CN114152664B - Method for testing concentration of magnesium acetate aqueous solution - Google Patents
Method for testing concentration of magnesium acetate aqueous solution Download PDFInfo
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- CN114152664B CN114152664B CN202111570355.0A CN202111570355A CN114152664B CN 114152664 B CN114152664 B CN 114152664B CN 202111570355 A CN202111570355 A CN 202111570355A CN 114152664 B CN114152664 B CN 114152664B
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- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 title claims abstract description 55
- 235000011285 magnesium acetate Nutrition 0.000 title claims abstract description 55
- 229940069446 magnesium acetate Drugs 0.000 title claims abstract description 54
- 239000011654 magnesium acetate Substances 0.000 title claims abstract description 54
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 34
- 238000012360 testing method Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 11
- 238000012937 correction Methods 0.000 claims abstract description 25
- 238000013178 mathematical model Methods 0.000 claims abstract description 5
- 238000004448 titration Methods 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims 1
- 229910052749 magnesium Inorganic materials 0.000 claims 1
- 239000011777 magnesium Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 12
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 229910002056 binary alloy Inorganic materials 0.000 description 2
- 229920002301 cellulose acetate Polymers 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000002898 library design Methods 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N29/00—Investigating or analysing materials by the use of ultrasonic, sonic or infrasonic waves; Visualisation of the interior of objects by transmitting ultrasonic or sonic waves through the object
- G01N29/02—Analysing fluids
- G01N29/024—Analysing fluids by measuring propagation velocity or propagation time of acoustic waves
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/02—Indexing codes associated with the analysed material
- G01N2291/022—Liquids
- G01N2291/0228—Aqueous liquids
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2291/00—Indexing codes associated with group G01N29/00
- G01N2291/02—Indexing codes associated with the analysed material
- G01N2291/028—Material parameters
- G01N2291/02809—Concentration of a compound, e.g. measured by a surface mass change
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Acoustics & Sound (AREA)
- Molecular Biology (AREA)
- Investigating Or Analyzing Materials By The Use Of Ultrasonic Waves (AREA)
Abstract
The invention discloses a method for testing the concentration of a magnesium acetate aqueous solution, which comprises the following steps: preparing magnesium acetate aqueous solution samples with different concentrations and different acidity, testing the concentration and acidity of the samples, and testing the density value and sound speed value of the samples by adopting an instrument; the measured concentration, density value and sound velocity value are imported into data analysis software, a concentration-density-sound velocity curve mathematical model is established, and a preliminary binary polynomial equation is fitted; a plurality of groups of magnesium acetate samples with the same concentration and different acidity are configured as model correction groups, and the density value and the sound speed value of the model correction group samples are measured; substituting the concentration, density and sound velocity values of the model correction group into the preliminary binary polynomial equation for correction to obtain a final binary polynomial equation. The invention establishes a multi-element combination correction system, thereby accurately measuring the content of magnesium acetate in the solution and avoiding the interference of acidity on the test result.
Description
Technical Field
The invention relates to concentration test, in particular to a method for testing the concentration of a magnesium acetate aqueous solution.
Background
The magnesium acetate aqueous solution is an important raw material in the production process of cellulose acetate, and has the important functions of neutralizing sulfuric acid and regulating the degree of the acetic acid reaction, so that in the production process of cellulose acetate, the concentration of the magnesium acetate aqueous solution needs to be accurately measured so as to accurately regulate the degree of the reaction.
At present, a chemical titration method is generally adopted for testing the magnesium acetate aqueous solution, and is more complicated; or the concentration of the magnesium acetate is obtained by measuring the density of the aqueous solution, but the method is greatly influenced by the acidity of the solution, the concentration of the magnesium acetate solution is measured by the traditional oscillation density method, the stability of the acidity of the solution is ensured, and the magnesium acetate solution is similar to a binary system of magnesium acetate and water on the premise of relatively stable acidity. However, in the case of unstable acidity, the change in acidity may destroy the binary system, thereby causing test deviation.
Disclosure of Invention
The invention aims to: the invention aims to provide a method for testing the concentration of a magnesium acetate aqueous solution, which solves the problem of large deviation of test results under the condition of unstable acidity in the existing test.
The technical scheme is as follows: the invention relates to a method for testing the concentration of a magnesium acetate aqueous solution, which comprises the following steps:
(1) Preparing magnesium acetate aqueous solution samples with different concentrations and different acidity, testing the concentration of the samples by using a titration method, and collecting the density value and the sound speed value of the samples tested by an instrument;
(2) The measured concentration, density value and sound velocity value are imported into data analysis software, a concentration-density-sound velocity curve mathematical model is established, and a preliminary binary polynomial equation is fitted;
(3) A plurality of groups of magnesium acetate samples with the same concentration and different acidity are configured as model correction groups, and the density value and the sound speed value of the model correction group samples are measured;
(4) Substituting the concentration, density and sound velocity values of the model correction group into the preliminary binary polynomial equation of the step (2) for correction to obtain a final binary polynomial equation.
