CN109613042A - A kind of pine class sawn timber Oleoresin Contents test method based on time domain nuclear magnetic resonance - Google Patents
A kind of pine class sawn timber Oleoresin Contents test method based on time domain nuclear magnetic resonance Download PDFInfo
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Abstract
The pine class sawn timber Oleoresin Contents test method based on time domain nuclear magnetic resonance that the present invention relates to a kind of.It is characterized by: using CPMG sequence in time domain Nuclear Magnetic Resonance, measure the standard specimen of the vacuum dried rear different quality of some tree species pine sawn timber, the original NMR relaxation attenuation curve of gained sample is obtained to the transverse relaxation distribution profile of standard specimen after Inversion Calculation, record each standard specimen transverse relaxation distribution spectral peak gross area, then Oleoresin Contents in soxhlet extraction methods measurement standard specimen are utilized, establish the standard curve of transverse relaxation distribution the spectral peak gross area and standard specimen Oleoresin Contents, the sample of Oleoresin Contents to be measured is measured again, bring the resulting relaxation distribution spectral peak gross area into standard curve, obtain the Oleoresin Contents of sample to be tested, and then sample to be tested Oleoresin Contents ratio can be acquired.Present invention detection speed is fast, as a result accurately, and without carrying out complicated chemical solvent extraction experiment.
Description
Technical field
The invention belongs to Wood abstract detection field, specific design is conducive to pine class sawn timber Oleoresin Contents detection method.
Background technique
According to the data of national forestry and the publication of grassland office, China's forestry gross output value reaches the 7.1 trillion yuan people within 2017
Coin, the preresearch estimates timber industry gross output value account for forestry gross output value ratio 40%, about 3,000,000,000,000 yuans.By decades
Development, China has become maximum timber processing, trade and country of consumption in the world, therefore wood consumption is huge, at present state
Interior timber annual consumption is more than 6 billion cubic meters, and wherein softwood accounts for about 65% or more total amount.With China's natural forest protection work
Journey iterative method has stopped wildwood commercial clear cutting in the whole country at present, and raw material needed for domestic timber industry are led at present
To depend on timber resources import and artificial fast-growing forest timber.Pine, pinus sylvestris var. mongolica etc. and south China in import softwood
The pines class resource such as masson pine planted extensively is always raw material important in timber industry production, in building, indoor dress
The industries such as decorations, furniture are widely applied.Due to pine class Wood Anatomical Structure feature, most pines contain resin canal, resin canal
Rosin can be generated, the rosin contained in sawn timber will affect the processes such as splicing, covering with paint, the coloring in woodwork production and processing.Especially
It is that the more pine sawn timber of Oleoresin Contents holds after woodwork is made if not in place without ungrease treatment or ungrease treatment
Easily there is rosin exudation, causes pull-away, jaundice, breakaway etc., seriously affect product appearance and product specification, therefore to pine
The high sawn timber of class sawn timber, especially Oleoresin Contents carries out ungrease treatment, and it is wood that Oleoresin Contents in sawn timber, which are controlled in a certain range,
It must be noted that in production of articles, the detection of pine class sawn timber Oleoresin Contents is to guarantee the important indicator of product quality.At this stage
The measuring method of Oleoresin Contents generally refers to National Standard of the People's Republic of China's GB/T2677.6-94 " paper making raw material in timber
The measurement of organic solvent extract content " in prescriptive procedure, wood sample is stripped as solvent using ether, analysis meter
Calculate Oleoresin Contents in timber.But this method is higher to operator's skill requirement, complicated operation for detection process, the time also compared with
It is long.According to examination criteria, extraction solvent must use ether, belong to the easily restrictive medicament of system poison, purchase, use, storage are all
Strict implement state organization of public security precursor chemicals administrative provisions are needed, therefore general wood processing enterprise is difficult to be produced
Middle real-time detection.
