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Stabilization of IPBC in wood through the use of organosilicon compounds
2012 - IRG/WP 12-30597
The aim of the research was to increase durability of wood treated with 3-Iodo-2-propynyl butylcarbamate (IPBC). The study used a blend of silanes. Biological examination against microfungi was performed to determine resistance of Scots pine wood treated with the tested formulations. Chemical analysis by the Electrospray Ionization Mass Spectrometry (ESI-MS) of water extracts from the leaching performed to assess the ability of silanes to stabilize of IPBC in wood. Through the use of methyltrimethoxysilane (MTMOS) and aminethyl-aminpropyl trimethoxysilane (AEAPTMOS) (1:1) increased stability of IPBC (0.05%) in wood subjected to leaching, thus increased its resistance to attack by microfungi.
B Mazela, W Perdoch

Exposure monitoring of creosote vapors
1989 - IRG/WP 3511
Creosote oils contain hundreds of compounds. During impregnation and handling of treated wood the main component in the vapors released in air is naphthalene. Other main components are alkyl naphthalenes, indene, phenol and its methyl derivatives, benzothiophene, diphenyl, acenaphthalene and fluorene. In the measurement of creosote vapors, naphthalene can be used as an indicator agent. One of the major urinary metabolites of naphthalene is 1-naphthol. To explore the relation between naphthalene concentration in the air and 1-naphthol in the urine of exposed workers we monitored air concentrations and collected urine samples from six men over a working week. 1-Naphthol concentrations in urine samples were analyzed by GC as a pentafluorobenzylbromide derivative. The average concentration of 1-naphthol in the Monday morning samples was 0.1 mg/l, in the Monday afternoon 3.1 mg/l, in the Friday morning 0.4 mg/l and in the Friday afternoon 2.9 mg/l.
P Heikkilä, M Loutamo, V Riihimäki, M Romo

Detection of brown rot decay in wood by ion mobility spectrometry
1991 - IRG/WP 2377
A test method for the detection of brown rot decay in wood is described and involves a two-step procedure: thermal release of vapours from wood samples followed by analysis using Ion Mobility Spectrometry (IMS), with results being obtained in 5-10 seconds. The advantages, limitations as well as the detection limit of the technique are presented.
A H Lawrence, T Nilsson

Soft rot fungi as possible sources of odor in impregnated wood in buildings
1993 - IRG/WP 93-20013
Wood preservatives are frequently used inside houses. In several cases impregnated wood, particularly when used in crawlspaces or other near-ground constructions, has been found to be a source of odor. Mold fungi, soft rot fungi actinomycetes or bacteria growing on impregnated wood are possible producers of the odor. Analyses of volatile emissions from impregnated wood with odor and pure cultures of the soft rot fungus Phialophora fastigiata were made with diffusive sampling on Tenax TA, thermal desorption and capillary GC-MS. 2-methylbutanol was found among compounds emitted from impregnated wood with odor taken from a house with odor. Among compounds produced by Phialophora fastigiata octanoic acid and 2-methylbutanol were found.
J Bjurman, J Kristensson

Identification of terminal structures in cellulose degraded by the brown-rot fungus Postia placenta
1989 - IRG/WP 1389
To gain insight into the biochemical mechanism employed by brown-rot fungi to depolymerize cellulose, we identified the end-groups of chemically pure cellulose that had been depolymerized by the brown-rot fungus, Postia placenta. The depolymerized cellulose was acid hydrolyzed and the anion fractions isolated by ion chromatography. Sugar acids were identified by gas chromatographic and mass spectrocopic analysis. Cellulose degraded by Fenton's reagent (H2O2/Fe2+) was also analyzed. The two systems generated the same sugar acids but not in the same quantities. The acids identified include glyceric and erythronic, indicating oxidative cleavage of the vicinal diol carbon-carbon bonds within glucosyl residues in the cellulose polymer. Gluconic and arabonic acids were also identified as major products. No uronic acids were produced in either systems.
T K Kirk, T L Highley, R E Ibach, M D Mozuch

