CN106053381A - Near infrared spectrum collecting device and method for online analysis of heteropical samples - Google Patents
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Abstract
本发明公开了非均匀性样品在线分析的近红外光谱采集装置及其方法。该装置包括近红外光谱仪、测量附件。测量附件对测试样品实行近红外光谱采集并传递至近红外光谱仪。测量附件包括光纤、光纤收集附件、近红外光源附件、近红外光源、参比物质、托盘。近红外光源附件内安装有一组光学镜片一，通过该光学镜片一将光束汇聚于测试样品的表面上。参比物质承载在托盘上，测试样品位于托盘的底部并位于参比物质的正下方。光纤收集附件内安装有一组光学镜片二，通过该光学镜片二收集光束，并通过光纤传输至近红外光谱仪以形成近红外光谱信号。本发还公开该装置的非均匀性样品在线分析的近红外光谱采集方法。
The invention discloses a near-infrared spectrum acquisition device and a method for on-line analysis of non-uniform samples. The device includes a near-infrared spectrometer and measurement accessories. The measurement accessory performs near-infrared spectrum collection on the test sample and transmits it to the near-infrared spectrometer. Measurement accessories include optical fiber, optical fiber collection accessories, near-infrared light source accessories, near-infrared light source, reference material, and tray. A group of optical lenses is installed in the near-infrared light source attachment, and the light beam is focused on the surface of the test sample through the optical lenses. The reference material is carried on the tray, and the test sample is located at the bottom of the tray directly below the reference material. A set of optical lens 2 is installed in the optical fiber collection accessory, through which the light beam is collected and transmitted to the near-infrared spectrometer through the optical fiber to form a near-infrared spectrum signal. The invention also discloses a near-infrared spectrum acquisition method for on-line analysis of heterogeneous samples of the device.
Description
技术领域technical field
本发明涉及一种近红外光谱采集装置及其近红外光谱采集方法，尤其涉及一种非均匀性样品在线分析的近红外光谱采集装置及其近红外光谱采集方法。The invention relates to a near-infrared spectrum acquisition device and a near-infrared spectrum acquisition method thereof, in particular to a near-infrared spectrum acquisition device for online analysis of non-uniform samples and a near-infrared spectrum acquisition method thereof.
背景技术Background technique
近红外光谱作为分析技术里的巨人，已成为一门独立的分析技术，其快速分析、非入侵测量方式、不产生二次污染、无需化学试剂的特点受到过程分析领域的青睐，其应用领域不断拓展，目前已广泛应用于农业、制药、化工、环境等行业，取得了良好的效果。As a giant in analytical technology, near-infrared spectroscopy has become an independent analytical technology. Its characteristics of rapid analysis, non-invasive measurement methods, no secondary pollution, and no chemical reagents are favored by the field of process analysis. Its application fields continue to It has been widely used in agriculture, pharmacy, chemical industry, environment and other industries, and has achieved good results.
近红外光谱仪、化学计量学软件和应用模型构成了现代近红外光谱技术，在线分析应用中多波长下吸光度的准确测量要求光谱仪具有较高的信噪比和良好的稳定性，测量得到的光谱数据通过模型分析得到定性和定量结果，分析结果有效的实时反馈样品成分含量信息。在实际应用中光谱仪对经过含氢基团样品(O-H，C-H，N-H等)吸收的近红外光谱信号进行检测，然而光谱仪只能对各波段的光强信息进行测试，需要通过参比光谱信号和样品光谱信号得到吸光度信息，具体计算公式为其中Aλ为波长λ处的吸光度，Is为光谱仪测试到样品在近红外光源下的光强信息，Ir为光谱仪测试到参比物质在近红外光源下的光强信息。Near-infrared spectrometers, chemometric software and application models constitute modern near-infrared spectroscopy technology. Accurate measurement of absorbance at multiple wavelengths in online analysis applications requires spectrometers to have a high signal-to-noise ratio and good stability. The measured spectral data Qualitative and quantitative results are obtained through model analysis, and the analysis results can effectively feed back the content information of the sample components in real time. In practical applications, the spectrometer detects the near-infrared spectral signals absorbed by samples containing hydrogen groups (OH, CH, NH, etc.). However, the spectrometer can only test the light intensity information of each band, and needs to pass the reference spectral signal and The absorbance information is obtained from the spectral signal of the sample, and the specific calculation formula is Where A λ is the absorbance at the wavelength λ, I s is the light intensity information of the sample under the near-infrared light source measured by the spectrometer, and I r is the light intensity information of the reference substance under the near-infrared light source measured by the spectrometer.
