CN106468670A - A kind of tobacco moisture percentage method of testing based on time domain nuclear magnetic resonance, NMR inverting peak area - Google Patents
A kind of tobacco moisture percentage method of testing based on time domain nuclear magnetic resonance, NMR inverting peak area Download PDFInfo
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- G01N24/08—Investigating or analyzing materials by the use of nuclear magnetic resonance, electron paramagnetic resonance or other spin effects by using nuclear magnetic resonance
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Abstract
The present invention relates to a kind of tobacco moisture percentage method of testing based on time domain nuclear magnetic resonance, NMR inverting peak area, it is characterized in that using CPMG sequence in time domain nuclear magnetic resonance analyser, the Nicotiana tabacum L. standard specimen of 4～6 different qualities of measurement, gained initial data obtains the transverse relaxation spectrum of standard specimen after SIRT inverting, the first peak-to-peak area of record transverse relaxation spectrum, then micro-wave drying method is utilized to measure the water content of standard specimen, set up the standard curve of first peak-to-peak area data and standard specimen water content, the sample treating measured moisture content again measures, the first peak-to-peak area value of gained is brought into standard curve, obtain the water content of testing sample, and then testing sample moisture content can be tried to achieve.The present invention can eliminate the interference of oily signal in tobacco sample, is not affected by oil in Nicotiana tabacum L., detection speed is fast, result is accurate.Sample and solvent consumption need not be prepared, overcome the defect that nuclear magnetic signal mensuration survey tobacco moisture percentage cannot be distinguished by profit signal in Nicotiana tabacum L., improve the accuracy of Nicotiana tabacum L. profit signal sample measurement of water ratio.
Description
Technical field
The invention belongs to time domain nuclear magnetic resonance, NMR is detecting tobacco moisture percentage detection field and in particular to tobacco moisture percentage detects
Method.
Background technology
Moisture content in Nicotiana tabacum L. is an important quality index in tobacco processing course.Moisture content is measured in tobacco business
Method mainly have Oven Method, karl Fischer titrimetry, gas chromatography, infrared method, microwave method, near infrared spectroscopy etc..Card
The requirement to operator and detectable of two methods of Er Feixiu titrimetry and gas chromatography is higher, and detection time is special
It is not that the pre-treatment time is long, testing cost is costly.Although infrared method, microwave method detection speed are fast, testing result is easily subject to
The impact of the color of material, temperature and external environment, detection data deviation is big.Oven Method detection time is longer, testing result
Delayed, lose the original effect of moisture content detection it is impossible to meet the requirement of Nicotiana tabacum L. processing adjustment in time.
Time domain nuclear magnetic resonance, NMR has been widely used in food, oil exploration, high score as a kind of detection method of quick nondestructive
The fields such as sub- material.Due to the presence of oil substances in Nicotiana tabacum L., using the side of NMR signal measurement tobacco moisture percentage
Method, the method that the low-field nuclear magnetic resonance as disclosed in CN 103837560 A measures tobacco moisture percentage cannot be distinguished by profit signal,
Obtained NMR signal amount is oil mixing with water semaphore summation, affects measurement result accuracy.Lacked based on this technology
Fall into, set up a kind of be based on nuclear-magnetism, profit signal can be distinguished, quick and precisely test tobacco moisture percentage is to the processing of Nicotiana tabacum L. and research
Suffer from highly important meaning.
Content of the invention
The present invention provides a kind of tobacco moisture percentage method of testing based on time domain nuclear magnetic resonance, NMR inverting peak area, existing to solve
Problem with the presence of technology.
The object of the invention is realized by following technical proposals：
This tobacco moisture percentage method of testing based on time domain nuclear magnetic resonance, NMR inverting peak area is it is characterised in that be total in time domain nuclear-magnetism
Using CPMG sequence on Vibration Meter, the Nicotiana tabacum L. standard specimen of 4～6 different qualities of measurement, gained initial data obtains after SIRT inverting
To the transverse relaxation spectrum of standard specimen, the first peak-to-peak area of record transverse relaxation spectrum, then measure containing of standard specimen using micro-wave drying method
The water yield, sets up the standard curve of first peak-to-peak area data and standard specimen water content, then treats the sample of measured moisture content and measure, will
The first peak-to-peak area value of gained brings standard curve into, obtains the water content of testing sample, and then can try to achieve testing sample moisture content.
