CN116642998A - Measurement alkaline desulfurization waste water absorption CO 2 Quantitative method of content - Google Patents
Measurement alkaline desulfurization waste water absorption CO 2 Quantitative method of content Download PDFInfo
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- 239000002351 wastewater Substances 0.000 title claims abstract description 60
- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 56
- 230000023556 desulfurization Effects 0.000 title claims abstract description 56
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 34
- 238000004445 quantitative analysis Methods 0.000 title claims abstract description 14
- 238000005259 measurement Methods 0.000 title claims description 11
- 239000000243 solution Substances 0.000 claims abstract description 73
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 229910001424 calcium ion Inorganic materials 0.000 claims abstract description 52
- 238000000034 method Methods 0.000 claims abstract description 35
- 239000012670 alkaline solution Substances 0.000 claims abstract description 13
- 239000002244 precipitate Substances 0.000 claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000012086 standard solution Substances 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000011575 calcium Substances 0.000 claims description 22
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 21
- 238000004448 titration Methods 0.000 claims description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 11
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 10
- 229910052791 calcium Inorganic materials 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 8
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 6
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000001110 calcium chloride Substances 0.000 claims description 6
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 230000035772 mutation Effects 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 3
- SGHZXLIDFTYFHQ-UHFFFAOYSA-L Brilliant Blue Chemical compound [Na+].[Na+].C=1C=C(C(=C2C=CC(C=C2)=[N+](CC)CC=2C=C(C=CC=2)S([O-])(=O)=O)C=2C(=CC=CC=2)S([O-])(=O)=O)C=CC=1N(CC)CC1=CC=CC(S([O-])(=O)=O)=C1 SGHZXLIDFTYFHQ-UHFFFAOYSA-L 0.000 claims 1
- 101001018064 Homo sapiens Lysosomal-trafficking regulator Proteins 0.000 claims 1
- 102100033472 Lysosomal-trafficking regulator Human genes 0.000 claims 1
- 235000010703 Modiola caroliniana Nutrition 0.000 claims 1
- 244000038561 Modiola caroliniana Species 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 8
- 238000005070 sampling Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 12
- 239000011777 magnesium Substances 0.000 description 9
- 238000001556 precipitation Methods 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 7
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000012528 membrane Substances 0.000 description 4
- 229910021532 Calcite Inorganic materials 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000010842 industrial wastewater Substances 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000002696 acid base indicator Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000000559 atomic spectroscopy Methods 0.000 description 2
- 229910000019 calcium carbonate Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- 238000004255 ion exchange chromatography Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- -1 iron ions Chemical class 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 238000003918 potentiometric titration Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000001568 sexual effect Effects 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 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
- 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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Abstract
The invention relates to a method for measuring CO absorption of alkaline desulfurization wastewater 2 The quantitative method of the content comprises the following specific steps: s1, measuring concentration epsilon of calcium ions in alkaline desulfurization wastewater 0 The method comprises the steps of carrying out a first treatment on the surface of the S2, CO 2 Introducing alkaline desulfurization wastewater to generate alkaline solution; s3, adding excessive calcium ions into the alkaline solution obtained in the step S2 to generate precipitate and solution A; s4, measuring the concentration epsilon of calcium ions in the solution A obtained in the step 1 Thereby calculating the absorption of CO by the alkaline desulfurization wastewater 2 Is contained in the composition. Compared with the prior art, the method for measuring CO absorption of desulfurization wastewater 2 The quantitative method of the content can be used for on-site sampling detection, and is independent of precise instruments and equipment with high requirements on environmental vibration, temperature and the like for quantitative detection.
Description
Technical Field
The invention relates to the technical field of analysis, in particular to a method for measuring CO absorption of alkaline desulfurization wastewater 2 Quantitative method of content.
