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Method for determining active ingredients of synthetic grease by using gas chromatography

A technology of gas chromatography and active ingredients, which is applied in the field of determining the composition of lubricating grease, can solve the problems of lack of detection standards for synthetic lubricating grease, and achieve the effects of lowering the gasification point, expanding the measurement range, and reducing the load

Active Publication Date: 2018-01-09
FOSHAN SHUNDE FUYANSHENG LUBRICANT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there is a lack of testing standards for the effective components of synthetic grease in the national standard, so it is necessary to propose a component detection method to determine the active components of synthetic grease

Method used

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  • Method for determining active ingredients of synthetic grease by using gas chromatography
  • Method for determining active ingredients of synthetic grease by using gas chromatography
  • Method for determining active ingredients of synthetic grease by using gas chromatography

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] In this example, unity comparison is used, petroleum ether is selected as the extractant, and two commonly used additives are used for gas chromatography detection to obtain the chromatogram of the additive test solution. The two additives are antioxidants and rust inhibitors. A total of 5 parallel tests were performed for each group of additives, and the chromatographic peak retention time of the obtained additive test solution was summarized in Table 1, and the chromatographic peak retention time range of the two additives was obtained.

[0051] Table 1

[0052]

[0053] In this embodiment, the antioxidant is diphenylamine, the rust inhibitor is sorbitol monooleate, and the obtained chromatogram of the additive test solution is a single-peak chromatogram. In order to improve the reliability of the test and ensure that the retention time of the chromatographic peak in Table 1 is the retention time of the peak of the additive test solution, a blank control gas chromatogram i...

Embodiment 2

[0055] The base oil used in the samples of this example is a synthetic oil containing pentaerythritol tetraester oil. This pentaerythritol tetraester oil is produced by the esterification reaction of pentaerythritol and two fatty acids. Its effective ingredients contain 5 effective substances, and, Because this kind of reaction is an incomplete and reversible reaction, in addition to additives, there are active ingredients and incomplete reaction by-products in the sample.

[0056] The sample quantitative test requires at least 3 parallel tests. In this example, a total of 4 parallel tests are performed. The chromatogram of the sample test solution obtained is as follows: Figure 2-Figure 5 As shown, get the retention time of each component chromatographic peak in the sample.

[0057] Calculation of analysis results of active ingredients

[0058] Using the area normalization algorithm, the content of component i is calculated by the following formula:

[0059]

[0060] A i =1.065×H i...

Embodiment 3

[0071] Example 3: The base oil used in the sample of this example is a synthetic oil containing pentaerythritol tetraester oil. This pentaerythritol tetraester oil is produced by the esterification reaction of pentaerythritol and two fatty acids. The effective ingredients contain 5 effective ingredients. Substance, and because this kind of reaction is an incomplete reversible reaction, in addition to additives, there are active ingredients and by-products of incomplete reaction in the sample.

[0072] Dilute 0.16g sample with petroleum ether to 10ml, call the gas chromatograph in the "DR301" operation mode for detection, measure 0.8μl of sample test solution into the sample, perform gas spectrum analysis and test, and establish a chromatogram of the sample test solution. The chromatogram of the sample test solution is as follows Image 6 As shown, get the retention time of each component chromatographic peak in the sample.

[0073] analysis Image 6 There are 10 chromatographic pea...

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Abstract

The invention discloses a method for determining active ingredients of synthetic grease by using gas chromatography. The method comprises the following steps: S1, extracting an additive by using petroleum ether or chromatographic methanol to obtain additive detection liquor; S2, regulating and optimizing gas chromatography parameters, performing quantitative sample injection on the tested additiveliquid, performing gas chromatography analysis and detection, establishing a chromatogram of the tested additive liquid to obtain a chromatographic peak retention time range of the additive, and establishing a chromatogram group of the additive detection liquor; S3, diluting and extracting the samples by using petroleum ether or alkane and other organic solvents so as to obtain sample detection liquor; S4, holding the gas chromatography a parameters, performing quantitative sample injection on the samples, performing gas chromatography analysis and detection, and establishing a chromatogram of the sample liquid tested; and S5, analyzing and calculating the chromatogram of the sample liquid tested, and determining the content of the active ingredients in the samples. According to the method, the ratio of each component in the synthetic grease can be easily analyzed, the detection result is accurate, and the method is time-saving and high-efficiency.

Description

Technical field [0001] The present invention relates to a method for determining the composition of grease used in machine parts, vehicles or other lubricating mechanisms, and in particular to a method for determining the effective components of synthetic grease using gas chromatography. Background technique [0002] Synthetic lubricating grease is a semi-solid mechanical part lubricant made of synthetic lubricating oil as the base oil, adding corresponding thickeners and lubricating additives. Compared with petroleum lubricating grease, this type of lubricant has better high and low temperature resistance, High vacuum resistance, chemical stability, flame retardancy and radiation resistance, etc., used for lubricating parts of military and civilian equipment with harsh working conditions. Synthetic grease is generally composed of 10%-20% thickener, 75%-90% base oil, 5% or less additives and fillers. The conversion rate of reaction into effective ingredients will directly affect ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 张军霍庆权
Owner FOSHAN SHUNDE FUYANSHENG LUBRICANT