In order to ensure that the magnesium acetate concentration-density-sound velocity model can accurately reflect the actual situation, the number of samples in the step (1) is 50, wherein the number of samples in the magnesium acetate aqueous solution concentration ranges from 0.1300 to 0.1350 and 0.1350 to 0.1400 is 5, and the number of samples in the magnesium acetate aqueous solution concentration ranges from 0.1400 to 0.1420, from 0.1420 to 0.1475, from 0.1500 to 0.1550 and from 0.1550 to 0.1600 is 10.
The preliminary binary polynomial equation in the step (2) is as follows:
Conc.＝C00+C01*Y+C02*Y 2 +C03*Y 3 +C10*X+C11*X*Y+C12*X*Y 2 +C20*X 2 +C21*X 2 *Y+C30*X 3
wherein X is the density value of the magnesium acetate aqueous solution, Y is the sound velocity value of the magnesium acetate aqueous solution, C00, C01, C02, C03, C10, C11, C12, C20, C21 and C30 are fitting constants, and Conc is the concentration of the magnesium acetate aqueous solution.
In order to achieve the aim of measuring the concentration of magnesium acetate without being influenced by the acidity, the model correction group in the step (3) selects 16 groups of samples, wherein the 16 groups of samples are divided into four groups, and each group comprises four groups of sample data with the same concentration and different acidity.
The final binary polynomial equation in the step (4) is:
Conc.＝-33.296053+0.266958*Y-0.000266452*Y 2 +7.211361*10 -8 *Y 3 -319.009588*X+0.354980*X*Y-0.000101*X*Y 2 +0*X 2 +0.001862*X 2 *Y+0*X 3
wherein Conc is the concentration of magnesium acetate, X is the density value of the aqueous solution of magnesium acetate, and Y is the sound velocity value of the aqueous solution of magnesium acetate.
The beneficial effects are that: according to the invention, by adding sound velocity measurement and utilizing the characteristic that the change of acidity can greatly change the sound velocity, the density-concentration relation model of the solution is corrected and optimized by simultaneously measuring the ultrasonic echo velocity, and a multi-element combination correction system is established, so that the content of magnesium acetate in the solution is accurately measured, and the interference of acidity on a test result can be avoided.
Drawings
FIG. 1 is a schematic representation of a mathematical model of the concentration-density-sonic velocity curve of the present invention.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
The invention discloses a method for testing the concentration of a magnesium acetate aqueous solution, which comprises the following steps:
(1) Preparing magnesium acetate aqueous solution samples with different concentrations and different acidity, testing the concentration of the samples by a titration method, and testing the density value and sound speed value of the samples at 20 ℃ by an instrument, wherein the concentration measured by the titration method comprises the following steps: transferring a certain amount of sample into a beaker, weighing and recording the weight of the sample; 55mL of glacial acetic acid and 200mL of chemically pure acetone are added; correcting the pH meter; with stirring, 1.0mol/l sulfuric acid (in 1/2H 2 SO 4 Meter) titrating the sample, continuously measuring the pH of the solution by using a pH meter while titrating until the titration is finished when the pH value is 1.00, and recording the consumed sulfuric acid content
The result is calculated according to the following formula:wherein: n1-sulfuric acid equivalent; a- -corrected milliliter of sulfuric acid; the mass concentration of the N-sulfuric acid titration solution; e— millimole mass of sulfuric acid; w is the weight of the sample;
in order to ensure that the magnesium acetate concentration-density-sound velocity model can accurately reflect the actual situation, the standard sample library is selected to be provided with more standard samples at common concentrations. From the practical production of magnesium acetate solution, the main magnesium acetate concentration is concentrated between 0.1400 and 0.1475, and the concentration of particular practical interest in the measurement is 0.1400 to 0.1420. Therefore, more samples are arranged in the interval when the standard sample library is designed, and the design concentration of the standard sample library is shown in the following table;
TABLE 1 Standard sample library design concentration Table
| Concentration of magnesium acetate | Number of samples |
| 0.1300-0.1350 | 5 |
| 0.1350-0.1400 | 5 |
| 0.1400-0.1420 | 10 |
| 0.1420-0.1475 | 10 |
| 0.1500-0.1550 | 10 |
| 0.1550-0.1600 | 10 |
And (3) preparing a magnesium acetate sample according to the design value, and measuring by using a titration method to form a standard sample library for establishing a magnesium acetate concentration-density-sound velocity model.