Background
The desulfurization wastewater treated by the triple tank process is usually alkaline and can be used for absorbing CO 2 Form a mixture containing CO 3 2- Or HCO 3 - And CO 3 2- Is a basic solution of (a) and (b). When the pH value of the solution is more than 11.50, the absorbed CO is absorbed 2 Completely with CO 3 2- In the form of (C), thus CO 2 Can be obtained by measuring the CO content in the desulfurization waste water after the reaction 3 2- To determine.
HCO 3 - And CO 3 2- The determination method mainly comprises an acid-base indicator titration method, a potentiometric titration method, an ultraviolet spectrophotometry method, an ion chromatography method, an electrode method, an inductively coupled plasma atomic spectrometry method and the like. The first mutation point of the acid-base indicator titration method has long phenolphthalein fading time, and the change limit from red to colorless is not easy to judge, so that the titration endpoint can not be accurately grasped. Potentiometric titration, ultraviolet spectrophotometry, ion chromatography, inductively coupled plasma atomic spectrometry, etc. can also be used for accurately measuring HCO 3 - And CO 3 2- However, these detection devices are not suitable for use in field conditions where movement is frequent and the environment is harsh. The double-electrode method can be used for rapidly measuring HCO in water on site 3 - And CO 3 2- But CO 3 2- The detection limit of (2) is lower than that of%<40 mg/L) of a metal ion (K + 、Mg 2+ ) And anions (Cl) - 、SO 4 2- ) The high concentration has influence on the measurement result, and the method is applicable to HCO 3 - And CO 3 2- Low concentration water bodies (such as groundwater and Hu Boshui), which are not suitable for high concentration HCO in wastewater 3 - And CO 3 2- And (5) measuring. Development of new methods for on-site rapid determination of CO is urgently needed 2 Absorption amount.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for measuring the CO absorption of alkaline desulfurization wastewater 2 Quantitative method for content, and determination of CO by quantitative determination of the amount of calcium ions 2 Is not limited, and the absorption amount of (a) is not limited.
The aim of the invention can be achieved by the following technical scheme:
measurement alkaline desulfurization waste water absorption CO 2 The quantitative method of the content comprises the following specific steps:
s1, measuring concentration epsilon of calcium ions in alkaline desulfurization wastewater 0 ；
S2, CO 2 Introducing alkaline desulfurization wastewater to generate alkaline solution;
s3, adding excessive calcium ion-containing solution into the alkaline solution obtained in the step S2 to generate precipitate and solution A;
s4, measuring the concentration epsilon of calcium ions in the solution A obtained in the step S3 1 Thereby calculating the absorption of CO by the alkaline desulfurization wastewater 2 Is used for absorbing CO 2 The calculation formula of the content of (2) is shown as formula (5):
wherein, theta is the concentration of calcium ions in the solution containing calcium ions, mg/L;
ε 0 -concentration of calcium ions in alkaline desulfurization wastewater, mol/L;
ε 1 -concentration of calcium ions in solution a, mol/L;
V 5 -volume of solution containing calcium ions, mL;
M 1 molar mass of calcium, M 1 ＝40.08g/mol；
M 2 —CO 2 44g/mol.
Further, in step S1, the concentration ε of calcium ions in alkaline desulfurization wastewater is measured 0 The specific steps of (a) are as follows: adding deionized water, triethanolamine solution, potassium hydroxide solution and calcium-carboxylic acid indicator into alkaline desulfurization wastewater, titrating with EDTA standard solution, and recording the consumption EDTA volume V when the reddish purple mutation of the solution color is changed into bright blue 1 。
The above further, ε 0 The calculation formula is formula (3):
wherein, the concentration of the C-EDTA standard solution and the mol/L are the same;
V 1 -titration of EDTA standard solution volume, L, consumed by calcium ions;
V 2 -the volume of alkaline desulphurized waste water sample taken at the time of dripping, mL;
M 1 molar mass of calcium, M 1 ＝40.08g/mol。
Further, in step S2, the alkaline solution contains HCO 3 - 、CO 3 2- Or HCO 3 - And CO 3 2- 。
In step S3, the pH value of the alkaline solution obtained in step S2 is adjusted to be more than 10.0, and then the solution containing calcium ions is added until no new precipitate is generated, and the precipitate and the solution A are obtained after heating, stirring and filtering.
