CN112345479B - Method for measuring chloride ion content in cobaltosic oxide by using double-beam turbidimetry - Google Patents
Method for measuring chloride ion content in cobaltosic oxide by using double-beam turbidimetry Download PDFInfo
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 77
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000004879 turbidimetry Methods 0.000 title claims abstract description 15
- 239000000243 solution Substances 0.000 claims abstract description 110
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 105
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000000706 filtrate Substances 0.000 claims abstract description 59
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 59
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 58
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 29
- 239000011259 mixed solution Substances 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000000523 sample Substances 0.000 claims description 30
- 238000012360 testing method Methods 0.000 claims description 26
- 239000012086 standard solution Substances 0.000 claims description 21
- 239000003153 chemical reaction reagent Substances 0.000 claims description 19
- 238000002156 mixing Methods 0.000 claims description 10
- 239000012496 blank sample Substances 0.000 claims description 7
- 238000002835 absorbance Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 12
- 239000002244 precipitate Substances 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 239000011780 sodium chloride Substances 0.000 description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000011550 stock solution Substances 0.000 description 4
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000012546 transfer 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
- 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)
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Abstract
The invention discloses a method for determining the content of chloride ions in cobaltosic oxide by using a double-beam turbidimetry method, which comprises the following steps: (1) Adding cobaltosic oxide to be detected into deionized water, uniformly stirring, heating to boil, and cooling to room temperature to obtain a mixed solution; (2) Adding a nitric acid solution into the mixed solution, and filtering to obtain a filtrate; (3) Adding a nitric acid solution, glycerol and a silver nitrate solution into the filtrate, and standing in the shade to obtain a sample to be detected; (4) And (3) carrying out color comparison on the sample to be detected on an ultraviolet spectrophotometer at the wavelength of 420nm, and calculating to obtain the content of chloride ions in the cobaltosic oxide to be detected according to the standard working curve value. The invention has good stability and high sensitivity, and can detect lower chloride ion content.
Description
Technical Field
The invention belongs to the technical field of detecting the content of chloride ions, and particularly relates to a method for determining the content of chloride ions in cobaltosic oxide by using a double-beam turbidimetry method.
Background
At present, a common 721 type spectrophotometer is used for detecting chloride ions, the sensitivity of instruments of the type is low, the linearity of curves is poor, the result has certain fluctuation, the accuracy of determination is reduced, and the phenomenon of filter leakage can occur when the traditional filter paper is used for filtering in the pretreatment process, so that the working efficiency is influenced. The method for detecting the content of chloride ions in the prior art generally comprises the following steps: weighing a sample, adding water, heating to boil, cooling, transferring to a volumetric flask, fixing the volume, and filtering, wherein if the solution leaks, the filtering needs to be repeated until the solution is clear; transferring the filtrate into a volumetric flask, adding a nitric acid solution, absolute ethyl alcohol and a silver nitrate solution, and standing; the absorbance was measured in a model 721 spectrophotometer at 420nm against a reagent blank as a reference. The method for detecting the content of the chloride ions has the following disadvantages: the 721 type spectrophotometer has low sensitivity, low chloride ion content in cobaltosic oxide, more samples need to be weighed, the dissolving time is longer, and powder precipitates are more and have large volume, so that the powder is difficult to transfer into a volumetric flask; the filter is leaked due to the fact that the amount of the precipitate is large and the powder is fine, the filter needs to be carried out for many times, the error is large, and the working efficiency is low; the silver nitrate reagent has large dosage.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the method for determining the content of the chloride ions in the cobaltosic oxide by using the double-beam turbidimetry, which has the advantages of good stability and high sensitivity and can detect the lower content of the chloride ions.
