CN112557313A - Improved method for determining aluminum ion content by chromium azure S method - Google Patents
Improved method for determining aluminum ion content by chromium azure S method Download PDFInfo
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- CN112557313A CN112557313A CN202011268685.XA CN202011268685A CN112557313A CN 112557313 A CN112557313 A CN 112557313A CN 202011268685 A CN202011268685 A CN 202011268685A CN 112557313 A CN112557313 A CN 112557313A
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 89
- 238000000034 method Methods 0.000 title claims abstract description 38
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229910052804 chromium Inorganic materials 0.000 title claims abstract description 18
- 239000011651 chromium Substances 0.000 title claims abstract description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- -1 aluminum ion Chemical class 0.000 claims abstract description 38
- 239000012482 calibration solution Substances 0.000 claims abstract description 28
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 239000007853 buffer solution Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 238000012360 testing method Methods 0.000 claims abstract description 8
- 238000002835 absorbance Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010998 test method Methods 0.000 claims description 6
- 238000007865 diluting Methods 0.000 claims description 5
- 239000006260 foam Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 3
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 239000012086 standard solution Substances 0.000 claims description 3
- 238000009472 formulation Methods 0.000 claims 1
- 238000005259 measurement Methods 0.000 abstract description 6
- 239000003651 drinking water Substances 0.000 description 5
- 235000020188 drinking water Nutrition 0.000 description 5
- 239000004411 aluminium Substances 0.000 description 2
- 239000000872 buffer Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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- 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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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1813—Specific cations in water, e.g. heavy metals
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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
- G01N21/75—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
- G01N2021/775—Indicator and selective membrane
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Abstract
The invention discloses an improved method for determining aluminum ion content by a chromium azure S method, and relates to the technical field of aluminum ion content measurement by the chromium azure S method. The method comprises a preparation method of a reagent A and a testing method of aluminum ions in a step B. The preparation method of the reagent in the step A further comprises the step A1 of preparing experimental water; step a2 preparing an aluminum calibration solution: rho is 100mg/L, and a calibration solution is prepared in the step A3; step A4 preparing an aluminum buffer solution; step a5 prepares an aluminum developer. The method for testing the aluminum ions further comprises a step B1 of transferring 5mL of aluminum calibration solution with corresponding concentration; b2 slowly adding 1mL of aluminum buffer solution into the colorimetric tube; step B3, adding 1mL of aluminum color developing agent into the colorimetric tube; in conclusion, the step B4 calculates the concentration of aluminum ions in the sample according to the calibrated absorbance, compared with the prior art, the present invention has the following advantages: the solution is simple to prepare, the determination steps are simple and convenient, and the measurement accuracy is high and the repeatability is good.
Description
Technical Field
The invention relates to the technical field of aluminum ion content measurement by a chromium azure S method, in particular to an improved method for measuring aluminum ion content by the chromium azure S method.
Background
Aluminum is a harmful element, and most researches on the harm of aluminum to human health are carried out at home and abroad. The aluminum content in drinking water is definitely specified in GB5749-2006 sanitary Standard for Drinking Water which specifies that the aluminum content in drinking water is not higher than 0.2 mg/L. The GB5750.6-2006 Standard test method for Drinking Water provides that the determination of aluminum in Drinking Water adopts a chromium azure S spectrophotometry, and the method has the following defects in the use process: the reagent types are multiple, and the operation steps are relatively complicated; the addition amount of the ethylenediamine buffer is insufficient, the pH value is difficult to control, and the reproducibility and stability of the sample are poor.
Disclosure of Invention
The invention aims to provide an improved method for determining the content of aluminum ions by a chromium azure S method for measuring the content of the aluminum ions, aiming at overcoming the defects and shortcomings in the prior art.
The method comprises the following processes: step a, a preparation method of a reagent and step b, a test method of aluminum ions.
a. Method for producing reagent
Unless otherwise stated, analytically pure reagents meeting national standards are used in the analysis.
Glass containers (volumetric flask, beaker, pipette, cuvette, etc.) used in reagent preparation and test process need to be soaked in 10% nitric acid to remove aluminum, and then the glass containers are cleaned with pure water for use (the cuvette needs to be dried).
1. Water for experiment
The water (hereinafter referred to as "water") used for reagent preparation is water meeting the third-level water specification in GB/T6682 and 2008 'analytical laboratory Water specification and test method' or water with the same purity.
2. Aluminum calibration solution: rho is 100mg/L
1.7582g of potassium aluminum sulfate KAI (SO) were weighed4)2·12H2O]Dissolving in water, diluting to 1000mL, and storing in polyethylene bottle.
3. Calibration solution
10mg/L aluminum calibration solution: accurately sucking 10mL of 100mg/L aluminum calibration solution into a 100mL volumetric flask, and metering the volume to a scale mark by using water;
0.3mg/L aluminum calibration solution: accurately sucking 3mL of 10mg/L aluminum calibration solution into a 100mL volumetric flask, and metering the volume to a scale mark by using water;
the calibration solution for aluminum with other concentrations can be prepared by diluting 0.3mg/L of the calibration solution for aluminum.
