CN112213279A - Method for measuring iron ions in denitration absorption liquid - Google Patents
Method for measuring iron ions in denitration absorption liquid Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 158
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 93
- 239000007788 liquid Substances 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 34
- -1 iron ions Chemical class 0.000 title claims abstract description 32
- 238000010521 absorption reaction Methods 0.000 title claims abstract description 20
- 239000000243 solution Substances 0.000 claims abstract description 125
- 238000002835 absorbance Methods 0.000 claims abstract description 66
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 239000012086 standard solution Substances 0.000 claims abstract description 25
- DGEZNRSVGBDHLK-UHFFFAOYSA-N [1,10]phenanthroline Chemical compound C1=CN=C2C3=NC=CC=C3C=CC2=C1 DGEZNRSVGBDHLK-UHFFFAOYSA-N 0.000 claims abstract description 24
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims abstract description 20
- 239000007974 sodium acetate buffer Substances 0.000 claims abstract description 16
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 16
- 238000007865 diluting Methods 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 12
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 10
- NDLPOXTZKUMGOV-UHFFFAOYSA-N oxo(oxoferriooxy)iron hydrate Chemical compound O.O=[Fe]O[Fe]=O NDLPOXTZKUMGOV-UHFFFAOYSA-N 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 229960005070 ascorbic acid Drugs 0.000 claims description 8
- 235000010323 ascorbic acid Nutrition 0.000 claims description 8
- 239000011668 ascorbic acid Substances 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000003085 diluting agent Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 abstract description 11
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 4
- 238000000691 measurement method Methods 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 229910001448 ferrous ion Inorganic materials 0.000 description 7
- 229910001447 ferric ion Inorganic materials 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 229940079593 drug Drugs 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000012847 fine chemical Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 125000005341 metaphosphate group Chemical group 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 150000002826 nitrites Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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- Spectroscopy & Molecular Physics (AREA)
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention discloses a method for determining iron ions in a denitration absorption liquid, which comprises the following steps: preparing an iron standard solution; establishing a standard curve by taking the absorbance of the solution as a vertical coordinate and the iron content in the reaction solution as a horizontal coordinate, and obtaining a standard curve equation; taking a preset amount of the denitration liquid, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the total iron concentration of the denitration liquid; sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline into the denitration liquid with the preset amount, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the ferrous concentration of the denitration liquid; and obtaining the concentration of the trivalent iron through the difference value of the total iron concentration and the ferrous iron concentration. The method solves the technical problems that the ferrous iron amount and the ferric iron amount can not be separately measured and the iron ion measurement efficiency is low in the existing iron ion measurement method.
Description
Technical Field
The invention relates to the technical field of iron ion detection, and particularly relates to a method for determining iron ions in a denitration absorption liquid.
Background
In the denitration absorption liquid, Fe (II) EDTA solution is easy to generate coordination reaction with NO and is directly absorbed and removed, and the method is an NO wet treatment technology with industrial development potential, but Fe (II) EDTA is easy to be oxidized into Fe (III) EDTA and loses the affinity of complexing NO. Therefore, a method for rapidly and accurately measuring the ferrous ions in the absorption liquid needs to be found to ensure that the concentration of the ferrous ions in the complex denitration liquid is higher, so that the absorption liquid has higher denitration efficiency.
At present, methods for detecting iron ions include high performance liquid chromatography, inductively coupled plasma emission spectrometry (ICP-AES), atomic absorption method and the like. The detection methods can only measure the total amount of the iron ions, the pretreatment of the sample is complicated, and the measurement efficiency of the iron ions is low.
Disclosure of Invention
Therefore, the embodiment of the invention provides a method for measuring iron ions in a denitration absorption liquid, which at least partially solves the technical problems that the ferrous iron amount and the ferric iron amount cannot be separately measured and the iron ion measurement efficiency is low in the conventional iron ion measurement method.