The invention adopts the following technical scheme:
a method for measuring the content of chloride ions in cobaltosic oxide by using a two-beam turbidimetry method, which is characterized by comprising the following steps:
(1) Adding cobaltosic oxide to be detected into deionized water, stirring uniformly, heating to boil, dissolving at 95-100 ℃ for 20-30 min, and cooling to room temperature to obtain a mixed solution; the solid-liquid ratio of the cobaltosic oxide to be detected to the deionized water is 1 (20-25);
(2) Adding a nitric acid solution into the mixed solution, shaking uniformly, standing for 20-30 min, and filtering to obtain a filtrate; the volume ratio of the mixed solution to the nitric acid solution is (10-15) to 1;
(3) Adding a nitric acid solution, a glycerol solution and a silver nitrate solution into the filtrate, and standing in the shade for 20-30 min to obtain a sample to be detected; the volume ratio of the filtrate to the nitric acid solution to the glycerol solution to the silver nitrate solution is (10-15): 2.5-3): 1;
(4) Transferring the filtrate obtained in the step (2) into a colorimetric tube, adding a chloride ion working standard solution into the colorimetric tube containing the filtrate, and performing the step (3) to obtain a filtrate containing the chloride ion working standard solution; drawing a standard working curve by taking the chloride ion content in the filtrate containing the chloride ion working standard solution as an abscissa and the absorbance as an ordinate;
(5) And (3) carrying out color comparison on the sample to be detected on an ultraviolet spectrophotometer at the wavelength of 420nm, simultaneously carrying out a sample blank test and a reagent blank test, and calculating the chloride ion content in the cobaltosic oxide to be detected according to the standard working curve value.
According to the method for measuring the content of chloride ions in the cobaltosic oxide by using the two-beam turbidimetry, the method is characterized in that the nitric acid solution in the step (2) and the nitric acid solution in the step (3) are both prepared from concentrated nitric acid and water, wherein the volume ratio of the concentrated nitric acid to the water is 1; in the step (3), the glycerol solution is prepared from glycerol and water in a volume ratio of 1; the concentration of the silver nitrate solution in the step (3) is 2-6 g/L.
The method for measuring the content of chloride ions in the cobaltosic oxide by using the double-beam turbidimetry is characterized in that the sample blank test in the step (5) is carried out by the following steps: adding a nitric acid solution and a glycerol solution into the filtrate, uniformly mixing, placing in the shade, and standing for 20-30 min to obtain a blank sample; the volume ratio of the filtrate to the nitric acid solution to the glycerol solution is (4-6) to 1.
The method for measuring the content of chloride ions in the cobaltosic oxide by using the double-beam turbidimetry is characterized in that the reagent blank test in the step (5) is carried out by the following steps: adding a nitric acid solution, a glycerol solution and a silver nitrate solution into the filtrate, uniformly mixing, placing the mixture in the shade, and standing for 20-30 min to obtain a reagent blank sample; the volume ratio of the filtrate to the nitric acid solution to the glycerol solution to the silver nitrate solution is (10-15): (2.5-3): 1.
The method for measuring the content of the chloride ions in the cobaltosic oxide by using the double-beam turbidimetry is characterized in that the concentration of the chloride ion working standard solution in the step (4) is 0.04mg/mL-0.2mg/mL.
The invention has the beneficial technical effects that: the method adopts the ultraviolet double-beam turbidimetry to measure the content of the chloride ions in the cobaltosic oxide, and has the advantages of less sample consumption and short dissolving time compared with the measuring method in the prior art. The detection result has good stability and high sensitivity, and can detect lower chloride ion content (detection limit: 0.00025% and quantification limit: 0.001%). The invention adds nitric acid (1 + 1) into the beaker before filtration, which can effectively prevent the phenomenon of filtration leakage in the filtration link. The original 17g/L of silver nitrate is changed into 2-6g/L, so that the using amount of the silver nitrate is greatly reduced.
Detailed Description
A method for measuring the content of chloride ions in cobaltosic oxide by using a double-beam turbidimetry method comprises the following steps:
(1) Adding cobaltosic oxide to be detected into deionized water, stirring uniformly, heating to boil, dissolving at constant temperature of 95-100 ℃ for 20-30 min, and cooling to room temperature to obtain a mixed solution; the solid-liquid ratio of cobaltosic oxide to deionized water to be detected is 1 (20-25); the solid-to-liquid ratio of the cobaltosic oxide to the deionized water to be measured is the ratio of the mass (g) of the cobaltosic oxide to be measured to the volume (mL) of the deionized water.
