Abstract:
A method and apparatus to produce an ion mobility signature representing a wood sample provides a method of comparing signatures to identify the species of the wood sample. A method of producing an ion drift time signature representing a wood species comprises heating at least a portion of a wood sample at a temperature in the range of about 220° to 350° C. to desorb and produce trace vapors from the wood sample, ionize the trace vapors at a temperature in the range of about 220° to 350° C., pulse ions through a gate into a drift region, measure the time of arrival of the ions and the ion flux for each pulse, with a collector electrode, located at the end of the drift region to produce an ionic signal, and amplify and average the ionic signal to provide an ion drift time signature for the wood sample.

Description:
BACKGROUND OF THE INVENTION 
     The present invention relates to sampling wood to identify wood species. More specifically the present invention provides a method of producing an ion mobility signature representing a wood sample and then comparing the signature with known signatures of wood species to determine the wood species of the sample. 
     When logs arrive at saw mills they are usually stacked, and in many cases it is difficult to tell the species of a specific log. It is known that different types of wood species have different commercial values and thus there is often an advantage for the saw mills to sort out different wood species in order to maximize the values of the more valuable woods. Today, distinguishing one species of wood from another is often done manually either in log form or when lumber is sorted, and this is not necessarily the most reliable or economical method. Once the species of the wood has been determined, there is generally a decision time of about 2 to 10 seconds while the wood moves along a conveyor to a position where the wood is sorted into a different species. 
     Ion mobility spectrometry (IMS) is recent technology which separates ionized compounds based on differences in their drift velocity through a gas under an applied electric field. This technique has the ability to produce a characteristic spectrum of the series of high molecular weight compounds in a matter of milliseconds. It is known that it can produce identifiable signatures for such items as drugs and explosives and is being developed for use by customs, airlines and police forces to detect such substances. Initial tests were carried out to determine if IMS could be used to identify different wood species. A report on these tests was published by A. H. Lawrence on Feb. 2, 1989 at the 75th annual meeting of the Technical Section of the Canadian Pulp and Paper Association entitled &#34;Rapid Characterization of Wood Species by Ion Mobility Spectrometry&#34;. Some tests were carried out in the &#34;positive mode&#34; and some in the &#34;negative mode&#34;. Positive mode is when polarity of the electric field is positive, i.e. positive ions present in the detection mode. Negative mode is when the polarity of the electric field is negative, i.e. negative ions present in the detection mode. The initial tests showed that some wood species could be identified one from the other provided the tests were conducted in both modes. However, there were a number of variable parameters that did not initially appear to be acceptable for use in the lumber industry. First of all sampling and analyzing by an IMS device took several seconds and this would hardly be feasible for fast moving conveyors used in saw mills. Secondly it seemed that only certain types of wood species could be identified and thirdly it was not clear how such a piece of equipment would work in a saw mill environment with saw dust, other types of particles as well as vapours from both machinery and wood are present. 
     Ion mobility spectrometers are known, and it is also known that specimens analyzed by such a spectrometer can produce different signatures, or plasmagrams as they are sometimes referred to, which are affected by many different variables, e.g. temperature, barometric pressure, humidity, etc. Furthermore, when one analyzes a specimen of wood, the wood may be dry or moist. Heartwood and sapwood from the same wood species have different ion mobility signatures, and there are other effects such as extraneous noises, radio signals, vibrations etc. that may effect the signature of a trace sample. 
     SUMMARY OF THE INVENTION 
     We have now found that by desorbing wood within a preferred temperature range to produce trace vapours, and ionizing the trace vapours at a further preferred temperature range, we can measure the time of arrival of the ions and the ion flux at a collector electrode and produce a weak electric current signal representing an ionic signal. The measurement can be made in the negative mode and the positive mode and different signals are produced in the two modes. Mobility of an ion is dependent at least partly, on the mass and shape of the ion, as well as the charge distribution. Mobilities are influenced by the media through which the ions travel, and by gas density variations which in turn depend on gas temperature and pressures. The density variations can be normalized by reducing the mobility to a standard temperature and pressure and thus produce a reduced ion mobility signature derived from the ion drift time signature for that particular wood species. It has been found that these different signatures can be used to identify most wood species regardless of the fact that the temperature, and pressure conditions vary for different locations. The signatures are identifiable regardless of the moisture content of the wood, and regardless of environmental conditions. Heartwood and sapwood signatures for the same wood species are different, but are specific for that species. 
