CN110873673A - Method for analyzing and testing ion content of corrosion product of petrochemical equipment - Google Patents

Method for analyzing and testing ion content of corrosion product of petrochemical equipment Download PDF

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Publication number
CN110873673A
CN110873673A CN201811020838.1A CN201811020838A CN110873673A CN 110873673 A CN110873673 A CN 110873673A CN 201811020838 A CN201811020838 A CN 201811020838A CN 110873673 A CN110873673 A CN 110873673A
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China
Prior art keywords
content
ion content
powder
corrosion
petrochemical equipment
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CN201811020838.1A
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Inventor
刘艳
黄贤滨
屈定荣
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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China Petroleum and Chemical Corp
Sinopec Qingdao Safety Engineering Institute
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Priority to CN201811020838.1A priority Critical patent/CN110873673A/en
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
    • G01N5/045—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder for determining moisture content
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
    • G01N2001/2866—Grinding or homogeneising

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Testing Resistance To Weather, Investigating Materials By Mechanical Methods (AREA)

Abstract

The invention relates to a method for analyzing and testing the content of ions in corrosion products of petrochemical equipment, which mainly solves the problem of poor accuracy of detection results in the prior art. The invention adopts a petrochemical equipment corrosion product ion content analysis and test method, the corrosion product is ground and sieved, the sieved powder is taken out, the water content is measured, and the weight is weighed; and then mixing the powder with water, stirring and filtering the mixture, taking clear filtrate, measuring the content of each ion in the filtrate, and finally converting the content of the ions in the solution into the content of the ions of corrosion products.

