids with liners removed, screwed down firmly and thenbacked off 1/4 turn (standard technique).

Type B. Metal lids with oiled paper liners, screwed down firmly.

Type C. Like Type B except for a 5/8-inch hole drilled through the center ofthe lid and tightly plugged with cotton.

Type D. Like Type B except for an opening drilled through the center of thelid and to which a glass venting tube, 6 mm. in diameter, was attached at a45 degree angle. The arrangement was patterned as closely as possible afterthat of Eades and Roff.

Upon removal from the bottles, the test blocks were weighed immediatelyafter brushing off the fungus mycelium, and as usual, after standard drying.By the extra weighing the final moisture content of the blocks, as well as theamount of decay caused by the fungi, could be measured.

Results and Conclusions

The amounts of decay in bottles with the four different types of closure areshown graphically in figure 5. There was no essential difference in amountsbetween bottles with the loose, unlined lids (Type A-Madison standard) andbottles with the glass tube vents (Type D). Moreover, in both cases and withall three test fungi, the maximum or near maximum amounts of decay wereobtained.

Venting through a cotton-plugged hole in the lid (Type C) resulted in consider-ably less decay than when venting was by the foregoing methods, apparently

Rept. No. 2114 -70-

because of excessive drying out of the test blocks. This was particularlynoticeable with decay by Lentinus lepideus.

Similarly, poor decay by L. trabea and P. monticola occurred in tightly cap-ped bottles (Type B), in this case undoubtedly because of an inadequate oxygensupply. However, decay by Lent. lepideus was not apparently retarded.

The final moisture contents in the test blocks (figure 6) indicate that wherethere was some provision for aeration (closures Type A and D) moisture wasthe factor contributing to the maximum decay. The much lower final moisturecontent in blocks contained in bottles with the cotton plugged vents (Type C) in-dicates that increased aeration had resulted and had led to moisture conditionsbelow the optimum for maximum decay. The final moisture content of blocksin bottles having the firmly attached lids with liners (Type B) was fully asfavorable for decay as that in blocks that incurred maximum decay, thus leav-ing deficient oxygen supply as the logical explanation for the reduced decay inthe B-type bottles.

It appears from the results that although some provision for aeration is essen-tial for rapid decay during the 12-week exposure period, the amount of aera-tion need not be large or critically controlled. Closure by loosely attachedlids without liners (Madison standard) or by lids with tube vents would seemto be about equally satisfactory for general testing. If there is any significantdifference between the two methods, it probably would result from the tendencyfor the tube venting to make the test blocks wetter than is optimal for decay.In any case, there is no evidence here that tube venting offers any advantageover the standard method of closure. It seems likely that the advantage ofsuch venting observed by Eades and Roff applies only when the aeration ofbottles is more restricted than it is by the standard closure, such as presum-ably is the condition when the liners are left in the lids.

Rept. No. 2114 -71-

REPRESENTATIVENESS OF THE PRESERVATIVE TOLERANCE OF

STANDARD MADISON ISOLATES OF LENTINUS LEPIDEUS,

LENZITES TRABEA, AND PORIA MONTICOLA

Three economically important species of fungi, Lentinus lepideus, Lenzitestrabea, and Poria monticola, represented by Madison isolates 534, 617, and698, have been extensively used in soil-block testing because they are particu-larly tolerant to creosote, pentachlorophenol, and copper naphthenate, respec-tively. However, it was recognized that the preservative tolerance betweenisolates of a given species of test fungus may vary considerably and, conse-quently, that the standard isolates being used might not suitably represent thegeneral tolerance of the species.

The purpose of the tests described here was to determine whether the Madisonisolates 534, 617, and 698 exhibit a tolerance to creosote, pentachlorophenol,and copper naphthenate that is prevalent in the species Lentinus lepideus, Len-zites trabea, and Poria monticola, and, therefore, are representative of theirrespective species for testing these preservatives by the soil-block method.

Methods

5Twenty-five isolates of Lentinus lepideus, — 17 of Lenzites trabea, and 28 ofPoria monticola were used. The majority were isolated from conifers, namelyfir, spruce, pine, cypress, hemlock, larch, and cedar; however, poplar, ma-hogany, oak, and apple were also among the host woods. The wood productsfrom which isolations were made included test stakes, logs, posts, telephonepoles, railroad ties, lumber, and structural timbers in boats, houses, and oil-well shafts. Some of the products were untreated, others were treated withcreosote, copper naphthenate, pentachlorophenol, zinc chloride, Greensalt,Minilith, fuel oil, and Tanalith. The products were obtained from widelyseparated parts of the United States. One isolate each of P. monticola (Madi-son 704) and Lent. lepideus (L-15) came from Europe.

5The preservative-tolerance tests of the Lentinus lepideus isolates were con-

ducted by Dr. Georg Schulz, Institut fur Forstliche Mykologie and Holzs -chutz Biologische Bundesanstalt, Hann. Munden, Germany, when at theForest Products Laboratory on a Fulbright Fellowship.

Rept. No. 2114 -74-

The tolerance of the isolates of a given species was determined for the pre-servative to which that species was known to be most tolerant, namely, Lent.lepideus for creosote, L. trabea for pentachlorophenol, and P. monticola forcopper naphthenate. In addition, to learn whether some isolates might beparticularly tolerant or intolerant to a variety of preservatives, pentachloro-phenol and copper naphthenate solutions as well as creosote, were testedwith the isolates of Lent. lepideus.

The preservatives characterized in more detail were: (1) A low residue coal-tar creosote, (2) Pentachlorophenol, 5 percent by weight, in an aromatic,high-boiling petroleum, (3) Copper naphthenate in an aromatic high-boilingpetroleum (providing 0.5 percent of copper metal).

The blocks were treated according to the standard soil-block procedure. Sincethe specific gravities of the blocks were similar, treatments with a given con-centration of preservative gave similar retentions. It was, therefore, possi-ble to observe the response of a given group of isolates in conjunction withessentially uniform amounts of a preservative.

After treatment, the blocks were conditioned for approximately 2 1 days,weighed, and placed in the decay test without any weathering.

Results

Lentinus lepideus Isolates

The weight losses in tests with the 25 isolates of Lentinus lepideus on blockstreated with creosote, pentachlorophenol, and copper naphthenate are shownin tables 40, 41, and 42. The preservative retentions bracketing the indicatedthresholds of the isolates were used as a basis for assigning threshold zones,and these are graphically shown in figure 7. These zones may also be re-garded as zones of relative tolerance.

The isolates of Lent. lepideus showed in general considerably less toleranceof the pentachlorophenol than of the other two preservatives. The toleranceof the majority of isolates for copper naphthenate and creosote was similar.But of more significance for the present study, the isolates varied consider-ably in tolerance to the same preservative. For example:

(1) The creosote threshold of 17 of the isolates was between 2.2 and 4.4 pounds(Zone II), whereas that of one isolate was below, and that of 7 isolates wasabove this zone.

Rept. No. 2 114 -75-

(2) The copper naphthenate-petroleum threshold of 18 isolates was between2.7 and 5.4 pounds whereas that of 2 isolates was below, and that of 5 isolateswas above this zone.

(3) The pentachlorophenol-petroleum threshold of 13 isolates was between 0.69and 1.4 pounds whereas that of 5 isolates was below, and that of 7 isolates wasabove this zone.

As might be expected, most of the isolates fell in the intermediate zone (II)of relative tolerance to the preservative in each case. Therefore, predicat-ing that the most prevalent level of tolerance is the most representative one,a majority of the isolates apparently would suitably represent L. lepideus fortesting preservatives of the kinds considered. However, this majority wouldnot consist altogether of the same isolates for the different preservatives.Only eight isolates exhibited intermediate or zone II tolerance to all threepreservatives and Madison 534 was one of these. Consequently, this isolatewas indicated to be suitably representative of the species for testing not onlycreosote, for which it was originally selected, but also for copper and penta-chlorophenol compounds.

Besides the 8 isolates that showed an intermediate level of relative toleranceto all 3 preservatives, 7 others showed a comparable tolerance to 2 preserva-tives, 3 to pentachlorophenol and copper naphthenate, 3 to copper naphthenateand creosote, and 1 to pentachlorophenol and creosote.

None of the isolates exhibited relatively low or high tolerance (zones I, andIII or IV, respectively) to all three preservatives. But again, some of themwere relatively low or high in tolerance to two preservatives. In zone I forinstance, 2 isolates exhibited comparable relative tolerance to pentachloro-phenol and copper naphthenate; in zones III or IV, 2 isolates were relativelyequitolerant to pentachlorophenol and copper naphthenate, 1 to copper naph-thenate and creosote, and 3 to pentachlorophenol and creosote.

Lenzites trabea Isolates •

The weight losses in the decay tests made with the 17 isolates of Lenzitestrabea on blocks treated with the pentachlorophenol solution are shown intable 43. These indicate that the thresholds of all the isolates but one whichwas exceptionally intolerant (R96), were in the comparatively narrow rangebetween 1.4 and 3.4 pounds per cubic foot of solution (equivalent to 0.07 and0.17 pound of dry pentachlorophenol). It is further indicated that within thisrange the isolates fell into three distinct threshold or tolerance groups.Thus, the thresholds of 4 isolates were between 1.4 and 2.0 pounds per cubic

Rept. No. 2114 -76-

foot, those of 6 isolates were between 2.0 and 2.7 pounds, and those of the re-maining 6 were in the highest retention range, 2.7 to 3.4 pounds. The standardtest isolate of Lenzites trabea, Madison 617, was in this last group.

Poria monticola Isolates

The weight losses in the decay tests made with the 28 isolates of Poria monti-cola on blocks treated with the copper naphthenate solution are shown in table44.

The thresholds of a majority of the isolates (16), including Madison 698, werebetween 3.5 and 4.6 pounds of copper naphthenate solution (0.0175 and 0.02 30pound of copper). The thresholds of 7 isolates were in a lower range of 2.1to 3.5 pounds per cubic foot and those of 5 isolates were in a higher range of4.6 to 6.2 pounds per cubic foot.

Conclusions

Isolates of the three species of test fungi considered here are too variablein tolerance to pentachlorophenol, creosote, and copper naphthenate to beused indiscriminantly in testing these preservatives if the results obtainedare to be regarded as representative of the species. The tests indicated thatthe isolates Madison 534 and 698 have a relative degree of tolerance to creo-sote and copper naphthenate, respectively, that is typical of a majority of the25 and 2 8 isolates of the species Lentinus lepideus and Poria monticola.Therefore, they may be considered to adequately represent their species insoil-block tests of the effectiveness of these preservatives and of compoundscontaining them. Judging from the same kind of evidence, Madison 534would also be suitably representative of L. lepideus for testing copper naph-thenate and pentachlorophenol.

Madison 617 was one of 6 among the 17 Lenzites trabea isolates tested thatshowed a relatively greater than intermediate tolerance to pentachlorophenol.Such deviation from the most prevalent response of the species indicates somedeficiency in representativeness of the isolates. The thresholds of these 6isolates, however, probably did not exceed those of intermediate level bymore than 1 pound per cubic foot (0.05 pound dry pentachlorophenol). Sincethis is not an excessively large difference for practical interpretation of soil-block tests of pentachlorophenol, continued use of Madison 617 seems war-ranted.

Rept. No. 2 114 -77-

A : 5096-12 : 25 13B • 5096-19 • 30 27G : West 76 : 32 25L : MC-33 : 36 22M : MC-34 : 35 20S : MD-13 : 28 28

81213181813

222222

Table 40.--Weight losses1- caused respectively, by the 25 Lentinus

lepideus isolates in unweathered blocks treated witha creosote

Lent. lepideus : Average retention (pounds per cubic foot)ofisolates : preservative in the test blocks?

