CN112881315A - Method for measuring concentration of octadecylamine in water and application - Google Patents
Method for measuring concentration of octadecylamine in water and application Download PDFInfo
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- CN112881315A CN112881315A CN202110095558.2A CN202110095558A CN112881315A CN 112881315 A CN112881315 A CN 112881315A CN 202110095558 A CN202110095558 A CN 202110095558A CN 112881315 A CN112881315 A CN 112881315A
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- octadecylamine
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- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 title claims abstract description 59
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 27
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229940090181 propyl acetate Drugs 0.000 claims abstract description 24
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000002835 absorbance Methods 0.000 claims abstract description 17
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 claims abstract description 11
- 229940012189 methyl orange Drugs 0.000 claims abstract description 11
- 239000007853 buffer solution Substances 0.000 claims abstract description 7
- 238000000605 extraction Methods 0.000 claims abstract description 7
- 238000012360 testing method Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims 1
- 239000001632 sodium acetate Substances 0.000 claims 1
- 235000017281 sodium acetate Nutrition 0.000 claims 1
- 231100000419 toxicity Toxicity 0.000 abstract description 6
- 230000001988 toxicity Effects 0.000 abstract description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 24
- 238000005259 measurement Methods 0.000 description 19
- 239000000523 sample Substances 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000012224 working solution Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003223 protective agent Substances 0.000 description 2
- 239000012088 reference solution Substances 0.000 description 2
- 239000012488 sample solution Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical class OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- 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
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- Spectroscopy & Molecular Physics (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)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention relates to a method for measuring the concentration of octadecylamine in water and application thereof, comprising the following steps: taking a water sample, adding a buffer solution into the water sample, and adding a methyl orange indicator to obtain a yellow mixed liquid; adding propyl acetate into the obtained yellow mixed liquid as an extracting agent to obtain an extract liquid; and testing the absorbance of the extraction liquid, and linearly corresponding the absorbance to obtain the concentration of the octadecylamine in the water sample. Compared with the prior art, the invention provides the novel extracting agent, namely propyl acetate, for measuring the concentration of the octadecylamine in the water. Meanwhile, the propyl acetate extractant has lower toxicity and better determination safety.
Description
Technical Field
The invention relates to a method for measuring the concentration of a protective agent, in particular to a method for measuring the concentration of octadecylamine in water and application thereof.
Background
With the development of the power industry, the start and stop of the unit become more and more frequent due to the requirements of power generation load and the change of the running state of the thermal equipment. During the period of unit shutdown, in order to prevent the corrosion problem of the unit, the shutdown protection of the unit is needed.
Octadecylamine, abbreviated as octadecylamine, belongs to aliphatic amine compounds, and has a molecular formula of CH3(CH2)16CH2NH2White crystal at normal temperature, easy to dissolve in chloroform, soluble in ethanol, ether and benzene, and slightly soluble in acetone. The octadecyl amine blowing-out protection method is characterized in that octadecyl amine is added into a thermodynamic system when the pressure and the temperature of a boiler are reduced to proper conditions in the unit sliding parameter blowing-out process, and a monomolecular or multi-molecular hydrophobic protective film can be formed on the inner surface of thermodynamic equipment, so that the aim of preventing an external medium from corroding metal is fulfilled. The method has the advantages of long protection time, wide protection range, simple application and the like, but has some problems in use, mainly the protection effect has a great relation with the concentration of the octadecylamine, so the concentration of the octadecylamine in furnace water is measured in the process of blowing out and adding chemicals so as to adjust the concentration of a blowing-out protective agent at any time; in addition, after the furnace is shut down for protection or before the unit is restarted, the concentration of octadecylamine in the discharged water needs to be measured so as to determine the waste liquid treatment mode and the unit grid connection time. Therefore, it is necessary to develop a method for rapidly and accurately measuring the concentration of octadecylamine in water.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for measuring the concentration of octadecylamine in water and application thereof. Meanwhile, the propyl acetate extractant has lower toxicity and better determination safety.
The purpose of the invention can be realized by the following technical scheme:
the first purpose of the invention is to protect a method for measuring the concentration of octadecylamine in water, which comprises the following steps:
s1: taking a water sample, adding a buffer solution into the water sample, and adding a methyl orange indicator to obtain a yellow mixed liquid;
s2: adding propyl acetate serving as an extracting agent into the yellow mixed liquid obtained in the step S1 to obtain an extraction liquid;
s3: and testing the absorbance of the extraction liquid in the S2, and performing linear correspondence according to the absorbance to obtain the concentration of the octadecylamine in the water sample.
Further, the concentration of octadecylamine in water was effectively measured in the range of 0-6 mg/L.
Further, the measurement wavelength of the absorbance in S3 was 420 nm.
Further, the buffer solution in S1 is an acetic acid-sodium acetate aqueous solution.
Further, the volume ratio of the buffer solution to the water sample in S1 was 1: 6.
Further, the volume ratio of the methyl orange indicator to the water sample in the S1 is 1:15, and the mass fraction of the methyl orange indicator is 0.05%.