In order to achieve the above object, the embodiments of the present invention provide the following technical solutions:
a method for determining iron ions in a denitration absorption liquid, comprising the following steps:
preparing an iron standard solution;
diluting the iron standard solution by a preset multiple to obtain a diluted solution, adding reactants into the diluted solution with different milliliters respectively, shaking up, and obtaining reaction solutions respectively;
measuring the solution absorbance of each reaction solution at a preset ultraviolet wavelength, establishing a standard curve by taking the solution absorbance as a vertical coordinate and the iron content in the reaction solution as a horizontal coordinate, and obtaining a standard curve equation;
taking a preset amount of the denitration liquid, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the total iron concentration of the denitration liquid;
sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline into the denitration liquid with the preset amount, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the ferrous concentration of the denitration liquid;
and obtaining the concentration of the trivalent iron through the difference value of the total iron concentration and the ferrous iron concentration.
Further, the preparation of the iron standard solution specifically comprises the following steps:
weighing 0.0001 g-0.0002 g of ferric oxide, and drying the ferric oxide at the temperature of 105-110 ℃ for 1h to obtain the ferric oxide;
adding 50ml of hydrochloric acid into a 400ml beaker, covering a watch glass, heating to dissolve, cooling to room temperature, transferring into a 1L volumetric flask, diluting with water to a scale, and shaking up to obtain the prepared iron standard solution.
Further, diluting the iron standard solution by a preset multiple to obtain a diluted solution, adding reactants into the diluted solution with different milliliters, shaking up, and obtaining reaction solutions respectively, wherein the method specifically comprises the following steps:
diluting the prepared iron standard solution by 10 times;
respectively sucking 0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL and 5.0mL of diluted iron standard solution, respectively injecting the diluted iron standard solution into a colorimetric tube of 100mL, sequentially and respectively adding ascorbic acid, acetic acid-sodium acetate and phenanthroline, diluting the mixture to a scale by using distilled water, and shaking up to respectively obtain reaction solutions.
Further, the determining of the solution absorbance of each reaction solution at a preset ultraviolet wavelength specifically includes:
and (3) developing each reaction solution for 10min, and respectively measuring the absorbance of each reaction solution at the wavelength of 510nm of an ultraviolet spectrophotometer by using a 1cm glass cuvette and a blank developer solution as reference.
Further, taking a preset amount of the denitration liquid, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the total iron concentration of the denitration liquid, wherein the method specifically comprises the following steps:
taking a preset amount of denitration liquid into a 100mL volumetric flask, diluting with constant volume, taking a proper amount of diluent into a 100mL colorimetric tube, sequentially adding ascorbic acid, acetic acid-sodium acetate buffer solution and phenanthroline, fixing the volume to a 100mL scale mark with distilled water, and shaking up;
developing for 10min, and measuring absorbance of the solution with a 1cm glass cuvette and a blank developer solution as reference at 510nm wavelength of an ultraviolet spectrophotometer;
and substituting the measured absorbance into a standard curve equation to calculate the total iron concentration.
Further, taking the denitration liquid with the preset amount, sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the ferrous concentration of the denitration liquid, wherein the method specifically comprises the following steps:
taking a preset amount of denitration liquid into a 100ml colorimetric tube, sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline, fixing the volume to 100ml scale mark with distilled water, and shaking up;
developing for 10min, and measuring absorbance of the solution with a 1cm glass cuvette and a blank developer solution as reference at 510nm wavelength of an ultraviolet spectrophotometer;
substituting the measured absorbance into a standard curve equation to calculate the ferrous concentration.
The method for measuring the iron ions in the denitration absorption liquid comprises the steps of establishing a standard curve, obtaining a standard curve equation, taking a preset amount of denitration liquid based on the standard curve equation, measuring the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the total iron concentration of the denitration liquid; sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline into the denitration liquid with the preset amount, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the ferrous concentration of the denitration liquid; and obtaining the concentration of the trivalent iron through the difference value of the total iron concentration and the ferrous iron concentration. The method is simple and convenient to operate, is rapid, has a good anti-interference effect, improves the detection efficiency of the iron ions in the denitration liquid, realizes the respective determination of the ferrous ions and the ferric ions, and solves the technical problems that the ferrous ion amount and the ferric ion amount can not be determined independently and the determination efficiency of the iron ions is low in the existing iron ion determination method.