目前在线分析的近红外光谱检测装置仍然存在不少缺陷，当近红外光源和光谱仪使用较长时间后，光强和光谱特性均会发生变化，导致测量得到的样品吸光度信息重复性变差，模型预测的结果也就会产生较大的偏差，不利于在线分析。为了满足在线运行的需求，在实际测试中需要通过参比物质进行自动测定才能对样品的吸光度数据进行实时校正，避免现场人工操作带来的不便和影响。At present, there are still many defects in the near-infrared spectrum detection device for online analysis. When the near-infrared light source and the spectrometer are used for a long time, the light intensity and spectral characteristics will change, resulting in poor repeatability of the measured absorbance information of the sample. The predicted results will also have a large deviation, which is not conducive to online analysis. In order to meet the needs of online operation, it is necessary to automatically measure the reference material in the actual test to correct the absorbance data of the sample in real time, avoiding the inconvenience and influence caused by on-site manual operation.
当实时获取的吸光度数据异常时，自动分析软件通常也会给出分析结果，这样的结果会降低整个在线分析系统的可靠性，在线分析应用中由于仪器设备长期的自动运行，不可避免的因为测量附件窗口堵塞、磨损、样品不均匀等因素导致数据出现异常。When the absorbance data obtained in real time is abnormal, the automatic analysis software will usually give the analysis results, which will reduce the reliability of the entire online analysis system. Accessory window clogging, wear, uneven sample, etc. can lead to abnormal data.
发明内容Contents of the invention
有鉴于此，本发明提供一种非均匀性样品在线分析的近红外光谱采集装置及其近红外光谱采集方法，本发明的装置可测定参比物质的光谱信号完成测试样品吸光度的自动校正，本发明的方法通过对异常数据的处理方法可以有效地避免测量窗口磨损、堵塞、样品非均匀性等因素对测量结果的影响，当异常数据出现时在线测试系统自动记录异常情况满足报警条件时给出警告信息，提高在线分析的可靠性，本方法和装置适用于固体粉末状、颗粒状尤其是非均匀性生物样品的实时在线的近红外光谱测量，为实时定性定量分析提供可靠的数据基础和解决方案。In view of this, the present invention provides a near-infrared spectrum collection device and a near-infrared spectrum collection method for online analysis of non-uniform samples. The device of the present invention can measure the spectral signal of a reference substance to complete the automatic correction of the absorbance of the test sample. The invented method can effectively avoid the influence of measurement window wear, clogging, sample non-uniformity and other factors on the measurement results by processing the abnormal data. When the abnormal data appears, the online test system automatically records the abnormal situation and gives an Warning information to improve the reliability of online analysis. This method and device are suitable for real-time online near-infrared spectrum measurement of solid powdery, granular, and especially heterogeneous biological samples, providing a reliable data basis and solution for real-time qualitative and quantitative analysis. .
本发明的解决方案是：一种非均匀性样品在线分析的近红外光谱采集装置，其包括近红外光谱仪、测量附件；测量附件对测试样品实行近红外光谱采集并传递至近红外光谱仪；测量附件包括光纤、光纤收集附件、近红外光源附件、近红外光源、参比物质、托盘；近红外光源附件内安装有一组光学镜片一，通过该光学镜片一将光束汇聚于测试样品的表面上；参比物质承载在托盘上，测试样品位于托盘的底部并位于参比物质的正下方；光纤收集附件内安装有一组光学镜片二，通过该光学镜片二收集光束，并通过光纤传输至近红外光谱仪以形成近红外光谱信号。The solution of the present invention is: a near-infrared spectrum acquisition device for on-line analysis of non-uniform samples, which includes a near-infrared spectrometer and a measurement accessory; the measurement accessory performs near-infrared spectrum collection on the test sample and transmits it to the near-infrared spectrometer; the measurement accessory includes Optical fiber, optical fiber collection accessories, near-infrared light source accessories, near-infrared light source, reference material, tray; a group of optical lenses 1 are installed in the near-infrared light source accessories, and the light beam is focused on the surface of the test sample through the optical lenses 1; The substance is carried on the tray, and the test sample is located at the bottom of the tray and directly below the reference substance; a set of optical lens 2 is installed in the optical fiber collection accessory, through which the optical lens 2 collects the light beam and transmits it to the near-infrared spectrometer through the optical fiber to form a near-infrared spectrometer. Infrared spectrum signal.