Analysis of volatile emissions as an aid in the diagnosis of dry rot
1992 - IRG/WP 92-2393
The dry rot fungus, Serpula lacrymans was grown in pure culture on malt extract and on sapwood of pine. The volatile compounds emitted from the cultures were determined by diffusion sampling on tubes filled with Tenax TA, thermal desorption and gas-chromatography-mass-spectrometry in order to find markers for attack of the fungus.
J Bjurman, J Kristensson

Oxalic acid quantification, oxaloacetase assay and ESI localization of P, C, and Fe from the brown rot fungus Postia placenta
1994 - IRG/WP 94-10063
The mechanism by which brown-rot fungi initiate depolymerization of holocellulose in wood remains unknown. Recently, oxalic acid (OA) has received considerable attention in cellulose breakdown by brown-rot fungi. The OA could serve as a proton donor for hydrolytic or an electron donor for oxidative (Fenton's reaction-H2O2/Fe2+) cleavages of cellulose. The acid may originate via oxaloacetase's action upon oxaloacetate. We report electron microscopic imaging (ESI) to localize Fe and HPLC/oxalic kit colorimetry to purify/quantify OA from hyphae upon agar, southern pine wood blocks (WBs) or in liquid culture. Comparative ESI at 25, 59, 110, 222, and 710 ev of hyphae grown upon agar or WBs demonstrated hyphal Fe (710 ev). Although Fe was not visualized in cell walls of uninoculated WBs, it was in certain wood cell walls of inoculated WBs. The Fe distribution differed from C and P. Oxaloacetase activity was not observed in either Amicon YM10 filter-retained intra-or extracellular fractions of liquid cultured hyphae or in homogenates from decayed WBs. In contrast, HPLC detected OA in both Postia placenta liquid cultures and decayed WBs. The less sensitive oxalic kit (mg vs. ug) did not detect OA in liquid cultures. These results constitute additional evidence for an OA Fe2+/H2O2-Fenton's mechanism for brown rot-induced cellulose degradation. However, OA's origin was not established.
C R Jordan, W V Dashek, T L Highley

Pyrolysis GC-MS as a tool for lignin analysis
1987 - IRG/WP 2201
Pyrolysis-GC-MS is a rapid process for analysis of rather complex organic compounds. The method has great application to petroleum shale oil and wood lignin. Small powdered samples (several mg) are placed in silica capillary tubes and rapidly heated in an inert atmosphere such as He or N2. Breakdown products of the pyrolysis are then trapped and held for an allocated time in an injector attached to a gas chromatograph (GC) before being introduced. Once introduced, the sample stream is chromatographed on a capillary column with programmable temperature control before being split into two streams. The first stream containing most of the sample travels directly to the GC detector and the second stream is electronically ionized and the fragmentation patterns read on a mass spectrometer (MS). All information is collected and stored for later retrieval and analysis by a large computer. The computer has software that can compare the fragmentation patterns of the compounds on the GC with known compounds stored in its library. Apart from uses already mentioned, there is great potential for use in lignin analysis of woods and wood products. Results to date indicate pyrolysis-GC-MS is extremely useful for characterisation of lignin from phenolic monomers in the pyrograms. Quantitation of these monomers is being studied.
L Doimo

Natural durability transfer from sawmill residues of white cypress (Callitris glaucophylla). - Part 4: Analysis of extracts and treated wood for active components
2000 - IRG/WP 00-20215
In order to facilitate the commercial implementation of a large project aimed at recovering 'waste' durability components from sawmill residues of Callitris glaucophylla, it has been essential to develop analytical methodology for the important bioactive components of the heartwood extract. This methodology will be used 1) to standardise the activity of successive production batches, ensuring that batch-to-batch variation is controlled, and 2) to monitor the penetration and retention of active components in extract-treated wood, ensuring that treatment quality is controlled. Analytical techniques used through the project have included both LC/MS and GC/MS, but as most of the extract activity against termites and fungi has now been demonstrated to reside in the lighter fractions, we have concentrated on GC/MS for the routine methodology for both extract activity and wood retention. Penetration is monitored by the application of a chromazurol S spot-test to a freshly cut transverse section. Both cypress heartwood and penetrated sapwood turn red-purple under the conditions of the test, which is not necessarily specific for cypress extractives, but nevertheless useful for routine monitoring of penetration of cypress extracts.
Hui Jiang, M J Kennedy, L M Stephens

