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Detection method of alkyl nitrate

A technology of an alkyl nitrate and a detection method, applied in the field of chemical analysis, can solve the problems of interfering measurement results, cumbersome operation steps, health of operators and adverse effects of laboratory environment, etc., and achieves the effect of eliminating interference and high selectivity

Pending Publication Date: 2021-03-30
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcomings of the existing determination method mainly include: 1. The operation steps of calibration solution preparation and sample pretreatment reaction extraction are cumbersome, and the analysis manual operation cycle is long; 2. Corrosive strong acid needs to be used in the sample pretreatment reaction extraction step And toxic, highly volatile meta-xylenol, which will adversely affect the health of operators and the laboratory environment; 3. Before testing, it is necessary to fully understand the type of alkyl nitrate added. If the calibration used The solution and the sample to be analyzed contain different alkyl nitrates, which will interfere with the determination results

Method used

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  • Detection method of alkyl nitrate
  • Detection method of alkyl nitrate
  • Detection method of alkyl nitrate

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preparation example Construction

[0034] (1) Preparation of calibration solution: by adding a certain amount of alkyl nitrate standard substance to carbon disulfide, prepare a series (at least 4) of carbon disulfide calibration solutions with known accurate concentration of alkyl nitrate.

[0035] (2) Spectrum measurement: inject the above-mentioned calibration solution into the sample cell with an optical path of 0.1-0.5mm, and record the infrared spectrum with the air spectrum as the background. The spectral scanning range is 4000-400cm -1 , with a resolution of 4cm -1 , and the number of scans is 32. The sample cell can be a fixed-thickness sample cell made of potassium bromide or calcium fluoride, and if the sensitivity allows, a mirror total reflection (ATR) accessory can also be selected.

[0036] (3) Calibration formula: use the calibration solution at 1620 ~ 1640cm -1 Or 1270~1285cm -1 The absorbance A at the place is the dependent variable, and the volume fraction q of alkyl nitrate is used as the ...

Embodiment 1

[0057] In this example, straight-run diesel oil (180° C. to 350° C. fraction) was used as the base to add isooctyl nitrate. The feasibility of the method was verified according to the precision and accuracy of the measurement results. The specific implementation steps are as follows.

[0058] (1) Preparation of calibration solution: Add 0 μL, 2 μL, 5 μL, 10 μL, 20 μL and 50 μL of isooctyl nitrate into six 10 mL volumetric flasks respectively. After constant volume with carbon disulfide, calibration solutions with volume fractions of isooctyl nitrate of 0%, 0.02%, 0.05%, 0.1%, 0.2% and 0.5% were obtained respectively.

[0059] (2) Spectrum measurement: inject the calibration solution into the sample cell with an optical path of 0.5mm, and record the infrared spectrum with the air spectrum as the background, and the spectral scanning range is 4000-400cm -1 , with a resolution of 4cm -1 , and the number of scans is 32. Scan results see figure 2 and image 3 .

[0060] (3) C...

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Abstract

The invention relates to the technical field of chemical analysis, and particularly relates to a detection method of alkyl nitrate. The detection method of alkyl nitrate comprises the steps of preparing a series of alkyl nitrate calibration solutions, and detecting the series of alkyl nitrate calibration solutions by using infrared rays to obtain a calibration formula; carrying out solid-phase extraction on vehicle diesel oil containing alkyl nitrate to form a to-be-detected test solution; and detecting the to-be-detected test solution by utilizing infrared rays, obtaining the volume fractionof alkyl nitrate according to thecalibration formula, and calculating the content of alkyl nitrate according to the formula. According to the detection method, alkyl nitrate does not need to react, and corrosive and toxic solvents are not adopted, so that the detection method is simpler, more convenient and safer. Meanwhile, the method has high selectivity, can eliminate the influence of saturatedhydrocarbon, aromatic hydrocarbon and other components in the diesel oil on detection, and ensures the accuracy and precision of the detection result.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a method for detecting alkyl nitrates. Background technique [0002] Alkyl nitrate has a good cetane number improving effect and dominates the market. However, alkyl nitrates may affect the color and stability of automotive diesel, and form associations with acid-type lubricity improvers in diesel to block engine filters, resulting in poor oil supply to the engine. In addition, the addition of alkyl nitrates to vehicle diesel will affect the determination of carbon residue in vehicle diesel, so it is necessary to control and measure the content of alkyl nitrates when conducting vehicle diesel blending and production research. [0003] At present, the determination of alkyl nitrate content in vehicle diesel mainly adopts ultraviolet spectrophotometry (SH / T 0559-1993, ASTM D4046-2014, ISO 13759-1996). Hydrolyze in sulfuric acid solution to generate nitric acid, add m-xy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/3577
CPCG01N21/3577
Inventor 李怿李翔蔡凌霄贾苒白正伟王乾李磊王飞龙金欣
Owner CHINA PETROLEUM & CHEM CORP