作为上述方案的进一步改进，测量附件还包括电磁铁；托盘具有磁性而能受电磁铁的牵引或推动，在电磁铁的通电情况下通过改变电磁铁的磁性以推动托盘位于测试样品上方、或牵引推动托盘复位。As a further improvement of the above scheme, the measurement accessory also includes an electromagnet; the tray is magnetic and can be pulled or pushed by the electromagnet, and the tray is positioned above the test sample by changing the magnetism of the electromagnet when the electromagnet is energized, or pulled Push the tray to reset.
作为上述方案的进一步改进，近红外光源附件与光纤收集附件对称设置，能使近红外光源附件出来的光线经过托盘折射后进入光纤收集附件内。As a further improvement of the above scheme, the near-infrared light source attachment and the optical fiber collection attachment are arranged symmetrically, so that the light from the near-infrared light source attachment can enter the optical fiber collection attachment after being refracted by the tray.
作为上述方案的进一步改进，近红外光源为卤素灯、或LED。As a further improvement of the above solution, the near-infrared light source is a halogen lamp or LED.
作为上述方案的进一步改进，该近红外光谱采集装置还包括电源系统，电源系统对近红外光源供电。As a further improvement of the above solution, the near-infrared spectrum acquisition device further includes a power supply system that supplies power to the near-infrared light source.
作为上述方案的进一步改进，该近红外光谱采集装置还包括传送机构，传送机构用于输送多个测试样品前后依次受测量附件的测量。As a further improvement of the above solution, the near-infrared spectrum collection device further includes a transmission mechanism, which is used to transport a plurality of test samples before and after being measured by the measurement accessories in sequence.
作为上述方案的进一步改进，该近红外光谱采集装置还包括计算机，计算机连接近红外光谱仪以接收近红外光谱信号进行分析。As a further improvement of the above solution, the near-infrared spectrum collection device further includes a computer connected to a near-infrared spectrometer to receive near-infrared spectrum signals for analysis.
本发明还提供一种上述任意非均匀性样品在线分析的近红外光谱采集装置的近红外光谱采集方法，该近红外光谱采集方法包含对多组测试样品的光谱数据的先验知识，根据测试样品的样品特征在多个波段处设定阈值范围，将采集的光谱数据与上述特定波段处的阈值范围进行比对，对连续多次光谱扫描不在阈值范围内的数据作异常处理并给出警告信息，对在阈值范围内的光谱数据取多次测量的平均值用于后续的定性定量分析。The present invention also provides a near-infrared spectrum acquisition method of the near-infrared spectrum acquisition device for online analysis of any non-uniform sample. The near-infrared spectrum acquisition method includes prior knowledge of the spectral data of multiple groups of test samples. The sample characteristics set the threshold range at multiple bands, compare the collected spectral data with the threshold range at the above-mentioned specific band, and perform abnormal processing for data that is not within the threshold range for multiple consecutive spectral scans and give a warning message , take the average value of multiple measurements for the spectral data within the threshold range for subsequent qualitative and quantitative analysis.
作为上述方案的进一步改进，多个波段处设定的阈值范围根据C-H/O-H/N-H特征吸收峰值范围设定。As a further improvement of the above solution, the threshold ranges set at the multiple bands are set according to the C-H/O-H/N-H characteristic absorption peak ranges.
