CN107561109A - Fresh peanut moisture content detecting method based on nuclear magnetic resonance transverse relaxation spectral technology - Google Patents

Fresh peanut moisture content detecting method based on nuclear magnetic resonance transverse relaxation spectral technology Download PDF

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CN107561109A
CN107561109A CN201710655641.4A CN201710655641A CN107561109A CN 107561109 A CN107561109 A CN 107561109A CN 201710655641 A CN201710655641 A CN 201710655641A CN 107561109 A CN107561109 A CN 107561109A
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China
Prior art keywords
transverse relaxation
drying
moisture content
fresh peanut
sample
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CN201710655641.4A
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钟鹏
王彦芳
王殿生
焦志勇
周丽霞
石志强
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China University of Petroleum East China
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China University of Petroleum East China
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Abstract

The present invention relates to a kind of fresh peanut moisture content detecting method based on nuclear magnetic resonance transverse relaxation spectral technology, the proportional relation of gross area rate of change is composed with the front and rear transverse relaxation of drying by the mass change before and after the drying of fresh peanut, to obtain the proportional relation of the transverse relaxation spectrum gross area rate of change before and after fresh peanut moisture content and its are dried and establish standard curve, so as to obtain fresh peanut moisture content to be measured.The present invention carries out high-moisture percentage detection for nuclear magnetic resonance technique and has opened up a new approaches, i.e., without using the difference at profit peak, and the variation relation that the gross area is composed using transverse relaxation obtains the change of moisture content.This method has wide significance and practical value for the measurement of water ratio of the high fresh crop of moisture with analysis.