Time domain nuclear magnetic resonance as a kind of detection method of quick nondestructive be widely used in food, geological prospecting, agricultural,
The fields such as high molecular material, medicine.Its principle is by applying radio-frequency pulse to the sample in stationary magnetic field, so that sample
Contained in proton resonate, realize transition from low-lying level to high level, after stopping excitation, the proton in sample returns again
To ground state, and generate NMR signal.Sample transverse relaxation attenuation curve is measured by CPMG sequence and carries out data inversion,
Different component is distributed containing protic component in available sample, and inverting spectral peak area represents its content of material.Since inverting is composed
There are certain proportion relationships with content of material for peak area, therefore can establish inverting spectral peak area and ratio that content of material directly subtracts
Relationship, thus quickly, it is accurate and lossless sample is detected.
Time domain nuclear magnetic resonance technique has been used for the research of moisture state in moisture content measurement and timber at present, but will
When it is applied to softwood determination of moisture, especially pine class softwood measurement, NMR signal actually contains timber
The summation of 2 kinds of fluid signals of water and rosin in sample.As shown in Figure 1, being the pine sawn timber sample of Oleoresin Contents very abundant
The transverse relaxation distribution spectrogram that the measurement of vacuum drying anteroposterior diameter CPMG sequence and inverting obtain.It can be seen that sample is dry by vacuum
Apparent transverse relaxation distribution (red curve) is still presented after dry exclusion moisture, it is seen that the original transverse relaxation distribution of sample is (black
Color curve) moisture and rosin two parts are contained, after removing moisture removal using vacuum drying, individually extract rosin transverse relaxation distribution
Then spectral peak area establishes the relationship with rosin quality, can be used for the detection of Oleoresin Contents in pine class timber, no
It can only save the plenty of time, and simplify subsequent cumbersome managed chemical reagent extracting treatment process processed.
Summary of the invention
The purpose of the present invention is based on above-mentioned prior art situation and provides one kind based on the measurement of time domain nuclear magnetic resonance technique
The method of Oleoresin Contents in pine class sawn timber, this method are suitable for Oleoresin Contents measurement, measurement process in pine class sawn timber and are not necessarily to
Sample destroy and chemical solvent extracting, time-consuming short and accuracy are high.
The present invention is achieved through the following technical solutions:
This pine class sawn timber Oleoresin Contents test method based on time domain nuclear magnetic resonance, it is characterised in that: in time domain core
CPMG sequence is used on magnetic resonance device, measures the standard specimen 15-20 of the vacuum dried rear different quality of some tree species pine sawn timber
It is a, the transverse relaxation that the original NMR relaxation attenuation curve of gained sample obtains standard specimen after Inversion Calculation is distributed
Spectrum records each standard specimen transverse relaxation distribution spectral peak gross area, then using Oleoresin Contents in soxhlet extraction methods measurement standard specimen, builds
The standard curve of vertical transverse relaxation distribution the spectral peak gross area and standard specimen Oleoresin Contents, then the sample of Oleoresin Contents to be measured is surveyed
Amount, by resulting relaxation distribution the spectral peak gross area bring standard curve into, obtain the Oleoresin Contents of sample to be tested, so can acquire to
Sample Oleoresin Contents ratio.