Further, the pH of the alkaline solution obtained in step S2 is adjusted to 10.0 or more by adding sodium hydroxide or potassium hydroxide solution, and the pH is preferably more than 11.57.
Mg 2+ Will replace Ca 2+ Insertion of CaCO 3 The calcite crystals of (2) increase calcite solubility, thereby inhibiting CaCO 3 And (3) generating a precipitate. Therefore, the solution to be measured is added with Ca 2+ Before, naOH solution is used for regulating the pH value of the solution to ensure that Mg 2+ By Mg (OH) 2 Form of (C) precipitates out, eliminating Mg 2+ For CaCO 3 Influence of precipitate formation. According to Mg (OH) 2 Solubility constant, when the pH value of the solution is 11.04 at normal temperature, mg in the solution 2+ The concentration is 1.0X10 -5 mol/L, the present study set the pH of the solution at 11.60, the reaction temperature at 60℃to ensure Mg 2+ By Mg (OH) 2 Complete precipitation, avoid Mg 2+ For CaCO 3 Influence of precipitation. Research shows that under the condition of low solution saturation, fe 2+ Will partially replace Ca 2+ Inhibiting CaCO 3 Conversion of vanadium stone to aragonite results in a decrease in aragonite number with increasing iron ions, thereby inhibiting CaCO 3 And (3) separating out a precipitate. But in an excessively high saturation state, fe 2+ For CaCO 3 The inhibition of crystallization was small and therefore its effect was negligible at higher supersaturation conditions in this study.
The above further, the calcium ion-containing solution is CaCl 2 Solution, so that the alkaline desulfurization wastewater absorbs CO 2 The calculation formula of the content of (2) is as follows:
wherein, the concentration of calcium ions in the theta-externally added calcium chloride standard solution is mg/L;
ε 0 -concentration of calcium ions in alkaline desulfurization wastewater, mol/L;
ε 1 -concentration of calcium ions in solution a, mol/L;
V 5 -adding the volume of the standard solution of calcium chloride, mL;
M 1 molar mass of calcium, M 1 ＝40.08g/mol；
M 2 —CO 2 44g/mol.
The stirring temperature is 50-100 ℃ and the stirring time is 3-10 min.
CaCO in general 3 The solubility of CaCO decreases with increasing temperature 3 The growth rate of the crystal increases with the increase of the reaction temperature, and the carbonate and Ca in the solution are in the higher reaction temperature 2+ The precipitation is more complete. Studies have shown CaCO when the temperature is above 50 DEG C 3 Most of the precipitation structures are calcite and acicular aragonite crystals, and the formed precipitation particles are large and easy to precipitate. CaCO at 50℃and pH 9.0 3 Complete precipitation was achieved within 5 minutes.
Further, in step S4, the concentration ε of calcium ions in the solution A obtained in the step is measured 1 The specific steps of (a) are as follows: adding deionized water, triethanolamine solution, potassium hydroxide solution and calcium-carboxylic acid indicator into the solution A obtained in the step S3, titrating with EDTA standard solution, and recording the consumption EDTA volume V when the reddish purple mutation of the solution color is bright blue 3 。
The above further, ε 1 The calculation formula is formula (4):
wherein, the concentration of the C-EDTA standard solution and the mol/L are the same;
V 3 -titration of EDTA standard solution volume, L, consumed by calcium ions;
V 4 -the volume of solution a taken when titrating the calcium ions, mL;
M 1 molar mass of calcium, M 1 ＝40.08g/mol。
Further, step S5 is provided after step S4: drawing of CO by indirect titration 2 The alkaline desulfurization wastewater obtained in the step S4 is absorbed with CO according to the standard curve of the content 2 The content rho of the desulfurization waste water is brought into a standard curve equation to finally obtain the CO absorption of the desulfurization waste water 2 Is contained in the composition.
