CN103743697A - Method for monitoring tea production in real time by adopting near infrared spectrum - Google Patents
Method for monitoring tea production in real time by adopting near infrared spectrum Download PDFInfo
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- CN103743697A CN103743697A CN201310710939.2A CN201310710939A CN103743697A CN 103743697 A CN103743697 A CN 103743697A CN 201310710939 A CN201310710939 A CN 201310710939A CN 103743697 A CN103743697 A CN 103743697A
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Abstract
The invention discloses a method for monitoring tea production in real time by adopting a near infrared spectrum. The method is characterized by comprising the following steps: (1) preparing a tea sample, namely collecting a tea sample with representativeness; (2) acquiring the near infrared spectrum, namely acquiring a diffuse reflection spectrum chart of the tea sample based on Workflow setting SOP (Standard Operation Process) and analysis method; (3) preprocessing the diffuse reflection spectrum chart, namely performing first-order or second-order derivative+Norris noise filtering processing on the spectrum chart; (4) establishing a model, namely establishing a mathematical model between data measured by the near infrared spectrum chart and the standard method by using special chemometrics software; (5) verifying the model, namely measuring a novel tea sample on a near infrared instrument according to a method which is identical to the step (2), predicting by using the model established in the step (4), and comparing the measured tea sample with the result measured according to a national standard method; and (6) performing field detection, namely performing near infrared spectrum scanning on a sample in the production field, measuring by using the model established in the step (4), and adjusting the field production conditions according to the measurement result.
Description
Technical field
The present invention relates to a kind of method of producing Real-Time Monitoring, particularly a kind of method that adopts near infrared spectrum to realize Tea Production Real-Time Monitoring.
Background technology
The complex chemical composition of tealeaves, according to GB regulation, in Tea Production and checkout procedure, need to analyze the many index compositions such as moisture content in tealeaves, Tea Polyphenols, amino acid.Measure these indexs, need to relate to complicated chemical method, as multiple instruments such as liquid chromatograph, baking oven, ultraviolet-visible pectrophotometers, sample analysis must carry out under laboratory condition.Examining report needs the time of several days just can obtain.Therefore, Tea Production mainly relies on the producer's experience, cannot realize the reliable quality control of online science.
In tealeaves, moisture is the key index that needs most control in Tea Production process, according to current methods GB/T 8304-2002 < < Measuring Moisture Content of Tea, measure > >, need in the baking oven in laboratory, heat 2 hours, or the longer time.Method operates length miscellaneous, consuming time, efficiency is low, cannot meet the On-line Control requirement of Tea Production process.Along with the development of technology and the raising of Quality Control requirement, Tea Production industry is in the urgent need to effective, can to carry out for the production of scene express-analysis analytical approach, to obtain in time reliable feedback data, for instructing production run, realize the line Quality Control of Tea Production.
Summary of the invention
The technical problem to be solved in the present invention is: for Measuring Moisture Content of Tea, measure and need under laboratory environment, carry out, and operate the defects such as loaded down with trivial details, length consuming time, a kind of online method detecting in real time of producing that can be used for is provided, does not need to pulverize, directly adopt tealeaves former state to analyze.Near infrared spectrum has reflected hydric group (C-H, N-H, O-H etc.) molecular vibration information, the important informations such as the moisture in very applicable measurement tealeaves, in conjunction with the multivariate data analysis method in Chemical Measurement, set up the analytical model of Measuring Moisture Content of Tea, thereby realize the line Quality Control of Tea Production process.
Technical scheme of the present invention is: a kind of method that adopts near infrared spectrum to realize Tea Production Real-Time Monitoring, comprises following steps:
(1) preparation of tealeaves sample: collected Tea Samples, after numbering, be contained in foil samples bag; Sealing refrigeration;
(2) collection of near infrared spectrum: based on Workflow established standards workflow (SOP) and analytical approach, gather the Tea Samples spectrogram that diffuses;
(3) diffuse reflection spectrum spectrum pre-service: spectrogram is carried out to " single order or second derivative+Norris filter is made an uproar " and process;
Data processing: the data processing of automatically being carried out all spectrum by TQ Analyst spectral analysis Chemical Measurement software;
(4) foundation of model: use TQ Analyst spectral analysis Chemical Measurement software, set up the mathematical model between the data that near infrared light spectrogram and standard method measured;
(5) checking of model: according to the identical method of the 2nd step, at nir instrument
The Tea Samples that upper measurement is new, and predict with the model that the 4th step establishes, compare with the result of measuring according to GB standard method;
(6) Site Detection: the sample of production scene is carried out near infrared spectrum scanning, and measure with the model that the 4th step establishes, adjust produced on-site condition according to measurement result.