Code : Isolate : 0 0.56 • 2.2 : 4.4 : 6.7: No. :

: Percent : Percent : Percent : Percent : Percent

THRESHOLD ZONE I (0.56 TO 2.2 POUNDS PER CUBIC FOOT)

J : MC-25 : 31 : 22 : (1) : (1) : (1)

THRESHOLD ZONE II (2.2 TO 4.4 POUNDS PER CUBIC FOOT)

X : 71167 : 34 17 : 2 (1) (1)

3 : TP357 : 22 22 : 6 (1) (1)Q 1 MD-6 : 21 :

1818 : 7 (1) . (1)

P : MC-38 : 10 14 8 (1) (1)O : Mc-36 : 16 15 : 9 (1) : (1)w : 66281 : 28 18 9 (1) (1)E : 5096-47 : 30 23 9 (1) (1)

K : MC-32 : 20 17 : 10 (1) (1)

I : Mad 534 : 27 25 10 : (1) (1)

U : P-72 : 30 : 20 : 11 (1) (1)

F : 86257 26 : 22 11 : (1) (1)

C : 5096-26 : 30 26 11 (1) (1)R : MD-10 : 27 25 12 (1) (1)

N • MC-35 : 38 28 : 12 : (1) (1)

H : Boat 187: 37 26 : 13 (1) .. (1)Y : L-15 : 31 29 14 : (1) -. (1)D : 5096-33 : 40 27 17 (1) :. (1)

THRESHOLD ZONE III (4.4 TO 6.7 POUNDS PERTUBIC FOOT)

THRESHOLD ZONE IV (ABOVE 6.7 POUNDS PER CUBIC FOOT)

T : MD-22 : 43 : 37 : 11 : 4 : 2

-Each weight loss is an average for 5 test blocks. Weight lossesin parentheses are attributed to factors other than decay.

2-Retentions in each group of 5 blocks subjected to decay by a

given isolate varied no more than t 0.01 pound at the lower or± 0.2 pound at higher absorptions from the values given.

Rept. No. 2114 -78-

GPO 813057-7

1 ,Table 41.--Weight losses caused, respectively, by 25 Lentinus

lepideus isolates in unweathered blocks treated with pentachlorophenol solution

Lent. lepideus : Average retention (pounds per cubic foot)isolates of preservative in the test blocks2

Code : Isolate : 0 : 0.14 : 0.28 0.69 : 1.4No.

: Percent : Percent : Percent : Percent : Percent

THRESHOLD ZONE I (0.28 TO 0.69 POUNDS PER CUBIC FOOT)

Q : MD-6 21 10 4 (1) (1)

K : MC-32 20 16 : 9 (1) (0)O : MC-36 16 16 8 (1) (1)

P : MC-38 18 12 8 •. (0) (0)W : 66281 28 25 21 '. (1) (1)

THRESHOLD ZONE II (0.69 TO 1.4 POUNDS PER CUBIC FOOT)

3 : TP357 : 22 17 : 13 2 (0)

F : 86257 : 26 26 : 20 : 2 • (1)

D : 5096-33 : 40 41 : 30 : 3 •. (1)R : MD-10 : 27 29 : 16 •. 3 •. (1)S : MD-13 : 28 28 : 22 : 3 •. (1)u : P-72 : 3o 18 16 : 4 •. (1)Y : L-15 : 31 21 •. 19 : 4 •. (1)

I : Mad 534 : 27 26 •. 21 : 5 •. (1)B : 5096-19 : 30 30 • 23 : 6 •. (1)G : West 76 : 32 33 31 : 6 •. (1)

A : 5096-12 : 25 : 23 25 : 8 -. (1)C : 5096-26 : 30 : 31 24 : 8 •. (1)

H : Boat 187: 37 •. 41 29 10 : (1)

THRESHOLD ZONE III (ABOVE 1.4 POUNDS PEE CUBIC FOOT)

M : MC-34 : 35 : 31 24 : 7 2

T : MD-22 : 43 4o 33 : 8 3

X : 71167 : 34 21 22 : 9 : 2E : 5096-47 : 30 29 24 10 : 2L : MC-33 : 36 29 20 : 10 : 2N : MC-35 : 38 38 3o : 10 : 3J : MC-25 : 31 28 27 15 : 3

_Each weight loss is an average for 5 test blocks. Weight lossesin parentheses are attributed to factors other than decay.

–.Retentions in each group of 5 blocks subjected to decay by agiven isolate varied only ± 0.02 at lower to ± 0.2 at higherabsorptions from the values given. The preservative was 5percent of pentachlorophenol in a high-boiling petroleum.

Rept. No. 2114 -79-

Table 42.--Weight losses- caused) respectively, by 25 Lentinus lepideus isolates in unweathered blocks treated withcopper naphthenate solution

Lent. lepideus : Average retention (pounds per cubic foot)isolates : of preservative in the test blocks

Code : Isolate : 0 • 0.68 : 1.4 : 2.7 : 5.4

0P

: No. : ••

: Percent : Percent : Percent : Percent : Percent

THRESHOLD ZONE I (1.4 TO 2.7 POUNDS PER CUBIC FOOT)

: MC-36 : 16 : 11 : 7 : (1) : (1): MC-38 : 18 : 9 : 7 : (1) : (1)

THRESHOLD ZONE II (2.7 TO 5.4 POUNDS PER CUBIC FOOT)

V : TP357 22 8 5 2 (2)K : MC-32 : 20 11 7 2 (1)A : 5096-12 : 25 17 12 2 (2)U : P-72 : 30 12 8 3 (2)w : 66281 28 17 10 3 (1)F : 86257 26 23 15 3 (2)J : MC-25 : 31 25 15 3 (2)D : 5096-33 : 40 37 26 4 (2)B : 5096-19 : 30 24 20 5 (2)R : MD-10 27 22 14 5 (2)s : MD-13 28 19 12 5 (2)x : 71167 : 34 21 13 5 (2)Y : L-15 : 31 18 16 6 (2)C : 5096-26 : 30 25 21 6 (2)I : Mad 534 : 27 23 20 7 (2)T : MD-22 : 43 37 22 8 (2)M : MC-34 : 35 22 : 15 9 (2)L : MC-33 : 36 22 : 16 9 (1)

THRESHOLD ZONE III (ABOVE 5.4 POUNDS PER CUBIC FOOT)

Q : MD-6 : 21 : 16 : 13 : 7 : 3G : West 76 : 32 : 31 : 28 : 17 : 4N : MC-35 : 38 : 33 : 33 : 22 : 5H : Boat 187: 37 : 37 : 25 : 16 : 6E 5096-47 : 30 : 27 : 25 : 19 : 10

1-Each weight loss is an average for 5 blocks. Weight losses in

brackets are attributed to factors other than decay.2-The preservative was copper naphthenate in an aromatic high-

boiling petroleum (0.5 percent copper) diluted in toluene toobtain different retentions. The listed retentions of stocksolution were equivalent to 0.0034, 0.007, 0.0135, and 0.027pound of copper metal per cubic foot. Retentions in eachgroup of 5 blocks subjected to decay by a given isolate variedless than + 0.04 from the values given.

Rept. No. 2114 -80-

Table 43.--Weight losses1– caused, respectively./ by 17 Lenzites trabea isolates in unweathered blocks treated with pentachlorophenol solution

Isolate No. Average retention (pounds per cubic foot)of preservative in the test blocks?

: 0 : 0.7 : . 1.4 : 2.0 : 2.7 : 3.4 : 4.1 : 4.7

;Percent :Percent :Percent :Percent :Percent :Percent :Percent :Percent

THRESHOLD ZONE: 0.7 TO 1.4 POUNDS PER CUBIC FOOT

R96 : 27 : 2 : (1) : (1) : (1) : (2) : (3) : (3)

THRESHOLD ZONE: 1.4 TO 2.0 POUNDS PER CUBIC FOOT

Boat 194 : 25 : 18 : 3 : (1) : (1) : (2)Minn. Cedar 1-15: 38 : 27 : 4 : (1) : (1) : (2)TP358 : 56 : 48 : 4 : (1) : (1) : (2)Boat 209 : 43 : 31 : 6 : (1) : (1) : (2)

THRESHOLD ZONE: 2.0 TO 2.7 POUNDS PER CUBIC FOOT

(3) : (3)(3) : (3)(3) : (3)(2) : (3)

Boat 288H4635096-15M. Say . Is.5060MD76

MD2051285123539Mad 617Boat 182B

32 : 29 : 12 : 2 : (1) : (1)51 : 43 : 14 : 3 : (1) : (2) :52 : 37 : 27 : 3 : (1) : (2)68 : 40 : 32 : 3 : (1) : (2)

: 54 : 46 : 29 : 4 : (1) : (2)59 32 : 25 : 5 : (1) : (2) :

THRESHOLD ZONE: 2.7 TO 3.4 POUNDS PER CUBIC FOOT

: 66 : 29 : 22 : 10 : 3 : (2)66 : 41 : 19 : 11 : 2 (1)43 : 24 : 25 : 12 : 3 ; (2)46 : 31 : 24 : 12 : 3 : (2)57 : 32 : 27 : 15 : 7 : (2) :48 : 43 : 29 : 18 : 11 : (2) :

(3) : (3)(3) : (4)(3) : (3)(3) : (3)(2) : (3)(3) : (3)

(3) (3)(3) (4)(3) : (3)(3) : (3)(3) : (3)(3) : (3)

2Each weight loss is an average of 4 blocks. Weightattributed to factors other than decay.

2–The preservative was 5 percent pentachlorophenol in

petroleum.

losses in parentheses are

an aromatic high-boiling

Rept. No. 2114 -81-

Table 44.--Weight losses! caused, respectively, by the 28 Poria monticolaisolates in unweathered blocks treated with copper naphthenate solution

Isolate No.

Average retention (pounds per cubic foot)of preservative in the test blocks

:

THRESHOLD

0 : 2.1 : 2.7 : 3.5 : 4.6 : 6.2 : 8.0: (o) :(0.0105):(0.0135):(0.0175):(o.o23o):(0.0310):(0.0400)

:Percent:Percent:Percent:Percent:Percent:Percent:Percent

ZONE: LESS THAN 3.5 POUNDS PER CUBIC FOOT

575 : 12 • (1) : (1) : (1) : (2) : (3) : (3)94264 : 6 : (1) : (1) : (1) : (2) : (2) : (3)4935 : 31 : 5 : (1) : (1) : (2) : (2) : (3)4752 : 26 : 5 • (1) • (1) : (2) • (2) : (3)H460 : 46 : 19 : 4 : (1) (2) : (2) : (3)22R : 42 : 9 : 3 : (1) - (2) : (2) : (3)94153 : 44 : 21 : 4 : (1) : (2) : (2) : (3)

THRESHOLD ZONE: 3.5 TO 4.6 POUNDS PER CUBIC FOOT

5096-22 : 48 : 35 : 14 •. 3 : (2) : (2) (3)94366 : 53 : 45 : 19 •. 4 : (2) : (3) (3)4718 : 25 : 18 : 10 : 5 : (2) : (2) (3)Boat 193 37 : 41 : 17 : 5 : (2) : (3) (3)Calif. 47-26 61 : 42 : 24 : 5 : (2) : (2) (3)5096-38 : 45 : 37 : 22 : 6 : (2) : (2) (3)U-10 • 47 : 49 : 22 . 6 : (2) : (2) : (3)West M21-2 + 0 . 46 : 40 : 23 •• 6 : (2) : (3) : (3)MD 60 47 : 42 : 26 : 6 : (2) : (3) : (3)21551 47 : 51 : 30 : 6 (2) : (2) : (3)Mad 698 41 : 45 : 23 : 7 : (2) • (3) : (3)4874 : 36 : 36 : 25 : 7 (2) • (2) • (3)White Plains 108 : 35 : 28 : 18 : 8 : (2) : (3) : (3)5096-45 : 55 • 35 • 20 : 8 (2) • (2) • (3)66236 40 : 44 : 28 : 8 : (2) : (2) (3)MD-65 44 : 45 : 23 : 9 (2) : (2) (3)

THRESHOLD ZONE: 4.6 TO 6.2 POUNDS PER CUBIC FOOT

MD-86 : 41 : 36 : 16 : 9 : 5 • (3) • (3)5096-11 49 : 32 19 : 11 : 5 : (3) • (3)94181 : 43 : 29 - 20 : 13 : 5 : (3) : (3)4764 : 44 41 : 30 20 : 5 : (2) : (3)704 : 56 24 : 15 : 11 6 : (3) • (3)

1Each weight loss is an average of 4 blocks. Weight losses in parentheses

are attributed to factors other than decay.

?Dilutions of the copper naphthenate aromatic high-boiling petroleumsolution (0.5 percent copper) were made in toluene to obtain differentretentions. Bracketed retentions represent pounds of copper metal.