     One aim of the present invention is to be able to analyze a wood sample within a short space of time, and detect the wood species in less than a second. To achieve this time and to repeat identifying different wood specimens, more than one apparatus may be required. Furthermore, under some conditions such as analyzing a cold wood sample, then longer times are necessary. It is a further aim to provide a sampling arrangement that works in the environment of a saw mill under conditions where saw dust and other dust is blowing about under extreme noise and vibration conditions, and still produce a signature so the wood species can be identified. 
     The present invention provides a method of producing an ion drift time signature representing a wood species, comprising the steps of, heating at least a portion of a wood sample at a temperature in the range of about 220° to 350° C. to desorb and produce trace vapours from the wood sample; ionizing the trace vapours in an ionizing zone at a temperature in the range of 220° to 350° C.; pulsing ions from the ionizing zone through a gate means into a drift region; measuring the time of arrival of the ions and the ion flux, for each pulse, with a collector electrode located at the end of the drift region to produce an ionic signal, and amplifying and averaging the ionic signal to provide an ion drift time signature for the wood sample. 
     There is further provided a method of identifying a wood species comprising the steps of heating at least a portion of a wood sample at a temperature in the range of about 220° to 350° C. to desorb and produce trace vapours from the wood sample; ionizing the trace vapours in an ionizing zone at a temperature in the range of about 220° to 350° C.; determining drift time of ions and ion flux produced in the ionizing zone, at a collector electrode spaced from the ionizing zone, to produce an ionic signal; amplifying and averaging the ionic signal to provide an ion drift time signature for the wood sample, and comparing the signature with known wood species signatures to determine the wood species of the wood sample. 
     In another embodiment there is also provided an apparatus for producing an ion drift time representing a wood species from a wood sample comprising heating means to heat at least a portion of the wood sample to a temperature in the range of about 220° to 350° C. to desorb and produce trace vapours from the wood sample; gas flow means for transferring the trace vapours to an ionizing zone, the ionizing zone being at a temperature in the range of about 220° to 350° C.; means to ionize the trace vapours in the ionizing zone; gate means adjacent the ionizing zone leading to a drift region having a collector electrode at the other side from the gate means, the collector electrode adapted to determine drift time of ions and ion flux in the drift region, and amplification means and averaging means to provide an ion drift time signature for the wood sample. 
    
    
     BRIEF DESCRIPTION OF THE DRAWINGS 
     In drawings which illustrate embodiments of the invention, 
     FIG. 1 is a schematic diagram showing an ion mobility spectrometer suitable for analyzing a wood sample according to the present invention. 
     FIG. 2 show six ion mobility signatures for different wood species. 
     FIG. 3 is a schematic diagram for air carrier flow and purge flow for the IMS and sample line. 
     FIG. 4 show six ion mobility signatures for different samples of jack pine showing the reproducibility of the signatures. 
     FIG. 5 show ion mobility signatures showing the effects of variable moisture content for jack pine. 
     FIG. 6 show ion mobility signatures showing the difference between sapwood and heartwood for jack pine. 
     FIG. 7 show ion mobility signatures at tree loading sites under both low and high vibrations. 
     FIG. 8 show ion mobility signatures at chipper and canter sites with an acoustical cover on and off. 
    
    
     DETAILED DESCRIPTION OF THE INVENTION 
     An ion mobility spectrometer (IMS) is illustrated in FIG. 1. For the purposes of experimentation a unit manufactured by Barringer Research Limited was modified for sampling wood. A desorber heater 10 is positioned at one end of a spectrometer 12 and a wood sample 14 rests on top of a filter above the desorber heater 10. A passage 16 from the desorber heater leads through a repelling ring 18 to an ionizing zone 20 which includes a weak radioactive source. An electronic gate 24 separates the ionizing zone 20 from a drift region 26. The drift region is a drift tube 28 with a series of stacked cylindrical guard rings 30 to produce a uniform electric field throughout the drift region 26. A collector electrode 32 at the top of the drift region 26 measures the drift time of the ions and also the ion flux. The electrode 32 produces a weak electric current which is an ionic signal. This signal is amplified by amplifier 34 then averaged by a signal averager 36 before being recorded on a chart recorder 38 as a representative ion mobility signature for the wood sample 14. A Nicolet signal averager was used for test purposes, however, intregated averagers are used for saw mill operations. 
