植物纤维原料化学成分定量分析方法研究
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摘要
随着石化资源的短缺以及人们对高质量生活的不断追求,天然纤维素纤维因其良好的服用舒适性、资源易得性和环境友好性而被大量的应用于纺织领域。同时植物资源作为天然纤维素纤维的重要来源,亦受到重视。
我国植物资源丰富,纺织用植物纤维原料种类繁多,如棉类、麻类、桑树皮、龙须草、棕叶、各种竹、椰壳、稻草等。目前对植物纤维及其资源化学成分进行定量分析通常采用国家标准GB/T5889-86《苎麻化学成分定量分析方法》。但是该标准是针对苎麻原料来制定的,在分析其它植物纤维原料时难免会存在一些问题,因此需要一种相对准确且普遍适用的方法来对植物纤维原料进行化学成分定量分析。
针对各种植物纤维原料化学成分含量不同的特点,在苎麻标准的基础上提出了多种定量分析方案,并通过实验对其优选,确立了相对准确的化学成分定量分析方法,最终方案确定为：
(1)将原料试样粉碎,大小可通过20目分样筛不过60目(1mm左右),用已知重量的200目筛绢布包包裹,并测试样含水率；
(2)用苯乙醇对测完含水率的试样进行提取,并对提取液进行蒸馏,取残液烘干称重测定脂蜡质含量；
(3)对提取脂蜡质后的试样进行沸水提取,并对提取液采用紫外-可见分光光度计测定水溶性果胶的含量A和分解的半纤维素的含量B,用试样失重减去(A+B)即为水溶物含量；
(4)利用草酸铵溶液对提取完水溶物的样品进行处理,并对提取液测试分解的半纤维素的含量C,用试样失重减去C并加上A即为果胶含量；
(5)对提取完果胶的试样用NaOH溶液处理,失重为半纤维素的含量和小部分木质素的含量D,用氯化法处理残渣,失重为部分木质素的含量E,剩余物为纤维素(含量为G),半纤维素的量就等于试样第一次失重减D再加上B和C；
(6)另取相同试样粉碎,大小可通过60目分样筛不过200目,烘干称重后用72%硫酸处理,剩余残渣即为总木质素,含量为F,同时木质素含量D就等于F减去E；
(7)对于含胶率和灰分的测定按照苎麻标准进行。
实验证明此方法对各种植物纤维原料化学成分的测定相对准确,且具有普遍适用性。但在实际操作过程中,由于步骤繁杂难免存在误差,从而对最终结果造成影响,并且某些化学试剂的应用对人体有一定的不良作用,因此需要进一步优化、完善各步骤或者引入新方法,使植物纤维原料化学成分定量分析更加安全、快捷、准确。
With the oil resource shortage and people's constant pursuit of high-quality live, natural cellulose fibers are utilization to the textile field because of its comfortable dressing, easy to get and environment-friendly properties. At the same time, the plant resources as an important source of natural cellulose fibers have been paid attention by the people.
The plant resource is rich in our country, and there are many kinds used in the textile, such as Cotton, Hemp, Flax, Jute, Ramie, Chinese Alpine Rush, Mulberry Bark, Palm Leaves, Bamboo, Coconut Shell, Rice Straw and so on. At present, the plant fiber chemical composition quantitative analysis is used to follow the National Standard GB/T5889-86 "the Method of the Ramie Chemical Composition Quantitative Analysis". The different plant has different chemical content, so here makes several plans according to the Ramie Standard, and confirms the final relative exact method, the particular steps as follows:
(Ⅰ) Mill the raw material samples to the size about 1mm, and bind up them by the 200-mesh sieves which have extracted by the organic solvent and known the weight, test ing the samples Moisture content;
(Ⅱ) Extract the samples by the Benzene-Ethanol, and distill and dry the residue. Weigh the residue to get the Lipid Classes content;
(Ⅲ) Extract the samples by the boiling water, the extracting liquid had a test by the UV-visible spectrophotometer, and get the content of the Water-soluble Pectin A and the decomposed Hemicellulose B. The content of Water-solubles equals to the lost weight minus the content of A and B;
(Ⅳ) Extract the samples by the Ammonium Oxalate, and test the decomposed Hemicellulose C from the extracting liquid. The content of Pectin equals to the lost weight minus the content of C plus the content of A;
(Ⅴ) Extract the samples by the NaOH liquor, the lost weight are Hemicellulose and a little of Lignin D. Chloridizing the residue, the lost is Lignin E, and the remains is Cellulose G. The content of Hemicellulose equals to the first lost weight minus the content of D plus the content of B and C;
(Ⅵ) Mill another same samples to the size passing the 60-mesh sub-sample screen, drying and weighing them. Treat the samples by concentrated sulfuric acid, the remains is the Lignin F, the same time, the content of D equaling to the content of F minus the content of E;
(Ⅶ) To the Cellulose, Gum content and Ash, the testing is conducted according to the Ramie Criterion.
The experiments prove that this method to test the various plant fibers'chemical composition is relatively accurate, and has a general applicability. However, in actual operation, there is inevitably errors because of the complicated steps, thus affects the final result and the application of some chemical reagents are harm for the people's health to a certain extent, therefore, it needs to have a further optimization and improve the various steps to make the chemical composition quantitative analysis of plant fibers more secure, fast and accurate.