Rept. No. 2114 -82-

DEVELOPMENT OF A WEATHERING PHASE

FOR THE SOIL-BLOCK TEST

A high initial toxicity is one of the requirements of a good preservative, butis of little value if much of the toxic material is soon lost in wood exposed toservice conditions. In order that the soil-block test might function as a com-bined appraisal of both toxicity and permanence of a preservative, "acceler-ated weathering" of the treated test blocks is, therefore, essential. The fol-lowing is an account of studies underlying the development of a suitableweathering phase.

Weathering Outdoors

Weathering was first accomplished by exposing the treated blocks outdoorsfor 60 days. The details of this procedure and the thresholds determined forvarious preservatives after outdoor weathering have appeared in several pub-lications (2, 3, 4, 5, 8, 10).

With outdoor weathering, it was recognized that differences in climatic con-ditions could affect the reproducibility of a threshold in the soil-block test.It was shown (6) for example, that the overall loss and threshold of a coal-_tar creosote varied with exposures in different seasons of the year. Thus itwas obvious that outdoor weathering could not be appropriately standardized;moreover, the 60-day exposure was excessively long. A permanence testwas needed, therefore, that could be sufficiently controlled to give repeat-able results, and preferably give results more quickly than outdoor weather-ing. This need led to trials of artificial weathering in the laboratory. Fromthese trials the present standard procedure was obtained.

Laboratory Weathering

In planning and conducting trials of artificial weathering, it was recognizedthat no procedure could be devised that would simulate all conditions to whichtreated wood is subjected in service. The primary purpose, therefore, wasto find a simple, reproducible procedure that would reveal significant differ-ences among preservatives in volatility and leachability likely to affect theprotection afforded by the preservatives in service. For lack of basic dataon preservative losses under field conditions, the severity of artificial

Rept. No. 2114 -84-

weathering was arbitrarily chosen. The general aim was to make it such thatlosses and threshold values of a low-residue coal-tar creosote would approxi-mate those previously obtained with outdoor weathering over a 60-day periodin the summer at Madison, Wis. Such weathering generally gave a loss ofcreosote constituents of about 50 percent by weight and a test threshold ofabout 8 pounds per cubic foot. Since further losses of creosote after 60 daysusually were small, it is not unlikely that the 50 percent figure is fairlyrepresentative of the amount of low residue creosote often lost from the outerzones of treated wood after several years of service. Creosote was chosenfor the weathering indicator because it was the most widely used oil preserva-tive and was the only standard preservative for which weathering losses canbe readily ascertained by weighing.

Laboratory Weathering by Means ofA Rotating Wheel

General. --Most weathering procedures used by different investigators toassess the permanence of preservatives have subjected the treated blocks tovarious schedules of alternate leaching and drying. None of these specificprocedures appeared to be adequate for integration with the soil-block test,however, because of shortcomings in either speed and simplicity of opera-tion or in capacity to reveal differences in permanence. Nevertheless,limited trials of a modification of one method used by Gillander et al (12)were made. These investigators placed the blocks on a wheel that rotated,passing the blocks successively through running water, an air steam for dry-ing and a hood in which they were exposed to radiant heat at approximately62 ° C.

In the trials connected with the present study, two motor driven bicyclewheels (11.5-inch radius), each with 72 clamps for holding test blocks ontheir outer circumference, were placed upright in a tank of running water.(See figure 8) The portion of a wheel submerged at one time could be changedby increasing or decreasing the amount of water in the tank. The water hada pH of approximately 7 and a temperature of approximately 12 ° C. , and itwas replenished at the rate of one liter per minute. The wheels were rotatedat a speed of one cycle every 24 hours. As the blocks emerged from thewater, they passed under an ultraviolet lamp or lamps that imparted a maxi-mum temperature at the surface of the blocks of 35 to 38° C. The apparatusthus provided automatic and precisely controlled cyclic wetting, heating, and.drying of the test blocks.

First trial. --During the first trial with the "weathering wheel" approximately40 percent of the blocks were submerged at one time, causing each block to

Rept. No. 2 114 -85-

be leached 10 of the 24 hours of a cycle. In this trial, one ultra-violet lightwas used. The blocks were treated with 8 pounds of a low residue creosoteand removed from the wheel at weekly intervals. The approximate loss ofcreosote during 7, 14, 21, and 28 revolutions (or days) was 27, 36, 40, and44 percent, respectively. None of the blocks were subsequently attacked byLentinus lepideus in the bioassay phase of the appraisal.

Second trial. --During the second trial, the leaching time was reduced to 7hours daily and another lamp was added at the opposite side of the wheels todouble drying time at 35° to 38° C.

The test blocks were treated with various amounts of a low residue coal-tarcreosote, a pentachlorophenol (5 percent by weight) petroleum solution, orzinc chloride. Eight blocks with each retention of three preservatives wereremoved after 7, 14, 21, and 28 cycles and bioassayed. Lent. lepideus was used for testing blocks treated with creosote, L. trabea for pentachloro-phenol, and P. monticola for zinc chloride.

The results of wheel-weathering trial No. 2 are shown in tables 45, 46, 47,and 48. Table 45 indicates that the longer drying time coupled with a longerexposure to elevated temperatures compared with trial No. 1 had increasedthe loss of creosote. The loss from an 8-pound treatment during 28 cyclesor days increased from 44 to 56 percent. The influence of increasing expo-sure to the weathering conditions of trial 2 itself is shown by progressivelosses of creosote and increases in threshold retentions or amounts of decayfor this and the other preservatives. Thus the loss from an 8-pound creo-sote treatment increased from 40 to 56 percent (table 45) and the thresholdfrom 5 to 8.6 pounds after 7 and 28 days, respectively (table 46). Thethreshold of a pentachlorophenol solution was between 2.0 and 3.9 poundsafter 7 days of weathering, but increased to 6.5 pounds after 28 days (table47). No threshold was obtained for zinc chloride since blocks treated withapproximately 4 pounds, the highest retention used, were decayed (table 48).

Discussion. --The results of these two trials indicate that the weatheringwheel is capable of removing appreciable amounts of preservative from testblocks. Under the conditions brought to bear, it apparently would take lessthan half the time to produce the same total losses of creosote that are ob-tained in 60 days of outdoor weathering in the summer at Madison. It ap-peared possible to shorten the weathering time even more by further increas-ing the drying temperature and decreasing the time in the leach water.Trials of the weathering wheel were discontinued, however, because of cer-tain practical limitations and possible sources of error. In any standardmethod, for instance, distilled rather than tap water undoubtedly would berequired for leaching; furthermore, separate tanks would seem necessary

Rept. No. 2 114 -86-GPO 813057-6

for tests of different preservatives or of different retentions of a given pre-servative. The large quantities of distilled water that would be required,coupled with the need of individual wheels for each particular treatment,made it seem advisable to seek a simpler and less costly method of weather-ing.

Preliminary Trials of CyclicLeaching and Drying

An account of trials of artificial weathering that led to the development ofthe standard weathering box has been published (7). In these trials blockswere subjected to a 24-hour cycle consisting of a short leaching phase (1 to8 hours) and a long drying phase -- with heat in the latter. The details ofthe trials appear in the publication so that only a summary of the informationis given here.

The major observations and conclusions were:

Amounts of drying and leaching. --A 3-week leaching phase alone resulted ina lower rather than an increased threshold for creosote. The reason for thishas not been fully understood (4). Therefore, subjection of the blocks strictlyto leaching did not provide adequate weathering. In subsequent trials, use ofboth a drying and leaching phase brought about increases in the threshold andthus eliminated the difficulty. In these cases the period of leaching was 1 to8 hours in the 24-hour cycle.

Rate of air exchange in the drying phase. --A standard weathering proceduremust provide a suitably controlled rate of access of fresh air to test blocks.The rate of exchange does not appear to be critical so long as it is rapidenough to dry the test blocks within about 4 hours after terminating the leach-ing phase. The forced renewal and circulation of air in the dry phase ofweathering produced a considerably more rapid loss of a low residue creo-sote from the test blocks than Was obtained in an ordinary oven with littleprovision for air exchange. Moreover, for the same total loss of creosoteproduced by artificial weathering, the initial retention (threshold) needed toprevent decay was greater when the air exchange was rapid than when it wasslow.

Temperature in the drying phase. --Comparatively mild drying temperatures,in the range of 120° to 140° F., seemed adequate to characterize the perman-ence of a creosote within a reasonably short time. With 2 hours of dailyleaching, losses of a low residue creosote obtained in 7 days at a dryingtemperature of 140° F. were practically the same as those obtained in 14

Rept . No. 2114 -87-

days with the drying temperature reduced to 120° F. Moreover, the thresholdretentions obtained with these two weathering conditions were essentially thesame, 8 to 10 pounds, and were similar to those obtained from 60 days of out-door weathering during the summer in Madison. These findings indicated thata temperature of 140° F. had not adversely affected the creosote. However,since 120° F. gave sufficiently rapid weathering and was less likely to causea typical loss of some other preservatives, this lower temperature was con-sidered more appropriate as a standard for general testing.

Semiautomatic weathering in a box heated by hot air. --To provide the indi-cated desirable weathering conditions with respect to alternate phases of dry-ing and leaching, rate of air exchange, and temperature on drying, and topreclude exchange of chemicals among blocks with different treatments, aweathering box with controlled hot air heating was found adequate (7). Usingthis weathering box, the treated blocks were carried at all times in glassbeakers. Weathering with this equipment was only semiautomatic since itrequired handling of beakers between the leaching and drying phases, andmanual introduction and removal of the leach water. However, these proced-ures in themselves were not sufficiently troublesome to require a modifica-tion of the method.

The hot-air weathering box offered virtually complete freedom from the inter-change of preservative materials between blocks in different treatment groups.In addition, results obtained with it indicated that the rate of access of freshair to the blocks during drying did not need to be controlled precisely. Thiswas indicated by the similarity of creosote losses and threshold retentionsbetween blocks weathered in a circulating oven or in the weathering box whenboth were maintained at the same temperature.

Adoption of Hot Water for Heatingthe Weathering Box

After some use of the weathering box in which hot air was used as the heat-ing medium, it was felt that hot water would provide more uniform controlof temperature, particularly by making the block temperature less subject tovariations from the influence of outside conditions. Such a box was construc-ted, therefore, and constitutes the present standard weathering apparatuswhich is described in "Tentative method of testing wood preservatives bylaboratory soil-block cultures. " (ASTM Designation: D1413-56T. 1956)

Results obtained with the two boxes were found to be similar if the beakerswere removed from the box and held at room temperature during the leach-ing phase (current standard procedure) rather than left inside the box at an

Rept. No. 2114 -88-

elevated temperature. With the beakers inside the box, the leach water inthe beakers tended to reach considerably higher temperatures with waterrather than air as the surrounding heating medium. With air, this tempera-ture of the leach water in the beakers raised slowly to approximately thatof the needed drying temperature (120° F.). With heated water, the leachwater in the beakers rather quickly attained a temperature of about 140° F. ,which was the water temperature needed to maintain the blocks at 120° F. ,during the drying phase.

Studies to Refine the Weathering Procedure

Influence of leaching temperature. --In 1954 this investigator it was reportedthat there was little difference in thresholds of a low-residue creosote, coppernaphthenate, or pentachlorophenol in petroleum when test blocks were leachedin water at room temperature or at 120° F. , by keeping the beakers in theweathering box during this phase of the weathering. This comparison wasmade when using the hot-air weathering box and a 2-hour leach period. Withthe adoption of the hot water weathering box, it became necessary to ascer-tain whether the higher temperature (140° F. ) reached by leach water in thebox would make it preferable to do the leaching outside the box.

Comparisons were again made of blocks treated with a low-residue coal-tarcreosote, copper naphthenate, and pentachlorophenol in petroleum, and inaddition with copperized chromated zinc chloride, using leach water at roomtemperature and 140° F.

The results of these comparisons are shown in table 49. They indicate thatsimilar thresholds of creosote and pentachlorophenol were obtained at bothleaching temperatures. However, the threshold of copper naphthenate-petroleum was slightly greater and that of copperized chromated zinc chlorideconsiderably greater with the higher temperature of the leach water. Theseresults and the fact that a 140° F. temperature might lead to a typical lossof some preservatives led to a decision to do the leaching at room tempera-ture.

Manner of applying the leach water . --Saturation of the blocks is never at-tained by merely submerging them in water for 2 hours. It, was thought,therefore, that saturation of the blocks at the start of leaching might hastenlosses of soluble materials and better screen the preservatives for leach-ability. With this in view, comparisons were made between treated blocksthat were either dry or saturated with water under reduced pressure beforebeing placed in the leach water.