The described tobacco moisture percentage method of testing based on time domain nuclear magnetic resonance, NMR inverting peak area is it is characterised in that include following
Step：
A. instrumental correction：Using standard oil sample correct time domain nuclear magnetic resonance analyser mid frequency be 21.2945～
21.2946MHz, pulse width is 90～180 degree；Correction uses FID sequence, and sampling number 2048, between adjacent multiple scanning
Be spaced apart 2000 ms；
B. Criterion curve：The tobacco sample taking 4～6 certain mass gradients, as standard specimen, measures mark using CPMG sequence
The transverse relaxation spectrum of sample, the data obtained records first peak-to-peak area figures after SIRT inverting, then tobacco sample is micro- at 105 DEG C
Ripple drying, to constant weight, is calculated the water content of described standard specimen, then standard specimen head peak-to-peak area value and standard specimen water content is entered
Row matching obtains standard curve：Y=kx+b, wherein y are standard specimen water content, and x is first peak-to-peak area value, and b is operation and instrumental error
The constant term causing；
C. sample measurement：Take the testing sample of certain known quality（m0）, the transverse relaxation of standard specimen is measured using CPMG sequence
Spectrum, extracts first peak-to-peak area value x after inverting0；
D. moisture content measuring and calculating：First peak area x by gained0Bring standard curve into, be calculated the water content of tobacco sample to be measured
y0, testing sample moisture content=y0/m0×100%.
CPMG parameter used by described transverse relaxation spectrum test is as follows：180 degree pulse number is 1000～1500,180 degree
Pulse spacing is 0.5 ms, and multiple scanning number of times is 16 times, is spaced apart 1000～2000 ms between adjacent multiple scanning.
The algorithm that described inverting CMPG attenuation curve uses is SIRT algorithm, and iterationses are 10000 times.
Although water and oil cannot be distinguish between in resultant signal amount, due to their different transport properties of molecules, they
It is distributed in different regions, this situation is particularly evident in Nicotiana tabacum L. in transverse relaxation spectrum.As shown in figure 1, moisture position in Nicotiana tabacum L.
In first peak of transverse relaxation spectrum, distribution of relaxation times is in the range of 0.1 ms to 1 ms.Meanwhile, the oil in Nicotiana tabacum L.
In the range of relaxation time 10 ms to 100 ms, water oil signal does not have overlap to cloth, therefore individually can be divided using transverse relaxation spectrum
The signal of moisture in analysis Nicotiana tabacum L., the interference of oily signal in exclusion Nicotiana tabacum L..The size of first peak-to-peak area in the transverse relaxation spectrum of Nicotiana tabacum L.
It is directly proportional with the water content of Nicotiana tabacum L..The first peak-to-peak area that the present invention is composed using water content and the transverse relaxation of standard specimen matching foundation
Standard curve, can accurately measure rapidly the moisture content of tobacco sample to be measured.
The invention has the beneficial effects as follows：The present invention can eliminate the interference of oily signal in tobacco sample, is not subject to oil in Nicotiana tabacum L.
Impact, the moisture content detecting method traditional compared to Oven Method, gas chromatography etc., detection speed of the present invention is fast, each sample
Product examine is surveyed and is only needed 1min, and testing result accurately, need not be prepared sample and solvent consumption and sample nondestructive consumption, need not in high volume be dried
Experiment, only carries out microwave drying to standard specimen, testing sample direct nuclear-magnetism measurement is obtained a result, overcomes nuclear magnetic signal mensuration survey cigarette
Careless moisture content cannot be distinguished by the defect of profit signal in Nicotiana tabacum L., improves Nicotiana tabacum L. and there is profit signal sample measurement of water ratio simultaneously
Accuracy, green energy conservation, suitable batch samples measure.
Brief description
Fig. 1 is the transverse relaxation spectrogram of different water cut equal in quality tobacco shred.
Fig. 2 is the fit standard curve synoptic diagram of Nicotiana tabacum L. standard specimen water content of the present invention and peak area semaphore.
