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Quantitative nuclear magnetic hydrogen spectrum valuing method for 2, 4, 6-trinitrotoluene standard substance

A technology of trinitrotoluene and standard substances, which is applied in the field of measurement and detection of energetic materials, can solve the problems of inapplicability of trinitrotoluene, etc., and achieve the effects of ensuring accuracy, less sampling amount, and accurate and reliable characteristic value determination

Pending Publication Date: 2020-04-14
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

None of the existing technologies are suitable for the determination of the purity standard substance of trinitrotoluene, so it is necessary to study and establish a new method that is faster and simpler and meets the special needs of the determination of the purity standard substance of trinitrotoluene

Method used

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  • Quantitative nuclear magnetic hydrogen spectrum valuing method for 2, 4, 6-trinitrotoluene standard substance
  • Quantitative nuclear magnetic hydrogen spectrum valuing method for 2, 4, 6-trinitrotoluene standard substance
  • Quantitative nuclear magnetic hydrogen spectrum valuing method for 2, 4, 6-trinitrotoluene standard substance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The purity of 2,4,6-trinitrotoluene standard substance was determined by quantitative NMR method with hexamethyldisiloxane standard substance as internal standard substance.

[0047] 1.1 Instrument and sample preparation

[0048]① Instruments: Bruker Ascend 800 superconducting NMR spectrometer (BRUKER, Germany), MettlerToledo XP6 one-hundred-thousandth balance (METTLER, Switzerland);

[0049] ② deuterated acetone (deuterated degree > 99.8%, American CIL company); 5mm standard NMR sample tube (American NORELL company); hexamethyldisiloxane solution standard product (Xi'an Institute of Modern Chemistry, content 0.102%, U= 2%), 2,4,6-Trinitrotoluene standard product (primary metering station for propellant and explosives in national defense science and technology industry)

[0050] 1.2 Preparation and determination of NMR samples to be tested

[0051] Accurately weigh about 20 mg of the 2,4,6-trinitrotoluene standard substance to be tested in a 5 mm NMR tube, then direct...

Embodiment 2

[0076] The purity of 2,4,6-trinitrotoluene standard substance was determined by quantitative NMR method with fumaric acid purity standard substance as internal standard substance.

[0077] 2.1 Instrument and sample preparation

[0078] ① Instruments: Bruker Ascend 800 superconducting NMR spectrometer (BRUKER, Germany), MettlerToledo XP6 one-hundred-thousandth balance (METTLER, Switzerland);

[0079] ② deuterated methanol (deuterated degree > 99.8%, American CIL company); 5mm standard NMR sample tube (American NORELL company); fumaric acid standard (Germany Dr.Ehrensforfer, purity 99.9%), 2,4, 6-Trinitrotoluene standard product (first-level metering station for explosives in national defense technology industry)

[0080] 2.2 Solution preparation

[0081] Accurately weigh about 150mg of the internal standard fumaric acid into a 10ml volumetric flask, then add the solvent deuterated methanol to make the volume to 10ml and accurately weigh, mix well and set aside.

[0082] 2.3 ...

Embodiment 3

[0104] 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 2,4,6-trinitrotoluene NMR samples to be tested 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 20...

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Abstract

The invention discloses a valuing method of a 2, 4, 6-trinitrotoluene standard substance. The content of a main component 2, 4, 6-trinitrotoluene in the standard substance is determined by using an internal standard substance with metering traceability based on quantitative 1H NMR technology. The method has the characteristics of simplicity, feasibility, low cost, good stability, high precision, strong specificity and the like, and has the broad application prospects in the 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 in particular relates to a quantitative nuclear magnetic hydrogen spectrum determination method for a purity standard substance of 2,4,6-trinitrotoluene. 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 ...

Claims

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Application Information

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IPC IPC(8): G01N24/08
CPCG01N24/08
Inventor 刘可王民昌徐敏张丽涵程瑞陈智群张皋常海赵嘉静何少蓉
Owner XIAN MODERN CHEM RES INST
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