Drawings
Fig. 1 is a flowchart of a method for determining iron ions in a denitration absorption liquid according to an embodiment of the present invention.
FIG. 2 is a diagram illustrating a relationship between absorbance and iron concentration of a solution according to an embodiment of the present invention.
Detailed Description
The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for determining iron ions in a denitration absorption liquid, which comprises the following steps of: ferric oxide (high-grade pure, chemical reagent company limited of national drug group), hydrochloric acid (analytical pure, fine chemical reagent company of Beijing modernization Oriental), ascorbic acid (analytical pure, chemical reagent company limited of national drug group), acetic acid (analytical pure, fine chemical reagent company of Beijing Yili), sodium acetate (analytical pure, chemical reagent company limited of national drug group), phenanthroline (analytical pure, chemical reagent company limited of national drug group). The apparatus used comprises: analytical balance (ME204/02, McLerland Torledo International trade (Shanghai) Co., Ltd.), pH meter (PHS-3C, Lemamoto instruments Co., Ltd.), pipette gun (Beijing Darongxing laboratory instruments Co., Ltd.), spectrophotometer (UV-8000, Shanghai Meta analytical instruments Co., Ltd.).
As shown in fig. 1, an embodiment of the present invention provides a method for determining iron ions in a denitration absorption liquid, including:
s1, preparing an iron standard solution.
S2, diluting the iron standard solution by a preset multiple to obtain a diluted solution, adding the diluted solutions with different milliliters into the reactants respectively, shaking up, and obtaining reaction solutions respectively.
S3, measuring the solution absorbance of each reaction solution at the preset ultraviolet wavelength, establishing a standard curve by taking the solution absorbance as a vertical coordinate and the iron content in the reaction solution as a horizontal coordinate, and obtaining a standard curve equation; fig. 2 is a schematic diagram showing a relationship between solution absorbance and iron concentration according to an embodiment of the present invention.
And S4, taking a preset amount of the denitration liquid, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into a standard curve equation to obtain the total iron concentration of the denitration liquid.
S5, taking a preset amount of denitration liquid, sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline, determining the solution absorbance of the denitration liquid, and substituting the determined solution absorbance into a standard curve equation to obtain the ferrous concentration of the denitration liquid.
And S6, obtaining the concentration of the ferric iron through the difference value of the total iron concentration and the ferrous iron concentration.
Specifically, in a specific embodiment, under the condition that the pH is 3-9, reducing solution ferric iron into ferrous iron, adding acetic acid-sodium acetate as a buffer solution, then adding phenanthroline and ferrous iron to form a complex, and measuring the absorbance of the complex at the wavelength of 510nm on an ultraviolet spectrophotometer. The method comprises the following steps:
preparing an iron standard solution; specifically, weighing 0.0001 g-0.0002 g of ferric oxide, and drying the ferric oxide at 105-110 ℃ for 1h to obtain the ferric oxide;
adding 50ml of hydrochloric acid into a 400ml beaker, covering a watch glass, heating to dissolve, cooling to room temperature, transferring into a 1L volumetric flask, diluting with water to a scale, and shaking up to obtain the prepared iron standard solution.
Diluting the iron standard solution by a preset multiple to obtain a diluted solution, adding reactants into the diluted solution with different milliliters respectively, shaking up, and obtaining reaction solutions respectively; specifically, the prepared iron standard solution is diluted by 10 times;
respectively sucking 0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL and 5.0mL of diluted iron standard solution, respectively injecting the diluted iron standard solution into a colorimetric tube of 100mL, sequentially and respectively adding ascorbic acid, acetic acid-sodium acetate and phenanthroline, diluting the mixture to a scale by using distilled water, and shaking up to respectively obtain reaction solutions.
Measuring the solution absorbance of each reaction solution at a preset ultraviolet wavelength, establishing a standard curve by taking the solution absorbance as a vertical coordinate and the iron content in the reaction solution as a horizontal coordinate, and obtaining a standard curve equation; further, the determining of the solution absorbance of each reaction solution at a preset ultraviolet wavelength specifically includes: and (3) developing each reaction solution for 10min, and respectively measuring the absorbance of each reaction solution at the wavelength of 510nm of an ultraviolet spectrophotometer by using a 1cm glass cuvette and a blank developer solution as reference.