The pine class sawn timber Oleoresin Contents test method based on time domain nuclear magnetic resonance, feature the following steps are included:
A instrumental correction: the centre frequency and pulse width of standard oil sample correction time domain Nuclear Magnetic Resonance, correction course are used
Using free damping FID sequence, sampling number 2048, sequence multiple scanning latency period is 2000ms；
B establishes standard curve: the pine sample for taking 10-15 quality size to have differences is sawed from a certain tree species pine sawn timber
Product, it is dry according to wood vacuum specified in National Standard of the People's Republic of China GB1931-91 " moisture content test method "
Drying method is dried in vacuo pine standard specimen, excludes the moisture in pine standard specimen, and record pine standard specimen quality at this time, this
The quality of Shi Songmu standard specimen is lumber quality and rosin quality sum.Then lateral the relaxing of CPMG sequence acquisition pine standard specimen is utilized
Henan attenuation curve obtains transverse relaxation distribution profile after carrying out inverting to it and records its peak gross area.It is total further in accordance with the Chinese people
With prescriptive procedure in state standard GB/T/T2677.6-94 " measurement of paper making raw material organic solvent extract content ", to
Pine standard specimen after vacuum drying carries out ether extraction, after the rosin ingredient dissolution in pine standard specimen, again according to middle Chinese
Prescriptive procedure is dried pine standard specimen with 103 ± 2 DEG C in people republic standard GB/T 1931-91 " moisture content test method "
To over dry, the absolute dry mass of pine standard specimen is recorded.Pine standard specimen quality and the difference of pine absolute dry mass are pine after vacuum drying
Rosin quality in standard specimen.Rosin quality in the pine standard specimen transverse relaxation distribution spectral peak gross area and standard specimen is fitted and is marked
Directrix curve: Y=AX+B, wherein Y is rosin quality in pine standard specimen, and X is the transverse relaxation distribution spectral peak gross area, B be operation and
Constant term caused by instrument error；
The measurement of c sample: taking the sample to be tested of certain mass, carries out obtaining after vacuum drying treatment to it after it removes moisture
Mass M 0, measure its transverse relaxation attenuation curve and carry out Inversion Calculation obtain relaxation distribution profile, record transverse relaxation distribution
Spectral peak gross area X0；
D Oleoresin Contents calculate: by resulting transverse relaxation distribution spectral peak gross area X0 bring standard curve into, be calculated to
Oleoresin Contents Y0 in Pine Samples is surveyed, and then rosin ratio Z0, Z0=100% × Y0/ (M0- contained by pine sample to be measured can be obtained
Y0)。
The pine standard specimen moisture vacuum drying parameter is as follows: not more than 50 DEG C of temperature, vacuum degree when vacuum drying
Not less than 0.88KPa, the quality for obtaining pine standard specimen is lumber quality and rosin quality sum, the Pine Samples after vacuum drying
It is extracted using ether, guarantee only removes rosin.
CPMG sequence parameter used by the pine standard specimen transverse relaxation is tested is as follows: between the adjacent multiple scanning of sample
Between be divided into 2000ms, 180 degree pulse number is 3000, and the 180 degree pulse echo time is 0.1ms, avoids collecting pine
Standard specimen solid signal, multiple scanning number 64-256 times.
It is SIRT algorithm that the Pine Samples transverse relaxation attenuation curve inverting, which obtains algorithm used in relaxation distribution spectrogram,
The number of iterations is 100000-1000000 times.
The beneficial effects of the present invention are: relative to traditional test method, test method of the present invention without pair
Pine Samples carry out managed chemical reagent ether extraction processing processed, and test process is nontoxic, harmless, and test method is quick and precisely.
Detailed description of the invention
Fig. 1 is that vacuum drying front and back pine sample transverse relaxation is distributed spectrogram
Fig. 2 is transverse relaxation distribution spectrogram after the multiple pine sample vacuum drying of the embodiment of the present invention
Fig. 3 is the fit standard song that pine of embodiment of the present invention sample Oleoresin Contents and transverse relaxation are distributed spectral peak area
Line schematic diagram
Fig. 4 is transverse relaxation distribution spectrogram after the multiple masson pine sample vacuum drying of the embodiment of the present invention
Fig. 5 is the fit standard song that masson pine of embodiment of the present invention sample Oleoresin Contents and transverse relaxation are distributed spectral peak area
Line schematic diagram
Specific embodiment
Embodiment 1
1 experimental material
Sawn timber of New Zealand's import pine log after the dry preliminary working of saw lumber, ether analysis are pure.
2 laboratory apparatus
Suzhou Niu Mai analysis instrument limited liability company production NMI-20 nuclear magnetic resonance spectroscopy tester (magnetic field strength 0.43T,
Bore probe 20mm), Shanghai Bo Xun Medical Devices Co., Ltd produces BZF-50 vacuum oven, Sai Duolisi scientific instrument (north
Capital) Co., Ltd's BSA224S-CW electronic balance, Soxhlet extractor.