Further, the volume ratio of propyl acetate to the water sample in S2 was 1: 15.
Further, after propyl acetate was added to S2, the liquid was shaken and left to stand to perform the extraction process, and the obtained extract was floated on the upper layer of the solution.
Further, in S3, the concentration of octadecylamine in the water sample is calculated according to a previously obtained standard curve.
The second purpose of the invention is to protect the application of the method for measuring the concentration of the octadecyl amine, in the process of unit slip parameter shutdown, when the pressure and the temperature of a boiler are reduced to proper conditions, the octadecyl amine is added into a thermodynamic system, then water is taken out from the thermodynamic system, and then the measurement of the concentration of the octadecyl amine in water is realized by the measuring method.
Compared with the prior art, the invention has the following technical advantages:
1) linear correlation coefficient R of standard curve2Can reach 0.9999, the measurement error can be controlled within 5 percent, and the accuracy of the octadecyl amine measurement is obviously improved.
2) The extractant propyl acetate has low toxicity, high boiling point, high safety and good application prospect.
3) When the power plant carries out furnace shutdown protection on the octadecylamine, the technical scheme can realize accurate octadecylamine measurement in a thermal power plant thermodynamic equipment system during the shutdown period.
Drawings
FIG. 1 is a standard curve for the determination of octadecyl amine concentration using chloroform as the extractant;
FIG. 2 is a standard curve for octadecyl amine concentration determination using propyl acetate as the extractant.
Detailed Description
The present invention is further described below with reference to examples, but the embodiments of the present invention are not limited thereto.
(1) Drawing of standard curve
Prepare 0.01mg/mL octadecyl amine working solution, and prepare a series of standard solutions by taking different working solution volumes, as shown in Table 3.
TABLE 3 Standard solutions
Adding 5mL of acetic acid-sodium acetate into the octadecyl amine working solution, and shaking up;
adding 2mL of 0.05% methyl orange indicator, shaking up, and standing for 5 min;
adding 25mL of propyl acetate as an extractant, shaking vigorously for at least 50 times, and standing for 5 min;
the upper layer of extract was poured out and absorbance was measured at a wavelength of 420nm in a 10mm cuvette, and a standard curve was drawn with deionized water as a reference solution.
(2) Determination of water samples
Taking a water sample with a certain volume, adding deionized water to the total volume of 30mL, determining according to the steps of the invention to obtain an absorbance value, and checking the concentration of octadecylamine through a standard curve.
Example 1
Preparing a 1mg/L octadecyl amine solution, taking 30mL, adding 5mL of acetic acid-sodium acetate, shaking uniformly, adding 2mL of 0.05% methyl orange indicator, shaking uniformly and standing for 5min, adding 2mL of propyl acetate, shaking vigorously for at least 50 times, standing for 5min, pouring an upper layer extract liquid in a 10mm cuvette, taking deionized water as a reference liquid, measuring absorbance at a wavelength of 420nm, and checking the octadecyl amine concentration in a standard curve. By error analysis, the relative standard deviation was 1.055%, i.e., precision was 1.055%. The measurement results and the analysis of measurement errors are shown in tables 4 and 5.
TABLE 4 measurement results of 1mg/L octadecylamine-like liquid at concentration
TABLE 5 analysis of measurement errors of 1mg/L octadecylamine-like liquid
Example 2
Preparing 2mg/L octadecyl amine solution, taking 30mL, adding 5mL of acetic acid-sodium acetate, shaking uniformly, adding 2mL of 0.05% methyl orange indicator, shaking uniformly and standing for 5min, adding 2mL of propyl acetate, shaking vigorously for at least 50 times, standing for 5min, pouring the upper layer extract in a 10mm cuvette, taking deionized water as reference solution, measuring absorbance at 420nm wavelength, and checking the octadecyl amine concentration on a standard curve. By error analysis, the relative standard deviation was found to be 0.711%, i.e. precision was 0.711%. The measurement results and the analysis of measurement errors are shown in tables 6 and 7.
TABLE 6 measurement results of octadecyl amine sample solution with concentration of 2mg/L
TABLE 7 analysis of measurement errors of octadecyl amine sample solution of concentration 2mg/L
Example 3
Preparing an octadecyl amine solution of 4mg/L, taking 30mL, adding 5mL of acetic acid-sodium acetate, shaking uniformly, adding 2mL of 0.05% methyl orange indicator, shaking uniformly and standing for 5min, adding 2mL of propyl acetate, shaking vigorously for at least 50 times, standing for 5min, pouring an upper layer of extract liquid in a 10mm cuvette, taking deionized water as a reference liquid, measuring absorbance at a wavelength of 420nm, and checking the octadecyl amine concentration in a standard curve. By error analysis, the relative standard deviation was found to be 0.366%, i.e. precision was 0.366%. The measurement results and the analysis of measurement errors are shown in tables 8 and 9.
