Method for accurately measuring purity of volatile substances by adopting quantitative HNMR

A technology of proton nuclear magnetic resonance spectroscopy and volatility, which is applied in the field of detection and analysis, and can solve problems that affect the accuracy of measurement results

Active Publication Date: 2018-11-16
NAT INST OF METROLOGY CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems in the prior art, the present invention provides a method for accurately measuring the purity of volatile substances by using quantitative p

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  • Method for accurately measuring purity of volatile substances by adopting quantitative HNMR
  • Method for accurately measuring purity of volatile substances by adopting quantitative HNMR
  • Method for accurately measuring purity of volatile substances by adopting quantitative HNMR

Examples

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Effect test

Embodiment 1

[0037] The purity of methyl tert-butyl ether (MTBE) was accurately measured by quantitative proton nuclear magnetic spectroscopy.

[0038] Target sample: methyl tert-butyl ether, a colorless, low-viscosity liquid, slightly soluble in water, miscible with many organic solvents, with a boiling point of 55°C, molecular formula C 5 h 12 O, the molar mass is 88.15. The sample was purchased from Sigma Company, and the gas chromatography (GC) purity was 99.94%.

[0039] At first adopt routine technology to measure: internal standard is the commonly used quantitative NMR solid internal standard acesulfame potassium (GBW (E) 100065, purity 99.6%, expanded uncertainty 0.6%, k=2), molecular formula C 4 h 4 KNO 4 S, the molar mass is 201.24.

[0040] Weigh about 32mg of acesulfame potassium solid internal standard into a 1.5mL solution bottle, weigh the mass of the internal standard, accurate to 0.01mg; use a pipette to pipette about 25mg of methyl tert-butyl ether, add the solution ...

Embodiment 2

[0050] The purity of tert-amyl methyl ether (TAME) was accurately measured by quantitative proton nuclear magnetic spectroscopy.

[0051] Target sample: methyl tert-amyl ether, boiling point 85°C, molecular formula C 6 h 14 O, the molar mass is 102.18. The sample was purchased from Sigma Company, and the gas chromatography (GC) purity was 98.60%.

[0052] Adopt the method of the present invention, the internal standard selects national primary standard substance ethyl acetate (GBW06114, purity 99.7%, expanded uncertainty 0.4%, k=2), boiling point 77.5 ℃, molecular formula C 4 h 8 o 2 , with a molar mass of 88.11.

[0053] Transfer 0.6mL of deuterated chloroform to a 1.5mL sealed sample bottle with a 1000 μL airtight needle, transfer about 19 mg of internal standard ethyl acetate into the sample bottle with a 50 μL airtight needle, and use a high-precision balance (d = 0.01 mg) weigh the mass of ethyl acetate; then use another 50 μL airtight needle to transfer about 15 mg...

Embodiment 3

[0058] The purity of isopropanol (IPA) was accurately measured by quantitative proton nuclear magnetic spectroscopy.

[0059] Target sample: Isopropanol, a colorless transparent liquid with an odor like a mixture of ethanol and acetone. Soluble in water, also soluble in alcohol, ether, benzene, chloroform and most other organic solvents. Boiling point is 82°C, molecular formula C 3 h 8 O, the molar mass is 60.1. The sample was purchased from Sigma Company, and the gas chromatography (GC) purity was 99.98%.

[0060] Adopt the method of the present invention, the internal standard selects national primary standard substance methanol (GBW06111, purity 99.7%, expanded uncertainty 0.3%, k=2), boiling point 65.4 ℃, molecular formula CH 4 O, the molar mass is 32.04.

[0061] Transfer 0.6mL deuterated dimethyl sulfoxide to a 1.5mL sealed sample vial with a 1000 μL airtight needle, transfer about 29 mg of internal standard methanol into the sample vial with a 50 μL airtight needle...

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Abstract

The invention discloses a method for accurately measuring the purity of volatile substances by adopting quantitative HNMR (Hydrogen Nuclear Magnetic Resonance). The method comprises the following steps: (1), taking a volatile substance as a to-be-detected target sample; (2), taking high-purity solvent standard substance with metrological traceability as an interior label; (3), accurately weighingthe target sample and the interior label in a sealed sample bottle through an air-tight needle and a high-precision balance, and dissolving in deuterated solvent to prepare solution; and (4), after mixing uniformly, transferring the solution into a sealed nuclear magnetic tube through the air-tight needle to perform HNMR measurement. The method can effectively solve the problem that the measurement result is not accurate due to weighing deviation caused by sample volatilization. The method provided by the invention has the characteristics that the degree of accuracy is high and the result cantrace to the source of SI, and the like, and the method can be applied to scientific researches such as high-accuracy analysis and detection and standard substance valuing.

Description

technical field [0001] The invention relates to the technical field of detection and analysis, and furthermore, relates to a method for accurately measuring the purity of volatile substances by using quantitative nuclear magnetic resonance proton spectrum. The result has accurate and reliable metrological traceability. Background technique [0002] Quantitative nuclear magnetic resonance technology is often used to measure the purity of organic compounds or the content of certain components. Its characteristic is that this technology does not need to separate the target compound, and the intensity of the generated signal depends entirely on the chemical structure and amount of the sample. Samples were quantified with internal standard peak responses to measure target sample purity. because 1 H proton nuclei have high sensitivity and relatively short relaxation time, making hydrogen spectroscopy 1 HqNMR is well suited for quantitative analysis. At present, the quantitativ...

Claims

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Application Information

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IPC IPC(8): G01N24/08
CPCG01N24/082
Inventor 全灿杨菡张伟黄挺何雅娟李红梅
Owner NAT INST OF METROLOGY CHINA
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