     A sampling gas flow 40 collects trace vapours from the wood sample 14, and transfers the vapours through a transfer line 16, in the test machine into the ionizing zone 20. The transfer lines 16 containing the trace vapours are heated to prevent condensation of the trace vapour. The entire cell is at atmospheric pressure and the ionizing source, which in one embodiment is Ni 63 , a radioactive isotope, generates certain reactant ions. These ionize a fraction of the trace sample molecules in the sampling gas flow. As a result of a complex interchange reaction which takes place in the of a spectrometer 12 and a wood sample 14 rests on top of a filter above the desorber heater 10. A passage 16 from the desorber heater leads through a repelling ring 18 to an ionizing zone 20 which includes a weak radioactive source. An electronic gate 24 separates the ionizing zone 20 from a drift region 26. The drift region is a drift tube 28 with a series of stacked cylindrical guard rings 30 to produce a uniform electric field throughout the drift region 26. A collector electrode 32 at the top of the drift region 26 measures the drift time of the ions and also the ion flux. The electrode 32 produces a weak electric current which is an ionic signal. This signal is amplified by amplifier 34 then averaged by a signal averager 36 before being recorded on a chart recorder 38 as a representative ion mobility signature for the wood sample 14. A Nicolet signal averager was used for test purposes, however, integrated averagers are used for saw mill operations. 
     A sampling gas flow 40 collects trace vapours from the wood sample 14, and transfers the vapours through a transfer line 16, in the test machine into the ionizing zone 20. The transfer lines 16 containing the trace vapours are heated to prevent condensation of the trace vapour. The entire cell is at atmospheric pressure and the ionizing source, which in one embodiment is Ni 63 , a radioactive isotope, generates certain reactant ions. These ionize a fraction of the trace sample molecules in the sampling gas flow. As a result of a complex interchange reaction which takes place in the ionizing zone, the molecules of certain species of trace vapours form ions while others do not. These ions are prevented from entering the drift region 26 by the electronic gate 24 and cannot return to the passageway 16 because of the repelling ring 18. When the gate 24 is open, the ions accelerate under the influence of a strong electric field through the drift region 26 towards the collector electrode 32. The gate 24 is repetitively opened at brief intervals (typically 0.2 milliseconds) emitting pulses of mixed ions into the drift region 26. A typical time between pulses is 20 milliseconds. As they pulse, the ions in any particular pulse separate into their individual chemical species based upon their differing intrinsic mobilities. The arrival of the individual ion pulses at the collector electrode 32 produces a characteristic ion arrival time spectrum. This ionic signal in the form of a weak electric current from the collector electrode 32 is amplified and then fed to the Nicolet signal averager where it is filtered, digitized and stacked to increase signal to noise ratio. The number of sweeps or cycles can be varied and the average signal is viewed on a screen in real time and subsequently displayed on the chart recorder 38. Because each ion travels at different velocities, the ions are separated in drift time as they arrive at the collector electrode 32. A plot of ion intensity as a function of drift time is referred to as a plasmagram or signature. 
     A drift gas flow 42 was maintained in the drift region 26 against the ion travel direction and exited at an exhaust 44 together with the sampling gas 40. A typical time between pulses is 20 milliseconds, this represents an analysis time for one pulse of the gate 24. 
     With regards to heating of the sample, the desorption temperature during tests varied from 170° to 400° C. and the tests were conducted with the negative ions analyzed and the positive ions analyzed. It was found that a temperature range of about 220° to 350° C. produced ion drift flow signatures that were distinguishable for different wood species. The results indicated that in the negative mode the signatures produced were distinctive in the desorption temperature range of about 250° to 315° C., with a preferred temperature of 300° C. when the species were well identified. Temperatures above 315° C. produced weaker peaks, and loss in distinguishing peaks. At 350° C. and above the peaks almost disappeared for some wood species. Further tests were carried out in the positive mode but weak signatures with peaks poorly defined were developed, and were often common for different wood species. It was found that in the negative mode peaks were more intense, and plasmagrams were unique for wood species. With regards to the temperatures in the ionizing zone 20, it was found that a range of about 220° to 350° C. produced satisfactory signals which allowed one species of wood to be distinguished from another. 
     The velocity with which ions travel through the drift region is given by the formula: 
     
         V.sub.d =K·E 
    
     where: 
     V d  is the drift velocity 
     E is the drift field strength, 
     K is the scalar mobility of the ions (cm 2  /V·s) for a drift length ld which is the length of the drift tube. 