The method for drawing the standard curve equation further comprises the following steps: quantitative Na was weighed with analytical balance 2 CO 3 Preparation of CO 2 CO at a concentration of 500mg/L to 2500mg/L 3 2- Standard solution, measuring CO according to steps S1-S4 3 2- CO in standard solution 2 Is used to obtain CO 2 Content measurement value x, CO 3 2- The standard solution is prepared to have a true value y by knowing the CO 2 CO at a concentration of 3 2- The measured value x and the true value y of the standard solution draw a standard curve, and the standard curve equation is expressed as follows: y=1.043 x, variance= 0.9996.
The principle of the invention is as follows:
the invention absorbs CO in the desulfurization wastewater 2 Produced HCO 3 - With OH - The reaction is completely converted into CO 3 2- Adding quantitative and excessive Ca 2+ And heating to make CO 3 2- Complete precipitation, determination of residual Ca in solution by EDTA titration 2+ Indirectly determining the concentration of HCO in solution 3 - And CO 3 2- I.e., EDTA indirect titration (hereinafter referred to as "indirect titration"). Provides a new alkali liquor for absorbing CO 2 Is a quantitative method of (a). By CO in solution 3 2- With Ca 2+ Combining to generate CaCO 3 Precipitation, EDTA titration method for measuring Ca 2+ The method is mature, the titration end point is changed from red to blue, and the end point change is obvious. The method can accurately obtain HCO with higher concentration in solution under certain conditions 3 - And CO 3 2- Is not shown in the drawing).
Principle of: the chemical equation for the reaction of carbonate with calcium ions is:
HCO 3 － +OH - → CO 3 2- +H 2 o type (1)
Ca 2+ + CO 3 2- → CaCO 3 ∈ (2)
Formula (2) shows that bicarbonate can be completely converted into carbonate under the condition that OH reaches a certain concentration (the pH value reaches a certain value); formula (2) shows that when calcium carbonate is completely precipitated, the consumption amount of calcium ions is equal to the amount of carbonate in the solution to be measured. The amount of calcium ions consumed can therefore be used to represent the original bicarbonate and total carbonate in the aqueous solution.
When the carbonate concentration reached 2500mg/L at room temperature, the pH of the sodium carbonate solution was measured to be 11.57. Therefore, in order to ensure complete precipitation of calcium carbonate at room temperature, the pH of the solution should be adjusted to above 11.57 before adding excess calcium ions.
Compared with the prior art, the invention has the following beneficial effects:
(1) According to the invention, the pH value of the solution to be detected is increased to convert bicarbonate into carbonate, and the influences of magnesium ions, iron ions and the like in the solution are removed, so that the problem of rapid quantitative detection of carbonate and bicarbonate in industrial wastewater with complex water quality is solved. The existing detection standard (DZ/T0064.49-93) is used for detecting carbonate and bicarbonate in underground water, the underground water is clear relative to the quality of industrial wastewater, the impurities are few, the content of carbonate and bicarbonate is low, and the method cannot be directly used for quantitatively detecting carbonate and bicarbonate in industrial wastewater with complex quality.
(2) The invention relates to a method for measuring CO absorption of desulfurization wastewater 2 The quantitative method of the content can be used for on-site sampling detection and is not dependent onThe quantitative detection is carried out on precise instruments and equipment with high requirements on vibration, temperature and the like.
Drawings
FIG. 1 is a schematic diagram of a carbonate indirect titration standard curve.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples.
