CN107860745A - 一种二醋酸纤维素结合酸快速检测方法 - Google Patents
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Abstract
一种二醋酸纤维素结合酸快速检测方法，包括以下步骤：（1） 建立标准样品的实验数据模型，模型是滴定法检测得到的结合酸数据与近红外光谱光谱图的对应关系；（2）采集所要检测的二醋酸纤维素片状样品；（3）将待检测的样品进行以下预处理：①粉碎至18‑25目；②粉碎后的醋片在80‑125℃干燥0.5‑2小时；③干燥好的醋片在干燥器中恒温至25℃的固定温度；（4）对待测样品通过近红外光谱仪进行扫描，获得待测样品的光谱图，通过建立的标准样品的实验数据模型中的光谱图和数据的对应关系，得到测定样品的结合酸。该方法快速、准确地实现了二醋酸纤维素结合酸的检测，可大大缩短分析检测时间，提高分析效率，及时为生产提供数据支持。
Description
技术领域
本发明涉及一种醋酸酯纤维素生产过程中最终产品结合酸检测的方法，属于醋片产品指标检测技术领域。
背景技术
醋酸纤维素(cellulose acetate)亦称醋酸酯纤维素，即以木材、棉短绒为原料，经与醋酸等化工原料反应制得纺丝原料醋酸酯纤维素，再经纺丝制得纤维。醋酸酯纤维素是纤维素与醋酸酐发生反应生产的纤维素乙酸酯纤维。由于纤维葡萄糖结构上的羟基被乙酰化，因此从原料、加工过程、产品性能来看，醋酸酯纤维素又被称为半合成纤维。
醋酸酯纤维素是从天然纤维素与醋酸经酯化合成，实际上纤维素分子中的羟基不可能全部酯化，不同酯化程度的醋酸纤维有不同的性能和用途。不同酯化程度的醋酸酯纤维素用途大致可以分为三大类：
(1)酯化程度2.30～2.40的，对应的结合酸为43-49％，用于制造涂料和塑料；
(2)酯化程度2.40～2.60的，对应的结合酸为53-58％，用于制人造丝和香烟的过滤嘴；
(3)酯化程度2.80～3.00的，对应的结合酸为60-62.5％，用于高性能电子薄膜与有机渗透膜的制造。
测定醋酸纤维素结合酸的传统方法为国标GB/T 32112015《工业用二醋酸纤维素片》中滴定法来检测，该方法对检验员的操作要求高，标准溶液需要配置和标定，滴定终点操作手法要求快速准确，同时分析过程耗时长，无法及时提供数据来指导生产。
为了去除操作误差和人为因素误差，亟需开发一种快速准确检验的方法。
近红外光谱(波长在700nm-2500nm(4000-14300cm-1)的光谱)是一种既快速又简便的测试手段，对样品作一步式组份分析而不需破坏样品。近红外光谱仪适用于对含有C-H,N-H,O-H和S-H化学键的化合物作组份分析。一些物质除在1450nm到2050nm之间产生第一谐波外，往往还会分别在1050nm-1700nm和700nm-1050nm谱带内产生第二及第三谐波。这些谐波的组合构成了被测物质在近红外光谱带内的特征吸收谱图-指纹图。
利用近红外图谱来对原材料或产品进行质量监控是利用统计学理论建立被测样品的数据库或校正曲线，而统计学之成败与校正曲线(数据库)的相互转移性有决定性的关系。在建立校正曲线或数据库之前,把日常的测试样品先作近红外扫描,然后再用传统分析法(如：GC、HPLC、TKN、FIA、折光仪、……)准确测定出样品的数值,具有不同指标的样品在近红外光谱中将产生不同强度的吸收图谱(不是某一吸收峰)，经过数据处理,便可得到校正曲线或数据库，分析人员可利用该校正曲线或数据库方便快速地通过测定未知样品的近红外谱图得知其被测指标的数据。
发明内容
本发明针对现有醋片结合酸检测技术存在的不足，提供一种快速、准确的二醋酸纤维素结合酸快速检测方法。
本发明的二醋酸纤维素结合酸快速检测方法，包括以下步骤：
(1)建立标准样品的实验数据模型，模型是滴定法检测得到的结合酸数据与近红外光谱光谱图的对应关系；
(2)采集所要检测的二醋酸纤维素片状样品；
(3)将待检测的样品进行以下预处理：
①粉碎至18-25目；
②粉碎后的醋片在80-125℃干燥0.5-2小时；
③干燥好的醋片在干燥器中恒温至25℃的固定温度；
(4)对待测样品通过近红外光谱仪进行扫描，获得待测样品的光谱图，通过建立的标准样品的实验数据模型中的光谱图和数据的对应关系，得到测定样品的结合酸。