In step (2), directly gather original Tea Samples spectrogram, do not need sample to carry out any pre-treatment.
In step (2), the spectrogram that diffuses of Tea Samples makes sample cup rotation when gathering, and acquisition parameter is: scanning times 64 times, resolution 8cm-1, spectral range 10000-3800cm-1.In step (4), building mathematical model algorithm used is partial least square method.
Beneficial effect of the present invention: set up Measuring Moisture Content of Tea on-line analysis model, utilize this model energy fast detecting to go out the moisture in testing sample, do not need to destroy sample, also do not need other pre-treatment; In Tea Processing process, the content of moisture plays a major role to the quality of tealeaves finished product, so the content control of the moisture to tealeaves in process of manufacture seems most important, the present invention can be used for the moisture control of the whole processing link from dark brownish green spreading for cooling to tealeaves finished product, thereby realizes the quality control of Tea Production overall process.Can to the sample on production line, detect in real time at processing site, thereby can by testing result, to production and processing condition, adjust fast.
Accompanying drawing explanation
Fig. 1 is the process flow diagram that the present invention sets up model;
Fig. 2 is the near infrared light spectrogram of sample;
Fig. 3 is correlogram and the residual distribution figure between modeling sample predicted value and water analysis value.
Embodiment
(1) preparation of tealeaves sample: collected each production phase (as before completing, electric heating complete after, after microwave de-enzyming etc.) Tea Samples, each 200 grams, after numbering, be contained in foil samples bag sealing refrigeration;
(2) collection of near infrared spectrum: the Antaris II near infrared spectrometer that adopts U.S. ThermoFisher to produce, software adopts based on Workflow established standards workflow (SOP) and analytical approach, the collection Tea Samples spectrogram that diffuses.Specific practice, for Tea Samples is placed in instrument quartz opening sample cup (4.78cm diameter), makes sample cup rotation, to reduce the error of bringing due to sample inequality during collection.Acquisition parameter is: scanning times 64 times, resolution 8cm-1, spectral range 10000-3800cm-1.High sensitivity InGaAs detecting device, gathers background automatically, sees accompanying drawing 2;
(3) diffuse reflection spectrum spectrum pre-service: in order to reduce sample; because physical property comprises that sample size, uniformity coefficient and color etc. are to the spectrum base-line shift causing; and improve spectral information resolution characteristic, spectrogram is carried out to " single order or second derivative+Norris filter is made an uproar " and process;
Data processing: the data processing of automatically being carried out all spectrum by TQ Analyst 7.1 spectral analysis Chemical Measurement softwares;
(4) foundation of model: use special Chemical Measurement software, set up the mathematical model between the data that near infrared light spectrogram and standard method measured; Modeling algorithm used is selected PLS (offset minimum binary); In the tealeaves of chamber traditional analysis (GB/T 8304-2002) test, moisture, with the association of near infrared light spectrogram, is used the related algorithm of Chemical Measurement by experiment, after optimization process, sets up moisture model in tealeaves.Fig. 3 is the correlogram between modeling sample predicted value and lab analysis value.As can be seen from Figure 3, the model related coefficient (Corr. Coeff.) of setting up is 0.9955, and proofreading and correct mean square deviation (RMSEC) is 0.109, good relationship, and correction mean square deviation is less.
(5) checking of model: according to the identical method of the 2nd step, at nir instrument
The Tea Samples that upper measurement is new, and measure with the model that the 4th step establishes.Compare with the result of measuring according to GB standard method.The result that two kinds of methods obtain is consistent, in Table 1.
Table 1: the water model predicted value of fresh tea leaf and National Standard Method (Oven Method) measured result
| Index | Laboratory evaluation | Near infrared value | Absolute deviation | Percentage deviation % relatively |
| 1 | 72.08 | 72.28 | 0.20 | 0.28 |
| 2 | 71.10 | 71.23 | 0.13 | 0.18 |
| 3 | 71.33 | 71.66 | 0.33 | 0.46 |
| 4 | 72.72 | 72.40 | -0.32 | -0.44 |
| 5 | 72.00 | 72.04 | 0.04 | 0.06 |
| 6 | 72.17 | 72.53 | 0.36 | 0.50 |
| 7 | 73.53 | 73.31 | -0.22 | -0.30 |
| 8 | 73.31 | 73.64 | 0.33 | 0.45 |
| 9 | 73.18 | 73.21 | 0.03 | 0.04 |
| 10 | 73.31 | 73.75 | 0.44 | 0.60 |
| Minimum deflection | 0.03 | 0.04 | ||
| Maximum deviation | 0.44 | 0.6 | ||
| Mean deviation | 0.13 | 0.18 |
(6) Site Detection: the sample of production scene is carried out near infrared spectrum scanning, and measure with the model that the 4th step establishes, can measure fast the moisture in sample, thereby adjust produced on-site condition according to measurement result, reach the object that real time and on line monitoring is produced.