Taking a preset amount of the denitration liquid, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the total iron concentration of the denitration liquid; specifically, a preset amount of denitration solution is taken in a 100mL volumetric flask, after constant volume dilution, a proper amount of diluent is taken in a 100mL colorimetric tube, ascorbic acid, acetic acid-sodium acetate buffer solution and phenanthroline are sequentially added, the constant volume is set to 100mL scale mark with distilled water, and the mixture is shaken up; developing for 10min, and measuring absorbance of the solution with a 1cm glass cuvette and a blank developer solution as reference at 510nm wavelength of an ultraviolet spectrophotometer; the measured absorbance was substituted into a standard curve equation to calculate the total iron concentration C (total Fe).
Sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline into the denitration liquid with the preset amount, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the ferrous concentration of the denitration liquid; taking a preset amount of denitration liquid into a 100ml colorimetric tube, sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline, fixing the volume to 100ml scale mark with distilled water, and shaking up; developing for 10min, and measuring absorbance of the solution with a 1cm glass cuvette and a blank developer solution as reference at 510nm wavelength of an ultraviolet spectrophotometer; the measured absorbance was substituted into a standard curve equation to calculate the ferrous iron concentration C (Fe2 +).
And obtaining the concentration of the trivalent iron through the difference value of the total iron concentration and the ferrous iron concentration. The concentration of ferric ions in the denitrated liquid, namely C (Fe3+) -C (total Fe) -C (Fe2+), can be obtained by subtracting the ferrous concentration from the measured total iron concentration.
The determination principle used by the method is that ferrous ions and phenanthroline in a solution with the pH value of 3-9 generate a stable orange-red complex, and the complex can be stable for half a year under the dark condition. The reaction formula is as follows:
strong oxidants, cyanides, nitrites, pyrophosphates, metaphosphates, and certain metal ions can interfere with the assay. Cyanide and nitrite can be removed by adding acid and boiling, and pyrophosphoric acid and metaphosphate can be converted into orthophosphate to reduce interference.
The interference of strong oxidants can be eliminated by adding ascorbic acid.
Phenanthroline can form colored complexes with certain metal ions to interfere with the assay. However, in acetic acid-sodium acetate buffer solution, copper, zinc, cobalt and chromium with concentration not more than 10 times of iron concentration and nickel with concentration less than 2mg/L do not interfere with measurement, and when the concentration is higher, excessive color developing agent can be added to eliminate the concentration. The mercury, cadmium, silver and the like can form precipitates with phenanthroline, and at low concentration, the excessive phenanthroline can be added to eliminate the precipitates.
If the iron content of each reagent batch is different, a curve needs to be drawn again every time a new test solution is prepared.
If the iron content of the water sample is higher, the water sample can be properly diluted and then measured.
The operation method is simple, convenient and quick, and has good anti-interference effect, so that the detection efficiency of the iron ions in the denitration liquid can be improved.
In the foregoing embodiment, the method for determining iron ions in a denitration absorption liquid provided by the invention includes establishing a standard curve, obtaining a standard curve equation, taking a preset amount of denitration liquid based on the standard curve equation, determining solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the total iron concentration of the denitration liquid; sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline into the denitration liquid with the preset amount, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the ferrous concentration of the denitration liquid; and obtaining the concentration of the trivalent iron through the difference value of the total iron concentration and the ferrous iron concentration. The method is simple and convenient to operate, is rapid, has a good anti-interference effect, improves the detection efficiency of the iron ions in the denitration liquid, realizes the respective determination of the ferrous ions and the ferric ions, and solves the technical problems that the ferrous ion amount and the ferric ion amount can not be determined independently and the determination efficiency of the iron ions is low in the existing iron ion determination method.
The above embodiments are only for illustrating the embodiments of the present invention and are not to be construed as limiting the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made on the basis of the embodiments of the present invention shall be included in the scope of the present invention.