Description

Method for analyzing and testing ion content of corrosion product of petrochemical equipment
Technical Field
The invention relates to a method for analyzing and testing the content of ions in corrosion products of petrochemical equipment.
Background
Corrosion is ubiquitous, economic loss caused by corrosion is more than 3% in GDP every year in each country, China reaches about 5%, and corrosion loss in the petrochemical industry accounts for about 6% of the total yield and is one time higher than that in other industries. The analysis of the components of the corrosion products has important significance for researching corrosion rules and corrosion failure analysis, but due to the particularity of the petrochemical industry, most of the corrosion products contain oil, and the conventional detection methods such as energy spectrum analysis, X-ray fluorescence analysis, X-ray diffraction analysis, X-ray photoelectron spectrum analysis, spectrophotometry and the like cannot directly carry out quantitative analysis on the components of oil-containing substances.
The current common method for analyzing the components of oil-containing substances is as follows: (1) and (3) taking toluene as a solvent, extracting the sample, and detecting and analyzing the extracted sample. The toluene used in the method belongs to an easily toxic substance, and is greatly harmful to human bodies after long-term use. (2) Heating the oil-containing substance at high temperature to decompose the organic substances, and analyzing and detecting the residual substances. After the method is heated at high temperature, the self component structure of the corrosion product, such as ammonium salt, is easily damaged, and the deviation of the detection result is caused.
CN200810138772.6 proposes a method for analyzing the content of salt and scale formation components of a turbine blade, which burns a scale sample at a high temperature, and is not suitable for the method due to the characteristic that the component structure of a corrosion product of petrochemical equipment is easy to change after being heated, and in addition, the ion type measured in the method is not suitable for the corrosion product of the petrochemical equipment.
Disclosure of Invention
The invention aims to solve the technical problem of poor detection result accuracy in the prior art, provides a novel method for analyzing and testing the ion content of corrosion products of petrochemical equipment, and has the advantage of good detection result accuracy.
In order to solve the problems, the technical scheme adopted by the invention is as follows: a petrochemical equipment corrosion product ion content analysis and test method, sieve the corrosion product after grinding, take the undersize powder and measure its moisture content, weigh; and then mixing the powder with water, stirring and filtering, taking clear filtrate, measuring the content of each ion in the filtrate, and finally converting the ion content in the solution into the ion content of a corrosion product.
In the above technical solution, preferably, the corrosion product is ground and sieved, and the sieved powder is taken out through a 100-mesh screen.
In the above technical solution, preferably, the water is deionized water.
In the above technical solution, preferably, a magnetic stirrer is used for stirring.
In the above technical scheme, preferably, the powder is mixed with water, and the mass ratio of the powder to the water is 1: 10-1: 15. In the above technical solution, preferably, the moisture content of the powder is measured by a moisture analyzer.
In the above technical solution, preferably, the ion content in the solution is converted into the ion content of the corrosion product according to the mass conservation law.
In the above technical solution, preferably, the stirring rotation speed enables the solution to form a stable vortex.
According to the invention, the corrosion product is dissolved in the deionized water, and the quantitative analysis of the components of the corrosion product is indirectly realized by measuring the ion content in the water, namely, the component structure of the corrosion product is not changed, the measuring process is safe, environment-friendly and pollution-free, and a better technical effect is obtained.
Drawings
FIG. 1 is a schematic flow diagram of the process of the present invention.
The present invention will be further illustrated by the following examples, but is not limited to these examples.
Detailed Description
[ example 1 ]
A method for analyzing and testing the ion content of corrosion products of petrochemical equipment, as shown in figure 1, comprises the following steps:
(1) grinding the corrosion product in an agate mortar, screening through a 100-mesh screen, taking the sieved powder, and measuring the water content (Karl Fischer coulometry);
(2) weighing a proper amount of corrosion product powder, weighing a proper amount of deionized water, mixing the deionized water and the corrosion product powder, and fully stirring the mixture on a magnetic stirrer;
(3) filtering with filter paper, taking clear filtrate, and measuring the content of each ion in the filtrate;
(4) the ion content in the filtrate is converted to the ion content of the corrosion products according to the law of mass conservation.
[ example 2 ]
The process was used in analytical testing of the ion content of corrosion products of the recycle hydrogen high pressure heat exchanger equipment according to the conditions and procedures described in example 1.
(1) Taking a proper amount of corrosion products, putting the corrosion products into an agate mortar for grinding, screening by a 100-mesh screen, and taking the screened powder;
(2) putting a proper amount of the powder into a Karl Fischer moisture analyzer, and measuring the moisture content of the powder to be 7.28%;
(3) weighing 8.9910g of the powder under the sieve by using an electronic balance with the precision of 0.1mg, and pouring the powder into a conical flask;
(4) weighing 100g of deionized water, pouring into the conical flask, and slightly shaking to enable the powder to be uniformly suspended in the solution;
(5) adding a rotor, sealing the conical flask with a preservative film, and stirring for 12 hours on a magnetic stirrer;
(6) filtering the solution by using filter paper, taking clear filtrate, and measuring the content of each ion in the solution by using a spectrophotometry method as follows: s2-30 mu g/L; 1160mg/L of ammonia nitrogen; cl-；1200mg/L。
(7) Converting the ion content in the solution into the ion content in the corrosion product according to the mass conservation law: s2-0.3599 mu g/g; 13.9147mg/g of ammonia nitrogen; cl-；14.3945mg/g。
[ example 3 ]
The method was used in analytical testing of the ion content of corrosion products from crude oil storage tank wall equipment according to the conditions and procedures described in example 1.
(1) Taking a proper amount of corrosion products, putting the corrosion products into an agate mortar for grinding, screening by a 100-mesh screen, and taking the screened powder;
(2) putting a proper amount of the powder into a Karl Fischer moisture analyzer, and measuring the moisture content of the powder to be 5.06%;
(3) weighing 8.0964g of the powder under the sieve by using an electronic balance with the precision of 0.1mg, and pouring the powder into a conical flask;
(4) weighing 100g of deionized water, pouring into the conical flask, and slightly shaking to enable the powder to be uniformly suspended in the solution;
(5) adding a rotor, sealing the conical flask with a preservative film, and stirring for 12 hours on a magnetic stirrer;
(6) filtering the solution by using filter paper, taking clear filtrate, and measuring the content of each ion in the solution by using a spectrophotometry method as follows: 120mg/L of total iron; s2-:65μg/L；SO4 2-:250mg/L；Cl-；4mg/L。
(7) Converting the ion content in the solution into the ion content in the corrosion product according to the mass conservation law: 1.5611mg/g of total iron; s2-:0.8456μg/g；SO4 2-:3.2524mg/g；Cl-；0.0521mg/g。
[ COMPARATIVE EXAMPLE ]
XRF analysis is carried out on the corrosion product components of the tank wall of the crude oil storage tank, and in view of the fact that the corrosion product contains crude oil, the corrosion product is extracted by taking toluene as a solvent, and the specific experimental steps are as follows:
(1) the oil bath was set to 130 ℃ and 10.5987g of sample were accurately weighed on an analytical balance.
(2) Qualitative filter paper was dried and weighed on an analytical balance, 3.7635 g.
(3) The weighed sample was placed in a small beaker (after wetting with toluene), and 200ml of toluene solvent was poured in and stirred well with a glass rod. And (3) placing the filter paper with constant weight in a Soxhlet extractor, and slowly pouring the diluted oil sample by using a glass rod for drainage when the filter paper is completely attached to the extractor.
(4) The samples were extracted for 5 hours.
(5) The solid product remaining after extraction and filter paper were weighed 12.3532 g.
(6) The extracted corrosion products were analyzed by XRF, and the results were as follows: iron content 5395 μ g/g; the sulfur content is 16000 mu g/g; chlorine content <12 mug
Obviously, the measurement result of the invention is similar to the traditional XRF analysis result, and the operation is simple, safe and environment-friendly.