Determination of N-cyclohexyl-diazeniumdioxide (HDO) containing compounds in treated wood using GC-MS
2000 - IRG/WP 00-20201
Beside the biological effectiveness the approval of a chemical wood preservative requires also techniques for the analytical determination of active ingredients in different matrices. Fulfilling of the last requirement is particularly difficult in the case of impregnated timber treated with wood preservatives containing organic compounds. This paper describes a procedure for the determination of the organic ingredient N-cyclohexyl- diazeniumdioxide (HDO) in solid phases using gas chromatography coupled with mass spectrometry (GC-MS) in connection with a previous thermal desorption step. For this powdered samples are placed in a glass tube. Then the tube is reinserted into the thermal desorption unit which is placed in the GC-oven and directly connected with the capillary column. Afterwards the sample was quickly heated up to 200°C. The resulting gas mixture is pushed onto the column and the separation of the gas components took place. The single components could be identified by means of the retention time and the mass spectrum. A quantitative determination seems to be possible by means of the intensity of the signals. The suitability and reproducibility of this method of the determination of HDO were tested successfully by analysing a number of impregnated wood specimens treated with different formulations containing HDO.
P Jüngel, J Wittenzellner, E Melcher

Incidence of soft rot in creosoted poles
1992 - IRG/WP 92-1554
A further population of creosote-treated poles has been assessed for the occurrence of soft rot, as a continuation of work reported in IRG Document No. IRG/WP/1368. The outer 1 cm of each core was assessed microscopically and graded for the presence of soft rot cavities in the wood cell walls; with further assessments taken at a consecutive 1cm interval for cores showing positive findings. Following this assessment each core was cultured on microbiological media in an attempt to isolate potential causative organisms and correlate their presence with the occurrence of soft rot cavities in the wood cell walls. The results indicate that a number of fungi may be important, either in causing soft rot decay or in creating the conditions necessary for such decay to occur. Of these, Hormoconis resinae seems to be particularly important. This fungus was found populating poles at a rate of 68% overall. Further work has also been undertaken, using gas chromatography and gas chromatography coupled with mass spectroscopy, to establish the amount of creosote present, its chemical composition in poles and to correlate this data with that for soft rot cavitation and microbiological assay.
D J Dickinson, P W McCormack, B Calver

The identification of organic compounds in wood using thermal desorption GC-MS - possibilities and limitations
2001 - IRG/WP 01-20224
There is a clear need for the analytical characterisation and identification of organic compounds and their derivatives in different phases especially in timber. In this context the paper describes a rapid and powerful gas chromatographic method for the determination of insecticides, biocides and "other" organic substances in treated and/or modified wood. The main advantage of this procedure is that wooden material can be analysed directly without any further sample preparation. In principle the technical equipment using a mass selective detector is suitable for identifying as well as quantifying thermal desorbable compounds in only one analytical run. The main emphasis of this contribution, however, is to show the possibilities and limitations of this technique.
P Jüngel, E Melcher

Formation of polychlorinated dibenzo-p-dioxins (PCDD) and polychlorinated dibenzofurans (PCDF) during the combustion of impregnated wood
1995 - IRG/WP 95-50040-19
Wood waste and industrial wood residues often contain various preservatives. The waste management for these residuals can be recycling, deposition or combustion. Among the three possibilities, combustion seems to be the most efficient way of disposal. To obtain detailed information about emissions of organic compounds with environmental impact, especially polychlorinated dibenzo-p-dioxins (PCDD) and furans (PCDF), different impregnated wood materials were incinerated in two furnaces after mixing with non-treated wood in a ratio of 1:4. The combustion process of residues containing organic or inorganic preservatives is influenced by the elementary composition of the preservative and the thermal and oxidative reaction paths in the flame. It was found that the concentrations of PCDD and PCDF in the exhaust gas can be kept low under good combustion conditions. However, a non-regular incineration process strongly supports increased emissions of PCDD and PCDF.
T Salthammer, H Klipp, R-D Peek