3 experimental procedures
Using the centre frequency and pulse width of standard oil sample correction time domain Nuclear Magnetic Resonance, correction course, which uses, freely to decline
Subtract FID sequence, sampling number 2048, sequence multiple scanning latency period is 2000ms；
The sample for taking 10 quality sizes to have differences is sawed from pine sawn timber, is marked according to country, the People's Republic of China (PRC)
Vacuum drying of wood method specified in quasi- GB1931-91 " moisture content test method ", is dried in vacuo standard specimen, row
Except the moisture in pine standard specimen, and record standard specimen quality at this time.Then the transverse relaxation of each standard specimen is acquired using CPMG sequence
Attenuation curve, between the adjacent multiple scanning of sample between be divided into 2000ms, 180 degree pulse number is 3000, and 180 degree pulse is returned
The wave time be 0.1ms, multiple scanning number 64 times.Sample transverse relaxation attenuation curve obtains relaxation point by the inverting of SIRT algorithm
Cloth spectrogram, the number of iterations are 100000 times, record its peak gross area.
According to National Standard of the People's Republic of China GB/T2677.6-94, " paper making raw material has after MRI scan
The measurement of solvent extract content " in prescriptive procedure to standard specimen carry out ether extraction, by sample rosin ingredient dissolve out
Afterwards, again according to prescriptive procedure in National Standard of the People's Republic of China GB1931-91 " moisture content test method " with 103
Sample is dried to over dry by ± 2 DEG C, records absolute dry mass, rosin quality in Mass Calculation sample after contrast sample vacuum drying.Its
After remaining sample also repeats above step, it is fitted after obtaining sample transverse relaxation distribution spectral peak area (Fig. 2) and rosin quality
Obtain standard curve (Fig. 3).
4 survey calculations
3 pine samples are taken, number is denoted as A, B, C respectively, is dried in vacuo to it, moisture in sample is excluded,
CPMG sequence acquires the transverse relaxation attenuation curve of each standard specimen, between the adjacent multiple scanning of sample between be divided into 2000ms, 180
Spend pulse number be 3000, the 180 degree pulse echo time be 0.1ms, multiple scanning number 64 times.Sample transverse relaxation decaying
Curve negotiating SIRT algorithm inverting obtains relaxation and is distributed spectrogram, and the number of iterations is 100000 times, records its peak gross area, gained peak
Area value brings calibration curve formula into, and Oleoresin Contents are calculated, and further calculates Oleoresin Contents ratio, after again to sample
Ether extraction is carried out, calculates Oleoresin Contents, then compare with the method for the present invention measurement result, concrete outcome such as table 1.
1 the method for the present invention of table and chemical solvent extraction process measure pine Oleoresin Contents Comparative result
Above-described embodiment is it can be proved that the method for the present invention testing result and chemical solvent extraction process measurement result relatively connect
Closely, Oleoresin Contents in pine sample more can be fast measured using nuclear magnetic resonance inverting peak area, avoided using by control
Organic solvent.
Embodiment 2
1 experimental material
Sawn timber of the masson pine log after the dry preliminary working of saw lumber, ether analysis are pure.
2 laboratory apparatus
Suzhou Niu Mai analysis instrument limited liability company production NMI-20 nuclear magnetic resonance spectroscopy tester (magnetic field strength 0.43T,
Bore probe 20mm), Shanghai Bo Xun Medical Devices Co., Ltd produces BZF-50 vacuum oven, Sai Duolisi scientific instrument (north
Capital) Co., Ltd's BSA224S-CW electronic balance, Soxhlet extractor.