Specific embodiment
The invention will be further described with reference to embodiments.
1st, experiment material
In Hebei, cigarette industry Co., Ltd produces three cigarette samples tobacco shred A, B, C.
2nd, experimental apparatus
Suzhou Niu Mai analytical tool limited company produces PQ-001 nuclear magnetic resonance analyser（Magnetic field intensity 0.5 T, bore probe
15mm）And microwave drying system；Mettler Toledo Inc. of Switzerland produces MS304S electronic balance.
3rd, experimental procedure
A. using standard configuration oil sample, PQ-001 nuclear magnetic resonance analyser is corrected, adjustment centre frequency be 21.2945～
21.2946MHz, 90 degree of adjustment and 180 degree pulse width, correction uses FID sequence, sampling number 2048, adjacent multiple scanning
Between be spaced apart 2000 ms.
B. take A sample 0.5g, 0.7g, 0.9g, 1.1g, 1.3g as standard specimen, measure the horizontal of each standard specimen with CPMG sequence
Relaxation spectrum, the data obtained extracts first peak-to-peak area value after SIRT inverting,（Inverting CMPG attenuation curve use algorithm be
SIRT algorithm, iterationses are 10000 times,）By tobacco sample after 105 DEG C of microwave drying are to constant weight, it is calculated standard specimen
Water content, then is fitted obtaining standard curve to standard specimen head peak-to-peak area value and standard specimen water content： y=43115x +
57.76（R2=0.999）, as shown in Fig. 2 wherein microwave dryer carries balance, temperature sense and temperature control accessory, connect core
Magnetic industrial computer, can under 105 DEG C of steady temperatures rapid draing Nicotiana tabacum L. standard specimen, take about 5 min, and automatically calculate water content.
C. measurement measuring and calculating：Take each 0.8g of cigarette shreds sample A, B, C respectively, horizontal using CPMG sequence measuring samples
Relaxation spectrum, extracts first peak-to-peak area value, and wherein CPMG parameter used by the test of transverse relaxation spectrum is：180 degree pulse number is 1000
～1500, the 180 degree pulse spacing is 0.5 ms, and multiple scanning number of times is 16 times, being spaced apart between adjacent multiple scanning
1000～2000 ms.3 Duplicate Samples surveyed by each sample, and gained peak area value brings above-mentioned standard curve into after calculating meansigma methodss public
Formula, is calculated water content, and then utilizes testing sample moisture content=y0/m0× 100% tries to achieve moisture content, concrete outcome such as table 1.
Table 1 present invention, micro-wave drying method and the contrast of nuclear magnetic signal mensuration moisture content testing result
Above-described embodiment may certify that, the inventive method testing result and micro-wave drying method are relatively, anti-using nuclear magnetic resonance, NMR
Drill the moisture content that peak area can preferably measure in tobacco sample；Compared with mensuration with nuclear magnetic signal, signal will not be subject to oils and fatss
Interference, result is more accurate.
Claims (4)
1. a kind of tobacco moisture percentage method of testing based on time domain nuclear magnetic resonance, NMR inverting peak area it is characterised in that：In time domain core
Using CPMG sequence on magnetic resonance device, the Nicotiana tabacum L. standard specimen of 4～6 different qualities of measurement, gained initial data is through SIRT（Simultaneous
Iterative reconstruction technique）Obtain the transverse relaxation spectrum of standard specimen, the first peak-to-peak area of record transverse relaxation spectrum after inverting, then utilize micro-
Ripple seasoning measures the water content of standard specimen, sets up the standard curve of first peak-to-peak area data and standard specimen water content, then contains to be measured
The sample of the water yield measures, and the first peak-to-peak area value of gained is brought into standard curve, obtains the water content of testing sample, and then
Testing sample moisture content can be tried to achieve.