Description

Fresh peanut moisture content detecting method based on nuclear magnetic resonance transverse relaxation spectral technology
Technical field
The present invention relates to a kind of fresh peanut moisture content detecting method, and in particular to one kind is composed based on nuclear magnetic resonance transverse relaxation The fresh peanut moisture content detecting method of technology.
Background technology
Fresh peanut moisture content is higher, and typically between 25% to 50%, the parameter is the selection of its processing technology and technology The foundation of parameter configuration, and instruct the important measures of packaging and safe storage.The method master of measure fresh peanut moisture content at present There are traditional Oven Method and the contact pin type water content detection method based on Theory of Electromagnetic Field.The new instrument of Oven Method has infrared moisture Analyzer, is such as preced with Asia/SFY-60, and the halogen heater of its ring-type ensures sample thermally equivalent during high temperature test, makes sample Product surface is not easily damaged, rapid draing, and in the drying process, the moisture that Moisture Meter test constantly and instant playback sample are lost contains Percentage is measured, after the completion of drying program, the locked display of moisture content value that finally determines.The peanut determination of moisture of contact pin method Instrument, such as the SH series contact pin type moisture detectors that Shenzhen Ai Gerui is produced, instrument can be around test probe in use The electromagnetic field sensitive to hydrone is produced, the characteristic that energy is absorbed using hydrone produces fixed electric field energy and the electric field lost It can be compared and draw accurate moisture value.For the different measured object of water content, instrument according to the energy difference that it absorbs from And draw different moisture values and come.
The advantages of Oven Method is simple to operate, and measurement is accurate, and shortcoming is to need all to dry the moisture of sample to obtain To moisture content data;Contact pin method need not dry moisture, can obtain sample moisture content in real time, but need to insert test probe Enter in sample, sample is caused damage.
The near infrared spectrum detection method of rising in recent years is a kind of lossless, quick determination method, but its algorithm is complicated, and by The affect traits such as thickness of sample, size, color are big, not general enough.
Low-field nuclear magnetic resonance (NMR) relaxation spectrum technology can quickly, nondestructively determine food water, study moisture in food Multidate information change.The method tested at present for peanut oil content and low-water-content nuclear magnetic resonance.But for containing The high fresh peanut of water rate, because the oil in its relaxation spectrum, water peak produce part and are folded, therefore be also not based on nuclear magnetic resonance technique Detection method.
The content of the invention
In view of the above-mentioned problems, the present invention provides a kind of difference without using profit peak, and use the transverse relaxation spectrum gross area Variation relation obtain the fresh peanut moisture content detecting method based on nuclear magnetic resonance transverse relaxation spectral technology of moisture content.
In view of the above-mentioned problems, the technical scheme that the present invention takes is:Fresh flower based on nuclear magnetic resonance transverse relaxation spectral technology Raw moisture content detecting method, comprises the following steps:
Step 1: randomly selecting fresh peanut sample, and weigh the initial mass of each sample, i.e. m respectively with balance0
Step 2: measuring the one-dimensional transverse relaxation spectrum of each sample respectively using CPMG pulse sequence, transverse relaxation spectrum is obtained Initial area, i.e. s0
Step 3: using thermostatic equipment by the matter after each sample drying that after the low constant temperature drying of each sample, makes to weigh with scale Amount, i.e. m1
Step 4: measuring the one-dimensional transverse relaxation spectrum after each sample drying respectively using CPMG pulse sequence, dried The area of transverse relaxation spectrum afterwards, i.e. s1
Step 5: the mass change before and after the drying of acquisition fresh peanut composes gross area change with the front and rear transverse relaxation of drying The proportional relation of rate:
Δ m is of poor quality before and after fresh peanut is dried, and Δ s is that the front and rear transverse relaxation spectrum gross area of fresh peanut drying is poor;
Under conditions of low temperature drying, the quality lost is entirely the water of various forms, therefore sets percentage of water lossSeparately If the rate of change of the relaxation spectrum gross areaThat is η '=a × K+b (2)
(1) a, b in formula, (2) formula are constant;
Step 6: obtain fresh peanut moisture content dries the proportional relation of front and rear transverse relaxation spectrum gross area rate of change with it And establish standard curve:
It is proportional i.e. that peanut moisture content η and percentage of water loss η ' under low temperature drying state can be demonstrate,proved by experiment
η=c × η '+d formulas (3)
(3) c, d in formula are constant;
A, b, c, d are constants, for intermediate variable of the formula during derived;
(2) formula substitution (3) formula is obtained into fresh peanut moisture content η and dries front and rear transverse relaxation spectrum gross area rate of change with it K proportional relation
η=e × K+f (4)
(4) e, f in formula are constant;
The transverse relaxation spectrum front and rear with drying of several water-cut variation values according to corresponding to abovementioned steps obtain each sample is total The average value of the average value of area change rate, i.e. Δ η and Δ K, establishes standard curve;
Wherein, the moisture content of each sample is to be calculated to obtain according to mass change, because the boiling point of peanut oil is left at 335 degree The right side, and temperature during low temperature drying is 103 degree, so the quality that peanut loses can determine whether to be entirely moisture, therefore standard is bent In line, the moisture content η of peanut is known, and due to magnetic nuclear resonance method, dry front and rear transverse relaxation spectrum gross area change Rate k values are also known, therefore, with several points are done, can fit e and f value.
Step 7: take a fresh peanut to be measured, measure that transverse relaxation before its drying composes respectively using CPMG pulse sequence just The area that transverse relaxation is composed after beginning area and drying;And then transverse relaxation spectrum gross area rate of change K is obtained, according to standard song Line, obtain fresh peanut moisture content η.
