ASTM D5974-15由美国材料与试验协会 US-ASTM 发布于 2015。
ASTM D5974-15在国际标准分类中归属于: 67.080.10 水果及其制品,67.200.10 动物和植物的脂肪和油。
ASTM D5974-15 采用毛细管气相色谱法测定妥尔油分馏产品中脂肪和树脂酸的标准试验方法的最新版本是哪一版?
最新版本是 ASTM D5974-20 。
3.1 Tall oil fractionated products derived from tall oil are important commercial materials, primarily composed of fatty acids and rosin acids, but also containing some neutral material (see Terminology D804). For many applications, it is necessary to know the level of the individual fatty acids and rosin acids present in these products. Gas chromatography has proven to be a useful tool for such determinations (see Test Methods D509), and capillary chromatography, described in these test methods, is considered to be the most effective gas chromatographic technique currently available. In particular situations, other techniques may be more suitable than gas chromatography. For example, the presence of fatty acid esters in the sample would result in transesterification during the derivatization step that may affect the results.
3.2 Due to hydrogen bonding, unmodified tall oil fatty acids and rosin acids cannot be volatilized at atmospheric pressure without undergoing decomposition. So, it is necessary to convert the free acids to the more volatile and more stable methyl esters, prior to chromatographic separation.
3.3 These test methods describe four ways to prepare methyl esters. The classic method is through the use of diazomethane, but diazomethane is a hazardous and toxic material, and so is no longer the preferred agent. The use of diazomethane is detailed in Appendix X1.
3.3.1 TMAH causes isomerization of a sample’s di- and polyunsaturated fatty acids, when it is used in even a slight excess. This leads to inaccurate results for the individual fatty acid components. TMAH should be used for materials containing only rosin acids, or when the identification or quantitation of individual fatty acid components is not important.
3.3.2 TMPAH is the recommended methylating agent when the identification or quantitation of individual di- and polyunsaturated fatty acids is required. TMPAH produces results that are very similar to those of diazomethane, but without the hazards that are associated with diazomethane. A considerable excess of TMPAH may cause isomerization of conjugated compounds similar to that encountered with TMAH.
3.3.3 DMF-DMA gives results comparable to TMPAH and is easy and safe to use. However, the reagent is moisture sensitive, requiring samples to be free of any significant levels of water.
3.4 Two test methods for calculating the amounts of the individual fatty acid and rosin acid methyl esters are included in these test methods. When the actual weight percentage of a given compound is required, the “internal standard” method must be used. This method involves adding a known amount of an internal standard to a known amount of test material, and comparing the area of the peak associated with the internal standard with the area of the peak of the individual fatty acid or rosin acid methyl esters. The “area percent” method will give the relative amount of each component, by comparing the area of the appropriate peak to the total area of all peaks. Non-eluting compounds will lead to erroneous (absolute) results with this method.
1、用于卫生质量监测和产品质量检验目前,白酒产品质量标准共有14项标准,其中有10项是用气相色谱法测定的,标准方法包括填充柱气相色谱法和毛细管柱气相色谱法。尽管有许多类型的标准,但甲醇和杂醇油的卫生标准有限公司需要进行测量,对国家白酒类泸州白酒类总量约占7 000,其次是汾酒白酒类,从生产或地理覆盖白酒类其他类型要小得多。...
根据脂肪酸组成与含量,即可鉴别油品种类。 2.气相色谱法测定脂肪酸,通常用硫酸-甲醇法,和AOAC-IUPAC 标准法,我们采用了氢氧化钾-甲醇法,经试验3种方法测定结果差异无显著性。...
根据脂肪酸组成与含量,即可鉴别油品种类。 2.气相色谱法测定脂肪酸,通常用硫酸-甲醇法,和AOAC-IUPAC 标准法,我们采用了氢氧化钾-甲醇法,经试验3种方法测定结果差异无显著性。...
在这个过程中还发生了裂化和成环的二级反应,变小了的分子透过催化剂的空隙在活化中心继续反应,在其后的冷却和物质分离阶段,气体和液体产物便分离开来。 废弃脂肪通过热催化转化所产生的液相和气相物质采用气相色谱法进行分离和测定。液相产物采用配置有低温致冷柱(应用液态氮)的气相色谱仪进行测量,柱温程序从0 ℃开始,以便测得易挥发性组分。 图2. 一种液体产物的GC/MS图谱。...
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