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Method for detecting BNST (Bed Nucleus of Stria Terminali) content in lubricants, printing ink, rubber and other products

A detection method and lubricant technology, which is applied in the field of BNST content detection in products, can solve the problems of no detection method, harmful aquatic organisms, etc., and achieve the effects of improving sensitivity and accuracy, accurate quantification, and simple operation

Active Publication Date: 2018-09-04
苏州市信测标准技术服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

BNST has not been registered in REACH Regulation (EC) No.1907 / 2006, but a company has notified the European Chemicals Agency (ECHA) that BNST is harmful to aquatic organisms and has lasting effects
However, there is no specific detection method in SOR / 2012-285 and REACH Regulation (EC) No.1907 / 2006

Method used

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  • Method for detecting BNST (Bed Nucleus of Stria Terminali) content in lubricants, printing ink, rubber and other products
  • Method for detecting BNST (Bed Nucleus of Stria Terminali) content in lubricants, printing ink, rubber and other products
  • Method for detecting BNST (Bed Nucleus of Stria Terminali) content in lubricants, printing ink, rubber and other products

Examples

Experimental program
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Effect test

Embodiment 1

[0023] This embodiment provides a method for detecting BNST content in products such as lubricants, inks, and rubber, which specifically includes the following steps:

[0024] Step 1: Weigh 3 samples with an electronic balance, each of which has the same mass of 0.2006g, and put the 3 samples into the sample bottles with labels 1, 2, and 3;

[0025] Step 2: Add 20 mL of dichloromethane + acetone as an extraction solvent mixed in a ratio of 1:1 by volume to each sample bottle, and seal it;

[0026] Step 3: After each sample is fully infiltrated, put them into an ultrasonic water bath for ultrasonic extraction. The extraction temperature of No. 1 sample is 25°C at room temperature, and the extraction time is 30 minutes. The extraction temperature of No. 3 sample is 60°C, and the extraction time is 90 minutes;

[0027] Step 4: After each extraction solution is cooled to room temperature, put it through a 0.22 μm needle-type PTFE filter membrane into the corresponding sampling bo...

Embodiment 2

[0032] In this example, the extraction solvent in Example 1 was replaced with toluene, and other steps were performed as in Example 1.

Embodiment 3

[0034] In this example, the extraction solvent in Example 1 was replaced with ethyl acetate, and other steps were performed as in Example 1.

[0035] Table 1: Factor and Level Table

[0036]

[0037] Table 2: Experimental plan and results

[0038]

[0039] Table 3: Experimental visual analysis table (based on the orthogonal table L 9 3 4 )

[0040]

[0041] from Table 3 and figure 1 It can be seen that: (1) Selection of extraction agent: the extraction solvent toluene and dichloromethane + acetone (1:1) have a better extraction effect, and dichloromethane + acetone (1:1) is preferred;

[0042] (2) Selection of extraction temperature: As the extraction temperature increases, the recovery rate increases, but the enhancement effect is not obvious.

[0043] (3) Selection of extraction time: When the extraction time is 60 minutes, the recovery rate reaches a maximum value, and the recovery rate does not change significantly when the extraction time increases.

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Abstract

The invention discloses a method for detecting BNST (Bed Nucleus of Stria Terminali) content in lubricants, printing ink, rubber and other products. The method specifically comprises the following steps: (1) weighing a sample by an electronic scale with the accuracy of 0.1mg, and putting the sample into a sample bottle; (2) adding an extracting solvent into the sample bottle, and sealing; (3) fully infiltrating the sample, adding the sample into an ultrasonic water bath, and performing ultrasonic extraction; (4) cooling the extracting solution to a room temperature, enabling the solution to enter a sample bottle via a filter membrane, performing GCMS (Gas Chromatography / Mass Spectrometry) testing analysis if a matrix effect does not occur in the extracting solution or obvious turbidity does not occur; performing purifying operations if the matrix effect occurs in the extracting solution or obvious turbidity occurs. The method disclosed by the invention is simple and convenient to operate, the analysis period is shortened, the detection sensitivity and accuracy are improved, the separation degree, linear coefficient and stability are excellent, quantification is accurate, and the recovery rate is 90% or higher.

Description

technical field [0001] The invention relates to the field of chemical analysis and detection, in particular to a method for detecting BNST content in lubricants, inks, rubber and other products. Background technique [0002] BNST, the Chinese name is alkylated diphenylamine, also known as the reaction product of diphenylamine, styrene and 2,4,4-trimethylpentene, the appearance is white powder or light yellow powder, CAS number: 68921-45- 9, the molecular formula is C 20 h 25 N 3 O, the molecular weight is 393.7, the melting point is 152°C~154°C, the flash point is 215°C, and the density is 1.1g / cm 3 , with a boiling point of 444°C at 760 mmHg, BNST is an antioxidant, mainly used as an antioxidant and or additive in lubricants in automotive engine oils, a small amount is used in inks, coatings, and as an additive in rubber. [0003] On December 14, 2012, Canada published the "Prohibition of Certain Toxic Substances Regulations 2012, SOR / 2012-285" in its official gazette, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/062
Inventor 杜适刘梦莹袁奇
Owner 苏州市信测标准技术服务有限公司