Example 1
This example provides an alkaline measurement of CO absorption by desulfurization wastewater 2 The quantitative method of the content comprises the following specific steps:
s1, measuring concentration epsilon of calcium ions in alkaline desulfurization wastewater 0 : adding deionized water, triethanolamine solution, potassium hydroxide solution and calcium-carboxylic acid indicator into alkaline desulfurization wastewater, titrating with EDTA standard solution, and recording the consumption EDTA volume V when the reddish purple mutation of the solution color is changed into bright blue 1 ；
ε 0 The calculation formula is formula (3):
wherein, the concentration of the C-EDTA standard solution and the mol/L are the same;
V 1 -titration of EDTA standard solution volume, L, consumed by calcium ions;
V 2 -the volume of alkaline desulphurized waste water sample taken at the time of dripping, mL;
M 1 molar mass of calcium, M 1 ＝40.08g/mol。
S2, CO 2 Introducing the alkaline desulfurization wastewater to generate wastewater containing HCO 3 - 、CO 3 2- Or HCO 3 - And CO 3 2- Filtering the alkaline solution with a 0.45 mu m filter membrane to obtain a water sample to be detected.
S3, taking 100mL of the water sample to be detected obtained in the step S2, placing the water sample to be detected on a digital display temperature-control magnetic stirrer for stirring, slowly dripping NaOH solution to adjust the pH value of the water sample to be detected to 12.0, and adding quantitative and excessive CaCl 2 The solution was stirred and heated to 60℃for 5min until no new precipitate formed, cooled to room temperature and filtered through a 0.45 μm filter to give precipitate and solution A.
S4, transferring the solution A obtained in the step S3 into a 100mL volumetric flask for constant volume, taking 10mL of water sample with constant volume, putting the water sample into a 250mL conical flask, and measuring the concentration epsilon of calcium ions in the solution A obtained in the step 1 Thereby calculating the absorption of CO by the alkaline desulfurization wastewater 2 Is contained in the composition;
in step S4 of this example, the concentration ε of calcium ions in the solution A obtained in the step was measured 1 The specific steps of (a) are as follows: adding deionized water, triethanolamine solution, potassium hydroxide solution and calcium-carboxylic acid indicator into the solution A obtained in the step S3, titrating with EDTA standard solution, and recording the consumption EDTA volume V when the reddish purple mutation of the solution color is bright blue 3 。
In step S4, ε 1 The calculation formula is formula (4):
wherein, the concentration of the C-EDTA standard solution and the mol/L are the same;
V 3 -titration of EDTA standard solution volume, L, consumed by calcium ions;
V 4 -the volume of solution a taken when titrating the calcium ions, mL;
M 1 molar mass of calcium, M 1 ＝40.08g/mol。
In step S4 of this embodiment, in step S4, the alkaline desulfurization wastewater absorbs CO 2 The calculation formula of the content of (2) is as formula (5):
wherein, the concentration of calcium ions in the theta-externally added calcium chloride standard solution is mg/L;
ε 0 concentration of calcium ion in alkaline desulfurization wastewater (counterCa in water sample to be measured before application 2+ Concentration), mol/L;
ε 1 concentration of calcium ions in solution A (Ca in the sample to be tested after reaction) 2+ Concentration), mol/L;
V 5 -adding the volume of the standard solution of calcium chloride, mL;
M 1 molar mass of calcium, M 1 ＝40.08g/mol；
M 2 —CO 2 44g/mol.
S5, analysis of standard solution measurement results and drawing of standard curves
Standard solution preparation: quantitative Na was weighed with analytical balance 2 CO 3 Preparation of CO 2 CO at a concentration of 500mg/L to 2500mg/L 3 2- Standard solutions are shown in table 1.
TABLE 1CO 3 2- CO of standard solution 2 Concentration of preparation of content
Measurement of CO according to steps S1-S4 3 2- CO in standard solution 2 Is used to obtain CO 2 Content measurement value x, CO 3 2- The standard solution is prepared to have a true value y by knowing the CO 2 CO at a concentration of 3 2- The standard curve is drawn by the measured value x and the true value y of the standard solution, and the results are shown in table 2 and fig. 1. The curve equation for the true value (y) and the measured value (x) can be expressed as: y=1.043 x, variance (R 2 ) Reaching 0.9993, the method is higher in accuracy.