我国植物资源丰富,纺织用植物纤维原料种类繁多,如棉类、麻类、桑树皮、龙须草、棕叶、各种竹、椰壳、稻草等。目前对植物纤维及其资源化学成分进行定量分析通常采用国家标准GB/T5889-86《苎麻化学成分定量分析方法》。但是该标准是针对苎麻原料来制定的,在分析其它植物纤维原料时难免会存在一些问题,因此需要一种相对准确且普遍适用的方法来对植物纤维原料进行化学成分定量分析。
针对各种植物纤维原料化学成分含量不同的特点,在苎麻标准的基础上提出了多种定量分析方案,并通过实验对其优选,确立了相对准确的化学成分定量分析方法,最终方案确定为：
(1)将原料试样粉碎,大小可通过20目分样筛不过60目(1mm左右),用已知重量的200目筛绢布包包裹,并测试样含水率；
(2)用苯乙醇对测完含水率的试样进行提取,并对提取液进行蒸馏,取残液烘干称重测定脂蜡质含量；
(3)对提取脂蜡质后的试样进行沸水提取,并对提取液采用紫外-可见分光光度计测定水溶性果胶的含量A和分解的半纤维素的含量B,用试样失重减去(A+B)即为水溶物含量；
(4)利用草酸铵溶液对提取完水溶物的样品进行处理,并对提取液测试分解的半纤维素的含量C,用试样失重减去C并加上A即为果胶含量；
(5)对提取完果胶的试样用NaOH溶液处理,失重为半纤维素的含量和小部分木质素的含量D,用氯化法处理残渣,失重为部分木质素的含量E,剩余物为纤维素(含量为G),半纤维素的量就等于试样第一次失重减D再加上B和C；
(6)另取相同试样粉碎,大小可通过60目分样筛不过200目,烘干称重后用72%硫酸处理,剩余残渣即为总木质素,含量为F,同时木质素含量D就等于F减去E；
(7)对于含胶率和灰分的测定按照苎麻标准进行。
实验证明此方法对各种植物纤维原料化学成分的测定相对准确,且具有普遍适用性。但在实际操作过程中,由于步骤繁杂难免存在误差,从而对最终结果造成影响,并且某些化学试剂的应用对人体有一定的不良作用,因此需要进一步优化、完善各步骤或者引入新方法,使植物纤维原料化学成分定量分析更加安全、快捷、准确。
With the oil resource shortage and people's constant pursuit of high-quality live, natural cellulose fibers are utilization to the textile field because of its comfortable dressing, easy to get and environment-friendly properties. At the same time, the plant resources as an important source of natural cellulose fibers have been paid attention by the people.
The plant resource is rich in our country, and there are many kinds used in the textile, such as Cotton, Hemp, Flax, Jute, Ramie, Chinese Alpine Rush, Mulberry Bark, Palm Leaves, Bamboo, Coconut Shell, Rice Straw and so on. At present, the plant fiber chemical composition quantitative analysis is used to follow the National Standard GB/T5889-86 "the Method of the Ramie Chemical Composition Quantitative Analysis". The different plant has different chemical content, so here makes several plans according to the Ramie Standard, and confirms the final relative exact method, the particular steps as follows:
(Ⅰ) Mill the raw material samples to the size about 1mm, and bind up them by the 200-mesh sieves which have extracted by the organic solvent and known the weight, test ing the samples Moisture content;
(Ⅱ) Extract the samples by the Benzene-Ethanol, and distill and dry the residue. Weigh the residue to get the Lipid Classes content;
(Ⅲ) Extract the samples by the boiling water, the extracting liquid had a test by the UV-visible spectrophotometer, and get the content of the Water-soluble Pectin A and the decomposed Hemicellulose B. The content of Water-solubles equals to the lost weight minus the content of A and B;
(Ⅳ) Extract the samples by the Ammonium Oxalate, and test the decomposed Hemicellulose C from the extracting liquid. The content of Pectin equals to the lost weight minus the content of C plus the content of A;
(Ⅴ) Extract the samples by the NaOH liquor, the lost weight are Hemicellulose and a little of Lignin D. Chloridizing the residue, the lost is Lignin E, and the remains is Cellulose G. The content of Hemicellulose equals to the first lost weight minus the content of D plus the content of B and C;
(Ⅵ) Mill another same samples to the size passing the 60-mesh sub-sample screen, drying and weighing them. Treat the samples by concentrated sulfuric acid, the remains is the Lignin F, the same time, the content of D equaling to the content of F minus the content of E;
(Ⅶ) To the Cellulose, Gum content and Ash, the testing is conducted according to the Ramie Criterion.
The experiments prove that this method to test the various plant fibers'chemical composition is relatively accurate, and has a general applicability. However, in actual operation, there is inevitably errors because of the complicated steps, thus affects the final result and the application of some chemical reagents are harm for the people's health to a certain extent, therefore, it needs to have a further optimization and improve the various steps to make the chemical composition quantitative analysis of plant fibers more secure, fast and accurate.
引文
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2杨淑蕙.植物纤维化学[M].北京：中国轻工业出版社,2001,4-20,43,50,69,112,163,214.
3郭建欣,王高升,陈夫山.植物纤维原料的液化及其应用[J].世界林业研究,2007,2,20(1)：55-60.
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