The one-dimensional transverse relaxation spectrum of CPMG pulse sequence measurement peanut, its major parameter include:Relaxation peak number, each peak rise The only parameter such as time, peak maximum time and peak area.Wherein, relaxation peak number characterizes contains in sample1The different material of H atom core Composition, the relaxation time of the peak maximum time representation material, peak area characterize1H atom core average proton signal amplitude.
In step 3, the mass change before and after sample drying is less than 0.2%, then assert constant mass, drying terminates; Otherwise, drying is continued until the mass change before and after sample drying is less than 0.2%, untill constant mass.
The present invention carries out high-moisture percentage detection for nuclear magnetic resonance technique and has opened up a new approaches, i.e., without using profit peak Difference, and the variation relation that the gross area is composed using transverse relaxation obtains the change of moisture content.This method is high for moisture The measurement of water ratio of fresh crop has wide significance and practical value with analysis.
Figure of description
Fig. 1 is that fresh peanut and the transverse relaxation of peanut oil nuclear magnetic resonance are composed;
Fig. 2 is the Establishing process figure that fresh peanut moisture content composes gross area rate of change standard curve with transverse relaxation;
Fig. 3 is the flow chart that fresh peanut moisture content is measured according to standard curve;
Fig. 4 is the graph of relation that fresh peanut moisture content composes gross area rate of change with transverse relaxation;
Fig. 5 is standard curve the result figure.
Embodiment
Fig. 1 is that fresh peanut and the transverse relaxation of peanut oil nuclear magnetic resonance are composed.Active ingredient in fresh peanut is:Fresh peanut is main Functional component is fat, protein, carbohydrate and moisture, therefore1H cores are essentially from fat, with reference to water, (protein is close With reference to water), semi-free water (carbohydrate) and Free water.Peanut oil component is denoted as:Protein, carbohydrate content For 0%, fat content 99.9%.Wherein fatty each component content:Saturated fat 17.8%;Single unsaturated lipid 43.9%;It is more Unsaturated fat 38.2%.Therefore the NMR relaxation peak of peanut oil is entirely fat.Using this peak as the fat in fresh peanut Composition is calibrated.With reference to the functional component of fresh peanut and the relaxation spectral curve of peanut oil, the explanation of fresh peanut relaxation spectrum, peak can obtain 1 is with reference to water, 2 semi-free water of peak;Peak 3 is Free water, and peak 4 is fatty peak 1, and peak 5 is fatty peak 2, due to peak 3 and the part of peak 4 It is overlapped, therefore oil, water peak can not be completely separable, it is impossible to the aqueous of fresh peanut is directly speculated according to the size of water peak peak area Situation.
Accordingly, the present invention provides a kind of fresh peanut moisture content detecting method based on nuclear magnetic resonance transverse relaxation spectral technology, As shown in Figure 2 and Figure 3, comprise the following steps:
Step 1: randomly selecting fresh peanut sample, and weigh the initial mass of each sample, i.e. m respectively with balance0
Step 2: measuring the one-dimensional transverse relaxation spectrum of each sample respectively using CPMG pulse sequence, transverse relaxation spectrum is obtained Initial area, i.e. s0
Step 3: using thermostatic equipment by the low constant temperature drying of each sample, the mass change before and after sample drying is less than 0.2%, then assert constant mass, drying terminates;Otherwise, drying is continued until the mass change before and after sample drying is less than 0.2%, untill constant mass;The quality for making to weigh with scale after each sample drying, i.e. m1
Step 4: measuring the one-dimensional transverse relaxation spectrum after each sample drying respectively using CPMG pulse sequence, dried The area of transverse relaxation spectrum afterwards, i.e. s1
Step 5: the mass change before and after the drying of acquisition fresh peanut composes gross area change with the front and rear transverse relaxation of drying The proportional relation of rate:
Δ m is of poor quality before and after fresh peanut is dried, and Δ s is that the front and rear transverse relaxation spectrum gross area of fresh peanut drying is poor;
Under conditions of low temperature drying, the quality lost is entirely the water of various forms, therefore
If percentage of water lossThe another rate of change for setting the relaxation spectrum gross area
That is η '=a × K+b (2)
(1) a, b in formula, (2) formula are constant;
Step 6: obtain fresh peanut moisture content dries the proportional relation of front and rear transverse relaxation spectrum gross area rate of change with it And establish standard curve:
It is proportional i.e. that peanut moisture content η and percentage of water loss η ' under low temperature drying state can be demonstrate,proved by experiment
η=c × η '+d formulas (3)
(3) c, d in formula are constant;
(2) formula substitution (3) formula is obtained into fresh peanut moisture content η and dries front and rear horizontal stroke with it
To relaxation spectrum gross area rate of change K proportional relation
η=e × K+f (4)
(4) e, f in formula are constant;
The transverse relaxation spectrum front and rear with drying of several water-cut variation values according to corresponding to abovementioned steps obtain each sample is total The average value of the average value of area change rate, i.e. Δ η and Δ K, establishes standard curve;
Step 7: take a fresh peanut to be measured, measure that transverse relaxation before its drying composes respectively using CPMG pulse sequence just The area that transverse relaxation is composed after beginning area and drying;And then transverse relaxation spectrum gross area rate of change K is obtained, according to standard song Line, obtain fresh peanut moisture content η.Two, fresh peanut sample is randomly choosed, (103 DEG C) of low temperature is dried 8 hours, during which small every 1 When, its quality and transverse relaxation spectrum are measured, fresh peanut moisture content η is obtained according to mass change η ', composed according to transverse relaxation Peak gross area rate of change obtains K, moisture content η and K relation curve such as Fig. 4, and y, X in figure correspond to η, K respectively.
η=1.0859K-0.0089 in figure
E i.e. in (4) formula is that 1.0859, f is square that -0.0089, R^2 is coefficient correlation, shows the fitted figure linearity Quality.
Using Fig. 4 relation curve as standard curve, randomly choose 5 sample low temperature dryings and carry out moisture content inspection in 1 hour Test card, as a result as shown in Figure 5.
Fig. 5 orbicular spots are the actual moisture content of each sample measured using Oven Method, and the relative error that both measure exists Between 10%, illustrate that this method can be estimated the moisture content of fresh peanut.