本发明通过建立标准样品的实验数据模型，利用近红外光谱仪对待检测的样品进行近红外扫描，快速、准确地实现了二醋酸纤维素结合酸的检测。与国标中的化学滴定法相比，可大大缩短分析检测时间，提高分析效率，及时为生产提供数据支持。
具体实施方式
本发明的二醋酸纤维素结合酸快速检测方法，是利用近红外光谱仪，由Vision软件控制运行，采用Partial Least Square回归方法来进行定量分析。下面通过实施例的方式进一步说明本发明，但并不因此将本发明限制在所述的实施例范围之中。下列实施例中未注明具体条件的实验方法，按照常规方法和条件，或按照商品说明书选择。
一.首先建立模型
建立标准样品的实验数据模型，该模型是滴定法检测得到的结合酸数据与近红外光谱仪扫描的光谱图的一个对应关系。模型的建立是在大量的滴定检测数据基础上，利用建模方法来建立。
在400-2500nm波长范围内，选择四个特征波长范围，分别是500-680nm、890-1186nm、1540-1720nm和1900-2500nm，得到其特征吸收光谱，对实验室滴定数据关联，采用PLS法(Partial Least Square回归方法)来进行定量分析，建立数据模型，获得标准样品的结合酸数据与近红外光谱扫描的光谱图的对应关系。
二.操作步骤
1.所需仪器与材料：近红外光谱仪、烘箱、电子天平、玻璃干燥器、50ml自动回零滴定管、粉碎机、振荡摇床、1mol/L硫酸标准溶液、1mol/L氢氧化钠标准溶液等。
2.预处理
由于样品颗粒大小及含水量对近红外光谱图强度有着较大的影响，因此需要对样品进行以下前期处理：
(1)采集具有代表性的二醋酸纤维素系列样品。
(2)片状二醋酸纤维素经过18-25目筛网的粉碎机粉碎，放入80-125℃的烘箱中干燥0.5-2小时，
(3)取出处理好的醋片在干燥器中恒温30分钟至25℃的固定温度，每份样品分为两份；
(4)利用电子天平、自动回零滴定管、振荡摇床、1mol/L硫酸标准溶液和1mol/L氢氧化钠标准溶液，将一份样品按照GB/T 32112015《工业用二醋酸纤维素片》中结合酸检测方法采用化学滴定法测定其结合酸。
(5)将另一份样品用近红外光谱仪扫描，得到样品的扫描光谱图，通过建立的标准样品的实验数据模型中的光谱图和数据的对应关系，得到测定样品的结合酸。
三.数据分析
按照上述操作过程，分别对软木浆二醋酸纤维素结合酸、硬木浆二醋酸纤维素结合酸和棉浆二醋酸纤维结合酸进行测定，结果如下各表所示。
①软木浆二醋酸纤维素结合酸
②硬木浆二醋酸纤维素结合酸
③棉浆二醋酸纤维结合酸
从上面3个表中可以得知，软木浆二醋酸纤维结合酸、硬木浆二醋酸纤维结合酸及棉浆二醋酸纤维结合酸的绝对偏差分别为0.038、0.053、0.052，表明本发明的检测方法重现性好，实用性强，检测人员在前期样品处理好后只需简单的装样操作即可用近红外光谱仪检测醋片的结合酸。与国标中的化学滴定法相比，可大大缩短分析检测时间，提高分析效率，及时为生产提供数据支持。
Claims (1)
1.一种二醋酸纤维素结合酸快速检测方法，其特征在于，包括以下步骤：
(1)建立标准样品的实验数据模型，模型是滴定法检测得到的结合酸数据与近红外光谱光谱图的对应关系；
(2)采集所要检测的二醋酸纤维素片状样品；
(3)将待检测的样品进行以下预处理：
①粉碎至18-25目；
②粉碎后的醋片在80-125℃干燥0.5-2小时；
③干燥好的醋片在干燥器中恒温至25℃的固定温度；
(4)对待测样品通过近红外光谱仪进行扫描，获得待测样品的光谱图，通过建立的标准样品的实验数据模型中的光谱图和数据的对应关系，得到测定样品的结合酸。
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| CN104198430A (zh) * | 2014-09-25 | 2014-12-10 | 四川北方硝化棉股份有限公司 | 醋酸丁酸纤维素取代基含量的检测方法 |
| CN106383094A (zh) * | 2016-10-25 | 2017-02-08 | 中国林业科学研究院热带林业研究所 | 一种快速测定尾细桉木材化学成分含量的方法 |
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