Method for detecting contents of glyceride and free fatty acid in biodiesel

A free fatty acid and biodiesel technology, which is applied in the direction of measuring devices, material separation, instruments, etc., can solve the problems of large instrument damage, inaccurate quantification, and low sensitivity, and achieve the effect of shortening the detection time

Active Publication Date: 2014-12-24
仕宝(天津)技术检测有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above methods often have shortcomings such as inaccurate quantification, incomplete information, low sensitivity, or large instrument damage, which limits their wide application.

Method used

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  • Method for detecting contents of glyceride and free fatty acid in biodiesel
  • Method for detecting contents of glyceride and free fatty acid in biodiesel
  • Method for detecting contents of glyceride and free fatty acid in biodiesel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: The detection of each fatty acid and glyceride in the biodiesel (sample 1) to be tested by thin-layer chromatography combined with heat-assisted hydrolysis methylation gas chromatography

[0030] (1) Separation process of thin-layer chromatography: firstly, 100 μL of the biodiesel sample to be tested (sample 1) was dissolved in 500 μL of ethyl acetate, and diluted 6 times. After mixing evenly, draw 1 μL with a liquid phase blunt needle, point it on one end of a 10 cm aluminum foil base chromatography silica gel plate, and develop it in the developer n-hexane / ethyl acetate / formic acid (90 / 10 / 2). When the front of the solvent extends to the other end of the TLC, the TLC is taken out, and after the solvent is evaporated, the color is developed with iodine vapor. At this time, the analytes to be measured on the thin layer appear as brown or yellow spots, and the thin layer chromatogram is shown in figure 1 far right, figure 1 On the left are thin layer chrom...

Embodiment 2

[0044] Example 2: Detection of Fatty Acids and Glycerides in 5 Kinds of Biodiesel to be Tested by Thin Layer Chromatography Combined with Heat-Assisted Hydrolysis Methylation Gas Chromatography

[0045] See Example 1 for the detection process and data of Sample 1. Samples 2, 3, and 4 were diluted 3 times, sample 5 was diluted 2 times, and other operations were the same as sample 1.

[0046] According to the peak area and standard curve of the gas chromatogram of the sample to be tested, the concentration of monoglyceride, di-ester, tri-ester and free fatty acid in the sample to be tested, and the distribution of fatty acid components in the molecule are obtained, see Table 2.

[0047] Table 2

[0048] Contents of residual glycerides and free fatty acids in 5 biodiesel samples, and their fatty acid composition distribution

[0049]

[0050]

[0051] *Fatty acid composition refers to the percentage of each methyl ester peak area to the total methyl ester peak area. Does...

Embodiment 3

[0053] In sample 4, add standard product stearic acid monoglyceride 2380mg / L, stearic acid diglyceride 1230mg / L, stearic acid triglyceride 2240mg / L, oleic acid 2460mg / L, obtain spiked sample 4, After mixing evenly, conduct thin-layer chromatography-heat-assisted hydrolysis methylation gas chromatography analysis. The operating conditions are the same as sample 4. Calculate respectively the content of monoglyceride, diglyceride, triglyceride and free fatty acid in this spiked sample 4 according to the standard curve, subtract the original content of each glyceride and free fatty acid in sample 4 in Table 2, can get its recovery rate. The spiked recoveries of monoglyceride, diglyceride, triglyceride and free fatty acid were 110.8%, 116.7%, 87.5%, 97.2%, respectively. The operation was repeated three times, and the obtained RSD values ​​were 9.7%, 10.3%, 5.8%, and 7.5%.

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Abstract

The invention discloses a method for detecting the contents of glyceride and free fatty acid in biodiesel. The method comprises the following steps: diluting a biodiesel sample, carrying out thin layer chromatograph with an aluminum matrix silica gel plate; with n-hexane, acetic ether and formic acid mixed solvent as a developer, developing with iodine steam, wherein the volume ratio of the n-hexane, acetic ether and formic acid is 90:10:2; after separating, cutting off the spots of monoglyceride, diglyceride, glycerin trilaurate and free fatty acid; putting the cut spots and carbinol solution of three methyl hydrogen trioxide into a sample cup; putting the sample in a cracker; placing the cracker at a GC sample feeding opening, and feeding the sample when the temperature of the cracker reaches 300-450 DEG C; carrying out gas chromatograph detection to obtain the gas chromatogram of the to-be-detected sample; comparing the gas chromatogram with the standard curves of monoglyceride, diglyceride, glycerin trilaurate and free fatty acid and calculating to obtain the contents of glyceride and free fatty acid in the to-be-detected sample. The method is simple in operation, accurate in quantization and comprehensive in information and has profound significance on quality control of the biodiesel.

Description

(1) Technical field [0001] The invention relates to a method for detecting the content of glyceride and free fatty acid in biodiesel, which can quickly and accurately measure the content of residual glyceride and free fatty acid in biodiesel through the method of thin layer chromatography combined with heat-assisted hydrolysis methylation gas chromatography. (2) Technical background [0002] Biodiesel is an emerging non-toxic, renewable and degradable green energy. It is mainly prepared from unprocessed or used vegetable oil and animal fat through different chemical reactions. It has become a high-quality substitutes for petroleum diesel. However, due to the incomplete reaction, a small amount of by-products such as monoglycerides, diglycerides, triglycerides, and free fatty acids often remain, seriously affecting the quality of biodiesel, thereby affecting the performance of the engine. The EU standard (EN 14214:2008) stipulates that the content of monoglyceride, diglyceri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/90G01N30/88
Inventor 王丽丽张佩佩孙杨黄忠平黄翌磊潘再法
Owner 仕宝(天津)技术检测有限公司
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