     Mobility was determined from the drift time t d  by the formula: ##EQU1## 
     Because mobility is dependent on the size of the ion, its shape and charge distribution mobilities are influenced by gas density variation which in turn depend on gas temperature and pressure. These variations are normalized out by referencing the mobility to standard temperature and pressure. 
     Thus reduced ion mobility is defined as: ##EQU2## where: l d  -- drift tube length (cm) 
     T o  --273° K 
     P o  --760 torr 
     P--drift tube pressure (usually equal to atmospheric pressure) torr 
     T--drift region temperature °K 
     t d  --drift time(s) 
     E--electric field (V/cm) 
     A wood sample in the form of saw dust was placed on a filter at room temperature. The filter with the particles thereon was then positioned over the desorber heater as shown in FIG. 1 and heated to a temperature of 300° C. The trace vapours generated were continuously carried by the sampling gas flow 40 into the ionizing zone 20 which was kept at a temperature of 240°C. Pulsing occurred every 20 milliseconds and a total of sixteen pulses were averaged for display which corresponds to 0.32 seconds of sampling time. The appearance of the signatures is illustrated in FIG. 2. The major peaks developed sufficiently within the 0.32 seconds so that positive identification was carried out. 
     The signatures represent the average mobility of the ions against time. The figures on top of the peaks are the reduced mobility determined by referring the average mobility to standard temperature and pressure. 
     In order to ensure that residual sample vapour was purged from the detector fast enough to facilitate the desired sampling cycle time, a sample or carrier flow arrangement with a purge line was prepared as shown in FIG. 3. A rotating sampling head or valve 50 allows the sample flow to pass through the transfer line 52 and enter the IMS 12. As soon as the sampling cycle is finished, the valve 50 switches through 90° , and clean air passes through the transfer line 50 and the IMS 12 to purge all trace vapours from the previous sample. The sampling flow flushes out through an exit line 54. 
     For each detection, at least a portion of the wood sample is heated to within the desired desorption temperature range. The trace vapours are then carried to the ionizing zone 20 of the IMS. A number of pulses occurs in each detection cycle and the complete detection cycle occurs in less than one second, preferably less than one half a second. The IMS and transfer line purge occur after each detecting cycle for a sufficient period of to remove all traces of the previous vapours. A time of one second was sufficient for the present tests. The results show that the detector can be purged rapidly between samples thus making it acceptable for use in a saw mill. 
     The steps of preheating, detecting, analyzing and purging occurs within a time range of about 1.5 to 5 seconds. Some of the steps, such as preheating and purging can have some overlap, however, the preheating time is generally the variable step as this is dependent on ambient temperature and moisture content of the wood sample. For analyzing wood samples faster than this time range, more than one IMS detector is provided, utilizing multiple transfer lines from one or more sampling positions. 
     The reproducibility of the samples were determined by taking six separate samples of jack pine and preparing signatures as shown in FIG. 4. Some intensity variations in the major peak and variation in the minor peaks are observed from sample to sample. However, it has no significant impact on identification of the species. In each case the 1.16 K o  reading clearly stands out as being an identifying signature. 
     
         ______________________________________WOOD SPECIES ANALYSED WITH BARRINGIMS DETECTOR                       IMSSPECIES                     SIGNATUREGROUP        SPECIES        K.sub.0 (cm.sup.2 /V.s)______________________________________Eastern SPF  Jack Pine      1.16(s)        Balsam Fir     1.86(s); 1.74(s)        Eastern Spruce 1.74(s); 1.54;                       1.41Eastern Pine Red Pine       1.74(s); 1.41        White Pine     1.16(s); 1.74;                       1.54; 1.41Western Interior        Western Larch  1.60(s); 1.74;                       1.51        Lodgepole Pine 1.74(s); 1.16(s)        Douglas-Fir    1.60(s); 1.74;                       1.48        Alpine Fir     1.86(s); 1.74(s)        Interior Spruce                       1.74(s); 0.98        Western Hemlock                       1.86(s); 1.74(s);        (interior samples)                       1.48; 1.24; 1.62Western Coastal        Sitka Spruce   1.41(s); 2.26;                       1.06        Douglas-Fir    1.60(s); 1.74;                       1.48        Western Hemlock                       1.39(s); 1.74        (costal samples)        Amabilis Fir   1.74(s); 1.41        Alpine Fir     1.86(s); 1.74______________________________________ (s) denotes the most prominent io peak in the plasmagram 
    
     Table 1 illustrates the wood species analyzed with the IMS detector. The signatures for the reduced ion mobility figures (Ko) are shown for the different wood species and also possible conflicts within the groups. The groups are selected for ones that grow in different areas and therefore are not likely to be mixed up in a mill. The most prominent peaks in the signatures are the distinguishing features of the signature. 
