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Quantitative nuclear magnetic hydrogen spectrum valuing method of pentaerythritol standard substance

A pentaerythritol and standard substance technology, which is applied in the field of quantitative hydrogen nuclear magnetic spectrum determination of pentaerythritol purity standard substances, can solve the problems of difficult pentaerythritol signal, low determination accuracy, etc. Accurate and reliable setting value

Active Publication Date: 2020-04-24
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high vaporization temperature of pentaerythritol, gas chromatographic detection usually requires derivatization treatment to complete the determination, and the corresponding determination accuracy is low; due to the limitation of ultraviolet detectors in high performance liquid chromatography, it is usually difficult to directly detect pentaerythritol Signal

Method used

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  • Quantitative nuclear magnetic hydrogen spectrum valuing method of pentaerythritol standard substance
  • Quantitative nuclear magnetic hydrogen spectrum valuing method of pentaerythritol standard substance
  • Quantitative nuclear magnetic hydrogen spectrum valuing method of pentaerythritol standard substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] With hexamethyldisiloxane standard substance as internal standard substance, the purity of pentaerythritol standard substance was determined by quantitative NMR method.

[0053] 1.1 Instrument and sample preparation

[0054] ① Instrument: BrukerAscend 800 superconducting nuclear magnetic resonance spectrometer (German BRUKER company), MettlerToledo XP6 1 / 100,000 balance (Switzerland METTLER company);

[0055] ② 5mm standard NMR sample tube (NORELL, USA); hexamethyldisiloxane deuterated acetone solution standard (Xi’an Institute of Modern Chemistry, content 0.102%, U=2%), pentaerythritol standard (National Defense Science and Technology Industry Explosive One level metering station)

[0056] 1.2 Preparation and determination of NMR samples to be tested

[0057] Accurately weigh about 20 mg of pentaerythritol standard substance to be tested in a 5 mm NMR tube, then directly pipette about 0.6 ml of deuterated acetone standard solution of hexamethyldisiloxane and weigh, m...

Embodiment 2

[0087] With fumaric acid purity standard substance as internal standard substance, the purity of pentaerythritol standard substance was determined by quantitative NMR method.

[0088] 2.1 Instrument and sample preparation

[0089] ① Instrument: BrukerAscend 800 superconducting nuclear magnetic resonance spectrometer (German BRUKER company), MettlerToledo XP6 1 / 100,000 balance (Switzerland METTLER company);

[0090] ② Deuterated methanol (deuterium degree > 99.8%, American CIL company); heavy water (deuteration degree > 99.8%, American CIL company) 5mm standard NMR sample tube (NORELL company in the United States); fumaric acid standard product (Germany Dr.Ehrensforfer, purity 99.9%), standard pentaerythritol (first-level metering station for explosives in national defense technology industry)

[0091] 1.2 Solution preparation

[0092] Accurately weigh about 150mg of the internal standard fumaric acid into a 10ml volumetric flask, then add a 2:1 mixed solvent of deuterated me...

Embodiment 3

[0117] Since the relaxation of protons in different chemical environments in the NMR samples to be tested is different, the time required for the relaxation to fully return to equilibrium after the protons are excited in the magnetic field environment is different. In the classical NMR theory, it is required to use a 90-degree pulse to achieve complete relaxation in quantitative NMR experiments, and the pulse delay time (d 1 ) must be greater than five times the spin-lattice relaxation time (T 1 ). For the NMR samples to be measured of pentaerythritol as the internal standard of fumaric acid and hexamethyldisiloxane, an inversion recovery experiment (180 ° and 90 ° pulse, d 1 Range: 0.01s~20s) to T 1 Determination of the spin-lattice relaxation time T of the characteristic hydrogen atoms on several compounds 1 As shown in Table 4 below. Then if the data shown in Table 4 shows that no matter which internal standard is used, the pulse delay time (d 1 ) must reach at least 2...

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Abstract

The invention discloses a valuing method of a pentaerythritol standard substance. Based on a quantitative nuclear magnetic resonance technology (1H NMR), an internal standard substance with metering traceability is adopted to directly determine a content of main component pentaerythritol in the standard substance. The method has characteristics of simplicity, feasibility, low cost, good stability,high precision, strong specificity and the like, and has a wide application prospect in aspects of standard substance calibration, intermediate check and the like.

Description

technical field [0001] The invention belongs to the field of measurement and detection of energetic materials, and relates to a method for quantitatively determining the value of pentaerythritol purity standard substances by proton nuclear magnetic spectrum. Background technique [0002] A standard substance is "a substance or material that has one or more sufficiently uniform and determined characteristic values ​​for calibrating measuring equipment, evaluating measuring methods, or assigning values ​​to materials", and its fundamental characteristic is that it has quantitative accuracy. Compared with ordinary purity substances, the characteristic value of the standard substance has traceability, which can be traced to the unit of measurement used to represent the characteristic value that is accurately reproduced, and is accompanied by an uncertainty of a given confidence level. As an important class of standard substances, purity standard substances are used to accurately...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 刘可陈智群王民昌徐敏常海张皋张丽涵赵嘉静何少蓉
Owner XIAN MODERN CHEM RES INST
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