Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for Determination of Hydrogen-containing Silicone Oil Residue in Trisiloxane Surfactant by One-dimensional Proton Nuclear Magnetic Resonance Spectroscopy

Active Publication Date: 2017-06-27
SUN YAT SEN UNIV
View PDF6 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the invention is to overcome the deficiencies in the prior art, to provide a simple, fast one-dimensional hydrogen nuclear magnetic resonance spectrum method to measure the residual amount of hydrogen-containing silicone oil in the trisiloxane surfactant, to solve the problem caused by the signal in the conventional hydrogen spectrum Overlap affects the accurate quantification of a compound and the problem of cumbersome testing

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for Determination of Hydrogen-containing Silicone Oil Residue in Trisiloxane Surfactant by One-dimensional Proton Nuclear Magnetic Resonance Spectroscopy
  • Method for Determination of Hydrogen-containing Silicone Oil Residue in Trisiloxane Surfactant by One-dimensional Proton Nuclear Magnetic Resonance Spectroscopy
  • Method for Determination of Hydrogen-containing Silicone Oil Residue in Trisiloxane Surfactant by One-dimensional Proton Nuclear Magnetic Resonance Spectroscopy

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] Determination of MD by one-dimensional proton NMR spectroscopy and chemical method H Consistency analysis of M hydrogen content:

[0061] In order to verify the feasibility of using the one-dimensional hydrogen nuclear magnetic resonance spectrum internal standard method to measure the hydrogen content of hydrogen-containing silicone oil, the present invention uses chemical titration to measure the hydrogen content of hydrogen-containing silicone oil as a comparison, and also in the determination of other embodiments The chemical titration method was also used as a comparison.

[0062] Reagents used and sample preparation: MD with a purity of 99% H M was purchased from West Asia Reagent Company, 99.9% deuterated chloroform (CDCl 3 ) were purchased from CIL (Cambridge Isotope Laboratories, Massachusetts, USA). Sodium thiosulfate (AR), potassium iodide (AR), soluble starch (AR) and concentrated sulfuric acid (AR) were purchased from Tianjin Damao Reagent Factory, potas...

Embodiment 2

[0079] Determination of residual MD in trisiloxane surfactants with an average molecular weight of 612 H M content

[0080] During the actual storage and production process, MD H M will produce hydrogen after standing for a period of time. Due to the residual MD in the production of trisiloxane surfactant H M, a certain amount of MD remains H M can cause the bag to bulge or even rupture. Therefore, the MD in the trisiloxane surfactant H The detection of M content plays an important guiding role in production.

[0081] When determining the content of hydrogen-containing silicone oil in trisiloxane surfactant, MD can be expressed by the hydrogen content H The size of the M residue.

[0082] Preparation of internal standard solution: Weigh 0.0600g of 1,3,5-tribromobenzene into a 5mL volumetric flask, add deuterated chloroform and ultrasonically dissolve, dilute to 5mL with deuterated chloroform, the concentration is 12mg / mL, pipette Take 0.25mL of the standard solution in...

Embodiment 3

[0085] Embodiment 3: Determination of the expansion of the hydrogen-containing silicone oil residual method in trisiloxane surfactants of different molecular weights

[0086]In order to further verify the feasibility of the method for determining the residual amount of hydrogen-containing silicone oil in trisiloxane surfactants, the present invention uses trisiloxane surfactant mixtures with different numbers of EO chain members as quantitative research objects. The preparation and pipetting of the internal standard solution were consistent with Example 2. The preparation and pipetting of the sample solution were consistent with Example 2.

[0087] Test according to the above-mentioned NMR test conditions to obtain a one-dimensional proton nuclear magnetic resonance spectrum, such as Figure 4 Shown is the one-dimensional proton nuclear magnetic resonance spectrum of the trisiloxane surfactant whose average molecular weight is 674. The results of three parallel determination...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a determination method of hydrogen-containing silicone oil residual quantity in a trisiloxane surfactant. The determination method comprises the following steps of adopting one-dimensional hydrogen nuclear magnetic resonance, and using single-peaked 1,3,5-tribromobenzene as a unified internal standard to perform quantitative analysis or concentration determination on the trisiloxane surfactant, wherein the quantitative analysis is performed by using the single-peaked internal standard as a one-dimensional nuclear magnetic resonance quantitative medium. The method not only can be used for determining the hydrogen content of methyl hydrogen silicone oil and block hydrogen silicone oil, but also can be used for the determination of the content of hydrogen-containing silicone oil in the trisiloxane surfactant. The concentration of each monomeric compound can be directly obtained through calculation according to a direct ratio relationship between the integral of a characteristic nuclear magnetism signal of a compound in a sample and the concentration thereof. According to the method, the problems that the determination is inaccurate and a test is complex due to overlapped signals of the trisiloxane surfactant are solved, and the experimental scheme of the method also has the possibility of accurately determining the content of multiple compounds in a mixture.

Description

technical field [0001] The invention belongs to the field of chemical instrument analysis methods, and in particular relates to the determination of the residual amount of hydrogen-containing silicone oil in trisiloxane surfactants by a one-dimensional hydrogen nuclear magnetic resonance spectrum method. Background technique [0002] NMR technology has become an essential tool in the qualitative research of compounds because it can provide the most detailed, true and reliable chemical structure information. With the development of nuclear magnetic resonance technology, one-dimensional nuclear magnetic resonance is often used in quantitative analysis because it has many unique advantages: [0003] For a defined nucleus, the signal intensity is proportional to the number of nuclei producing the signal and has nothing to do with the chemical nature of the nucleus. When using the internal standard method or relative measurement method to analyze a certain compound in the mixtur...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): G01N24/08
Inventor 纪红兵符国华李玮
Owner SUN YAT SEN UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com