This model can be used for:
1, the application in fresh leaf purchase stage, cooperation expert's experience
2, the application in process segment
2.1 from the moisture of complete-microwave de-enzyming-Li of spreading for cooling (completing)-electric heating bar-shaping-Tuo Hao-dry-form slection-dry-each manufacturing procedure of choosing weight-Se choosing-far infrared Titian detect in real time, heating-up temperature-heat time-quality stability monitors, and arrives the quality monitoring of finished product.Find the moisture range of control of each procedure of processing, instruct and produce.
For example, for the electric heating process that completes, can reduce loss in production (broken, black etc.) by controlling heating-up temperature, inventory.Can improve the utilization factor of fresh leaf.
Claims (4)
1. adopt near infrared spectrum to realize a method for Tea Production Real-Time Monitoring, it is characterized in that: comprise following steps:
(1) preparation of tealeaves sample: collect Tea Samples, after numbering, be contained in foil samples bag, sealing refrigeration;
(2) collection of near infrared spectrum: based on Workflow established standards workflow (SOP) and analytical approach, gather the Tea Samples spectrogram that diffuses;
(3) diffuse reflection spectrum spectrum pre-service: spectrogram is carried out to " single order or second derivative+Norris filter is made an uproar " and process;
Data processing: the data processing of automatically being carried out all spectrum by TQ Analyst spectral analysis Chemical Measurement software;
(4) foundation of model: use TQ Analyst spectral analysis Chemical Measurement software, set up the mathematical model between the data that near infrared light spectrogram and standard method measured;
(5) checking of model: according to the identical method of the 2nd step, at nir instrument
The Tea Samples that upper measurement is new, and predict with the model that the 4th step establishes, compare with the result of measuring according to GB standard method;
Site Detection: the sample to each operation in producing carries out near infrared spectrum scanning, and measure with the model that the 4th step establishes, according to measurement result, adjust produced on-site condition.
2. a kind of method that adopts near infrared spectrum to realize Tea Production Real-Time Monitoring according to claim 1, is characterized in that: in step (2), directly gather original Tea Samples spectrogram, do not need sample to carry out any pre-treatment.
3. a kind of method that adopts near infrared spectrum to realize Tea Production Real-Time Monitoring according to claim 1, it is characterized in that: in step (2), the spectrogram that diffuses of Tea Samples makes sample cup rotation when gathering, acquisition parameter is: scanning times 64 times, resolution 8cm-1, spectral range 10000-3800cm-1.
4. a kind of method that adopts near infrared spectrum to realize Tea Production Real-Time Monitoring according to claim 1, is characterized in that: in step (4), building mathematical model algorithm used is partial least square method.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104049624A (en) * | 2014-07-07 | 2014-09-17 | 蓝星（北京）技术中心有限公司 | Chemical product production mode optimization method and device and continuous type chemical system |
| CN110308111A (en) * | 2019-06-14 | 2019-10-08 | 湖北省农业科学院果树茶叶研究所 | A method of using the near-infrared spectrum technique quick predict Yuanan yellow tea bored yellow time |
| CN110308110A (en) * | 2019-06-14 | 2019-10-08 | 湖北省农业科学院果树茶叶研究所 | Non-destructive prediction method |
| CN113376103A (en) * | 2021-06-04 | 2021-09-10 | 广东省农业科学院茶叶研究所 | Method for measuring content of tea components by using hyperspectral image technology and application |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104049624A (en) * | 2014-07-07 | 2014-09-17 | 蓝星（北京）技术中心有限公司 | Chemical product production mode optimization method and device and continuous type chemical system |
| CN110308111A (en) * | 2019-06-14 | 2019-10-08 | 湖北省农业科学院果树茶叶研究所 | A method of using the near-infrared spectrum technique quick predict Yuanan yellow tea bored yellow time |
| CN110308110A (en) * | 2019-06-14 | 2019-10-08 | 湖北省农业科学院果树茶叶研究所 | Non-destructive prediction method |
| CN113376103A (en) * | 2021-06-04 | 2021-09-10 | 广东省农业科学院茶叶研究所 | Method for measuring content of tea components by using hyperspectral image technology and application |
| CN113376103B (en) * | 2021-06-04 | 2023-03-07 | 广东省农业科学院茶叶研究所 | Method for measuring content of tea components by using hyperspectral image technology and application |
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