2. the tobacco moisture percentage method of testing based on time domain nuclear magnetic resonance, NMR inverting peak area according to claim 1, it is special
Levy and be to comprise the following steps：
A. instrumental correction：Using standard oil sample correct time domain nuclear magnetic resonance analyser mid frequency be 21.2945～
21.2946MHz, pulse width is 90 degree and 180 degree；Correction use FID sequence, sampling number 2048, adjacent multiple scanning it
Between be spaced apart 2000 ms；
B. Criterion curve：The tobacco sample taking 4～6 certain mass gradients, as standard specimen, measures mark using CPMG sequence
The transverse relaxation spectrum of sample, the data obtained records first peak-to-peak area figures after SIRT inverting, then tobacco sample is micro- at 105 DEG C
Ripple drying, to constant weight, is calculated the water content of described standard specimen, then standard specimen head peak-to-peak area value and standard specimen water content is entered
Row matching obtains standard curve：Y=kx+b, wherein y are standard specimen water content, and x is first peak-to-peak area value, and b is operation and instrumental error
The constant term causing；
C. sample measurement：Take the testing sample of certain known quality（m0）, measure its transverse relaxation spectrum, extract first peak-to-peak area value
x0；
D. moisture content measuring and calculating：First peak area x by gained0Bring standard curve into, be calculated the water content of tobacco sample to be measured
y0, and then tobacco sample moisture content=y to be measured can be obtained0/m0×100%.
3. the tobacco moisture percentage method of testing based on time domain nuclear magnetic resonance, NMR inverting peak area according to claim 2, it is special
Levy and be that CPMG parameter used by described transverse relaxation spectrum test is as follows：180 degree pulse number is 1000～1500,180 degree arteries and veins
Punching is spaced apart 0.5 ms；Multiple scanning number of times is 16 times, is spaced apart 1000～2000 ms between adjacent multiple scanning.
4. the tobacco moisture percentage method of testing based on time domain nuclear magnetic resonance, NMR inverting peak area according to claim 2, it is special
Levy and be that the algorithm that described inverting CMPG attenuation curve uses is SIRT algorithm, iterationses are 10000 times.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106959315A (en) * | 2017-03-10 | 2017-07-18 | 河北中烟工业有限责任公司 | A kind of method of testing of tobacco moisture diffusion velocity |
| CN107064240A (en) * | 2017-04-11 | 2017-08-18 | 江南大学 | A kind of on-line monitoring system based on dielectric property dynamic change |
| CN107247064A (en) * | 2017-05-09 | 2017-10-13 | 江南大学 | A kind of analysis method of low field nuclear-magnetism Non-Destructive Testing Daqu moisture |
| CN108333075A (en) * | 2018-02-08 | 2018-07-27 | 中原工学院 | Hygroscopic water transmission testing method in fire-retardant Thermal Protective Fabric under a kind of simulation scene of a fire |
| CN109115823A (en) * | 2018-08-27 | 2019-01-01 | 南京农业大学 | One kind being based on LF-NMR pork moisture content rapid detection method |
| CN109490349A (en) * | 2019-01-16 | 2019-03-19 | 江南大学 | A kind of analysis method of low field nuclear-magnetism non-destructive testing white wine distiller's yeast water activity |
| CN109613042A (en) * | 2018-12-27 | 2019-04-12 | 中国林业科学研究院木材工业研究所 | A kind of pine class sawn timber Oleoresin Contents test method based on time domain nuclear magnetic resonance |
| CN110879234A (en) * | 2019-12-27 | 2020-03-13 | 中国矿业大学 | Method for rapidly detecting total moisture of coal based on low-field nuclear magnetic resonance |
| CN110887860A (en) * | 2019-11-28 | 2020-03-17 | 同济大学 | Method for detecting water content of sand based on low-field nuclear magnetic resonance |
| CN111007096A (en) * | 2019-11-29 | 2020-04-14 | 同济大学 | Method for measuring water content of sand |
