CN111220563B - 一种采用红外光谱检测回收油的方法 - Google Patents

一种采用红外光谱检测回收油的方法 Download PDF

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CN111220563B
CN111220563B CN201811462195.6A CN201811462195A CN111220563B CN 111220563 B CN111220563 B CN 111220563B CN 201811462195 A CN201811462195 A CN 201811462195A CN 111220563 B CN111220563 B CN 111220563B
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李大军
杨美玉
申秀娟
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Jilin Agricultural University
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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    • G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
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    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
    • G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR

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Abstract

本发明公开了一种红外光谱偏度值望大望小极差法测定回收油，建立红外光谱的电子表格软件数学分析方法。该方法以红外吸收峰区域偏度分布为依据，筛选望大与望小值，计算极差值，确定限值。低于限值判定为原油，高于限值判定为回收油。

Description

一种采用红外光谱检测回收油的方法
技术领域
本发明公开了一种采用研究型红外光谱，分析植物原油、烹饪回收油，围绕特征基团，对全波数透光度采用偏度SKEW(array1；array2)望大和望小进行筛选保留，求累积极差，得到以特定限值以下与以上作为界定原油与回收油的参数。本发明属于农产品及食品加工安全控制领域。
背景技术：
傅立叶红外光谱分析技术，是解决回收油可能带来的化学变化的潜在的有力工具。通常扫描波数范围在3600～400 1/λ，能够分析大多数有机物化学基团。回收油的检测是目前检测的难点，被业界称为“一群科学家对付不了几个二道贩子”，目前没有回收油检测的国家标准。回收油来源、精炼方法多种多样，成分复杂，溴化钾压片和油脂涂层厚度难以均衡和定量。本发明关键在于提出通过多样本分析建立恰当的数学模型，消除分析误差，总结出规律性的解决方案。
回收油对比原油的直接性变化包括a、油脂混合，b、动物油，c、熔点降低。
回收油对比原油的化学变化包括a、饱和脂肪含量，b、掺入极性基团(氨基、亚胺、硝基、磷酸、硫酸、氯、磷脂等)，c、生成极性基团(羧基、酯羧基、甘油伯或叔位羟基、氨基、反式脂肪酸等)。
上述特征可利用研究型红外光谱进行分子基团分析，判断油脂特性。
发明内容：
本发明的目的是采用傅立叶红外光谱分析技术，结合不同波数透光度的偏度累计差值，对回收油进行检测分析。本发明的目的是通过如下的技术方法来实现的：
A、测定几种植物原油和若干回收油的红外扫描光谱透光度值，利用红外基团检索图，在适当位置标记分子基团波数区。
B、查找基团波数区或波数前后3～5个分辨率的透光度极小值。
C、计算极小值附近3～5个波数分辨率的偏度值。
D、分析确定回收油对比原油不同分子基团波数附近的偏度值的望大与望小，并进行筛选。
C、分别累计筛选后的偏度的望大与望小值。
D、计算望大与望小的累计值的极差。
E、观测原油与回收油的偏度累计极差分布区间，重新筛选、优化极差分布，确定原油与回收油的极差限值。
F、测定待检测油脂的偏度望大与望小值累计极差，判断油脂性质。
本发明的有益效果是，采用傅立叶红外光谱分析技术，对油脂进行检测分析。达到快速识别回收油的目的。
具体实施方式
以下为判断回收油示例(相关操作方法、原理参见说明书附图1～5)：
用红外Prestage21红外光谱仪，涂布200mg溴化钾压片，设置分辨率2cm-1，扫描菜籽油、花生油、玉米油原油、若干回收油的红外光谱。标记分子基团波数区。查找基团波数区或波数前后5个分辨率的透光度极小值。利用Excel计算极小值附近5个波数分辨率的偏度值，分析确定回收油对比原油不同分子基团波数附近的偏度值的望大与望小，并进行筛选。分别累计筛选后的偏度的望大(7.80～26.00)与望小值(-13.80～4.05)。计算望大与望小的累计值的极差(原油-5.20～4.24；回收油5.88～27.55)。重新筛选、优化极差分布，确定原油与回收油的极差限值为5.00，即极差限值大于5.00判断为回收油。
附图说明
图1是偏度的电子表格图形示例和计算公式；
图2是红外基团快速检索图；
图3是操作流程实体示例；
图4是偏度SKEW(array1；array2)的计算计算值演示示例；
图5是回收油累计偏度极差示例。