Claims (6)
1. A method for measuring iron ions in a denitration absorption liquid is characterized by comprising the following steps:
preparing an iron standard solution;
diluting the iron standard solution by a preset multiple to obtain a diluted solution, adding reactants into the diluted solution with different milliliters respectively, shaking up, and obtaining reaction solutions respectively;
measuring the solution absorbance of each reaction solution at a preset ultraviolet wavelength, establishing a standard curve by taking the solution absorbance as a vertical coordinate and the iron content in the reaction solution as a horizontal coordinate, and obtaining a standard curve equation;
taking a preset amount of the denitration liquid, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the total iron concentration of the denitration liquid;
sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline into the denitration liquid with the preset amount, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the ferrous concentration of the denitration liquid;
and obtaining the concentration of the trivalent iron through the difference value of the total iron concentration and the ferrous iron concentration.
2. The method for determining iron ions in the denitration absorption liquid according to claim 1, wherein the preparing of the iron standard solution specifically comprises:
weighing 0.0001 g-0.0002 g of ferric oxide, and drying the ferric oxide at the temperature of 105-110 ℃ for 1h to obtain the ferric oxide;
adding 50ml of hydrochloric acid into a 400ml beaker, covering a watch glass, heating to dissolve, cooling to room temperature, transferring into a 1L volumetric flask, diluting with water to a scale, and shaking up to obtain the prepared iron standard solution.
3. The method for determining iron ions in the denitration absorbing liquid according to claim 2, wherein the method comprises the steps of diluting the iron standard solution by a preset multiple to obtain a diluted solution, adding reactants into the diluted solution with different milliliters, shaking up the reactant to obtain reaction solutions, and specifically comprises the following steps:
diluting the prepared iron standard solution by 10 times;
respectively sucking 0mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL and 5.0mL of diluted iron standard solution, respectively injecting the diluted iron standard solution into a colorimetric tube of 100mL, sequentially and respectively adding ascorbic acid, acetic acid-sodium acetate and phenanthroline, diluting the mixture to a scale by using distilled water, and shaking up to respectively obtain reaction solutions.
4. The method for measuring iron ions in the denitration absorption liquid according to claim 3, wherein the measuring of the solution absorbance of each reaction solution at a preset ultraviolet wavelength specifically comprises:
and (3) developing each reaction solution for 10min, and respectively measuring the absorbance of each reaction solution at the wavelength of 510nm of an ultraviolet spectrophotometer by using a 1cm glass cuvette and a blank developer solution as reference.
5. The method for measuring iron ions in the denitration absorption liquid according to claim 3, wherein a preset amount of the denitration liquid is taken, the solution absorbance of the denitration liquid is measured, and the measured solution absorbance is substituted into the standard curve equation to obtain the total iron concentration of the denitration liquid, and specifically comprises:
taking a preset amount of denitration liquid into a 100mL volumetric flask, diluting with constant volume, taking a proper amount of diluent into a 100mL colorimetric tube, sequentially adding ascorbic acid, acetic acid-sodium acetate buffer solution and phenanthroline, fixing the volume to a 100mL scale mark with distilled water, and shaking up;
developing for 10min, and measuring absorbance of the solution with a 1cm glass cuvette and a blank developer solution as reference at 510nm wavelength of an ultraviolet spectrophotometer;
and substituting the measured absorbance into a standard curve equation to calculate the total iron concentration.
6. The method for determining iron ions in a denitration absorption liquid according to claim 5, wherein the method comprises the steps of taking a preset amount of the denitration liquid, sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline, determining the solution absorbance of the denitration liquid, and substituting the measured solution absorbance into the standard curve equation to obtain the ferrous concentration of the denitration liquid, and specifically comprises the following steps:
taking a preset amount of denitration liquid into a 100ml colorimetric tube, sequentially adding acetic acid-sodium acetate buffer solution and phenanthroline, fixing the volume to 100ml scale mark with distilled water, and shaking up;
developing for 10min, and measuring absorbance of the solution with a 1cm glass cuvette and a blank developer solution as reference at 510nm wavelength of an ultraviolet spectrophotometer;
substituting the measured absorbance into a standard curve equation to calculate the ferrous concentration.
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