(2) Adding a nitric acid solution into the mixed solution, transferring the obtained solution and the precipitate into a volumetric flask, fixing the volume with water, shaking up, standing for 20min-30min, and filtering to obtain a filtrate; the volume ratio of the mixed solution to the nitric acid solution is (10-15) to 1; the nitric acid solution is prepared by concentrated nitric acid and water with the volume ratio of 1;
(3) Transferring a proper amount of intermediate filtrate into a colorimetric tube, adding a nitric acid solution, a glycerol solution and a silver nitrate solution into the filtrate, fixing the volume, uniformly mixing, placing in the shade, and standing for 20-30 min to obtain a sample to be detected; the volume ratio of the filtrate to the nitric acid solution to the glycerol solution to the silver nitrate solution is (10-15): 2.5-3): 1; the nitric acid solution is prepared by concentrated nitric acid and water with the volume ratio of 1; the glycerol solution is prepared by glycerol and water with the volume ratio of 1; the concentration of the silver nitrate solution is 2g/L-6g/L.
(4) Drawing a standard addition method curve: and (3) respectively transferring the filtrates in the step (2) into a 50mL colorimetric tube, adding different volumes of chloride ion working standard solutions into the colorimetric tube containing the filtrates, and preparing at least 5 standard solutions according to the method in the step (3), wherein the chloride ion concentration of the sample to be detected is within the standard series range. Preparing to obtain filtrate containing chloride ion working standard solution; and (3) drawing a standard working curve by taking the chloride ion content in the filtrate containing the chloride ion working standard solution as an abscissa and the absorbance as an ordinate. The concentration of the chloride ion working standard solution is 0.04mg/mL-0.2mg/mL.
(5) And (3) carrying out color comparison on the sample to be detected on an ultraviolet spectrophotometer at the wavelength of 420nm, simultaneously carrying out a sample blank test and a reagent blank test, and calculating the chloride ion content in the cobaltosic oxide to be detected according to the standard working curve value. The sample blank test is carried out as follows: transferring the filtrate into a colorimetric tube, adding a nitric acid solution and a glycerol solution into the filtrate, uniformly mixing, fixing the volume, and standing in the shade for 20-30 min to obtain a blank sample; the volume ratio of the filtrate to the nitric acid solution to the glycerol solution is (4-6) to 1. The reagent blank test is carried out as follows: transferring the filtrate into a colorimetric tube, adding a nitric acid solution, a glycerol solution and a silver nitrate solution into the filtrate, uniformly mixing, fixing the volume, placing in the shade, and standing for 20-30 min to obtain a reagent blank sample; the volume ratio of the filtrate to the nitric acid solution to the glycerol solution to the silver nitrate solution is (10-15): 2.5-3): 1.
Example 1
Weighing 2.0000g of cobaltosic oxide sample to be detected (batch number KL 2010050) in a 250mL beaker, adding 50mL of deionized water into the beaker, uniformly stirring, placing the beaker on a heating plate, heating at 95 ℃ for boiling for 20min, taking off the beaker, and cooling the beaker to room temperature to obtain a mixed solution.
Adding a nitric acid solution into the mixed solution, transferring the obtained solution and the precipitate into a 100mL volumetric flask, fixing the volume with water, shaking up, standing for 20min, and filtering in an original beaker by using filter paper (the filtrate is clear) to obtain a filtrate; the volume ratio of the mixed solution to the nitric acid solution is 10; the nitric acid solution is prepared by concentrated nitric acid and water with the volume ratio of 1.
And (3) transferring 20.0mL of filtrate into a 50mL colorimetric tube, adding 5.0mL of nitric acid solution, 5.0mL of glycerol solution and 2.0mL of silver nitrate solution with the concentration of 2g/L into the filtrate, fixing the volume by using water, uniformly mixing, placing in the shade, and standing for 20min to obtain the sample to be detected. The nitric acid solution is prepared by concentrated nitric acid and water with the volume ratio of 1; the glycerol solution is prepared by mixing glycerol and water in a volume ratio of 1.