Rept. No. 2114 -89-

Results of these comparisons are shown in tables 50 and 51. They indicatethat the thresholds of 'creosote and pentachlorophenol were similar whetheror not the treated blocks were saturated with water at the start of the leach-ing phase. However, the thresholds for copper naphthenate and a proprietarysalt were somewhat higher when the blocks were initially saturated with water.Furthermore, the threshold for copperized chromated zinc chloride wasgreatly increased by saturating the blocks, and similar results seemed to betrue for zinc chloride.

It appeared from these results that saturation of the blocks with water at thestart of the leaching phase has little effect on the threshold of oil-type pre-servatives, but causes excessive losses of some waterborne preservatives.Until better guiding data on losses of waterborne preservatives under fieldconditions are available, it seemed best to forego saturation of blocks at thestart of the leaching phase.

Interval between treating and start of artificial weathering. --It is generallyagreed that the toluene used as a diluent for testing oil-type preservativesshould be allowed to evaporate from the treated blocks before the start ofartificial weathering. Snoke' s use of radio-active toluene discussed earlierin this report indicated that all toluene is gone from creosote-treated blocksin 7 days when kept at 80° F. With the present standard procedure (ASTMDesignation: D1413-56T, 1956), it is suggested that artificial weathering bestarted with the 22-hour period of the dry phase at 120° F. This shouldeliminate much of the toluene. There seems to be no need of more time forthe toluene to evaporate, based on tests indicating that the threshold valueof a coal-tar creosote or a pentachlorophenol solution is about the same whenweathering was started 3 days and 14 days after treatment.

In the case of waterborne salts, it has been assumed that the interval betweentreating and the start of the leach phase should permit drying of the blocks toapproximately 12 percent moisture. This is accomplished in the 22-hour dry-ing phase at 120° F. at the start of weathering...

Appraisal of the Severity ofLaboratory Weathering

As mentioned previously, the severity of laboratory weathering was gaged toapproximate the reduction in effectiveness of a low-residue coal-tar creosoteduring 60 days of outdoor weathering of test blocks in the summer at Madison.

6–It is the practice after treatments with waterborne salts to dry the blocks to

approximately 12 percent moisture at a temperature no greater than 80° F.,before starting artificial weathering.

Rept. No. 2114 -90-

This outdoor weathering included spraying the blocks with water for 5 minutesthree times. a week except when a heavy rain occurred on these days. Thethresholds of such a creosote have stayed between 7 to 9 pounds even whenoutdoor weathering was done in different seasons (6). Thus, it seemed prob-able that several schedules of cyclic wetting and drying in laboratory weather-ing might give thresholds within this range for a similar creosote. Testswere made, therefore, of a sample of low-residue coal-tar creosote, as wellas other creosotes and preservatives, to ascertain how nearly the thresholdsobtained after a 14-day laboratory weathering schedule would approximatethose obtained in outdoor weathering.

The preservatives tested were low, medium, and high-residue coal-tarcreosotes, coke-oven and vertical retort tar English creosotes, a penta-chlorophenol-petroleum solution, a copper naphthenate-petroleum solution,a proprietary salt, copperized chromated zinc chloride, and zinc chloride.

The results, shown in tables 52 and 53, indicate that laboratory weatheringwas somewhat more severe than outdoor weathering on the low-residue coal-tar creosote,-7 the two English creosotes, and the pentachlorophenol solution,whereas the reverse was true for the medium and high-residue creosotes.The two types of weathering were approximately equal in their effect on thecopper naphthenate and the proprietary salt. The other salts, copperizedchromated zinc chloride and zinc chloride, were affected more by outdoorthan laboratory weathering, the former particularly so.

It would appear that for creosotes and oil-borne preservatives in whichlosses are mainly through volatilization, the severity of laboratory weather-ing approximated that of the outdoor weathering. With waterborne preserva-tives, the outdoor weathering apparently caused considerably more leachingin some cases than the laboratory method. Judging from the apparent heavyleaching of zinc chloride (table 52: threshold greater than 4.2 pounds percubic foot), however, it seems doubtful that the severity of laboratoryweathering should be increased for salts. But if this ultimately is wanted,it can be accomplished by giving more emphasis to the leaching phase.Supplementary tests show that heating the leach water and saturating theblocks at the start of the leach phase will increase the loss of salt preserva-tives.

7Laboratory weathering was shown to be somewhat more severe than out-

door weathering on another low-residue coal-tar creosote, and two lowtemperature tar creosotes.

Rept. No. 2 114 -91-

Modifications of the 14-Day ContinuousCyclic Weathering

In the preceding tests, the schedule generally used in developing the weather-ing box consisted of 14 daily cycles of 22 hours drying at 120° F. and 2 hoursleaching in water at room temperature or in water gradually heated to 12 5° F.(where hot air was the heating medium). Such a schedule had the obvious dis-advantage of requiring an operator' s attention on two Saturdays and Sundays.Tests were made, therefore, to determine if threshold values would be sig-nificantly changed by interrupting the continuous cyclic schedule on weekendsthrough continuous drying or leaching during these periods.

The principal features of the different weathering schedules considered aregiven in table 54. Schedule I followed the usual pattern of 14 days of cyclicweathering without interruption. Schedules II, III, and IV utilized continuousdrying on weekends, and Schedule V continuous leaching. The test blockswere treated with a low-residue coal-tar creosote, pentachlorophenol-petroleum, copper naphthenate-petroleum, and copperized chromated zincchloride.

The results are shown in table 55. The thresholds of none of the oil pre-servatives were materially changed by the modified weathering schedulesincorporating continuous drying on the weekends (Schedules II, III, and IV).However, where a 72-hour leach was used on the weekend (Schedule V) thethresholds of these oil preservatives were somewhat reduced, and that ofthe waterborne preservative, copperized chromated zinc chloride, was in-creased. Omitting the number of 2-hour cyclic leach periods (Schedules IIand IV) tended to lower the threshold of copperized chromated zinc chloride.

On the basis of these results, it appeared that thresholds of oil- and water-borne-preservatives of the type considered here are not likely to be changedmaterially by substituting continuous drying at 120° F. for the cyclic weather.ing on weekends. However, continuous leaching over a weekend would tendto lower the thresholds of oil preservatives and raise those of the salts.

Reproducibility of the Laboratory Weathering Phase as Indicated by Bioassay

The ultimate goal in laboratory weathering has been to develop a procedurewhich would give a repeatable reduction in effectiveness of a preservative,as determined by bioassay. To observe whether this was being accom-plished, a number of preservatives were tested three or more times atthree main stages in improving or working out schedules for the use of theweathering box.

Rept. No. 2 114 -92-

The weathering involved in each case was a preliminary 22- to 24-hour dry-ing period and daily cycles of 2 hours leaching and 22 hours drying. Thedrying temperature was always 120° F.

The three weathering schedules were:

1. Fourteen continuous daily cycles of 2 hours leaching and 22 hours drying.During leaching the blocks were left in the weathering box heated by hot air,and the temperature of the leach water gradually reached 125° F.

2. Nine cycles of 2 hours leaching and 22 hours drying, with 48 hours of dry-ing at the end of the fourth and ninth cycles. During leaching the blocks wereremoved from the weathering box, which in this case was heated by hot water,and the temperature of the leach water approximated that of the room (68° to80° F.).

3. Seven cycles of 2 hours leaching and 22 hours drying, with 72 hours leach-ing at room temperature between the third and fourth cycles.

The results of the comparisons (table 56, 57, 58, and 59), indicate that thereis a comparatively high degree of repeatability in the threshold of a preserva-tive when the test blocks are exposed to any one of the selected weatheringschedules.

Rept. No. 2 114 -93-

Table 45.--Weathering losses of a low residue coal-tar creosotefrom blocks exposed to cyclic wetting and drying on the rotating wheel (trial No. 2)1

Weathering : Loss2- of creosote from blocks treated tocycles (or days): the'indicated retentions

. (lb. per cu. ft.) of creosote

: 2.2 : 4.1 : 6.3 : 8.4 : 10.2 : 12.1: : : : : •

Number :Percent:Percent:Percent:Percent:Percent:Percent. . . . . .

7 : 46 : 42 : 4o : 4o : 37 • 35. . . . . .

14 : 52 : 5o : 49 : 48 : 46 : 46•

21 : 55 : 53 53 : 52 • 51 • 5o

28 56 57 56 : 56 : 55 • 55

1-Leaching 7 hours in running tap water, drying 17 hours with

temperatures of 35-38° C.2-Average loss from 8 blocks.

Table 46.--Weight losses in creosote-treated and wheel-weathered blocks whensubjected to decay by Lentinus lepideus trial No.

Weathering:Weight loss in blocks treated to the indicated:Retentions:Estimated2

cycles : retentions (lb. per cu. ft.) of creosote : tested :threshold2.

(or days) : : nearest :2.2 : 4.1 : 6.3 : 8.4 : 10.2 : 12.1 :threshold :

Number :Percent:Percent:Percent:Percent:Percent:Percent: Lb. per : Lb. per

•.

.

•.

.

:

.

•

: : : cu. ft. : cu. ft.

7 : 11.9. 4.0 : (0.2) : (0.7) : (1.1) : (1.7) : 4.1-6.3 : 5.0

14 : 16.2. 9.6 : 3.9 : (1.o) : (1.5) : (1.8) : 6.3-8.4 : 7.3. . : .

21 : 23.2 : 11.5 : 7.0 : (1.2) : (1.7) : (1.9) : 6.3-8.4 : 8.2

28 : 29.5 : 18.2 : 11.5 : 2.2 : (1.7) : (2.3) : 8.4-10.2 : 8.6

1-Leaching 7 hours in running tap water, drying 17 hours with temperature of

35-38° C.

2Each weight loss is an average of 8 blocks. Weight losses in parentheses areattributed to factors other than decay.

Threshold for the conditions of the test estimated by the method of intersect-ing lines.

Rept. No. 2114 -94- GPO 8 t 3057-.8

Table 47.--Weight losses in pentachlorophenol-treated and wheel-weathered blocks when subjected to decay by Lenzites trabea (trial No. 2)1

Weathering: Weight loss in blocks treated to the :Retentions:Estimated4

cycles : indicated retentions (lb. per cu. ft.) : tested :threshold-

(or days) : of pentachlorophenol-petroleuml : nearest : : threshold:2.0 : 3.9 : 6.2 : 8.1 : 10.3 : 12.5 :

Number :Percent:Percent:Percent:Percent:Percent:Percent: Lb. per : Lb. per: : : cu. ft. : cu. ft.

• - • • • :. . . : . . .

7 : 14.5 : (1.5) : (2.2) : (2.4) : (3.0) : (3.4) : 2.0-3.9 •

14 : 17.4. 2.5 : (2.3) : (2.6) : (2.9) : (3.5) : 3.9-6.2 : 4.1

21 : 27.2 : 10.2 : (2.5) • (3.0) • (3.5) : (3.9) • 3.9-6.2 : 5.1

28 : 41.7 : 17.4 : 4.1 : (3.1) : (3.4) : (4.o) : 6.2-8.1 : 6.5

1-Leaching 7 hours in running tap water; drying 17 hours with temperature of

35-38° c.

2Each weight loss is an average of 8 blocks. Weight losses in parentheses areattributed to factors other than decay.

-Five percent pentachlorophenol in a light naphthenic-base petroleum oil.

-Threshold for the conditions of the test estimated by the method of intersect-ing lines when data was sufficient to permit it.

Table 48.--Weight losses in zinc chloride treated and wheel-weathered blocks when subjected to decay by Poriamonticola (trial No. 2)1

Weathering:Weight loss in blocks treated to the indicated :Retentionscycles : retentions (lb. per cu. ft.) of zinc chloride : tested

(or days) : : nearest1.0 : 1.6 : 2.2 : 2.8 : 3.4 : 3.9 : threshold

Number :Percent:Percent:Percent:Percent:Percent:Percent: Lb. per: cu. ft.

7 : 52.4 : 51.6 : 48.9. 38.2. 22.8. 15.7. > 3.9

14 : 55.6 : 54.2. 50.5 : 48.9 : 47.o : 40.2 : > 3.9

21 : 56.1. 55.4 : 55.3 : 52.6 : 50.2. 48.9. > 3.9

28 : 57.2 : 53.2 : 55.6. 54.8 : 52.6 : 56.o : > 3.9

1-Leaching 7 hours in running tap water; drying 17 hours with tem-

perature of 35-38° c.2Each weight loss is an average of 8 blocks.