作为上述方案的进一步改进，该近红外光谱采集方法包括以下步骤：As a further improvement of the above scheme, the near-infrared spectrum collection method includes the following steps:
一、通过测试多个测试样品获取在近红外光谱仪得到对应测试样品的近红外光谱信号，并建立参考数据库，分析多次测试的吸光度数据Aλ的分布特征；1. Obtain the near-infrared spectrum signal of the corresponding test sample in the near-infrared spectrometer by testing a plurality of test samples, and establish a reference database to analyze the distribution characteristics of the absorbance data A λ of multiple tests;
二、确定吸光度数据Aλ在O-H键的强吸收带1450nm/1900nm/2100nm处、在C-H键的强吸收带1750nm/1400nm处、在N-H的强吸收带1450nm/2100nm处的吸光度范围，设置3-5个特征波长点处的吸光度范围；2. Determine the absorbance data A λ is at the strong absorption band of OH bond at 1450nm/1900nm/2100nm, at the strong absorption band of CH bond at 1750nm/1400nm, and at the strong absorption band of NH at 1450nm/2100nm, set 3- Absorbance range at 5 characteristic wavelength points;
三、将每次扫描得到的吸光度数据与步骤二中设定的特征波长点处的吸光度范围进行比较，在预设范围之外的数据作为异常信息处理，连续扫描得到在预设范围之内的光谱数据取均值，作为有用信号输入定性、定量模型；3. Compare the absorbance data obtained by each scan with the absorbance range at the characteristic wavelength point set in step 2. The data outside the preset range will be treated as abnormal information, and the data within the preset range will be obtained by continuous scanning. Take the mean value of the spectral data and input the qualitative and quantitative models as useful signals;
四、如果步骤三中连续得到的异常信息，则判定测量附件、近红外光谱仪产生异常，需要进行维护处理；4. If the abnormal information is continuously obtained in step 3, it is determined that the measurement accessories and the near-infrared spectrometer are abnormal and need to be maintained;
重复步骤三，实现在线近红外光谱信号的连续自动采集和分析。Repeat step three to realize continuous and automatic collection and analysis of online near-infrared spectrum signals.
本发明在获取在线分析的近红外光谱数时，可以根据大量样品的测量数据设置多个特定波长处的吸光度范围，通常用于近红外光谱分析的样品均带有含氢基团(O-H，C-H，N-H等)，因此可以根据样品在上述含氢基团的近红外吸收分布来确定测试结果是否正常，每一次自动测量的数据结果与预先设定的阈值范围进行对比，不符合要求的样品数据代表着测量附件需要清洗维护或者样品本身出现异常波动，通过预设光谱阈值范围的判定方法可以有效提高在线分析的可靠性。When the present invention obtains the near-infrared spectrum number of on-line analysis, the absorbance range at a plurality of specific wavelengths can be set according to the measurement data of a large number of samples, and the samples usually used for near-infrared spectrum analysis all have hydrogen-containing groups (O-H, C-H , N-H, etc.), so it can be determined whether the test result is normal according to the near-infrared absorption distribution of the sample in the above-mentioned hydrogen-containing groups. The data results of each automatic measurement are compared with the preset threshold range, and the sample data that does not meet the requirements It means that the measurement accessories need to be cleaned and maintained or the sample itself has abnormal fluctuations. The reliability of online analysis can be effectively improved by the judgment method of the preset spectral threshold range.
附图说明Description of drawings
图1为本发明较佳实施例提供安装有非均匀性样品在线分析的近红外光谱采集装置的结构示意图。FIG. 1 is a schematic structural diagram of a near-infrared spectrum acquisition device equipped with an on-line analysis of non-uniform samples provided by a preferred embodiment of the present invention.
图2为图1中的近红外光谱采集装置的状态变化图。FIG. 2 is a state transition diagram of the near-infrared spectrum acquisition device in FIG. 1 .
图3为本发明实施例提供安装有非均匀性样品在线分析的近红外光谱采集方法的流程图。Fig. 3 is a flowchart of a near-infrared spectrum collection method provided with online analysis of non-uniform samples according to an embodiment of the present invention.
图4为传统的在线测试过程中光谱仪多次采集得到的在线分析的单籽粒水稻种子近红外光谱数据图。Fig. 4 is a graph of the near-infrared spectrum data of a single-grain rice seed analyzed online obtained by the spectrometer multiple times during the traditional online testing process.
图5为图4中通过本发明的光谱采集方法得到的单籽粒水稻种子近红外光谱数据图。Fig. 5 is a graph of near-infrared spectrum data of a single-grain rice seed obtained by the spectral collection method of the present invention in Fig. 4 .
图6为传统的在线测试过程中光谱仪多次采集得到的在线分析的肥料样品近红外光谱数据图。Fig. 6 is a graph of the near-infrared spectrum data of the fertilizer sample analyzed on-line obtained by the spectrometer multiple times during the traditional on-line testing process.
图7为图4中通过本发明的光谱采集方法得到的肥料样品近红外光谱数据图。Fig. 7 is a graph of the near-infrared spectrum data of the fertilizer sample obtained by the spectral collection method of the present invention in Fig. 4 .