Claims (2)

1. the fresh peanut moisture content detecting method based on nuclear magnetic resonance transverse relaxation spectral technology, it is characterised in that including following step Suddenly:
Step 1: randomly selecting fresh peanut sample, and weigh the initial mass of each sample, i.e. m respectively with balance0
Step 2: measuring the one-dimensional transverse relaxation spectrum of each sample respectively using CPMG pulse sequence, the first of transverse relaxation spectrum is obtained Beginning area, i.e. s0
Step 3: using thermostatic equipment by the quality after each sample drying that after the low constant temperature drying of each sample, makes to weigh with scale, i.e., m1
Step 4: the one-dimensional transverse relaxation spectrum after each sample drying is measured respectively using CPMG pulse sequence, after being dried The area of transverse relaxation spectrum, i.e. s1
Step 5: the mass change before and after the drying of acquisition fresh peanut composes gross area rate of change with the front and rear transverse relaxation of drying Proportional relation:
<mrow> <mfrac> <mrow> <mi>&amp;Delta;</mi> <mi>m</mi> </mrow> <msub> <mi>m</mi> <mn>0</mn> </msub> </mfrac> <mo>=</mo> <mi>a</mi> <mo>&amp;times;</mo> <mfrac> <mrow> <mi>&amp;Delta;</mi> <mi>s</mi> </mrow> <msub> <mi>s</mi> <mn>0</mn> </msub> </mfrac> <mo>+</mo> <mi>b</mi> <mo>-</mo> <mo>-</mo> <mo>-</mo> <mrow> <mo>(</mo> <mn>1</mn> <mo>)</mo> </mrow> </mrow>
Δ m is of poor quality before and after fresh peanut is dried, and Δ s is that the front and rear transverse relaxation spectrum gross area of fresh peanut drying is poor;
Under conditions of low temperature drying, the quality lost is entirely the water of various forms, therefore
If percentage of water lossThe another rate of change for setting the relaxation spectrum gross area
That is η '=a × K+b (2)
(1) a, b in formula, (2) formula are constant;
Dry the proportional relation of front and rear transverse relaxation spectrum gross area rate of change Step 6: obtaining fresh peanut moisture content with it and build Day-mark directrix curve:
It is proportional i.e. that peanut moisture content η and percentage of water loss η ' under low temperature drying state can be demonstrate,proved by experiment
η=c × η '+d formulas (3)
(3) c, d in formula are constant;
(2) formula substitution (3) formula is obtained into fresh peanut moisture content η and dries front and rear transverse relaxation spectrum gross area rate of change K's with it Proportional relation
η=e × K+f (4)
(4) e, f in formula are constant;
The transverse relaxation spectrum gross area front and rear with drying of several water-cut variation values according to corresponding to abovementioned steps obtain each sample The average value of the average value of rate of change, i.e. Δ η and Δ K, establishes standard curve;
Step 7: taking a fresh peanut to be measured, the primary face of transverse relaxation spectrum before its drying is measured respectively using CPMG pulse sequence The area that transverse relaxation is composed after product and drying;And then transverse relaxation spectrum gross area rate of change K is obtained, according to standard curve, ask Go out fresh peanut moisture content η.
2. the fresh peanut moisture content detecting method according to claim 1 based on nuclear magnetic resonance transverse relaxation spectral technology, its It is characterised by:
In step 3, the mass change before and after sample drying is less than 0.2%, then assert constant mass, drying terminates;It is no Then, drying is continued until the mass change before and after sample drying is less than 0.2%, untill constant mass.
CN201710655641.4A 2017-08-03 2017-08-03 Fresh peanut moisture content detecting method based on nuclear magnetic resonance transverse relaxation spectral technology Pending CN107561109A (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
WO2019192088A1 (en) * 2018-04-04 2019-10-10 江南大学 Method for smart detection of moisture content and texture in fruits high in sugar for microwave spray/freeze drying
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Application publication date: 20180109