4. Aluminium buffer
Dissolving 16g of anhydrous sodium acetate in 90mL of water, adding about 1.4mL of acetic acid, uniformly mixing, adjusting the pH value to 5.5, and fixing the volume to 100 mL; before use, 0.05g of hexadecyl trimethyl ammonium bromide is added to be dissolved and mixed evenly, and the mixture is kept stand for use after bubbles disappear.
5. Aluminium colour developing agent
0.02g of chromium azure S (C) is weighed23H13O9SC12Na3) Dissolved in 50mL (1+1) ethanol solution and made up to 100mL with water.
b. Method for testing aluminum ions
Transferring 5mL of aluminum calibration solution or a sample to be detected with corresponding concentration into a colorimetric tube (the aluminum ion content in a water sample needs to be diluted when exceeding 0.3 mg/L), slowly adding 1mL of aluminum buffer solution into the colorimetric tube, screwing a colorimetric bottle cap, and shaking the colorimetric bottle to uniformly mix the solution. Standing for 1min until the foam near the colorimetric tube opening is broken. And adding 1mL of aluminum color developing agent into the colorimetric tube, screwing the colorimetric tube cover, and shaking the colorimetric tube to uniformly mix the solution. And developing for 15min, wiping off the moisture on the outer wall, measuring the absorbance at the wavelength of 620nm, and calculating the concentration of the aluminum ions of the sample according to the calibrated absorbance (during calibration, only the aluminum ion standard solution with known concentration is used for replacing a water sample, and the other steps are consistent with the measurement of the water sample).
Note that: foam is easily generated in the adding process of the aluminum buffer solution, and the adding process is slow; the aluminum buffer solution and the aluminum color developing agent are added with care not to be polluted by other reagents.
As mentioned above, the improved method for determining the content of aluminum ions by the chromium azure S method comprises the preparation method of the reagent for determination and the test method of the aluminum ions, and compared with the prior art, the method has the following advantages: the solution is simple to prepare, the determination steps are simple and convenient, and the measurement accuracy is high and the repeatability is good.
Drawings
FIG. 1 is a flow chart of an improved method for determining aluminum ion content by a chromium azure S method according to the invention;
FIG. 2 is an aluminum ion working curve according to an embodiment of the present invention.
Detailed Description
The invention is further described in the following with reference to the figures and examples
An improved method for determining the content of aluminum ions by a chromium azure S method is characterized by comprising the following steps: step A, a preparation method of a reagent; and B, testing the aluminum ions (shown in the attached figure 1).
The preparation method of the reagent further comprises the following steps:
step A1. preparing water for experiment
The water (hereinafter referred to as "water") used by the reagent is water meeting the third-level water specification in GB/T6682-;
step A2, preparing an aluminum calibration solution: rho is 100mg/L
1.7582g of potassium aluminum sulfate KAI (SO) were weighed4)2·12H2O]Dissolving in water, diluting to 1000mL, and storing in polyethylene bottle.
Step A3. preparing a solution for calibration
10mg/L aluminum calibration solution: accurately sucking 10mL of 100mg/L aluminum calibration solution into a 100mL volumetric flask, and metering the volume to a scale mark by using water;
0.3mg/L aluminum calibration solution: accurately sucking 3mL of 10mg/L aluminum calibration solution into a 100mL volumetric flask, and metering the volume to a scale mark by using water;
the aluminum calibration solution with other concentrations can be diluted and prepared by 0.3mg/L aluminum calibration solution;
step A4. preparing an aluminum buffer solution
Dissolving 16g of anhydrous sodium acetate in 90mL of water, adding about 1.4mL of acetic acid, uniformly mixing, adjusting the pH value to 5.5, and fixing the volume to 100 mL; before use, 0.05g of hexadecyl trimethyl ammonium bromide is added to be dissolved and mixed evenly, and the mixture is kept stand for use after bubbles disappear.
Step A5, preparing an aluminum color developing agent
0.02g of chromium azure S (C) is weighed23H13O9SC12Na3) Dissolving in 50mL (1+1) ethanol solution, and adding water to 100 mL;
the analysis uses analytically pure reagents meeting the national standard;
glass containers (volumetric flask, beaker, pipette, colorimetric tube and the like) used in the reagent preparation and test processes are soaked in 10% nitric acid to remove aluminum and are cleaned by pure water for use, wherein the colorimetric tube needs to be dried.