Detection of dry rot by air analysis
1992 - IRG/WP 92-2399
Detection of dry rot (Serpula lacrymans) at an early stage appears to be very difficult in practice. Also control inspections in buildings, after remedial treatment of dry rot, have a limited accuracy. The use of trained dogs in Denmark initiated the idea for this research on the possible use of air analysis as a detection method. The Centre for Timber Research-TNO (TNO-CHT) and the Institute for Biotechnology and Chemistry therefore started a research programme sponsored by the Ministry of Housing, Physical Planning and Environmental Management in the Netherlands. The Centre for Timber Research has cultured under controlled laboratory conditions Serpula lacrymans and seven other fungi, which frequently occur in building structures. From these cultures air samples were taken and analysed by IBC-TNO, using GC-MS. Results indicate, that each fungus has it's own specific "blueprint" of volatile metabolic compounds. Though this is a promising start, further research is necessary to see, how growth conditions and environment may influence the consistency of the air analysis. This air analysis, could have application as another non-destructive detection method for decay caused by fungi. Other potential applications also need exploring.
P Esser, A C Tas

The quantitative determination of N-cyclohexyl-diazeniumdioxide (HDO) containing compounds in treated wood using TD-GC-MS
2001 - IRG/WP 01-20223
Last year we presented the paper (IRG/WP/00-20201) "Determination of N-cyclohexyl-diazeniumdioxide (HDO) containing compounds in treated wood using GC-MS". Based on the intensive discussion at the meeting, the first experiences made with the calibration of the system for this application will be reported. For the quantitative determination of N-cyclohexyl-diazeniumdioxide in treated wood, milled material containing a known concentration of the active ingredient were placed in special liners which were sealed with magnetic caps. The liners were then stored in a sample rack. Depending on the analytical program a certain liner was transported automatically into the thermal desorption unit. Afterwards the sample was quickly heated to 200°C. Only a part of the resulting gas mixture was pushed onto the column where the separation of the components took place. The component of interest could be identified by means of the retention time and the mass spectrum. The calibration of the system and the quantification are based on 5 different values (TIC, peak height/area with and without background subtraction, peak height/area of a selected mass fragment with and without background subtraction) received from the spectrum. For the quantification it is necessary to analyse at least 5 samples of identical concentration.
P Jüngel, J Wittenzellner, E Melcher

Anti-fungal properties of pyrolytic oils derived from softwood bark
2000 - IRG/WP 00-30218
Thermal decomposition of balsam fir and white spruce mixed bark residues at 450°C and under vacuum (< 20 kPa abs.) results in high yields of pyroligneous liquors rich in phenolic content. This vacuum pyrolysis process has been scaled-up to a pyrolysis plant with a feed capacity of 3.5 t/h of softwood bark, which is the largest plant of this type in the world. The pyrolytic aqueous condensates have been tested for their anti-fungal properties. One of the major objectives of this study was to identify which groups of chemical compounds were the most active to inhibit the growth of wood decay fungi. The fractionation of the pyrolytic aqueous phase in four distinct parts was accomplished by a liquid-liquid extraction method. The four fractions were named F1 (ether extractibles), F2 (ethyl acetate extractibles), F3 (neutral compounds) and F4 (phenolic compounds). Petri tests were conducted using two brown rot fungi (P. placenta and G. trabeum) and two white rot fungi (I. lacteus and T. versicolor). The composition of these fractions was analysed by GC/MS. Fraction F1, with concentrations of organic acids, phenols and derivatives (3.0% by weight), benzenediols (3.9% by weight), and a variety of other products (quinones, furans, etc.), was the most promising to inhibit the growth of decay fungi, while fraction F3 showed no inhibitive effect in the Petri dish agar test. C. versicolor was most sensitive to these fractions, while I. lacteus was the least. The addition of CuSO4 to the water soluble organics improved their ability against decay.
D Mourant, Dian-Qing Yang, Xiao Lu, C Roy