具体实施方式detailed description
为了使本发明的目的、技术方案及优点更加清楚明白，以下结合附图及实施例，对本发明进行进一步详细说明。应当理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限定本发明。In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments. It should be understood that the specific embodiments described here are only used to explain the present invention, not to limit the present invention.
请一并参阅图1及图2，本发明的非均匀性样品在线分析的近红外光谱采集装置主要包括近红外光谱仪12、测量附件3、电源系统10、传送机构1。测量附件3对测试样品2实行近红外光谱采集并传递至近红外光谱仪12，近红外光谱仪12由此形成近红外光谱信号。也可以特地配置计算机13，计算机13连接近红外光谱仪12以接收近红外光谱信号进行分析。当然也可以采用智能手机、掌上通等具有数据处理功能的电子设备。传送机构1用于输送多个测试样品2前后依次受测量附件3的测量。Please refer to FIG. 1 and FIG. 2 together. The near-infrared spectrum acquisition device for online analysis of non-uniform samples of the present invention mainly includes a near-infrared spectrometer 12 , a measurement accessory 3 , a power supply system 10 , and a transmission mechanism 1 . The measurement accessory 3 collects the near-infrared spectrum of the test sample 2 and transmits it to the near-infrared spectrometer 12, and the near-infrared spectrometer 12 forms a near-infrared spectrum signal accordingly. The computer 13 can also be specially configured, and the computer 13 is connected to the near-infrared spectrometer 12 to receive near-infrared spectrum signals for analysis. Certainly also can adopt the electronic equipment that has data processing function such as smart mobile phone, handheld communication. The transmission mechanism 1 is used to transport a plurality of test samples 2 to be measured by the measurement accessory 3 sequentially.
测量附件3包括光纤11、光纤收集附件4、近红外光源附件5、近红外光源6、参比物质7、电磁铁8、托盘14。近红外光源附件5内安装有一组光学镜片一，通过该光学镜片一将光束汇聚于测试样品2的表面上，该光学镜片可采用光纤接口将光束传输至近红外光谱仪12。参比物质7承载在托盘14上，测试样品2位于托盘14的底部并位于参比物质7的正下方。光纤收集附件4内安装有一组光学镜片二，通过该光学镜片二收集光束，并通过光纤11传输至近红外光谱仪12以形成近红外光谱信号。测量附件3配合近红外光源6可以实现反射、透射光谱测量，测量附件3可以结合各种基线、背景扣除方法实现光谱的准确测量，消除近红外光谱仪12因素对光谱信号的影响。测量附件12适用于非均匀性固体颗粒态/粉末态样品的光谱测量。The measuring accessory 3 includes an optical fiber 11 , an optical fiber collecting accessory 4 , a near-infrared light source accessory 5 , a near-infrared light source 6 , a reference substance 7 , an electromagnet 8 , and a tray 14 . A group of optical lenses one is installed in the near-infrared light source attachment 5, through which the light beam is converged on the surface of the test sample 2, and the optical lens can transmit the light beam to the near-infrared spectrometer 12 through an optical fiber interface. The reference substance 7 is carried on the tray 14 , and the test sample 2 is located at the bottom of the tray 14 and directly below the reference substance 7 . A set of optical lenses 2 is installed in the optical fiber collection accessory 4, through which the light beams are collected and transmitted to the near-infrared spectrometer 12 through the optical fiber 11 to form a near-infrared spectrum signal. The measurement accessory 3 cooperates with the near-infrared light source 6 to realize reflection and transmission spectrum measurement. The measurement accessory 3 can combine various baseline and background subtraction methods to realize accurate measurement of the spectrum, and eliminate the influence of the near-infrared spectrometer 12 factors on the spectral signal. Measuring accessory 12 is suitable for spectral measurement of non-uniform solid granular/powder samples.
托盘14具有磁性而能受电磁铁8的牵引或推动，在电磁铁8的通电情况下通过改变电磁铁8的磁性以推动托盘14位于测试样品2上方、或牵引推动托盘14复位。近红外光源附件5可与光纤收集附件4对称设置，能使近红外光源附件5出来的光线经过托盘14折射后进入光纤收集附件4内。电源系统10对近红外光源6供电，电源系统10可通过导线9与近红外光源6电连接。托盘14可为U型。The tray 14 has magnetism and can be pulled or pushed by the electromagnet 8. When the electromagnet 8 is energized, the magnetism of the electromagnet 8 is changed to push the tray 14 above the test sample 2, or pull the tray 14 to reset. The near-infrared light source attachment 5 can be arranged symmetrically with the optical fiber collection attachment 4, so that the light from the near-infrared light source attachment 5 can enter the optical fiber collection attachment 4 after being refracted by the tray 14. The power supply system 10 supplies power to the near-infrared light source 6 , and the power supply system 10 can be electrically connected to the near-infrared light source 6 through a wire 9 . Tray 14 may be U-shaped.