3 experimental procedures
Using the centre frequency and pulse width of standard oil sample correction time domain Nuclear Magnetic Resonance, correction course, which uses, freely to decline
Subtract FID sequence, sampling number 2048, sequence multiple scanning latency period is 2000ms；
The sample for taking 10 quality sizes to have differences is sawed from Lumber of Pinus Massoniana, is marked according to country, the People's Republic of China (PRC)
Vacuum drying of wood method specified in quasi- GB1931-91 " moisture content test method ", is dried in vacuo standard specimen, row
Except the moisture in pine standard specimen, and record standard specimen quality at this time.Then the transverse relaxation of each standard specimen is acquired using CPMG sequence
Attenuation curve, between the adjacent multiple scanning of sample between be divided into 2000ms, 180 degree pulse number is 3000, and 180 degree pulse is returned
The wave time be 0.1ms, multiple scanning number 64 times.Sample transverse relaxation attenuation curve obtains relaxation point by the inverting of SIRT algorithm
Cloth spectrogram, the number of iterations are 100000 times, record its peak gross area.
According to National Standard of the People's Republic of China GB/T2677.6-94, " paper making raw material has after MRI scan
The measurement of solvent extract content " in prescriptive procedure to standard specimen carry out ether extraction, by sample rosin ingredient dissolve out
Afterwards, again according to prescriptive procedure in National Standard of the People's Republic of China GB1931-91 " moisture content test method " with 103
Sample is dried to over dry by ± 2 DEG C, records absolute dry mass, rosin quality in Mass Calculation sample after contrast sample vacuum drying.Its
After remaining sample also repeats above step, it is fitted after obtaining sample transverse relaxation distribution spectral peak area (Fig. 4) and rosin quality
Obtain standard curve (Fig. 5).
4 survey calculations
3 masson pine samples are taken, number is denoted as A, B, C respectively, is dried in vacuo to it, moisture in sample is excluded,
CPMG sequence acquires the transverse relaxation attenuation curve of each standard specimen, between the adjacent multiple scanning of sample between be divided into 2000ms, 180
Spend pulse number be 3000, the 180 degree pulse echo time be 0.1ms, multiple scanning number 64 times.Sample transverse relaxation decaying
Curve negotiating SIRT algorithm inverting obtains relaxation and is distributed spectrogram, and the number of iterations is 100000 times, records its peak gross area, gained peak
Area value brings calibration curve formula into, and Oleoresin Contents are calculated, and further calculates Oleoresin Contents ratio, after again to sample
Ether extraction is carried out, calculates Oleoresin Contents, then compare with the method for the present invention measurement result, concrete outcome such as table 2.
2 the method for the present invention of table and chemical solvent extraction process measure masson pine Oleoresin Contents Comparative result
Above-described embodiment is it can be proved that the method for the present invention testing result and chemical solvent extraction process measurement result relatively connect
Closely, Oleoresin Contents in masson pine sample more can be fast measured using nuclear magnetic resonance inverting peak area, avoided using by control
Organic solvent.
Claims (5)
1. a kind of pine class sawn timber Oleoresin Contents test method based on time domain nuclear magnetic resonance, it is characterised in that: in time domain nuclear-magnetism
CPMG sequence is used on resonance instrument, the standard specimen for measuring the vacuum dried rear different quality of some tree species pine sawn timber is multiple, will
The original NMR relaxation attenuation curve of gained sample obtains the transverse relaxation distribution profile of standard specimen after Inversion Calculation, record
Each standard specimen transverse relaxation is distributed the spectral peak gross area, then using Oleoresin Contents in soxhlet extraction methods measurement standard specimen, establishes laterally
Relaxation is distributed the standard curve of the spectral peak gross area and standard specimen Oleoresin Contents, then measures to the sample of Oleoresin Contents to be measured, will
The resulting relaxation distribution spectral peak gross area brings standard curve into, obtains the Oleoresin Contents of sample to be tested, and then acquire sample to be tested
Oleoresin Contents ratio.