The action of siderophores isolated from Gloeophyllum trabeum on the structure and crystallinity of cellulose compounds
1991 - IRG/WP 1479
Low molecular weight, high affinity iron-binding compounds (siderophores) were isolated from the brown-rot fungus Gloeophyllum trabeum. The compounds were shown to be inducible by iron starvation and could be purified by ultra-filtration, ethyl acetate extraction, column chromatography and preparative HPLC. The isolated compounds were shown by analytical and immunological techniques to be produced in both culture and in degraded wood. GC-mass spectroscopy and NMR allowed characterization showing their phenolate nature and molecular mass. The chelators are capable of cleaving selected cellulose model compounds and preliminary results suggest siderophores may be able to effect the percent crystallinity of milled poplar wood. Siderophores, together with other non-enzymatic factors, may function as readily diffusible agents catalyzing the initial degradation of wood cell walls.
J Jellison, V Chandhoke, B Goodell, F Fekete, N Hayashi, M Ishihara, K Yamamoto

Characterization of wood decay enzymes by MALDI-MS for post-translational modification and gene identification
2002 - IRG/WP 02-10442
The recent sequencing of the Phanerochaete chrysosporium genome presents many opportunities, including the possibility of rapidly correlating specific wood decay proteins of the fungus with the corresponding gene sequences. Here we compare mass fragments of trypsin digests, determined by MALDI-MS (Matrix Assisted Laser Desorption Ionization-Mass Spectrometry), with predicted mass fragments derived from genome sequence. Glyoxal oxidase of P. chrysosporium is used for proof of concept because its genomic organization is known. Glyoxal oxidase was also chosen because it is a glycoprotein, as are many other fungal proteins, and post-translational sites are predicted by MALDI-MS.
T H de Koker, P J Kersten

Characterization of protein patterns from decayed wood of loblolly pine (Pinus taeda L.) by proteomic analysis
2008 - IRG/WP 08-10654
The primary biotic decomposers of wood belong to the basidiomycetes. The members of this group can attack and biodegrade both wood in the forest and in service. By the time wood decay is visible, there has already been a significant loss of strength. The identification of basidiomycetes and other organisms on wood only tell us what is present, not what is actively decaying the wood. When organisms are metabolically active, such as during wood decay, they produce proteins, some of which are unique to the decay process. Detection and identification of the fungal proteins involved in wood biodegradation would be an advantage in helping to understand the complex biodegradation pathways. In this study, we concentrated on proteomics as a tool to decipher biodeterioration-linked proteins. Proteomic analysis of fresh wood (southern yellow pine), decayed wood, inoculated decayed wood, and Gloeophyllum trabeum were performed. More than 170 proteins from four treatments were visualized on Commassie-stained two-dimensional polyacrylamide gels with a high resolution and reproducibility. These protein spots were subjected to in-gel digestion with trypsin for peptide fingerprint analysis by MALDI-TOF-MS. The tryptic peptides were identified with the aid of a BLAST homology search which found 76 unique proteins from inoculated decayed wood. No proteins were detected from fresh wood. Over 110 proteins were visualized from Gloeophyllum trabeum grown in culture. Among the proteins identified were oxidative enzymes and hydrogen peroxidases. Only actin was identified from decayed wood, but inoculated decayed wood contained wood degradation proteins such as alcohol oxidase, lipoxygenase, and catalases.
Young-Min Kang, L Prewitt, S Diehl