Claims (6)

1.一种红外光谱偏度值望大望小极差法测定回收油的方法，其特征在于，该方法通过以下的步骤来实现：
A、测定几种植物原油和若干回收油的红外扫描光谱透光度值，利用红外基团快速检索图，在适当位置标记分子基团波数区；
B、查找基团波数区或波数前后3~5个分辨率的透光度极小值；
C、计算极小值附近3~5个波数分辨率的偏度值；
D、分析确定回收油对比原油不同分子基团波数附近的偏度值的望大与望小，并进行筛选，
E、分别累计筛选后的偏度的望大与望小值；
F、计算望大与望小的累计值的极差；
G、观测原油与回收油的偏度累计极差分布区间,重新筛选、优化极差分布，确定原油与回收油的极差限值；
H、测定待检测油脂的偏度望大与望小值累计极差，判断油脂性质。
2.根据权利要求1所述的红外光谱偏度值望大望小极差法测定回收油的方法，其特征在于：步骤A所述的利用红外基团快速检索图；其红外基团快速检索图是把分子基团红外扫描波数分布做成快速检索简图，列入说明书附图。
3.根据权利要求1所述的红外光谱偏度值望大望小极差法测定回收油的方法，其特征在于：步骤C所述的计算极小值附近3~5个波数分辨率的偏度值；其偏度值是红外特征基团透光度减少与回复的数学函数值，具有特征性变化，可利用办公或统计软件进行分析。
4.根据权利要求1所述的红外光谱偏度值望大望小极差法测定回收油的方法，其特征在于：步骤D所述的分析确定回收油对比原油不同分子基团波数附近的偏度值的望大与望小；其望大与望小是回收油对比原油的透光度偏度值增大与减小趋势。
5.根据权利要求1所述的红外光谱偏度值望大望小极差法测定回收油的方法，其特征在于：步骤F所述的计算望大与望小的累计值的极差；其极差是优选后的偏度望大与望小的累计值的差值。
6.据权利要求1所述的红外光谱偏度值望大望小极差法测定回收油的方法，其特征在于：步骤G所述的定原油与回收油的极差限值；其极差限值是判定油脂来源的依据。
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Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001004612A2 (en) * 1999-07-09 2001-01-18 Foss Electric A/S A method of determining the content of a component in a fluid sample and an apparatus therefor
EP1199555A1 (en) * 2000-10-17 2002-04-24 JAPAN as represented by DIRECTOR GENERAL OF NATIONAL FOOD RESEARCH INSTITUTE, MINISTRY OF AGRICULTURE, FORESTRY AND FISHERIES Analytical method and apparatus for liquid samples using near infrared spectroscopy
WO2004012586A2 (en) * 2002-08-05 2004-02-12 Infraredx, Inc. Near-infrared spectroscopic analysis of blood vessel walls
WO2007062196A2 (en) * 2005-11-21 2007-05-31 State Of Oregon Acting By And Through The State Board Of Higher Educ. On Behalf Of Oregon State Univ Portable meter to measure chlorophyll, nitrogen and water and methods
KR20110006887A (ko) * 2009-07-15 2011-01-21 대한민국(농촌진흥청장) 참기름 진위 판별 장치
CN102405402A (zh) * 2008-09-23 2012-04-04 阔达生命有限公司 基于液滴的测定系统
CA2859951A1 (en) * 2011-12-19 2013-06-27 Opticul Diagnostics Inc. Spectroscopic means and methods for identifying microorganisms in culture
CN103398970A (zh) * 2013-07-24 2013-11-20 骆驰 一种定性和定量分析食用油并进而检测地沟油的方法
CN103592256A (zh) * 2013-11-29 2014-02-19 重庆市计量质量检测研究院 基于傅里叶变换中红外光谱识别正常食用植物油和精炼潲水油的方法
CN104142311A (zh) * 2014-08-15 2014-11-12 华南农业大学 一种用近红外光谱技术预测火炬松松脂产量的方法
CN104568820A (zh) * 2014-10-17 2015-04-29 芜湖扬宇机电技术开发有限公司 一种水质检测方法
JP2018205226A (ja) * 2017-06-08 2018-12-27 昭和産業株式会社 近赤外分光分析を用いたフライ用油脂組成物の分析
CN212780503U (zh) * 2020-10-09 2021-03-23 南京昆磊泓锐仪器技术有限公司 傅里叶近红外光谱干涉仪及用于在线物料检测的仪器