Rept. No. 2114 -95-

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Rept . No. 2114 -96-

Table 50.--Differences in decay and threshold associated with oil-type preservatives when starting the leaching phase of weather-ing1 with dry blocks and with saturated blocks

2

Preservative retention: Weight losses- in the decay test

:Blocks initially dry:Blocks initially saturated

: when leached when leached

Lb. per cu. ft.

Percent

Percent

LOW RESIDUE COAL-TAR CREOSOTE TESTED BY LENT. LEPIDEUS

3.9 20.2 14.05.8 10.7 8.97.9 2.2 2.19 .8. (.9) (1.0)11.9 (1.2) (1.4)

PENTACHLOROPEENOL- PETROLEUM TESTED BY L. TRABEA

2.0 29.1 20.43.6 15.4 12.95.o 7.2 5.46.o (.6) (.5)7.8 (.9) (.7)

COPPER NAPHTBENATE-PETROLEUM TESTED BY P. MONTICOLA

4.1 17.5 21.16.o 9.2 11.28.o (1.0) 2.2

10.2 (1.2) (1.1)12.4 (1.5) (1.6)

2-Fourteen cycles: 22 hours dryinon two Saturdays and Sundays.

-Each weight loss is an averageparentheses not attributed to

g at 120° F. with 2-hour leach except

of 6 blocks. Weight losses indecay.

Rept. No. 2114 -97-

Table 51.--Differences in decay and threshold associated with salt-typepreservatives when starting the leaching phase of weather-ing1.- with dry blocks and with saturated blocks

Preservative retention: Weight losses 2- in the decay test

:Blocks initially dry:Blocks initially saturatedwhen leached when leached

Lb. per cu. ft. Percent Percent

A PROPRIETARY SALT TESTED BY P. MONTICOLA

0.1.15.20•25.35•45

12.2(.3)(.2)(.4)(.3)(.2)

30.46.3(.1)(.3)(.2)(.3)

COPPERIZED CBROMATED ZINC CHLORIDE TESTED BY P. MONTICOLA

.4 45.6 55.o

.7 12.1 48.2

1.0 2.5 43.7

1.5 (.6) 35.1

2.0 (.7) 7.6

2.5 (.9) 2.0

ZINC CHLORIDE TESTED BY P. MONTICOLA

.5 57.2 57.2

1.0 55.0 58.0

2.0 44.4 56.4

3.0 38.0 55.8

4.1 32.3 54.7

5.0 20.1 50.3

1Fourteen cycles: 22 hours drying at 120° F. with 2-hour leach except

on two Saturdays and Sundays.2Each weight loss is an average of 6 blocks. Weight losses in

parentheses are not attributed to decay.

Rept. No. 2114 -98-

Table 52.--Comparison of the effects of laboratory-- and outdoor weathering on2 creosoteeg

Preservative:Losses of creosote:Losses during the :Retentions tested nearestretention at: during weathering: decay test.1 after: threshold and indicated

treatment : : weathering : threshold:Outdoor:Laboratory:

:Outdoor:Laboratory:

Lb. per :Percent: Percent :Percent: Percent : Lb. per cu. ft.

cu. ft, :

LOW RESIDUE COAL-TAR CREOSOTE

4.3 : 50 : 56 : 9.0 : 13.0 :Outdoor 6.2-8.2 (8.1)

6.2 : 48 : 56 : 5.6 : 7.6 :Laboratory 8.2-10.2 (8.9)

8.2 •

. 48 : 57 : (.6) : 2.6 :

10.2 : 47 : 57 : (1.0) : (1.0) :

12.3 •

. 46 : 57 : (1.2) : (1.4) :

MEDIUM RESIDUE COAL-TAR CREOSOTE

4.3 : 42 : 46 : 13.1 : 8.6 :Outdoor 8.2-10.2 (8.4)

6.2 : 39 : 47 : 7.9 : 4.5 :Laboratory 6.2-8.2 (7.7)

8.2 : 40 : 47 : 1.8 : • (.5) :10.2 : 39 : 47 : (1.0) : (.9) :

12.3 : 37 • 47 : (1.5) : (1.3) :

HIGH RESIDUE COAL-TAR CREOSOTE

4.3 : 24 : 31 : 16.2 : 6.6 :Outdoor 8.1-10.2 (9.7)

6.2 : 22 : 29 : 9.6 : 3.1 :Laboratory 6.2-8.1 (7.4)

8.1 : 22 : 30 : 5.8 : (.4) :

10.2 : 21 : 30 : (.8) : (.8) :

12.4 : 20 : 30 : (1.4) : (1.3) :

VERTICAL-RETORT-TAR CREOSOTE

4.2 : 36 : 43 : 7.1 : 11.3 :Outdoor 6.1-8.1 (6.8)

6.1 : 34 : 41 : 2.5 : 7.4 :Laboratory 8.1-10.0 (9.4)8.1 : 33 : 41 : (1.0) : 3.9 :

10.0 : 33 : 40 : (1.5) : (1.6) :

12.1 : 30 : 40 : (1.7) : (1.8) :

COKE-OVEN-TAR CREOSOTE

4.2 : 51 : 57 : 7.4 : 12.8 :Outdoor 6.2-8.2 (6.8)

6.2 : 48 : 57 : 2.6 : 6.6 :Laboratory 6.2-8.2 (8.0)

8.2 : 48 : 57 : (1.2) : (1.1) :

10.2 : 46 : 57 : (1.5) : (1.6) :

12.1 : 45 : 56 : (1.6) : (1.7) :

1-Fourteen daily cycles of 2 hours leaching at roan temperature and 22 hours

drying at 120° F.

2The creosotes were not the same as those for which threshold results werepublished in 1951 (AWPA Proceedings 47:275-287).

2Each weight loss is an average of 6 blocks. Weight, losses in parenthesesnot attributed to decay. All the creosotes were tested with Lent.lepideus.

4-Threshold for the conditions of the test estimated by the method of inter-

secting lines.

Rept. No. 2114 -99-

1Table 55.--Comparieon of effects of laboratory and outdoor weathering

on oil and waterborne preservatives

Preservative retention:Losses2- in decaytest:Retentions tested nearest

at treatment : after weathering : threshold and estimated: : threshold./: Outdoor :Laboratory:

Lb. per cu. ft. : Percent : Percent : Lb. per cu. ft.

PENTACHLOROPHENOL-PETROLEUM, 11 TESTED WITH L. TRABEA

1.9 22.4 : 20.4 :Outdoor 4.0-6.2 (5.4)4.0 8.6 : 11.5 :Laboratory 6.2-8.4 (6.3)6.2 (.6) : 1.7 :8.4 (1.2) : (1.4)

10.5 (1.8) : (2.0) :

COPPER NAPHTHENATE-PETROLEUM, 11 TESTED WITH P. MONTICOLA

2.0 29.5 : 25.6 :Outdoor 8.2-10.6 (8.5)4.2 18.2 : 17.2 :Laboratory 8.2-10.6 8.6)5.9 11.1 : 12.1 :8.2 2.9 : 3.1 :

10.6 : (1.6) : (1.9) :

A PROPRIETARY SALT,1 TESTED WITH P. MONTICOLA

.1 : 20.3 : 6.7 :Outdoor 0.1-0.15

.15 (.5) • (.7) :Laboratory 0.1-0.15

.20 (.7) : (.8) :25 (.6) : (.6) :35 (.4) : (.6) :

COPPERIZED CHROMATED ZINC CHLORIDE, TESTED WITH P. MONTICOLA

5 : 55.3 • 45.5 :Outdoor >2.5

1.1 45.3 : 10.8 :Laboratory-1.6-2.0 (1.8)

1.6 20.4 : 8.9

2.0 : 16.9 : (.7) :

2.5 14.2 : (1.0) :

ZINC CHLORIDE, TESTED WITH P. MONTICOLA

.5 : 58.2 : 50.1 :Outdoor >4.21.0 : 40.6 : 45.3 :Laboratory >4.22.2 : 38.9 : 37.0 :3.o : 35.4 : 34.2 :4.2 : 37.5 : 30.6 :

1Fourteen daily cycles of 2 hours leaching at room temperature and 22

hours drying at 120° F.

2Each weight loss is an average of 6 blocks. Weight losses in paren-theses not attributed to decay.

hreshold for the conditions of the test estimated by the method ofintersecting lines.

An aromatic high-boiling petroleum containing either 5 percent penta-chlorophenol by weight or 0.5 percent copper metal.

2A salt known to have little solubility in water.

Rept. No. 2114 -100-

Table 54.--Schedules considered in attempting to avoid weekend attention tothe weathering

: drying at :: 120° F. :

leachingtime and : time and

:temperature : temperature

I : 22 hours : 14 continuous cycles: 2 hours: 330 hours : 28 hours: leaching (125° F.) and 22

hours drying.(120° F.) : (125° F.)

II : 24 hours : 9 cycles: 2 hours leaching : 318 hours : 18 hours: (125° F.) and 22 hours drying:

with 48 hours drying at end :(120° F.) : (125° F.)

III

•: of 4th and 9th cycles.

: 64 hours : 12 cycles: 2 hours leaching 340 hours : 28 hours(125° F.) and 22 hours drying: (120° F.) : (125° F.)with a 2-hour leach plus 6 128 hours :hours drying (120° F.) and (80° F.) :64 hours drying (80° F.) at :end of 4th and 8th cycles. :

•

IV : 24 hours : 9 cycles: 2 hours leaching : 318 hours : 18 hours(72° F.) and 22 hours drying :with 48 hours drying at end :

(120° F.) : (72° F.)

of 4th and 9th cycles.• • •

V : 24 hours : 7 cycles: 2 hours leaching 178 hours : 86 hours(72° F.) and 22 hours drying : (120° F.) : (72° F.)with a 72-hour leaching •

•

: (72° F.) following 3rd cycle.:

1–Drying unless otherwise indicated was done at 120° F. Leaching temperature

given indicates maximum reached at end of leach period.

Schedule:Preliminary: Cyclic change1– :Total drying:Total

Rept. No. 2114 -101-

Table 55.--Bioanalysis of treated blocks after laboratory weathering with thedifferent schedules shown in table 54

2Preservative: Weight losses in blocks weathered : Indicated differences amongretention at: by indicated schedules :schedules in their effect ontreatment 1 : : raising the threshold

I : II : III : IV : V retention

Lb. per :Percent:Percent:Percent:Percent:Percent:cu. ft. : . •. . •

. .

LOW RESIDUE COAL-TAR CREOSOTE, TESTED BY LENT. LEPIDEUS

3.0 : 16.5 : 20.0 : 21.9 : 19.2 : 12.4 :I, II, III, IV, show no ma-

4.0 : 12.7 : 16.4 : 17.1 : 15.6 : 8.5 : terial differences but all

6.0 : 6.1 : 7.7 : 9.5 • 5.9 • (.9): had a greater effect than V

8.0 : (.8): (1.4): (1.0): (1.1): (1.2):

10.0 (.9): (1.4): (1.3): (1.2): (1.3):

PENTACHLOROPHENOL (5 PERCENT)-PETROLEUM,2 TESTED BY L. TRABEA

1.0 : 40.6 : 30.9: 42.4: 30.3 : 24.9 :I, II, III, IV show no ma-

2.0 : 27.5 : 21.5 : 25.0 : 22.6 : 18.5 : terial differences but all

4.0 : 19.2 : 14.9 : 14.5 : 15.2 : 10.4 : had a greater effect than V

6.0 : 5.1 : 4.1 : 3.8 : 3.5 • (.5):

8.0 : (.9): (1.2): (1.4): (1.1): (1.2):

COPPER NAPHTBENA1E-PETROLEUM- (0.5 PERCENT COPPER), TESTED BY P. MONTICOLA

3.0 29.9 : 32.3 : 35.6 : 33.0 : 27.8 :I, III, IV show no ma-

4.0 20.1 : 18.6 : 22.6: 25.6 : 17.6 : terial differences but all

6.0 : 13.6 : 9.5 : 11.1 : 14.9 : 8.6 : had a greater effect than V

8.0 : 3.4 : 1.6 : 3.2 : 3.1 : (.9):

10.0 : (1.6): (2.1): (1.8): (1.7): (1.9):

COPPERIZED CHROMATED ZINC CHLORIDE, TESTED BY P. MONTICOLA

.5 • 37.2 : 30.1 : 40.4 : 42.8 : 43.2 :Effect increasing somewhat

1.0 : 21.9 : 18.2 : 19.9 : 19.7 : 38.6 : from II, IV, to I, III,

1.5 : 2.0 : (.5): 1.8 : (.7) : 14.5 : with greatest in V

2.0 (.4): (.4): (.3): (.4•: 1.8 :

2.5 (.8): (.9): (.7): (1.0): (.4):

1-Groups of blocks weathered by the different schedules were treated separately,

but the average retentions varied no more than± .03 pound from those shown.