故，本实施例的非均匀性样品在线分析的近红外光谱采集装置，主要包括一个近红外光源6、一个近红外光谱仪12(或者光电转换模块)、一个在线测量附件3以及一种配套的光谱数据采集方法。近红外光源6和在线测量附件3可以采用反射、透射等测量方式，在线测量附件3可以结合光纤接口将光谱信息传输至近红外光谱仪12或者光电转换模块，测量附件3和光谱数据采集方法适用于便携式光纤光谱仪、滤光片型光谱仪、光栅扫描光谱仪、傅立叶变换光谱仪、声光可调滤光型光谱仪以及固定光路多通道型光谱仪。Therefore, the near-infrared spectrum collection device for on-line analysis of non-uniform samples in this embodiment mainly includes a near-infrared light source 6, a near-infrared spectrometer 12 (or photoelectric conversion module), an on-line measurement accessory 3 and a supporting spectrum Data collection method. The near-infrared light source 6 and the online measurement accessory 3 can adopt measurement methods such as reflection and transmission. The online measurement accessory 3 can transmit spectral information to the near-infrared spectrometer 12 or a photoelectric conversion module in combination with an optical fiber interface. The measurement accessory 3 and the spectral data acquisition method are suitable for portable Fiber optic spectrometer, filter spectrometer, grating scanning spectrometer, Fourier transform spectrometer, acousto-optic tunable filter spectrometer and fixed optical path multi-channel spectrometer.
近红外光源6可以采用卤素灯、LED等窄带和宽谱带光源器件，通过光学镜片将光束汇聚于待测样品表面。The near-infrared light source 6 can use narrow-band or wide-band light source devices such as halogen lamps and LEDs, and converge the light beams on the surface of the sample to be tested through optical lenses.
本发明配套的光谱数据采集方法，即该非均匀性样品在线分析的近红外光谱采集装置的近红外光谱采集方法包含对多组待测样品光谱数据的先验知识，根据样品特征在多个波段处设定阈值范围，将采集的光谱数据与上述特定波段处的阈值范围进行比对，对连续多次光谱扫描不在阈值范围内的数据作异常处理并给出警告信息，对在阈值范围内的光谱数据取多次测量的平均值用于后续的定性定量分析。The supporting spectral data acquisition method of the present invention, that is, the near-infrared spectrum acquisition method of the near-infrared spectrum acquisition device for online analysis of non-uniform samples includes prior knowledge of multiple sets of spectral data of samples to be tested, and according to the characteristics of the samples in multiple bands Set the threshold range at the threshold range, compare the collected spectral data with the threshold range at the above-mentioned specific band, perform abnormal processing and give a warning message for data that is not within the threshold range for multiple consecutive spectral scans, and give a warning message for data within the threshold range The average value of multiple measurements was taken for the spectral data for subsequent qualitative and quantitative analysis.
多个波段处设定的阈值范围可以根据C-H/O-H/N-H特征吸收峰值范围设定，更进一步剔除光谱数据波动对预测结果的影响。The threshold range set at multiple bands can be set according to the C-H/O-H/N-H characteristic absorption peak range, further eliminating the influence of spectral data fluctuations on the prediction results.