Evaluation and identification of extractives from Iranian walnut (Juglans regia L.) by GC/MS technique for protection of non-decay resistant species
2008 - IRG/WP 08-10670
The use of walnut extractives is interest as environment friendly wood preservatives in the wood preservation industry. In this study, organic solvents were used to remove extractives from Iranian walnut heartwood samples. The solvent was removed by rotoevaporation, and Identification of chemical compounds in the Walnut extractives was done by using GC/MS technique. The toxicity of various extracts concentrations against white rot was tested on agar media and the relative toxicity threshold determined at 0.15mg/ml of agar for Coriolus versicolor. Extracts were used to treat poplar blocks at three concentrations percent (1.5%, 2.5% and 3.5%). Treated blocks were exposed to white rot fungi to determine the biological performance of such treatment. Results showed that treated blocks weight loss to extracts retention of 1.99% in contrast with untreated poplar blocks against white rot, meanly decreased amounting to 15.65 percent, but for purposes of statistically have had not significant difference in 5 and 1 percent level. Also, resistant to tangential and radial hardness and resistant to compression parallel to grain of poplar blocks treated, for purposes of statistically have had not significant difference in 5 and 1 percent level. The most abundant identified compound in heartwood of walnut species was benzoic acid, 3,4,5-tris(hydroxy)/Gallic acid amounting to (44.57%) and the most toxic identified compounds, that caused decrease treated blocks weight loss, was Juglone (5.15%) and 2,7- dimethyle phenanthrene (5.81%).
S K H Hashemi, D Parsapajouh, H Khademi Eslam

Utilization of thermodesorption coupled to GC-MS to study kinetics of thermodegradation of different wood species
2011 - IRG/WP 11-40559
Thermdesorption coupled to Gas Chromatography coupled to Mass Spectroscopy (TD-GC-MS) has been investigated to identify volatile degradation products generated during wood heat treatment by mild pyrolysis. For this purpose, wood samples of different softwood and hardwood species have been heat treated under nitrogen for different temperatures comprised between 180 and 230°C during 15 min. in the glass thermal desorption tube of the thermodesorber and the volatile wood degradation products trapped. The trapped products were then thermodesorbed and analysed by GC-MS. Chromatograms of the different samples indicated the formation of different products resulting from degradation of lignin and hemicelluloses. The important formation of acetic acid is concomitant with the formation of most degradation products and at the origin of the difference of reactivity observed between softwoods and hardwoods.
K Candelier, M Chaouch, S Dumarçay, A Pétrissans, M Pétrissans, P Gérardin

Above Ground Field Evaluation and GC-MS Analysis of Naturally Durable Wood Species
2012 - IRG/WP 12-10764
Nine wood species are being evaluated in above ground field studies in Mississippi and Wisconsin. Candidate naturally durable wood (NDW) species are being rated at yearly intervals for resistance to decay, cupping, and checking. Field ratings after 12 months exposure are presented. To date, Paulownia tomentosa (PAW) and southern yellow pine (SYP) are least durable and cedars are the most durable in above ground exposure. Wood samples are being taken from the deck-boards and subjected to chemical analysis using GC-MS. Fatty acids from NDW species were extracted, derivatized, and analyzed along with commercial fatty acid methyl ester (FAME) standards. With few exceptions, results indicate that FAMEs are more abundant in NDW species. However, preliminary bioassays found no inhibition of select wood decay fungi by FAMEs at naturally occurring concentrations.
G T Kirker, A B Blodgett, S T Lebow, C A Clausen

Utilization of thermodesorption coupled to GC-MS to characterize volatiles formation kinetics during wood thermodegradation
2012 - IRG/WP 12-40587
Identification of volatile degradation products produced during wood mild pyrolysis is important to have better insight on thermodegradation mechanisms. Previous studies have shown that thermodesorption coupled to GC-MS is an attractive tool to characterize and quantify products formed during wood thermodegradation indicating an higher susceptibility of hardwoods to thermodegradation compare to softwoods. The aim of this study is to give better insights on wood thermodegradation pathways during wood heat treatment with special emphasis on the kinetics of thermodegradation. For this purpose, one hardwood species (beech) and one softwood species (Sylver fir) have been subjected to thermal treatment directly in the thermal desorption glass tube of the thermodesorber under helium at temperatures of 210 and 230°C for different times ranging from 10 to 80 minutes and volatiles compounds formed analysed by gas chromatography coupled to mass spectroscopy. Starting from these results, it’s was possible to visualize the different products formed as a function of time allowing determination of the kinetic curves of formation of the main degradation products. Making the assumption that acetic acid is representative of hemicelluloses degradation and vanillin representative of lignin degradation, it was possible using Arrhenius equation to determine a mean activation energy of formation of this two products leading to indirect informations on lignin and hemicelluloses stability for each wood species.
K Candelier, S Dumarçay, A Pétrissans, M Pétrissans, P Kamdem, P Gérardin