2. the pine class sawn timber Oleoresin Contents test method according to claim 1 based on time domain nuclear magnetic resonance, feature
Be the following steps are included:
A instrumental correction: using the centre frequency and pulse width of standard oil sample correction time domain Nuclear Magnetic Resonance, correction course is used
Free damping FID sequence；
B establishes standard curve: the Pine Samples for taking 10-15 quality size to have differences are sawed from a certain tree species pine sawn timber,
According to vacuum drying of wood side specified in National Standard of the People's Republic of China GB1931-91 " moisture content test method "
Method is dried in vacuo pine standard specimen, excludes the moisture in pine standard specimen, and record pine standard specimen quality at this time, loose at this time
The quality of the wooden standard specimen is lumber quality and rosin quality sum；Then it is declined using the transverse relaxation of CPMG sequence acquisition pine standard specimen
Subtract curve, obtain transverse relaxation distribution profile after inverting is carried out to it and records its peak gross area；Further in accordance with the People's Republic of China (PRC)
Prescriptive procedure in standard GB/T/T2677.6-94 " measurement of paper making raw material organic solvent extract content ", to vacuum
Pine standard specimen after drying carries out ether extraction, total again according to the Chinese people after the rosin ingredient dissolution in pine standard specimen
Pine standard specimen is dried to absolutely with 103 ± 2 DEG C with prescriptive procedure in state standard GB/T 1931-91 " moisture content test method "
It is dry, record the absolute dry mass of pine standard specimen；Pine standard specimen quality and the difference of pine absolute dry mass are pine standard specimen after vacuum drying
Interior rosin quality；Rosin quality in the spectral peak gross area and standard specimen is distributed to pine standard specimen transverse relaxation to be fitted to obtain standard song
Line: Y=AX+B, wherein Y is rosin quality in pine standard specimen, and X is the transverse relaxation distribution spectral peak gross area, and A is fitting parameter, B
It is constant term caused by operation and instrument error；
The measurement of c sample: taking sample to be tested, obtains the mass M 0 after its removing moisture, measurement after vacuum drying treatment is carried out to it
Its transverse relaxation attenuation curve simultaneously carries out Inversion Calculation acquisition relaxation distribution profile, and record transverse relaxation is distributed spectral peak gross area X0；
D Oleoresin Contents calculate: bringing resulting transverse relaxation distribution spectral peak gross area X0 into standard curve, pine to be measured is calculated
Oleoresin Contents Y0 in the wooden sample, and then obtain rosin ratio Z0, Z0=100% × Y0/ (M0-Y0) contained by pine sample to be measured.
3. the pine class sawn timber Oleoresin Contents test method according to claim 2 based on time domain nuclear magnetic resonance, feature
It is to carry out vacuum drying treatment before sample carries out time domain MRI scan to exclude the moisture in pine standard specimen, is dried in vacuo
Not more than 50 DEG C of Shi Wendu, vacuum degree is not less than 0.88KPa, and the quality for obtaining pine standard specimen is lumber quality and rosin matter
The sum of amount, the Pine Samples after vacuum drying are extracted using ether, and guarantee only removes rosin.
4. the pine class sawn timber Oleoresin Contents test method according to claim 2 based on time domain nuclear magnetic resonance, feature
It is as follows to be that used CPMG sequence parameter is tested in pine standard specimen transverse relaxation: being divided between the adjacent multiple scanning of sample
2000ms, 180 degree pulse number are 3000-5000, and the 180 degree pulse echo time is 0.1ms, avoids collecting pine standard specimen
Solid signal, multiple scanning number are greater than 64 times.
5. the pine class sawn timber Oleoresin Contents test method according to claim 2 based on time domain nuclear magnetic resonance, feature
Being that the Pine Samples transverse relaxation attenuation curve inverting obtains algorithm used in relaxation distribution spectrogram is SIRT algorithm, iteration
Number is 100000-1000000 times.
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| CN112834548B (en) * | 2021-01-08 | 2022-08-19 | 上海纽迈电子科技有限公司 | Cross-linking density measuring method and device |
| CN113030148A (en) * | 2021-03-24 | 2021-06-25 | 浙江省林业科学研究院 | Microscopic on-line detection method for phase state change of water-soluble low-molecular-weight resin |
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