Each weight loss is an average of 6 blocks. Weight losses in parentheses arenot attributed to decay.

o. 2 fuel oil.

An aromatic high-boiling petroleum.

Rept. No. 2114 -102-GPO 8 I 3057...4

Table 56.--Comparison of weight losses and thresholds obtained in different tests in which the blocks had been subjected to nominally the same labora-tory weatherinz_-- 14 cycles of 2-hour leaching (125° F.) and 22-,hour drying (120° F.) in the weathering box

Preservative: Weight loss1- in test blocks :Retentions tested

retention : :nearest threshold: Test I : Test II : Test III: Test IV : Test V : and indicated: : : : : threshold?

Lb. per : Percent : Percent : Percent : Percent : Percent : Lb. per cu. ft. cu. ft. : : : :

LOW RESIDUE COAL-TAR CREOSOTE, TESTED BY LENT. LEPIDEUS

2.2 : 29.1 24.0 : 26.5 : 30.6 : 20.5 : I. 8-10 (8.4)

4.1 : 17.9 15.6 : 16.8 : 20.7 : 12.4 : II. 8-10 (8.6)

6.2 11.3 : 9.5 : 10.4 : 10.1 : 7.6 : III. 8-10 (8.5)

8.0 : 2.5 • 2.6 : 2.6 : 2:0 : 2.7 : IV. 8-10 (8.5)

10.1 (.7) • (.9) : (.9) : (.6) : (.9) : v. 8-10 (8.7)

PENTACHLOROPHENOL (5 PERCENT) IN 3285 PETROLEUM, TESTED BY L. TRABEA

2.0 : 34.9 : 29.1 : 39.2 : 35.0 : 24.8 : I. 6-8 (7.2)

3.9 : 19.2 17.2 : 27.6 : 19.4 : 14.6 : II. 6-8 (7.5)

6.o 7.6 : 7.5 : 12.2 : 7.o : 7.2. : III. 6-8 (7.6)

8.o : (1.0) : (.9) : (1.2) (1.2) (1.1) : Iv. 6-8 (7.1)10.2 : (1.5) : (1.4) : (1.7).: (1.6) (1.6) : v. 6-8 (7.6)

1-Each weight loss is an average of 6 blocks. Weight losses in parentheses are

attributed to factors other than decay.

-The threshold for the condition of the test was estimated by the method ofintersecting lines.

Rept. No. 2114 -103-

Table 57.--Comparison of weight losses and thresholds obtained in different tests in which the blocks had been subjected to nominally the same laboratorj weathering -- 9 cycles of 2-hour leaching (roomtemperature) and 22-hour drying (120° F.) in the weathering boxwith 48-hour drying (120° F.) at the end of the 4th and 5th

2E122

Preservative:retention :

: Test I : Test II : Test III: Test IV

Lb. per : Percent : Percent : Percent : Percent cu. ft.

:Retentions tested nearest: threshold and indicated

threshold?

: Lb. per cu. ft.

Weight losses in test blocks1-

A LOW RESIDUE COAL-TAR CREOSOTE TESTED BY, LENT. LEPIDEUS

2.9 15.0 17.6 : 22.6 : 14.6 : I. 7.4-8.2 (8.2)4.2 10.2 12.2 : 18.1 : 9.7 : II. 7.4-8.2 (7.8)5.0 8.9 11.4 : 13.9 : 8.6 : III. 7.4-8.2 (7.6)6.1 6.7 6.6 : 8.5 : 7.3 : Iv. 7.4-8.2 (8.2)7.4 2.1 : 2.0 : 2.0 : 3.08.2 (1.0) : (.9) : (1.1) : (1.2) :9.2 (1.2) : (1.1) : (1.4) : (1.3) :

10.5 (1.2) : (1.3) : (1.4) : (1.4) :

PENTACHLOROPHENOL (5 PERCENT) IN PETROLEUM 5012, TESTED BY L. TRABEA

2.1 29.8 : 26.2 : 28.5 : 30.1 : I. 6.3-7:4 (6.4)3.0 19.5 : 11.2 15.0 15.6 : II. 6.3-7.4 (6.3)4.2 14.6 : 7.7 10.6 : 11.3 : III. 6.3-7.4 (6.6)5.0 9.2 : 5.1 7.4 : 7.4 : Iv. 6.3-7.4 (6.7)6.3 1.6 : 1.0 : 2.4 : 2.57.4 : (1.0) : (1.0) : (1.2) : (1.3) :8.7 : (1.3) : (1.4) : (1.4) : (1.4) :

COPPERTZED CHROMATED ZINC CHLORIDE TESTED BY P. MONTICOLA

.4 : 44.2 : 47.6 : 40.1 42.8 : I. 1.0-1.4

.7 : 39.4 : 40.2 : 39.4 38.9 : II. 1.0-1.41.0 : 7.8 : 5.9 : 4.7 7.8 : III. 1.0-1.41.4 : (.5) • (.7) • (.4) : (.5) : IV. 1.0-1.41.8 : (.8) : (.9) • (.7) : (.8) :

2.2 : (1.4) : (1.3) : (1.2) : (1.4) :

1-Each weight loss is an average value for 6 blocks. Weight losses in paren-

theses attributed to factors other than decay.

2The threshold for the condition of the test was estimated by the method ofintersecting lines. In some cases the data did not permit this to be done.

Rept. No. 2114 -104-

Table 58.--Comparison of weight losses and thresholds obtained indifferent tests in which the blocks had been subjected to nominally the same laboratory weathering -- 9 cyclesof 2 hours leaching (room temperature) and 22 hoursdrying (120° F.) in the weathering box with 48 hours drying (120° F.) at the end of the 4th and 5th cycle!

Preservative: Weight losses2- in blocks :Retentions tested nearest

retention : in indicated tests : threshold and indi-: : cated threshold.: Test I : Test II : Test III:

122,2LI : Percent : Percent : Percent : Lb. per cu. ft. cu. ft. .

LOW RESIDUE CREOSOTE TESTED BY LENT. LEPIDEUS

0 45.o : 49.6 : 42.3 : I. 6.8-8.2 (7.5)4.o 10.2 : 7.9 : 9.9 • II. 6.8-8.2 (7.7)5.4 6.4 : 5.8 : 6.8 : III. 6.8-8.2 (7.5)6.8 2.6 : 3.o : 2.5 :8.2 (1.0) : (1.1) : (1.1) :

10.3 (1.5) : (1.5) : (1.5)

PENTACHLOROPHENOL (5 PERCENT) IN A HIGH-BOILINGPETROLEUM TESTED BY L. TRABEA

o •• 59.9 : 61.4 : 56.7 : 1. 3.8-5.o (4.8)2.8 •. 10.6 : 14.6 : 9.4 : II. 3.8-5.o (4.9)3.8 •. 5.5 : 8.1 : 5.1 : III. 3.8-5.o (4.8)

••

(.7) : (.9) : (.4)6.0.7 •. (.8) : (.8) : (.6) :

8.5 .• (.9) • (.9) : (.7) :

COPPERIZED CHROMATID ZINC CHLORIDE TESTED BY P. MONTICOLA

o -. 52.5 : 56.7 , 53.5 : I. 1.0-1.5.52 •. 43.3 : 43.7 : 40.8 : II. 1.0-1.5

1.0 •. 6.2 : 4.4 : 4.5 : III. 1.0-1.51.5 : (.5) : (.8) : (.9)2.0 •. (1.0) : (1.2) : (1.2) :

2.6 •. (2.0) : (2.1) : (2.2) :

ZINC CHLORIDE TESTED BY P. MONTICOLA

0 53.3 • 55.1 : 54.7 : 1. >4.21.0 52.0 : 52.7 : 53.4 : II. >4.21.5 51.4 : 54.8 : 54.3 : III. >4.22.1 51.1 : 55.2 : 50.1 :2.7 50.1 : 52.8 : 48.64.2 48.6 : 46.8 : 48.2 :

-1-For comparative effects of the 2 weathering schedules, results inthis table can be compared directly with those in table 59 sincethe same preservatives were used.

2-Each weight loss is an average of 6 blocks. Weight losses in

parentheses are attributed to factors other than decay.

2The threshold for the condition of the test was estimated by themethod of intersecting lines. In same cases the data did notpermit this to be done.

Rept. No. 2114 -105 -

Table 59.--Comparison of weight losses and thresholds obtained in different tests in which the blocks had been subjected to nominally the same laboratory weathering -- 7 cycles of 2-hour leaching (room temperature) and 22-hour drying(120° F.) in the weathering box with a 72-hour leachingat the end of the 3rd cycle

Preservative: Weight losses2- in blocks in :Retentions tested nearest

retention : the indicated separate tests: threshold and estimatedthreshold.

: Test I : Test II : Test III:

Lb. per : Percent : Percent : Percent : Lb. per cur ft. cu. ft. :

LOW RESIDUE CREOSOTE TESTED BY LENT. LEPIDEUS

0 : 45.5 : 48.9 : 42.4 : I. 5.4-6.8 (6.o)4.o 4.4 : 5.9 : 5.9 : II. 5.4-6.8 (5.9)5.4 1.7 : 2.0 : 2.4 : III. 5.4-6.8 (5.9)6.8 (.9) : (1.0) : (1.2) :8.2 : (1.1) : (1.2) : (1.1) :

10.3 : (1.6) : (1.3) : (1.5) :

PENTACHLOROPHENOL (5 PERCENT) IN A HIGH-BOILINGPETROLEUM TESTED BY L. TRABEA

o 60.8 : 65.4 : 58.2 : I. 3.8-5.o (4.8)2.8 7.1 : 6.2 : 8.4 : II. 3.8-5.o (4.9)3.8 3.8 : 3.7 : 3.6 : III. 3.8-5.0 (4.5)5.o (.7) • (.8) • (.5)6.7 (.7) : (.8) • (.9) •8.5 : (1.1) : (1.2) : (1.1) :

COPPERIZED CBROMATED ZINC CHLORIDE TESTED BY P. MONTICOIA

0 53.8 : 55.2 : 53.7 : I. 1.5-2.0.52 : 48.2 : 49.7 46.3 : II. 1.5-2.0

1.0 : 41.0 : 37.3 : 41.5 : III. 1.5-2.01.5 4.1 : 5.4 : 5.1 :2.0 (.7) : (.4) : (.5) :2.6 (.5) : (.5) • (.5) •

ZINC CHLORIDE TESTED BY P. MONTICOLA

o •. 52.4 : 56.1 : 54.o : I. >4.21.0 •. 51.2 : 53.9 : 50.4 : II. >4.21.5 •. 51.5 : 54.3 : 51.5 : III. >4.22.1 53.o : 53.4 : 53.5 •2.7 •. 50.3 : 53.1 : 52.4 :4.2 •. 51.1 : 50.2 : 50.6 :

1-For comparative effects of 2 weathering schedules, results in this

table can be compared directly with those in table 58, since thesame preservatives were used.

2-Each weight loss is an average for 6 blocks. Weight losses in

parentheses are attributed to factors other than decay.

-The threshold for the condition of the test was estimated by themethod of intersecting lines. In some cases the data did notpermit this to be done.

Rept. No. 2114 -106 -

Figure 8. --Rotating weathering wheel.