Claims (8)

1. A petrochemical equipment corrosion product ion content analysis and test method, sieve the corrosion product after grinding, take the undersize powder and measure its moisture content, weigh; and then mixing the powder with water, stirring and filtering, taking clear filtrate, measuring the content of each ion in the filtrate, and finally converting the ion content in the solution into the ion content of a corrosion product.
2. The method as claimed in claim 1, wherein the corrosion products are ground and sieved, and the sieved powder is sieved through a 100-mesh sieve.
3. The analytical test method for the ion content of corrosion products of petrochemical equipment as recited in claim 1, wherein the water is deionized water.
4. The analytical test method for ion content in corrosion products of petrochemical equipment according to claim 1, wherein the stirring operation is performed by a magnetic stirrer.
5. The analytical test method for the ion content of corrosion products of petrochemical equipment according to claim 1, wherein the powder is mixed with water, and the mass ratio of the powder to the water is 1: 10-1: 15.
6. The analytical test method for ion content of corrosion products of petrochemical equipment according to claim 1, wherein the moisture content of the powder is measured by a moisture analyzer.
7. The analytical test method for the ion content of corrosion products of petrochemical equipment according to claim 1, wherein the ion content of the solution is converted into the ion content of the corrosion products according to the mass conservation law.
8. The analytical test method for the ion content of corrosion products of petrochemical equipment according to claim 1, wherein the stirring speed is such that the solution forms a stable vortex.
CN201811020838.1A 2018-09-03 2018-09-03 Method for analyzing and testing ion content of corrosion product of petrochemical equipment Pending CN110873673A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112378936A (en) * 2020-10-28 2021-02-19 中国石油化工股份有限公司 Analysis method for corrosion unknown composition of oil refining device
CN116203187A (en) * 2023-01-17 2023-06-02 青岛双鲸药业股份有限公司 Method for measuring water content of soft capsule shell

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103884620A (en) * 2014-03-05 2014-06-25 中国石油天然气股份有限公司 Method for analyzing and detecting scale sample of scaled oil well

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103884620A (en) * 2014-03-05 2014-06-25 中国石油天然气股份有限公司 Method for analyzing and detecting scale sample of scaled oil well

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112378936A (en) * 2020-10-28 2021-02-19 中国石油化工股份有限公司 Analysis method for corrosion unknown composition of oil refining device
CN116203187A (en) * 2023-01-17 2023-06-02 青岛双鲸药业股份有限公司 Method for measuring water content of soft capsule shell
CN116203187B (en) * 2023-01-17 2023-09-19 青岛双鲸药业股份有限公司 Method for measuring water content of soft capsule shell

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Application publication date: 20200310