     The effects of variable moisture content are illustrated in FIG. 5. Wood samples in different states of drying were investigated. Jack pine in three different moisture conditions was analyzed, the green sample contains a higher percentage of moisture than the air dried sample. However, the signatures differ only in the time required to heat the sample to a high enough temperature for the plasmagram to develop. Traces B and C in FIG. 5 show 10 ms segments of the signature A expanded in four consecutive analysis time slots of 0.64 seconds. There is little difference between the signatures for the three samples thus the moisture content does not modify the appearance of the signature provided the sample is heated to the required desorption temperature preferably 300° C. Similar tests were carried out with balsam fir with similar results. This means that IMS can be used anywhere in the sequence of processing wood products, even after the wood has been dried. 
     Sapwood samples and heartwood samples were taken from jack pine and analyzed. The signatures, as shown in FIG. 6, indicate that the sapwood samples contain a strong peak of reduced mobility of 1.39 K o . For the heartwood samples a 1.16 K o  peak occurs and it is clear that the signatures for heartwood and sapwood within the same species are reproducible but differ one from the other. Other species of wood were looked at with similar results. 
     In order to assess the feasibility of an IMS installation in the field, tests were conducted at a tree loading site and the equipment was set up in an area where tree lengths are loaded on conveyors to be sent to a debarker. Large amplitude shocks were experienced and vibration signals were picked up by the IMS detector as shown in FIG. 7. Tests were also conducted at six additional locations in a saw mill. 
     These locations were chosen as suitable positions in the saw mill where the logs or lumber could be sorted dependent upon wood species, and conveyed to different areas. The locations took into account the different environmental conditions in the mill. 
     Throughout the mill testing, ambient air was used without predrying or filtering for the sample carrier flow. The ambient air was coarsely filtered and partially dried for the drift gas flow. No additional background peaks were observed from the ambient air, as illustrated in trace 1 of FIG. 7, and no chemical interference was detected. Acoustic and vibration effects from falling and bumping trees were severe as can be seen in trace 2. Traces 3 and 4 are the signatures from jack pine samples from the mill run at low and high vibration noise and trace 5 is a sample of spruce run under low vibrational noise. In both cases positive detection and identification is evident. 
     Further tests were conducted at a chipper and canter site where many electric motors were generally running continuously. The hydraulic system was intermittent and settled wood dust was present on all surfaces. The air was estimated to contain about 100 particles per cubic foot. Vibration noise was low with only occasional shocks as logs were fed into the conveyor, however, acoustical noise levels were severe as shown in FIG. 8. Traces 1 and 2 show the background signatures before and after an acoustical protection cover was placed on the IMS system. Traces 3 and 4 show the signatures of jack pine and spruce on this site. Both the jack pine and spruce samples were reliably detected. 
     The 2.90 K o  peak in FIG. 8 represents the partially hydrated chloride ion, (H 2  O) n  Cl - , which is present in the reaction region and ion mixture allowed into the drift region. In a preferred embodiment in the negative mode, chloride reactant ions are generated in the reaction region from chlorinated compounds, typically methylene chloride (dichloromethane), introduced as a dopant into the sample carrier gas. Under the usual operating conditions these are partially hydrated, resulting in the reduced mobility constant of 2.90 cm 2  /Vs. Upon introduction of sample molecules into the reaction region, analyte ions are formed at the expense of the chloride ions, and the reactant ion concentration decreases and may become even completely depleted. 
     Other reactant ions that may be used as indicators are bromides and iodides in the negative mode, and nicotinamide in the positive mode. 
     In certain locations acoustical protectors either in the form of an acoustical cover or by utilizing electronic circuits are provided to eliminate extraneous noise from vibrations and other spurious electronic signals which are often present in industrial locations. 
     The tests have shown that there is an unambiguous signature for different wood species. Furthermore, the IMS application can handle wood with moisture contents varying from about 0 to 200%. The machine can operate with mill background atmosphere and in a mill environment. For the purposes of the test sampling was conducted with saw dust, however, other types of sampling may be developed. 
     Various changes may be made to the embodiments described herein without departing from the scope of the present invention which is limited only by the following claims.