The step B, the test method of the aluminum ions comprises the following steps:
b1, transferring 5mL of aluminum calibration solution or a sample to be detected with corresponding concentration into a colorimetric tube, and diluting when the content of aluminum ions in a water sample exceeds 0.3 mg/L;
b2, slowly adding 1mL of aluminum buffer solution into the colorimetric tube, screwing a colorimetric bottle cap, and shaking the colorimetric bottle to uniformly mix the solution; standing for 1min until the foam near the colorimetric pipe orifice is broken;
b3, adding 1mL of aluminum color developing agent into the colorimetric tube, screwing a colorimetric tube cover, and shaking the colorimetric tube to uniformly mix the solution; developing for 15min, and wiping off water on the outer wall; measuring absorbance at a wavelength of 620 nm;
step B4., calculating the concentration of aluminum ions of the sample according to the calibrated absorbance (as shown in fig. 2), and during calibration, only the aluminum ion standard solution with known concentration is needed to replace the water sample, and the rest steps are consistent with the steps b1 to b3.
In summary, the improved method for determining the content of aluminum ions by the chromium azure S method, which comprises the preparation method of the reagent for determination and the test method of aluminum ions, has the following advantages compared with the prior art: the solution is simple to prepare, the determination steps are simple and convenient, and the measurement accuracy is high and the repeatability is good.
Claims (3)
1. An improved method for determining the content of aluminum ions by a chromium azure S method is characterized by comprising the following steps: step A, a preparation method of a reagent; and B, testing the aluminum ions.
2. The improved method for determining the content of aluminum ions by the chromium azure S method as claimed in claim 1, characterized in that the preparation method of the reagent in step A. further comprises:
step A1. preparing water for experiment
The water used by the reagent is called as water which meets the third-level water specification in GB/T6682-;
step A2, preparing an aluminum calibration solution: rho is 100mg/L
1.7582g of potassium aluminum sulfate KAI (SO) were weighed4)2·12H2O]Dissolving in water, fixing the volume to 1000mL, and storing in a polyethylene bottle;
step A3. preparing a solution for calibration
10mg/L aluminum calibration solution: accurately sucking 10mL of 100mg/L aluminum calibration solution into a 100mL volumetric flask, and metering the volume to a scale mark by using water;
0.3mg/L aluminum calibration solution: accurately sucking 3mL of 10mg/L aluminum calibration solution into a 100mL volumetric flask, and metering the volume to a scale mark by using water;
the aluminum calibration solution with other concentrations can be diluted and prepared by 0.3mg/L aluminum calibration solution;
step A4. preparing an aluminum buffer solution
Dissolving 16g of anhydrous sodium acetate in 90mL of water, adding about 1.4mL of acetic acid, uniformly mixing, adjusting the pH value to 5.5, and fixing the volume to 100 mL; before use, 0.05g of hexadecyl trimethyl ammonium bromide is added to be dissolved and mixed evenly, and the mixture is kept stand for use after bubbles disappear.
Step A5, preparing an aluminum color developing agent
0.02g of chromium azure S (C) is weighed23H13O9SC12Na3) Dissolving in 50mL (1+1) ethanol solution, and adding water to 100 mL;
the analysis uses analytically pure reagents meeting the national standard;
all glass containers during reagent formulation and testing: the volumetric flask, the beaker, the pipette and the colorimetric tube are soaked in 10 percent nitric acid to remove aluminum and are used after being cleaned by pure water, wherein the colorimetric tube needs to be dried.
3. The improved method for determining the content of aluminum ions by the chromium azure S method as claimed in claim 1, wherein the step B. the test method for aluminum ions comprises the following steps:
b1, transferring 5mL of aluminum calibration solution or a sample to be detected with corresponding concentration into a colorimetric tube, and diluting when the content of aluminum ions in a water sample exceeds 0.3 mg/L;
b2, slowly adding 1mL of aluminum buffer solution into the colorimetric tube, screwing a colorimetric bottle cap, and shaking the colorimetric bottle to uniformly mix the solution; standing for 1min until the foam near the colorimetric pipe orifice is broken;
b3, adding 1mL of aluminum color developing agent into the colorimetric tube, screwing a colorimetric tube cover, and shaking the colorimetric tube to uniformly mix the solution; developing for 15min, and wiping off water on the outer wall; measuring absorbance at a wavelength of 620 nm;
step B4., the concentration of the aluminum ions of the sample is calculated according to the calibrated absorbance, when the calibration is carried out, only the aluminum ion standard solution with the known concentration is needed to replace the water sample, and the other steps are consistent with the steps B1 to B3.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011268685.XA CN112557313A (en) | 2020-11-13 | 2020-11-13 | Improved method for determining aluminum ion content by chromium azure S method |
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| CN202011268685.XA CN112557313A (en) | 2020-11-13 | 2020-11-13 | Improved method for determining aluminum ion content by chromium azure S method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113945533A (en) * | 2021-11-09 | 2022-01-18 | 上海仪电科学仪器股份有限公司 | Treatment and application method of extraction colorimetric bottle |
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| CN108333125A (en) * | 2017-12-04 | 2018-07-27 | 上海仪电科学仪器股份有限公司 | A kind of Chrome azurol s colorimetry measurement aluminium ion method |
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Patent Citations (6)
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Application publication date: 20210326 |