R.ept. No. 2.114 -107-

DIFFERENCES AMONG TEST FUNGI IN THEIR TOLERANCE OF

PRESERVATIVES WHEN APPRAISED BY THE SOIL-BLOCK METHOD

It is expected that eventually the tolerances of many wood-destroying fungito several types of preservatives will be determined by the soil-block method.At present this is being accomplished gradually by including fungi other thanthose called for by the standard method in various tests. Information aboutthe tolerances of a variety of selected fungi, as well as of different isolatesof a particular species of fungus, are needed as a guide to the most suitablecultures to use for general or special appraisals of preservatives. In thefollowing observations, differences among a number of fungi in their abilityto attack blocks treated with a given preservative are considered. Fungi notregularly used in the soil-block test were generally selected for the frequencywith which they have been found in treated wood, especially wood with a pre-servative of the same type as that under consideration, or for their generalimportance as wood destroyers.

Tolerances to Copper Naphthenate

A. Carried in an Aromatic High-Boiling Petroleum

Eleven species of fungi, not heretofore used in the soil-block method of test-ing, were evaluated for their respective tolerances to copper naphthenate inan aromatic high-boiling petroleum. Tolerances to the same preservativewere also determined for 28 isolates of Poria monticola, including thestandard test isolate of this species, Madison 698. The findings for theseisolates have already been given in table 44.

The tests were made in the standard manner, on conditioned but unweatheredblocks. The fungi used, other than P. monticola, were:

White-rot species

Odontia bicolor (Flo. 126 A), Poria nigrescens (4856).

Brown-rot species

Coniophord. puteana (515), Daedalia quercina (59058),Fomes subroseus (701), Poria cocos (MD 104), Poria

Rept. No. 2114 -108-

incrassata (563), Poria oleraceae (4907), Poria radiculosa(5096-29), Poria vaillantii (FP90877), and Poria xantha(5096-35).

The test results for the 12 species, including P. monticola (Madison 698), aresummarized in table 60. They indicate that the range of tolerances of the 11new species for copper naphthenate (0.5 percent copper metal) in an aromatichigh-boiling petroleum is considerable. The highest estimated threshold (6.5pounds per cubic foot) was more than three times the lowest (< 2.1 poundsper cubic foot). Despite the fact that different species were represented, thetolerance range was fairly similar to that found for the 28 isolates of Poriamonticola (table 44). Inasmuch as Madison 698 occupied an essentially cen-tral position of tolerance among the P. monticola isolates, it also was com-parably located with respect to the 11 species (table 60). Five of the fungishowed a slightly higher tolerance, one a similar tolerance, and five, in-cluding the two white-rot fungi, a lower tolerance to the copper naphthenatesolution. This circumstance, of course, favors continuation of P. monticola(Madison 698) for testing copper preservatives.

B. Carried in Toluene Alone

In this series of tests, the tolerances to copper naphthenate in toluene alonewere ascertained for the same 11 species of fungi listed above, for 28 isolatesof P. monticola and for the 3 additional species used in standard testing.Earlier soil-block tests indicated that the ability of P. monticola (Madison698) to decay blocks treated with similar amounts of copper naphthenate wasmarkedly increased when a low rather than a high-boiling petroleum carrierwas used. Also, a preliminary test showed that this fungus could decayblocks treated with nine times more copper naphthenate carried in straighttoluene than when carried in an aromatic high-boiling petroleum. The pur-pose of the present tests was both to explore the fungi for differences intolerance to copper naphthenate and to learn whether the earlier evidenceon the greater effectiveness of this preservative when carried in petroleumapplies also to other isolates of P. monticola and to other fungi.

Blocks of southern pine sapwood were treated with two copper naphthenate-toluene solutions containing .5 and .2-5 percent copper metal. These treat-ments gave the wood .085 and .175 pound of copper per cubic foot. Thetreated blocks were conditioned for 3 weeks, but not weathered. As therewere only two retentions of the preservative, thresholds were not estimated;instead, the tolerances of the fungi are compared on the basis of amounts ofdecay (weight loss) caused by them in blocks having the same retention.

Rept. No. 2 114 -109-

The weight losses (table 61) indicate that all the isolates of P. monticolaattacked blocks containing .085 pound copper, although in markedly differentdegrees. This amount of copper had only slight effect in retarding decay byfour of the isolates, but permitted the others to cause weight losses of 22 to54 percent. The larger copper retention, 0.175 pound, essentially preventeddecay by 9 isolates, but only retarded decay by the other 19, including Madi-son 698.

Among the species of other fungi, the weight losses indicate that Lent.lepideus, and the 3 white-rot fungi, P. nigrescens, 0. bicolor, and Poly.versicolor did not attack blocks containing .085 pound copper; however, suchblocks were attacked by the 10 other brown-rot species. Three of these, P.radiculosa, P. vaillantii, and P. cocos also decayed blocks with .175 poundcopper.

With respect to the influence of the carrier, it is apparent that the earlier-observed greater effectiveness of copper naphthenate in petroleum oil ap-plies not alone to P. monticola (Madison 698) but also for many other P.monticola isolates and other brown-rot species. The copper thresholds forthe fungi tested were previously found (tables 44 and 60) to be no more thanapproximately .03 pound per cubic foot when treatments were made with cop-per naphthenate in an aromatic high-boiling petroleum. However, for coppernaphthenate carried in toluene alone, the thresholds for all 28 isolates of P.monticola and for all but one of the brown-rot fungi were indicated to be con-siderably greater than .03 pound (table 61). Therefore, the presence ofpetroleum oil apparently improves the effectiveness of copper naphthenateagainst brown-rot fungi in general, although to various degrees.

Tolerances to Pentachlorophenol

Tests of tolerances to pentachlorophenol were made with 8 brown- and 9white-rot fungi, none of which was a standard species. The pentachloro-phenol tolerance of the standard fungi was already known from earlier testsin which several types of carriers were used.

The pentachlorophenol, 5 percent by weight, was carried in a medium-boiling petroleum oil. The test blocks were conditioned but not weathered.The conditioning period in this case was longer than standard, being 2 monthsinstead of the usual 2 weeks. Two species of wood were used: southern pineblocks were used for all the fungi and sweetgum blocks for 7 of the 9 white-

rot fungi that were tested.

Rept. No. 2114 -110-GPO 813057-3

The results of the tests employing the pine and sweetgum blocks appear,respectively, in tables 62 and 63. As may be observed in table 62, thethreshold on pine for six of the brown-rot fungi tested against the 5 percentpentachlorophenol-petroleum was approximately 4 pounds, while that of theother two was less than 4 pounds (smallest, 2.1). Thus, none of the brown-rot fungi showed any greater tolerance for pentachlorophenol than that gen-erally shown by Lenzites trabea (4 pounds), the most tolerant of the standardtest fungi for pentachlorophenol in pine. A considerable range of tolerances(< 0.7 to 2.7 pounds) for pentachlorophenol in the pine blocks was exhibitedby the white-rot fungi. The tolerance of the standard white-rot fungus, P.versicolor (1.7 pounds), was in this case not far above an intermediateposition.

In sweetgum blocks, the pentachlorophenol tolerances of the white-rot fungi(table 63) were mostly similar in relative order to those observed on thepine blocks. Here, however, P. versicolor occupied a position of maximumrather than near intermediate tolerance. Two additional things may be notedabout the results obtained with the sweetgum blocks: (1) the absolute levelsof tolerance were mostly greater than those associated with the pine blocks,and (2) the spread of tolerances was about twice as great (range -<0.7 to 5.8pounds).

All white rotters, except Schizophyllum commune, attacked the untreatedgum much more than the pine, and are also known to do this under naturalconditions. Therefore, sweetgum blocks obviously are preferable to pinefor conducting soil-block tests with fungi of this type.

Tolerance to Boliden S-25 Salt

The response of various fungi to Boliden S-25 salt was of interest becauseof the mixture of chemicals involved -- namely, chromium oxide (24 per-cent), cupric oxide (4 percent), zinc oxide (11 percent), arsenic pentoxide(37 percent), and water (24 percent).

This test was of a simpler type than the others dealing with tolerance in thatall the data were obtained on blocks with a single retention of the preserva-tive. Moreover, the test blocks were not treated in the laboratory but werecut from a 2- by 4- by 18-inch southern pine stake pressure treated with0.31 pound of Boliden S-25 salt. Three positions were sampled (end, fourinches from the end and center), and two blocks from each of the three posi-tions were tested against each fungus. The blocks were unweathered.

Rept. No. 2114 -111-

The fungi used were Lentinus lepideus (Madison 534), Lenzites trabea (Madi-son 617), Poria monticola (Madison 698), Coniophora puteana (Madison 515),Poria incrassata (Madison 563), Odontia spathulata (5096-21), and 9 isolatesof Poria radiculosa (5096-29, 94392, 97451, 90848, 2996, 94373, 3538, 1331,and B9). 0. spathulata, a white-rot fungus, is not considered to be of impor-tance in the decay of untreated softwoods; however, it has been isolatedseveral times from southern pine treated with salt preservatives. P. radicu-losa (5096-29) was isolated from a southern pine stake treated with Bolidensalts and exposed in the field at Madison, Wis.

The test results (table 64) indicate that L. trabea, P. incrassata, and 4 ofthe 9 isolates of P. radiculosa caused considerable decay of the test blocks,whereas 5 other isolates of P. radiculosa caused only a slight amount of decayand the 4 other species caused none. Obviously, it is important in testing apreservative of the Boliden S-25 type that the test fungus be selected withspecial care.

Tolerance to Copper-8 Quinolinolate

The comparatively high tolerance of certain of the brown-rot fungi for coppernaphthenate (60 and 61) made it of interest to learn whether such tolerancemight hold for other copper compounds also. Accordingly, tests were madeto determine the tolerance of the three standard brown-rot fungi to copper-8quinolinolate.

Southern pine test blocks were treated with copper-8 quinolinolate carried at0.75 percent, by weight, in No. 2 fuel oil. 8— The treating solutions, obtainedby diluting with toluene, contained 0.0875, .125, .175, .25, .35, and .50 per-cent copper-8 quinolinolate. Part of the blocks were tested after condition-ing and part after weathering (ASTM D1413-56T).

The decay weight losses and estimated thresholds (table 65) indicate that ap-proximately .06, .04, and less than .02 pound of copper-8 would prevent decayby P. monticola, L. trabea, and Lent. lepideus, respectively, in conditionedblocks. This relative difference in tolerance among the three fungi is some-what like that exhibited by the same fungi for copper naphthenate applied intoluene (table 61).

8—Obtained by adding 7.5 grams Cunilate 2174 (10 percent copper-8 quinolino-

late) to 92.5 grams of No. 2 fuel oil.

Rept. No. 2114 -112-

Weathering approximately doubled the threshold of copper-8 for P. monticola,making it about 0.12 pound per cubic foot. The copper metal equivalent ofthis threshold, nevertheless, is still only about 0.02 pound per cubic foot.

It is possible that the properties of the oil carrier were a factor in the effec-tiveness of copper-8 just as it is in the effectiveness of copper naphthenate.Therefore, these tolerances of copper-8 might have been smaller or greaterthan those observed here, if the oil had been significantly heavier or lighterthan the No. 2 fuel oil.

Tolerance to Copper Formate

A third organic copper compound, copper formate with the application of heatafter treatment, was brought into the studies. This preservative has beendescribed in recent literature to be promising for wood protection purposes.

Blocks were treated with seven water solutions of the chemical containing0.04, 0.08, 0.14, 0.20, 0.26, 0.33, and 0.40 percent copper. The blockswere left submerged in the treating solutions in covered containers for 20hours before the absorptions were determined. Then they were autoclavedfor 1 hour at 15 pounds pressure per square inch (121° C. ).

Part of the blocks were tested after conditioning and the remainder afterstandard weathering. The untreated control blocks were subjected to thesame heat treatment as the treated blocks.

The three standard brown-rot test fungi, Lentinus lepideus, (Madison 534),Lenzites trabea (Madison 617), and Poria monticola (Madison 698) were usedin testing both the conditioned and weathered blocks. The conditioned blockswere also tested with two additional brown rotters, Poria cocos (MD-104)and P. xantha (5096-35). P. xantha, as well as P. monticola, is known tobe copper tolerant. The copper tolerance of P. cocos was not known, but ithas recently been isolated in several localities from wood treated with pre-servatives containing copper.

The test results, shown in table 66, indicate that P. monticola, P. xantha,and P. cocos were very tolerant to copper formate. Even the 0.18 pound ofcopper (highest retention used) in the unweathered blocks had little effect inretarding decay. Since copper formate was ineffective in unweathered woodagainst these three fungi, its effectiveness was expected to be even less inthe weathered wood. This was indicated to be the case by the large weightlosses caused by P. monticola.