本实施例的非均匀性样品在线分析的近红外光谱采集装置在使用时，测试样品2在传送机构1的传送带上随着传送到移动，到测量附件3对应的区域时，计算机13操作近红外光谱仪12记录测试样品的有效数据并保存，测量附件3通过光纤耦合的方式将信号通过光纤11传输至近红外光谱仪12。当需要对参比光谱进行校正时，电磁铁8牵引放置于U型托盘14中的参比物质7抵达样品测试窗口，此时记录参比光谱信息用于校正样品的吸光度信息，校正完成后电磁铁牵引参比物质返回初始位置等待下一次校正。其中样品2可以是颗粒状样品也可以是粉末状样品。When the near-infrared spectrum acquisition device for on-line analysis of non-uniform samples in this embodiment is in use, the test sample 2 moves along with the transmission on the conveyor belt of the transmission mechanism 1, and when it reaches the area corresponding to the measurement accessory 3, the computer 13 operates the near-infrared spectrum. The spectrometer 12 records and saves the effective data of the test sample, and the measurement accessory 3 transmits the signal to the near-infrared spectrometer 12 through the optical fiber 11 through optical fiber coupling. When the reference spectrum needs to be calibrated, the electromagnet 8 pulls the reference substance 7 placed in the U-shaped tray 14 to the sample testing window. At this time, the reference spectrum information is recorded for correcting the absorbance information of the sample. After the calibration is completed, the electromagnetic The iron pulls the reference substance back to its initial position and waits for the next calibration. Wherein sample 2 can be a granular sample or a powder sample.
如图3所示，本发明的非均匀性样品在线分析的近红外光谱采集方法，其具体步骤如下：As shown in Fig. 3, the near-infrared spectrum acquisition method of the heterogeneity sample online analysis of the present invention, its specific steps are as follows:
一、多次离线测量分别获取多个待测样品在该类型光谱仪得到对应样品的近红外光谱信号，建立参考数据库，分析多次测试的吸光度数据Aλ分布特征。1. Multiple off-line measurements obtain multiple samples to be tested respectively. Get the near-infrared spectral signals of the corresponding samples in this type of spectrometer, establish a reference database, and analyze the absorbance data A λ distribution characteristics of multiple tests.
二、确定Aλ在O-H键的强吸收带1450nm/1900nm/2100nm处、在C-H键的强吸收带1750nm/1400nm处、在N-H的强吸收带1450nm/2100nm处吸光度范围，设置3-5个特征波长点处的吸光度范围。2. Determine the absorbance range of A λ at the strong absorption band of OH bond at 1450nm/1900nm/2100nm, at the strong absorption band of CH bond at 1750nm/1400nm, and at the strong absorption band of NH at 1450nm/2100nm, and set 3-5 features Absorbance range at wavelength points.
三、将每次扫描得到的吸光度数据与步骤二中设定的特征波长点处的吸光度范围进行比较，在预设范围之外的数据作为异常信息处理，连续扫描得到在预设范围之内的光谱数据取均值，作为有用信号输入定性、定量模型。3. Compare the absorbance data obtained by each scan with the absorbance range at the characteristic wavelength point set in step 2. The data outside the preset range will be treated as abnormal information, and the data within the preset range will be obtained by continuous scanning. The average value of the spectral data is used as a useful signal input to the qualitative and quantitative models.
四、如果步骤三中连续得到的异常信息，则判定测量附件、光谱仪产生异常，需要进行维护处理。4. If the abnormal information is continuously obtained in step 3, it is determined that the measurement accessories and the spectrometer are abnormal and need to be maintained.
重复步骤三，实现在线近红外光谱信号的连续自动采集和分析。Repeat step three to realize continuous and automatic collection and analysis of online near-infrared spectrum signals.
本发明在获取在线分析的近红外光谱数时，可以根据大量样品的测量数据设置多个特定波长处的吸光度范围，通常用于近红外光谱分析的样品均带有含氢基团(O-H，C-H，N-H等)，因此可以根据样品在上述含氢基团的近红外吸收分布来确定测试结果是否正常，每一次自动测量的数据结果与预先设定的阈值范围进行对比，不符合要求的样品数据代表着测量附件需要清洗维护或者样品本身出现异常波动，通过预设光谱阈值范围的判定方法可以有效提高在线分析的可靠性。When the present invention obtains the near-infrared spectrum number of on-line analysis, the absorbance range at a plurality of specific wavelengths can be set according to the measurement data of a large number of samples, and the samples usually used for near-infrared spectrum analysis all have hydrogen-containing groups (O-H, C-H , N-H, etc.), so it can be determined whether the test result is normal according to the near-infrared absorption distribution of the sample in the above-mentioned hydrogen-containing groups. The data results of each automatic measurement are compared with the preset threshold range, and the sample data that does not meet the requirements It means that the measurement accessories need to be cleaned and maintained or the sample itself has abnormal fluctuations. The reliability of online analysis can be effectively improved by the judgment method of the preset spectral threshold range.
接下来，本实施例采用两个试验案例以举证本发明的有益效果。Next, this embodiment adopts two test cases to demonstrate the beneficial effects of the present invention.