TABLE 2 CO in Standard solution 2 Comparison of the measured value of the content with the actual value
Example 2
Taking 100mL of absorbing CO 2 Post alkaliFiltering sexual desulfurization waste water 1 with 0.45 μm filter membrane, stirring with digital display temperature-controlled magnetic stirrer, slowly dripping NaOH solution to adjust pH value of water sample to be detected to 12.0, adding quantitative and excessive CaCl 2 The solution was heated to 60℃with stirring for 5min, cooled to room temperature, filtered through a 0.45 μm filter, and transferred to a 100mL volumetric flask for constant volume. Taking 10mL of water sample with constant volume, putting the water sample into a 250mL conical flask, and titrating Ca 2+ The concentration of CO is calculated according to formula (5) 2 Absorption of CO 2 The absorption ρ is carried into the standard curve equation y=1.043x to obtain CO 2 The absorption amount was 1347.37mg/L, and the Relative Standard Deviation (RSD) was 1.28 (as shown in Table 3).
Example 3
Taking 100mL of absorbing CO 2 Filtering the alkaline desulfurization wastewater 2 with a 0.45 mu m filter membrane, placing the filtered alkaline desulfurization wastewater on a digital display temperature-control magnetic stirrer for stirring, and adding quantitative and excessive CaCl 2 Slowly dripping NaOH solution into the solution to adjust the pH value of a water sample to be measured to 12.0, stirring and heating to 80 ℃ and keeping for 5min, cooling to room temperature, filtering with a 0.45 mu m filter membrane, and transferring the solution into a 100mL volumetric flask for constant volume. Taking 10mL of water sample with constant volume, putting the water sample into a 250mL conical flask, and titrating Ca 2+ The concentration of (3) is recorded and CO is calculated according to formula (5) 2 Absorption and averaging the CO 2 The absorption ρ is brought into the standard curve equation y=1.043x, and CO is measured 2 The absorption amount was 1457.04mg/L, and the Relative Standard Deviation (RSD) was 0.92 (as shown in Table 3).
TABLE 3 CO of alkaline desulfurization waste water 1 and alkaline desulfurization waste water 2 2 Absorption capacity
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments 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-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. Measurement alkaline desulfurization waste water absorption CO 2 The quantitative method of the content is characterized by comprising the following specific steps:
s1, measuring concentration epsilon of calcium ions in alkaline desulfurization wastewater 0 ；
S2, CO 2 Introducing alkaline desulfurization wastewater to generate alkaline solution;
s3, adding excessive calcium ion-containing solution into the alkaline solution obtained in the step S2 to generate precipitate and solution A;
s4, measuring the concentration epsilon of calcium ions in the solution A obtained in the step S3 1 Thereby calculating the absorption of CO by the alkaline desulfurization wastewater 2 Is used for absorbing CO 2 The calculation formula of the content of (2) is shown as formula (5):
wherein, theta is the concentration of calcium ions in the solution containing calcium ions, mg/L;
ε 0 -concentration of calcium ions in alkaline desulfurization wastewater, mol/L;
ε 1 -concentration of calcium ions in solution a, mol/L;
V 5 -volume of solution containing calcium ions, mL;
M 1 molar mass of calcium, M 1 ＝40.08g/mol；
M 2 —CO 2 44g/mol.
