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Method for measuring water contents of organic matters by virtue of nuclear magnetic resonance instrument

A nuclear magnetic resonance apparatus and nuclear magnetic resonance technology, which is applied in the direction of using nuclear magnetic resonance for analysis, etc., can solve the problems of low measurement accuracy and achieve the effect of good measurement accuracy

Active Publication Date: 2015-11-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The centrifuge method for measuring water and sediment in crude oil (GB / T6533-86) has low measurement accuracy, and is more suitable for rough on-site determination of crude oil with high water content and low accuracy requirements

Method used

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  • Method for measuring water contents of organic matters by virtue of nuclear magnetic resonance instrument
  • Method for measuring water contents of organic matters by virtue of nuclear magnetic resonance instrument
  • Method for measuring water contents of organic matters by virtue of nuclear magnetic resonance instrument

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0031] Determine the water content of crude oil by standard methods.

[0032] Take a crude oil sample and determine the water content in it according to GB / T8929-2006 Crude Oil Water Content Determination Method (Distillation Method): add xylene solvent to the crude oil sample and heat and distill under reflux conditions. The condensed solvent and water are continuously separated in the receiver, the water settles to the volume scale part of the receiver, and the solvent is returned to the distillation flask. Calculate the percentage of water in the sample based on the volume of water in the receiver and the sample amount.

[0033] The amount of samples and solvents used in the above distillation method to determine the water content of crude oil is shown in Table 1.

[0034] Table 1

[0035] Item

example 2

[0037] Establish a standard curve for the determination of crude oil water content and investigate the linear range of the determination curve.

[0038] Take 26 crude oil samples, measure the water content of each sample according to the method of Example 1, then take 3 mL samples, preheat in a water bath at 42°C for 15 minutes, and measure their hydrogen spectrum with a 58MHz nuclear magnetic resonance analyzer to obtain Fourier transform. After the frequency domain spectrum, the proton nuclear magnetic resonance spectra of 4 samples are shown in figure 1 . by figure 1 It can be seen that the peak positions of hydrogen atoms in water are far away from the peak positions of hydrogen atoms in other hydrocarbons.

[0039] Integrate the peak intensity in the characteristic region with a chemical shift of 4.0 to 5.5 ppm (corresponding to 340 to 400 points) in the hydrogen spectrum of the crude oil sample to obtain the peak area in this range. Correlate the measured peak area of ​​each...

example 3

[0042] It illustrates the repeatability of the method of the present invention to determine the water content.

[0043] Take two crude oil samples, use the standard method described in Example 1 to determine their water content, and then use the method of Example 2 to measure their proton nuclear magnetic resonance spectrum. Each crude oil sample is collected three times repeatedly, and the chemical shift is calculated to be 4.0~ The peak area in the characteristic area of ​​5.5 ppm is substituted into the standard curve to obtain the predicted value of the water content of the sample. The predicted value of the water content and the measured value by the standard method are shown in Table 2.

[0044] It can be seen from Table 2 that the relative standard deviation of the water content of crude oil samples determined by this method is within 0.025% by mass, indicating that the method of the present invention has good repeatability.

[0045] Table 2

[0046]

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Abstract

The invention provides a method for measuring the water contents of organic matters by virtue of a nuclear magnetic resonance instrument. The method comprises the following steps: (1) selecting a series of organic matter samples with different water contents and measuring the water contents of the samples by use of a standard method; (2) detecting the organic matter samples by use of the nuclear magnetic resonance instrument so as to obtain a 1H NMR spectrum, calculating peak areas with the chemical displacement of 4.0-5.2ppm, associating the detected peak areas of the samples in a spectrum region and the water contents obtained by the standard method, and establishing a standard curve; and (3) measuring the 1H NMR spectrum of the to-be-measured samples, calculating peak areas with the chemical displacement of 4-5.2ppm, and taking the peak area values into the standard curve, so as to obtain the water contents of the to-be-measured samples. The method is capable of measuring the water contents of the organic matters by virtue of measuring the 1H NMR spectrum of the to-be-measured samples, so that the method is convenient, rapid and accurate in operation.

Description

Technical field [0001] The present invention is a method for measuring the water content in organic matter by a nuclear magnetic resonance instrument, specifically, a method for measuring the water content in a sample according to the hydrogen nuclear magnetic resonance spectrum. Background technique [0002] In the process of crude oil processing, excessive water content will cause the operation of the distillation tower to be unstable. In severe cases, the material will easily flush out of the distillation tower. At the same time, too much water content will increase the energy consumption of the atmospheric and vacuum unit and increase the consumption of cooling water. In addition, when trading crude oil, the level of water content affects the interests of both sides of the trade. Therefore, the water content must be accurately measured before the crude oil enters the factory and the equipment is processed to provide reference data for crude oil trade and processing. [0003] T...

Claims

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Application Information

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IPC IPC(8): G01N24/08
Inventor 冯云霞田松柏褚小立许育鹏王京
Owner CHINA PETROLEUM & CHEM CORP
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