TABLE 8 measurement results of 4mg/L octadecylamine-like liquid at concentration
TABLE 9 analysis of measurement errors of 4mg/L octadecylamine-like liquid at concentration
Comparative example 1
The method for measuring the octadecylamine in the water in the comparative example also adopts a spectrophotometric method, firstly uses chloroform as an extracting agent to extract the octadecylamine in the water, the octadecylamine in the extracting agent reacts with a color developing agent under an acidic condition to generate a water-insoluble colored complex, measures the absorbance value of the complex under a certain wavelength, and compares the absorbance value with the content of the octadecylamine in the extracting agent to obtain the concentration of the octadecylamine in the water by a reference to a pre-made standard curve.
When the concentration of the octadecylamine is measured, a standard curve equation drawn by using chloroform as an extracting agent is as follows: a is 0.45775c-0.02168, and the linear correlation coefficient is: r2The concentration has a good linear relationship with the absorbance, and the concentration range of the octadecyl amine is 0.9997.
In the embodiment of the technical scheme, when propyl acetate is used as the extracting agent, the standard curve equation is drawn as follows: a is 0.08368c +0.09911, and the linear correlation coefficient is: r2The concentration is 0.9999, the concentration has a good linear relation with the absorbance, and the measuring concentration of the octadecylamine is 0-6 mg/L. Compared with chloroform as an extracting agent, the linear relation of the standard curve with propyl acetate as the extracting agent is better, and the tested concentration range is wider.
Table 1 shows the comparison of physical and chemical properties and toxicity of two kinds of extractant, propyl acetate has boiling point 40 deg.c higher than that of chloroform and toxicity far lower than that of chloroform. Table 2 shows the relative standard deviation of octadecyl amine concentration measurements using these two extractants, and it can be seen that the relative standard deviation for propyl acetate is much smaller.
Table 1 comparison between extractants
TABLE 2 results of the precision test
On the other hand, compared with visible chloroform, the chloroform has high toxicity, and can react with oxygen in the air to generate HCl and virulent phosgene under the action of light, so that the measurement result is interfered; the boiling point of the propyl acetate is higher than that of the chloroform, namely the propyl acetate is relatively difficult to volatilize, and the toxicity of the propyl acetate is lower than that of the chloroform; the propyl acetate has high precision as an extracting agent.
Chloroform is used as an extracting agent in the prior determination of the concentration of octadecylamine, has the advantage of low solubility, but has strong toxicity, certain harm is caused to the health of operators, in addition, the boiling point is low, and when the room temperature is high, test errors are easily caused by the volatilization of the extracting agent.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (10)
1. A method for measuring the concentration of octadecylamine in water is characterized by comprising the following steps:
s1: taking a water sample, adding a buffer solution into the water sample, and adding a methyl orange indicator to obtain a yellow mixed liquid;
s2: adding propyl acetate serving as an extracting agent into the yellow mixed liquid obtained in the step S1 to obtain an extraction liquid;
s3: and testing the absorbance of the extraction liquid in the S2, and performing linear correspondence according to the absorbance to obtain the concentration of the octadecylamine in the water sample.
2. The method as claimed in claim 1, wherein the concentration of octadecyl amine in water is effectively measured in the range of 0-6 mg/L.
3. The method according to claim 1, wherein the absorbance at S3 is measured at 420 nm.
4. The method of claim 1, wherein the buffer solution in S1 is an aqueous solution of acetic acid and sodium acetate.
5. The method for determining the concentration of octadecylamine in water according to claim 4, wherein the volume ratio of the buffer solution to the water sample in S1 is 1: 6.
6. The method for determining the concentration of octadecylamine in water according to claim 1, wherein the volume ratio of the methyl orange indicator to the water sample in S1 is 1:15, and the mass fraction of the methyl orange indicator is 0.05%.
7. The method for determining the concentration of octadecylamine in water according to claim 1, wherein the volume ratio of propyl acetate to water sample in S2 is 1: 15.
8. The method for determining the concentration of octadecylamine in water as claimed in claim 1, wherein the extraction process is carried out by shaking the liquid and standing after adding propyl acetate to S2, and the obtained extract floats on the upper layer of the solution.
9. The method as claimed in claim 1, wherein the concentration of octadecylamine in the water sample is calculated according to a pre-obtained standard curve in S3.
10. Use of a method for determining the concentration of octadecylamine, characterized in that during a unit slip parameter shutdown, when the boiler pressure and temperature are reduced to suitable conditions, octadecylamine is added to a thermodynamic system, then water is taken out of the thermodynamic system, and then the determination of the concentration of octadecylamine in water is achieved by the determination method as claimed in any one of claims 1 to 9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114184607A (en) * | 2021-12-09 | 2022-03-15 | 中国科学院青海盐湖研究所 | System, method and application for determining content of octadecylamine based on ninhydrin |
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| CN114184607A (en) * | 2021-12-09 | 2022-03-15 | 中国科学院青海盐湖研究所 | System, method and application for determining content of octadecylamine based on ninhydrin |
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