2. A method for measuring the absorption of CO by alkaline desulfurization waste water according to claim 1 2 A method for quantifying the content of calcium ions, characterized in that in step S1, the concentration epsilon of calcium ions in alkaline desulfurization wastewater is measured 0 The specific steps of (a) are as follows: adding deionized water and triethanolamine into alkaline desulfurization wastewaterAmine solution, potassium hydroxide solution and calcium-carboxylic acid indicator, titrate with EDTA standard solution, when the color of the solution changes from mauve to brilliant blue, the end point is reached, and the volume V of EDTA consumed is recorded 1 。
3. A method for measuring the absorption of CO by alkaline desulfurization waste water according to claim 2 2 A method for quantifying the content of epsilon 0 The calculation formula is formula (3):
wherein, the concentration of the C-EDTA standard solution and the mol/L are the same;
V 1 -titration of EDTA standard solution volume, L, consumed by calcium ions;
V 2 -the volume of alkaline desulphurized waste water sample taken at the time of dripping, mL;
M 1 molar mass of calcium, M 1 ＝40.08g/mol。
4. A method for measuring the absorption of CO by alkaline desulfurization waste water according to claim 1 2 A method for quantifying the content, characterized in that in step S2, the alkaline solution contains HCO 3 - 、CO 3 2- Or HCO 3 - And CO 3 2- 。
5. A method for measuring the absorption of CO by alkaline desulfurization waste water according to claim 1 2 The quantitative method of the content is characterized in that in the step S3, the pH value of the alkaline solution obtained in the step S2 is adjusted to be more than 10.0, and then the solution containing calcium ions is added until no new precipitate is generated, and the precipitate and the solution A are obtained after heating, stirring and filtering.
6. A method for measuring the absorption of CO in alkaline desulfurization waste water as claimed in claim 5 2 A method for quantifying the content, characterized in that in step S2, sodium hydroxide or potassium hydroxide solution is addedThe pH value of the obtained alkaline solution is adjusted to be more than 10.0;
the solution containing calcium ions is CaCl 2 Solution, formula (5): theta-is added with the concentration of calcium ions in the standard solution of calcium chloride, mg/L; v (V) 5 -adding the volume of the standard solution of calcium chloride, mL;
the stirring temperature is 50-100 ℃, and the stirring time is 3-10 min.
7. A method for measuring the absorption of CO by alkaline desulfurization waste water according to claim 1 2 A method for quantifying the content, characterized in that in step S4, the concentration epsilon of calcium ions in the solution A obtained in the step is measured 1 The specific steps of (a) are as follows: adding deionized water, triethanolamine solution, potassium hydroxide solution and calcium-carboxylic acid indicator into the solution A obtained in the step S3, titrating with EDTA standard solution, and recording the consumption EDTA volume V when the reddish purple mutation of the solution color is bright blue 3 。
8. A method for measuring the absorption of CO in alkaline desulfurization waste water as claimed in claim 7 2 A method for quantifying the content of epsilon 1 The calculation formula is formula (4):
wherein, the concentration of the C-EDTA standard solution and the mol/L are the same;
V 3 -titration of EDTA standard solution volume, L, consumed by calcium ions;
V 4 -the volume of solution a taken when titrating the calcium ions, mL;
M 1 molar mass of calcium, M 1 ＝40.08g/mol。
9. A method for measuring the absorption of CO by alkaline desulfurization waste water according to claim 1 2 The quantitative method of the content is characterized in that step S5 is arranged after step S4: drawing of CO by indirect titration 2 Content ofIs used for absorbing CO by the alkaline desulfurization wastewater obtained in the step S4 2 The content rho of the desulfurization waste water is brought into a standard curve equation to finally obtain the CO absorption of the desulfurization waste water 2 Is contained in the composition.
10. A method for measuring the absorption of CO by alkaline desulfurization waste water according to claim 9 2 The quantitative method of the content is characterized in that the drawing method of the standard curve equation is as follows: quantitative Na was weighed with analytical balance 2 CO 3 Preparation of CO 2 CO at a concentration of 500mg/L to 2500mg/L 3 2- Standard solution, measuring CO according to steps S1-S4 3 2- CO in standard solution 2 Is used to obtain CO 2 Content measurement value x, CO 3 2- The standard solution is prepared to have a true value y by knowing the CO 2 CO at a concentration of 3 2- The measured value x and the true value y of the standard solution draw a standard curve, and the standard curve equation is expressed as follows: y=1.043 x, variance= 0.9996.
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