Developing Analytical Methods for Determination of Quaternary Ammonium Compounds (DDAC) using HPLC and HPLC-MS (Application to treating solution and preservatives treated wood)
2013 - IRG/WP 13-20516
Korea preservative treating industry has mainly used alkaline copper quaternary (ACQ) expected over 80% of market share in Korea. ACQ employs dodecyl dimethyl ammonium chloride (DDAC) and benzyl dimethyl dodecyl ammonium chloride (DBAC) for active ingredient along with copper. The strongly increasing domestic applications for wood preservatives require developing accurate and reproducible analytical methods. Although a long historical titration method has been successfully applied to quantify quaternary ammonium compounds (QACs), the method cannot tell DBAC from DDAC in the analytes. The objective of this study was to develop and optimize a method for the quantification of QACs in treating solutions and preservatives treated woods using HPLC and HPLC-MS. This study showed that the both HPLC-UV and HPLC-MS analysis resulted in accurate and reproducible analytical data for QACs quantification, compared to a titration method. The HPLC-MS method, however, produced more sensitive and specific results than HPLC-UV. The MS method was reliable for the determination of the pure DDAC in treating solution and preservative treated wood.
Sung-Mo Kang, Kwon-Min Kim, Won-Mo Koo, Myeong-Won Cho

Recycling of used railroad ties via two-staged pyrolysis for fractionation of wood preservatives and bio-oil: pyrolytic characterization by TGA and Py-GC/MS
2015 - IRG/WP 15-50311
Creosote and copper naphthenate (CuNap) (in an oil carrier) treated railroad tie materials (crossties or sleepers) were initially heat-treated at 200 – 300 oC and subsequently pyrolyzed via thermogravimetric analysis (TGA) and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) to recover wood preservatives and produce a higher quality bio-oil. Preservative-desorptive temperatures at 200 and 250 oC by TGA removed water and creosote (6.6 – 9.3 wt%) from the creosote-treated crosstie materials, and water and CuNap components (21.2 – 23.3 wt%) from the CuNap-treated crossties. Temperature at 300 oC removed a shoulder DTG peak at 305 - 325 oC and weight loss accounted for 25.5 wt% in the creosote-treated tie and 30.6 wt% in the CuNap-treated tie. Temperature at 200 – 300 oC by Py-GC/MS desorbed creosote-derived chemicals such as naphthalene, acenaphthene, fluorine, anthracene, fluoranthene, pyrene and other polycyclic aromatic hydrocarbon (PAHs) derived from the creosote-treated tie; and mineral oil (alkane hydrocarbons such as tetradecane, nonadecane, hexadecane and octadecane, and heptacosane) from the CuNap-treated ties. Pyrolysis of the wood tie with elevated temperature produced a high amount of carbohydrate- and lignin-derived compounds from wood ties. Fast pyrolysis of the 200 oC-treated crossties by Py-GC/MS produced a high fraction of creosote- and CuNap compounds most of which were then not subsequently recovered through fast pyrolysis of the 250 and 300 oC-treated samples. Fast pyrolysis of the thermally preservatives-removed tie samples produced high anhydrosugars such as levoglucosan and low acetic acid, furfural and ketones as well as high pyrolytic lignin-derived compounds, which shows good potential for phenolic-based chemical production. The results demonstrate that a thermal preservative-removal step (similar to a torrefaction step) can successfully remove valuable creosote and CuNap components for re-use as preservatives and subsequently supply a clean wood without significant levels of contaminant hazardous air pollutants for use as boiler fuel, more efficient pyrolysis to produce higher quality bio-oil, gasification or other uses.
Pyoungchung Kim, J Lloyd, Jae-Woo Kim, N Labbe

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