| CN111122636A (en) * | 2019-12-10 | 2020-05-08 | 同济大学 | Method for measuring setting time of sulphoaluminate cement by using hydrogen proton low-field nuclear magnetic resonance technology |
| CN111595885A (en) * | 2019-04-22 | 2020-08-28 | 苏州纽迈分析仪器股份有限公司 | Calibration standard sample for testing fluorine content and sealing method and application thereof |
| CN112649459A (en) * | 2019-10-12 | 2021-04-13 | 中国石油化工股份有限公司 | Time-domain nuclear magnetic resonance-based composite material component content determination method and system |
| CN112730497A (en) * | 2020-12-21 | 2021-04-30 | 贺州学院 | Vacuum fried pleurotus eryngii strip moisture and grease rapid detection technology based on low-field nuclear magnetic resonance |
| CN112834541A (en) * | 2020-01-03 | 2021-05-25 | 上海纽迈电子科技有限公司 | Method for testing sodium content and sodium distribution |
| CN112834546A (en) * | 2020-12-01 | 2021-05-25 | 上海纽迈电子科技有限公司 | Method for testing water content and oil content in plant grains and application thereof |
| CN114609324A (en) * | 2022-02-28 | 2022-06-10 | 中南林业科技大学 | Method for rapidly judging and judging drying effect of rice |
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Cited By (18)
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|---|---|---|---|---|
| CN106959315A (en) * | 2017-03-10 | 2017-07-18 | 河北中烟工业有限责任公司 | A kind of method of testing of tobacco moisture diffusion velocity |
| CN107064240A (en) * | 2017-04-11 | 2017-08-18 | 江南大学 | A kind of on-line monitoring system based on dielectric property dynamic change |
| CN107247064A (en) * | 2017-05-09 | 2017-10-13 | 江南大学 | A kind of analysis method of low field nuclear-magnetism Non-Destructive Testing Daqu moisture |
| CN108333075A (en) * | 2018-02-08 | 2018-07-27 | 中原工学院 | Hygroscopic water transmission testing method in fire-retardant Thermal Protective Fabric under a kind of simulation scene of a fire |
| CN109115823A (en) * | 2018-08-27 | 2019-01-01 | 南京农业大学 | One kind being based on LF-NMR pork moisture content rapid detection method |
| CN109613042A (en) * | 2018-12-27 | 2019-04-12 | 中国林业科学研究院木材工业研究所 | A kind of pine class sawn timber Oleoresin Contents test method based on time domain nuclear magnetic resonance |
| CN109490349A (en) * | 2019-01-16 | 2019-03-19 | 江南大学 | A kind of analysis method of low field nuclear-magnetism non-destructive testing white wine distiller's yeast water activity |
| CN111595885A (en) * | 2019-04-22 | 2020-08-28 | 苏州纽迈分析仪器股份有限公司 | Calibration standard sample for testing fluorine content and sealing method and application thereof |
| CN112649459A (en) * | 2019-10-12 | 2021-04-13 | 中国石油化工股份有限公司 | Time-domain nuclear magnetic resonance-based composite material component content determination method and system |
| CN110887860A (en) * | 2019-11-28 | 2020-03-17 | 同济大学 | Method for detecting water content of sand based on low-field nuclear magnetic resonance |
| CN111007096A (en) * | 2019-11-29 | 2020-04-14 | 同济大学 | Method for measuring water content of sand |
| CN111122636A (en) * | 2019-12-10 | 2020-05-08 | 同济大学 | Method for measuring setting time of sulphoaluminate cement by using hydrogen proton low-field nuclear magnetic resonance technology |
| CN110879234A (en) * | 2019-12-27 | 2020-03-13 | 中国矿业大学 | Method for rapidly detecting total moisture of coal based on low-field nuclear magnetic resonance |
| CN112834541A (en) * | 2020-01-03 | 2021-05-25 | 上海纽迈电子科技有限公司 | Method for testing sodium content and sodium distribution |
| CN112834546A (en) * | 2020-12-01 | 2021-05-25 | 上海纽迈电子科技有限公司 | Method for testing water content and oil content in plant grains and application thereof |
| CN112730497A (en) * | 2020-12-21 | 2021-04-30 | 贺州学院 | Vacuum fried pleurotus eryngii strip moisture and grease rapid detection technology based on low-field nuclear magnetic resonance |
| CN114609324A (en) * | 2022-02-28 | 2022-06-10 | 中南林业科技大学 | Method for rapidly judging and judging drying effect of rice |
| CN114609324B (en) * | 2022-02-28 | 2024-05-17 | 中南林业科技大学 | Method for rapidly judging rice drying effect |
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