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107228924B (zh) * 2017-06-20 2019-08-20 中国农业科学院农产品加工研究所 一种适宜蛋白加工用花生原料品质测定及其评价方法

Patent Citations (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2001004612A2 (en) * 1999-07-09 2001-01-18 Foss Electric A/S A method of determining the content of a component in a fluid sample and an apparatus therefor
EP1199555A1 (en) * 2000-10-17 2002-04-24 JAPAN as represented by DIRECTOR GENERAL OF NATIONAL FOOD RESEARCH INSTITUTE, MINISTRY OF AGRICULTURE, FORESTRY AND FISHERIES Analytical method and apparatus for liquid samples using near infrared spectroscopy
WO2004012586A2 (en) * 2002-08-05 2004-02-12 Infraredx, Inc. Near-infrared spectroscopic analysis of blood vessel walls
WO2007062196A2 (en) * 2005-11-21 2007-05-31 State Of Oregon Acting By And Through The State Board Of Higher Educ. On Behalf Of Oregon State Univ Portable meter to measure chlorophyll, nitrogen and water and methods
CN102405402A (zh) * 2008-09-23 2012-04-04 阔达生命有限公司 基于液滴的测定系统
KR20110006887A (ko) * 2009-07-15 2011-01-21 대한민국(농촌진흥청장) 참기름 진위 판별 장치
CA2859951A1 (en) * 2011-12-19 2013-06-27 Opticul Diagnostics Inc. Spectroscopic means and methods for identifying microorganisms in culture
CN103398970A (zh) * 2013-07-24 2013-11-20 骆驰 一种定性和定量分析食用油并进而检测地沟油的方法
CN103592256A (zh) * 2013-11-29 2014-02-19 重庆市计量质量检测研究院 基于傅里叶变换中红外光谱识别正常食用植物油和精炼潲水油的方法
CN104142311A (zh) * 2014-08-15 2014-11-12 华南农业大学 一种用近红外光谱技术预测火炬松松脂产量的方法
CN104568820A (zh) * 2014-10-17 2015-04-29 芜湖扬宇机电技术开发有限公司 一种水质检测方法
JP2018205226A (ja) * 2017-06-08 2018-12-27 昭和産業株式会社 近赤外分光分析を用いたフライ用油脂組成物の分析
CN212780503U (zh) * 2020-10-09 2021-03-23 南京昆磊泓锐仪器技术有限公司 傅里叶近红外光谱干涉仪及用于在线物料检测的仪器

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
A detection method of vegetable oils in edible blended oil based on three-dimensional fluorescence spectroscopy technique;Xu Jing;<Food Chemistry>;20161201;第212卷;第72-77页 *
Authentication of edible vegetable oils adulterated with used frying oil by Fourier Transform Infrared Spectroscopy;Qing Zhang;<Food Chemistry>;20111208;第132卷(第3期);第1607-1613页 *
两种国标方法测定油脂过氧化值的比较与方法改进;李大军;《农业机械》;20111130(第32期);第68-70页 *
傅里叶变换红外光谱-加热顶空法鉴别地沟油;许洪勇;《中国油脂》;20131231;第38卷(第1期);第118-124页 *
斜率截距校正算法在食用油酸值和过氧化值上的近红外光谱模型转移的研究;李天瑞;《中国粮油学报》;20180131;第33卷(第1期);第64-66页 *

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