Rept. No. 2114 -113-

By comparison, Lent. lepideus and L. trabea were strikingly less tolerantof copper formate. Retentions in the unweathered (conditioned) blocks of .06and .12 pound of copper essentially prevented decay by these two fungi, andin the weathered blocks little or no decay occurred at .15 to .18 pound.

The high tolerance of the Porias to copper formate corresponds to similartolerance to copper naphthenate (tables 60 and 61) and copper-8 quinolinolate(table 65). In contrast, Lentinus lepideus and Lenzites trabea exhibited arelatively low order of tolerance to all 3 copper compounds (tables 61 and65). It seems likely that indications of tolerance of a wood-destroying fungusfor a particular copper compound are evidence that similar tolerance extendsto a variety of other copper-containing materials.

Rept. No. 2114 -114-

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Test fungus : Isolate: number

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•

•

1Weight loss- in

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Lentinus lepideus : 534 : 41 : 0 : 0Poria xantha : 5096-35 : 40 : 1.2 : 0Lenzites trabea : 617 : 52 2.1 : 0Daedalia quercina : 59058 : 45 3.5 : 0Coniophora puteana : 515 : 38 : 10.0 : 0Poria oleraceae : 4907 : 42 : 12.2 : 0Fomes subroseus : 701 : 39 : 14.8 .5Poria incrassata : 563 : 63 : 52.0 .8Poria radiculosa : 5096-29 : 9 : 8.1 • 2.5Poria vaillantii : FP 90877: 35 : 18.2 • 13.1Poria cocoa : MD 104 : 61 : 60.1 46.1Poria monticola • 94264 • 6 1.6 : .8

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2Each weight loss is an average of 4 blocks.

Rept. No. 2114 -116-

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Table 64.--Results obtained with 7, species of fungi and 9 iso-lates of one of them on unweathered southern pine blocks treated with Boliden S-25 salt

Test fungus :Isolate

:

Lentinus lepideus

number: Weight

:0.31

534

698

515

5096-21 :

B-9

B-31

2996

94392

94373

617

563

5096-29

97451

90848

3538

: nominallyloss in blocks

containingpound per cubic foot-

Percent

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1

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13

25

25

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24

27

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Coniophora puteana :

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Poria radiculosa

Do

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Lenzites trabea

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-Each weight loss is an average for six blocks.

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Rept . No. 2124 -121-

MISCELLANEOUS DATA

1. Thresholds in Relation to the Calculated Amount ofCreosote Distilling Below 355° C.

A number of separate soil-block tests in which the laboratory or outdoorweathering procedures followed some of those described in the section onthe development of a weathering phase for the soil-block test have indicatedthat 2 to 2.5 pounds of residual creosote oil distilling below 355° C. remainedin the blocks at the thresholds. The treating solutions in these cases involvedcreosote diluted with toluene, and initial retentions of creosote usually rangedbetween 8 to 12 pounds.

The present test. was directed at learning whether a critical amount of resid-ual creosote distilling below 355° C. was required to reach a threshold pointregardless of the amount of residue distilling above 355° C. that might bepresent.

Methods

An American Wood-Preservers' Association No. 1 coal-tar creosote with 20percent residue was used. The 3/4-inch southern pine blocks were treatedto refusal with 100 percent creosote or 50 percent creosote carried in toluene.The blocks in each treatment were of two specific gravity groups, so thatcreosote absorptions of about 35 and 40 pounds were obtained in those treatedwith 100 percent creosote and about one half such amounts in those treatedwith the 50 percent solution.

The treated blocks were allowed to stand in the laboratory for 10 days andwere then placed in either a circulating-air oven or the weathering box main-tained at 120° F. No leaching was involved in the weathering. It was notpossible to proceed with a definite weathering and conditioning schedule be-cause the weathering apparatus was used for other tests. However, allblocks were handled similarly for a given weathering period. The blockswere removed at irregular intervals, conditioned, weighed, and the loss ofcreosote determined.

When the loss of creosote from the blocks treated with either toluene-dilutedor straight creosote solutions was about 56 and 71 percent, respectively,ten blocks from each treatment were placed in the bioassay test. Weather-ing and conditioning continued for the remaining blocks. Thereafter, groups

Rept. No. 2114 -122-

were removed periodically and placed in the bioassay test until weights indi-cated that the blocks treated with the two types of solutions had lost 74 and 78percent of the creosote, respectively. Lentinus lepideus (Madison 534) wasused in all the bioassay tests.

Results

The average percent loss of creosote, the residual creosote, and the resultsof the bioassay test are summarized in table 67.

At the end of the first weathering period, the percentage loss of creosotefrom the blocks treated by the toluene-dilution method with about 15 and 20pounds of creosote was 11 percent higher than that from the blocks treatedwith about 35 and 40 pounds of straight creosote. This difference, however,was gradually decreased to about 3 percent by the end of the fifth weatheringperiod and this difference remained constant through the eighth and final periodfor which comparisons were possible.

The bioassay test indicated that the blocks treated with creosote-toluene wereattacked when the residual of creosote distilling below 355° C. was reduced byweathering to less than 2 pounds, and the residual above 355°, assuming noloss, was 3 to 4 pounds. For those blocks treated with straight creosote,there was no or only slight decay even when the residual distilling below 355°C. was finally reduced to below one pound. The residual above 355° forthese treatments, assuming no loss, was 7 to 8 pounds.

Conclusions

At thresholds, the residual creosote distilling below 355° C. was differentfor blocks treated with about 20 pounds of creosote by the toluene-dilutionmethod as compared to those treated with about 40 pounds of straight creo-sote. It appears that the amount of residue above 355° C. that remains inthe wood influences threshold determinations when blocks treated with highretentions of creosote are tested. With large amounts of residue, thresholdsmay be reached in blocks that have considerably less than 2 pounds of residualoil distilling below 355° C.

Rept. No. 2114 -123-

Table 67.--Loss of creosote and the amount of decay in blocks treated torefusal with straight creosote and 50 percent creosote intoluene and weathered far different 1eriods

Weathering:Creosote: Initial :Loss of : Residual creosote :Amountperiods : in : creosote :creosote: +- :of decay1

:treating:absorption-: : Total Z>355°C.:<355°C.::solution:

:Percent : Lb. per

•

:Percent :Lb. per:Lb. per:Lb. per:Percent

.cu. ft. :

.:cu. ft.:cu. ft.:cu. ft.:

1 •. 50 : 14.99 : 56.04 : 6.59 : 3.00 : 3.59 : o2 •. 50 •. 14.99 : 62.04: 5.69: 3.00: 2.69: 03 •. 50 •. 14.99 : 65.04 : 5.24: 3.00: 2.24: o4 •. 5o 14.99 : 68.04 : 4.79 : 3.00 : 1.79 : 1.885 •. 5o 14.99 : 70.51 : 4.42 : 3.00 : 1.42 : 4.936 : 50 14.99 : 71.12 : 4.33 : 3.00 : 1.33 : 7.117 •. 5o 14.99 : 72.32: 4.15: 3.00 : 1.15: 8.868 •. 5o 14.99 : 74.12: 3.88: 3.00 : .88 : 11.13

: . . . . .1 •. 5o : 20.05 : 56.31 : 8.76 : 4.01 : 4.75 : 02 : 50 : 20.05 : 61.70 : 7.68 : 4.01 : 3.67 : o3 •. 5o : 20.05 : 65.34: 6.96: 4.01: 2.95: o4 •. 5o : 20.05 : 68.03 : 6.41 : 4.01 : 2.4o : o5 •. 5o : 20.05 : 69.83 : 6.05: 4.01: 2.04: 06 •. 5o : 20.05 : 70.72 : 5.87 : 4.01 : 1.86 : 2.107 •. 5o : 20.05 : 71.62 : 5.69 : 4.01 : 1.68 : 4.6o8 •. 5o : 20.05 : 74.32 : 5.15 : 4.01 : 1.14 : 8.14

•. . . . . .1 : 100 35.22 : 45.14 : 19.32 : 7.04 :. 12.28 •2 : 100 : 35.22 : 55.14 : 15.80: 7.04: 8.76 3 : 100 : 35.22 : 60.25 : 14.00 : 7.04 : 6.96 4 : 100 : 35.22 : 64.11 : 12.64 : 7.04 : 5.60 5 : 100 : 35.22 : 66.67 : 11.74 : 7.04 : 4.7o 6 : 100 35.22 : 67.94 : 11.29 : 7.04 : 4.25 7 : 100 35.22 : 69.22 : 10.84 : 7.04 : 3.8o 8 : 100 35.22 : 70.53 : 10.38 : 7.04 : 3.34 : o

: 100 35.22 : 73.08: 9.48: 7.04: 2.44: 010 : 100 : 35.22 : 74.36 : 9.03 : 7.04 : 1.99 : 011 : 100 : 35.22 : 74 .87 : 8.85 : 7.04 : 1.81 : o12 : 100 35.22 : 75.64 : 8.58 : 7.04 : 1.54 : 013 : 100 : 35.22 : 76.92: 8.13 : 7.04: 1.09: 014 : 100 : 35.22 : 77.94 : 7.77 : 7.04 : .73 : o15 : 100 : 35.22 : 77.94 : 7.77 : 7.04 : .73 : 1.0

•. . . . . .1 : 100 40.18 : 45.17 : 22.0 : 8.04 : 13.99 •2 : 100 : 40.18 : 55.05 : 18.06 : 8.04 : 10.023 : 100 : 40.18 : 60.23 : 15.98: 8.04: 7.94 4 : 100 : 40.18 : 64.04 : 14.45 : 8.04 : 6.41 •5 : 100 : 40.18 : 66.53 : 13.45 : 8.04 : 5.41 •6 : 100 40.18 : 68.09 : 12.82 : 8.04 : 4.78 7 : 100 40.18 : 69.21 : 12.37 : 8.04 : 4.33 8 : 100 : 40.18 : 70.56 : 11.83: 8.04: 3.79: o

9 : 100 : 40.18 : 73.02 : 10.84 : 8.04 : 2.8o : o1 : 100 40.18 : 73.69 : 10.57 : 8.04 : 2.53 : o11 : 100 : 40.18 : 74.84 : 10.11 : 8.04 : 2.07 : 0

12 : 100 : 40.18 : 75.96 : 9.66 : 8.04 : 1.62 : o

13 : 100 : 40.18 : 77.08 : 9.21 : 8.04 : 1.17 : o

14 : 100 40.18 : 78.20 : 8.76 : 8.04 : .72 : o

15 : 100 40.18 : 78.20: 8.76: 8.04: .72 : o

-Two groups of blocks of different specific gravity were subjected toeach type of treatment.

Rept. No. 2114 -124-

Literature Cited

1. BOUYOUCOS, G. J. A.1935. A Comparison Between the Suction Method and the Centrifuge

Method for Determining the Moisture Equivalent of Soils.Soil Science 40: 165-170.

2. DUNCAN, C. G., and RICHARDS, C. A.1950. Evaluating Wood Preservatives by Soil-Block Tests: 1. Effect

of the carrier on pentachlorophenol solutions. 2. Comparisonof a coal-tar creosote, a petroleum containing pentachlorophenolor copper naphthenate and mixtures of them. AWPA Proceed-ings 46:131-145.

3.1951. Evaluating Wood Preservatives by Soil-Block Tests: 3. The

effect of mixing a coal-tar creosote and a pentachlorophenolsolution with a petroleum; a creosote with a coke-oven tar orpentachlorophenol solution. AWPA Proceedings 47:264-274.

1951. Evaluating Wood Preservatives by Soil-Block Tests: 4. Creo-sotes. AWPA Proceedings 47:275-287. 1951.

1952. Evaluating Wood Preservatives by Soil-Block Tests: 5. Lignite-tar and oil-tar creosotes. AWPA Proceedings 48:99-104.

1953. Evaluating Wood Preservatives by Soil-Block Tests: 6. Ex-ploratory tests toward improving the method. AWPA Proceed-ings 49:49-55.

1954. Evaluating Wood Preservatives by Soil-Block Tests: 7. Progresson the development of a laboratory weathering method. AWPAProceedings 50:41-51.

1955. Evaluating Wood Preservatives by Soil-Block Tests: 8. Lowtemperature coal-tar creosote. AWPA Proceedings 51:11-15.

4.

5.

6.

7.

8.

Rept. No. 2114 -125-

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