The total content of 50 magnesium acetates in the actual standard sample library is as follows:
TABLE 2 Standard sample library concentration data
| Sequence number | Concentration of | Sequence number | Concentration of | Sequence number | Concentration of | Sequence number | Concentration of | Sequence number | Concentration of |
| 1 | 0.1313 | 11 | 0.1404 | 21 | 0.1419 | 31 | 0.1491 | 41 | 0.1550 |
| 2 | 0.1329 | 12 | 0.1405 | 22 | 0.1426 | 32 | 0.1499 | 42 | 0.1555 |
| 3 | 0.1339 | 13 | 0.1406 | 23 | 0.1439 | 33 | 0.1501 | 43 | 0.1560 |
| 4 | 0.1353 | 14 | 0.1407 | 24 | 0.1449 | 34 | 0.1503 | 44 | 0.1569 |
| 5 | 0.1355 | 15 | 0.1409 | 25 | 0.1452 | 35 | 0.1504 | 45 | 0.1578 |
| 6 | 0.1358 | 16 | 0.1410 | 26 | 0.1453 | 36 | 0.1513 | 46 | 0.1584 |
| 7 | 0.1373 | 17 | 0.1412 | 27 | 0.1456 | 37 | 0.1517 | 47 | 0.1587 |
| 8 | 0.1389 | 18 | 0.1413 | 28 | 0.1474 | 38 | 0.1534 | 48 | 0.1593 |
| 9 | 0.1392 | 19 | 0.1414 | 29 | 0.1475 | 39 | 0.1540 | 49 | 0.1602 |
| 10 | 0.1401 | 20 | 0.1418 | 30 | 0.1477 | 40 | 0.1545 | 50 | 0.1612 |
(2) The measured concentration, density value and sound velocity value are imported into data analysis software, a concentration-density-sound velocity curve mathematical model is established, and a preliminary binary polynomial equation is fitted:
Conc.＝C00+C01*Y+C02*Y 2 +C03*Y 3 +C10*X+C11*X*Y+C12*X*Y 2 +C20*X 2 +C21*X 2 *Y+C30*X 3
wherein X is the density value of the magnesium acetate aqueous solution, Y is the sound velocity value of the magnesium acetate aqueous solution, C00, C01, C02, C03, C10, C11, C12, C20, C21 and C30 are fitting constants, and Conc is the concentration of the magnesium acetate aqueous solution.
(3) A plurality of groups of magnesium acetate samples with the same concentration and different acidity are configured as model correction groups, and the density value and the sound speed value of the model correction group samples are measured;
the method comprises the steps of using samples with the same concentration and different acidity as a correction sample library, correcting and optimizing fitting constants, setting up a correction group to optimize the fitting constants in order to achieve the aim of measuring the concentration of magnesium acetate without being influenced by the acidity because the acidity possibly influences a magnesium acetate concentration-density-sound velocity model, and mainly concentrating the acidity in a range of 1-2% in actual production, so that the samples are configured for correction, a reliable confirmation model is obtained, and the correction sample library data are shown in the following table:
table 3 correction of sample library data
(4) Substituting the concentration, density and sound velocity values of the model correction group into the preliminary binary polynomial equation of the step (2) for correction to obtain a final binary polynomial equation, wherein the final binary polynomial equation is as follows:
Conc.＝-33.296053+0.266958*Y-0.000266452*Y 2 +7.211361*10 -8 *Y 3 -319.009588*X+0.354980*X*Y-0.000101*X*Y 2 +0*X 2 +0.001862*X 2 *Y+0*X 3
wherein Conc is the concentration of magnesium acetate, X is the density value of the aqueous solution of magnesium acetate, and Y is the sound velocity value of the aqueous solution of magnesium acetate.
Claims (1)
1. The method for testing the concentration of the magnesium acetate aqueous solution is characterized by comprising the following steps of:
(1) Preparing magnesium acetate aqueous solution samples with different concentrations and different acidity, testing the concentration of the samples by using a titration method, and testing the density value and sound velocity value of the samples at 20 ℃ by using an instrument;
(2) The measured concentration, density value and sound velocity value are imported into data analysis software, a concentration-density-sound velocity curve mathematical model is established, and a preliminary binary polynomial equation is fitted;
(3) A plurality of groups of magnesium acetate samples with the same concentration and different acidity are configured as model correction groups, and the density value and the sound speed value of the model correction group samples are measured;
(4) Substituting the concentration, the density value and the sound velocity value of the model correction group into the preliminary binary polynomial equation of the step (2) for correction to obtain a final binary polynomial equation;
the number of the samples in the step (1) is 50;
the preliminary binary polynomial equation in the step (2) is as follows: conc=c00+c01+c02×y 2 +C03*Y 3
+C10*X+C11*X*Y+C12*X*Y 2 +C20*X 2 +C21*X 2 *Y+C30*X 3 Wherein X is the density of the aqueous solution of magnesium acetateThe degree value, Y is the sound velocity value of the magnesium acetate aqueous solution, C00, C01, C02, C03, C10,
c11, C12, C20, C21, C30 are fitting constants, conc. is magnesium acetate aqueous solution concentration;
the model correction group in the step (3) selects 32 samples, the 32 samples are divided into eight groups, and each group comprises four groups of sample data with the same concentration and different acidity;
the final binary polynomial equation in the step (4) is: conc=
-33.296053+0.266958*Y-0.000266452*Y 2 +7.211361*10 －8 *Y 3 -319.009588*X+0.354980*X*Y-0.000101*X*Y 2 +0*X 2 +0.001862*X 2 *Y+0*X 3
Wherein Conc is the concentration of the aqueous solution of magnesium acetate, X is the density value of the aqueous solution of magnesium acetate, and Y is the sound velocity value of the aqueous solution of magnesium acetate.
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