试验案例一Test case one
采用本发明介绍的光谱采集方法和装置得到的水稻种子的近红外光谱，其中图4为传统的单颗种子在通量化测试过程中光谱仪多次采集得到的结果，可以看出在通量化在线测试过程中由于样品和测量附件的相对运动，导致光谱信号质量下降。通过本发明介绍的光谱采集方法可以在1450nm处设置吸光度阈值范围为0.1-0.5，在1950nm和2100处设置光谱阈值范围为0.4-0.7，将测量得到的每一条光谱信息与上述阈值范围比对，可以剔除异常信息得到图5中的结果，将阈值范围内的多条光谱取均值用于进一步的定性定量分析。Adopt the near-infrared spectrum of the rice seed that the spectral collection method and device that the present invention introduces obtains, and wherein Fig. 4 is the result that the traditional single seed is collected by spectrometer multiple times in the flux quantization test process, it can be seen that in the flux quantization on-line test Due to the relative movement of the sample and measuring accessories during the process, the quality of the spectral signal is degraded. Through the spectral acquisition method introduced in the present invention, the absorbance threshold range can be set at 1450nm to be 0.1-0.5, and the spectral threshold range can be set at 1950nm and 2100 to be 0.4-0.7, and each piece of spectral information obtained by measurement is compared with the above-mentioned threshold range, Abnormal information can be eliminated to obtain the results in Figure 5, and the average value of multiple spectra within the threshold range is used for further qualitative and quantitative analysis.
试验案例二Test case two
采用本发明介绍的光谱采集方法和装置得到的肥料样品的近红外光谱，其中图6为在线测试过程中光谱仪多次采集得到的结果，可以看出在线测试过程中由于样品和测量附件的相对运动，导致光谱信号质量下降。通过本发明介绍的光谱采集方法可以在1320nm处设置吸光度阈值范围为0.3-0.8，在1750nm处设置光谱阈值范围为0.5-0.8，在2050nm处设置光谱阈值范围为1-1.6，将测量得到的每一条光谱信息与上述阈值范围比对，可以剔除异常信息得到图7中的结果，将阈值范围内的多条光谱取均值用于进一步的定性定量分析。The near-infrared spectrum of the fertilizer sample obtained by the spectrum acquisition method and device introduced in the present invention, wherein Fig. 6 is the result obtained by the spectrometer multiple acquisitions in the online test process, it can be seen that in the online test process due to the relative motion of the sample and the measurement accessory , leading to the degradation of spectral signal quality. The spectrum acquisition method introduced by the present invention can set the absorbance threshold range at 1320nm to be 0.3-0.8, set the spectrum threshold range at 1750nm to be 0.5-0.8, set the spectrum threshold range at 2050nm to be 1-1.6, and measure each obtained Comparing a piece of spectral information with the above threshold range, the abnormal information can be eliminated to obtain the result in Figure 7, and the average value of multiple spectra within the threshold range is used for further qualitative and quantitative analysis.
因此，本发明不仅有效避免外界环境对测量信号的影响，有效，所以本发明可以方便、准确的实现固体粉末状、颗粒状样品的在线近红外光谱采集，提高样品测量的准确性和模型分析的鲁棒性。并且本装置结构紧凑、体积小、本方法简便易操作，适用于固体、液体和气体样品的实时、在线近红外光谱分析。Therefore, the present invention not only effectively avoids the influence of the external environment on the measurement signal, but also is effective, so the present invention can conveniently and accurately realize the online near-infrared spectrum collection of solid powdery and granular samples, and improve the accuracy of sample measurement and model analysis. robustness. Moreover, the device has a compact structure and a small volume, and the method is simple and easy to operate, and is suitable for real-time and online near-infrared spectral analysis of solid, liquid and gas samples.
上述实施例的描述是为便于该技术领域的普通技术人员能理解和应用本发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于这里的实施例，本领域技术人员根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。The descriptions of the above embodiments are for those of ordinary skill in the art to understand and apply the present invention. It is obvious that those skilled in the art can easily make various modifications to these embodiments, and apply the general principles described here to other embodiments without creative effort. Therefore, the present invention is not limited to the embodiments herein. Improvements and modifications made by those skilled in the art according to the disclosure of the present invention without departing from the scope of the present invention should fall within the protection scope of the present invention.
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