Preparing a standard solution: a) Chloride ion standard stock solution: weighing 1.6488g of sodium chloride burned at 550 ℃, putting the sodium chloride into a beaker, adding water to dissolve the sodium chloride, and metering the volume of the solution into a 1000mL volumetric flask, wherein 1mL of the solution contains chloride ions and the magnesium is left on the magnesium. b) Chloride ion standard solution: 20.00mL of the standard stock solution of chloride ions was transferred to a 500mL volumetric flask and the volume was determined by water, and 1mL of the solution containing chloride ions was measured on a mg.
Transferring 6 parts of 20mL of sample filtrate to be detected, respectively placing the filtrate in 50mL of colorimetric tubes, and sequentially adding 0.00mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL and 5.00mL of chloride ion standard solution according to the sample determination method. And drawing a working curve by taking the chloride ion content as an abscissa and the absorbance as an ordinate.
And (3) performing a sample blank test and a reagent blank test, and measuring the content of chloride ions at a wavelength of 420nm by using a TU-1950 double-beam ultraviolet-visible spectrophotometer in a 3cm quartz cuvette and taking a reagent blank sample as a reference. And automatically obtaining the corresponding mass concentration of the chloride ions in the cobaltosic oxide to be detected from the working curve according to the standard working curve value, wherein the detection result is shown in table 1. The sample blank test is carried out as follows: transferring 20.0mL of the filtrate into a 50mL colorimetric tube, adding 5.0mL of nitric acid solution and 5.0mL of glycerol solution into the filtrate, and fixing the volume with water. The reagent blank test is carried out as follows: transferring 20.0mL of the filtrate into a 50mL colorimetric tube, adding 5.0mL of nitric acid solution, 5.0mL of glycerol solution and 2.0mL of silver nitrate solution with the concentration of 2g/L into the filtrate, fixing the volume by using water, shaking uniformly, and then placing in a dark place for 20min.
The chloride ion content of the sample was calculated as follows:
in the formula: m is a unit of 1 -the amount of chloride ions, μ g, found from the working curve;
m 0 -amount of test material, g.
Table 1 test results of example 1 repeated 6 times
Example 2
Weighing 2.0000g of cobaltosic oxide sample to be detected (batch number KL 2010050) in a 250mL beaker, adding 50mL of deionized water into the beaker, uniformly stirring, placing the beaker on a heating plate, heating at 95 ℃ for boiling for 20min, taking off the beaker, and cooling the beaker to room temperature to obtain a mixed solution.
Adding a nitric acid solution into the mixed solution, transferring the obtained solution and the precipitate into a 100mL volumetric flask, fixing the volume with water, shaking up, standing for 20min, and filtering in an original beaker by using filter paper (taking care that the filtrate is clear) to obtain a filtrate; the volume ratio of the mixed solution to the nitric acid solution is 10; the nitric acid solution is prepared by concentrated nitric acid and water with the volume ratio of 1.
And (3) transferring 20.0mL of filtrate into a 50mL colorimetric tube, adding 5.0mL of nitric acid solution, 5.0mL of glycerol solution and 2.0mL of silver nitrate solution with the concentration of 17g/L into the filtrate, fixing the volume by using water, uniformly mixing, placing in the shade, and standing for 20min to obtain the sample to be detected. The nitric acid solution is prepared by concentrated nitric acid and water with the volume ratio of 1; the glycerol solution is prepared by mixing glycerol and water in a volume ratio of 1.
Preparing a standard solution: a) Chloride ion standard stock solution: weighing 1.6488g of sodium chloride burned at 550 ℃, putting the sodium chloride into a beaker, adding water to dissolve the sodium chloride, and metering the volume of the solution into a 1000mL volumetric flask, wherein 1mL of the solution contains chloride ions and the magnesium is left on the magnesium. b) Chloride ion standard solution: 20.00mL of the standard stock solution of chloride ions was transferred to a 500mL volumetric flask and the volume was determined by water, and 1mL of the solution containing chloride ions was measured on a mg.
Transferring 6 parts of 20mL of sample filtrate to be detected, respectively placing the filtrate in 50mL of colorimetric tubes, and sequentially adding 0.00mL, 1.00 mL, 2.00 mL, 3.00 mL, 4.00 mL and 5.00mL of chloride ion standard solution according to the sample determination method. And drawing a working curve by taking the chloride ion content as an abscissa and the absorbance as an ordinate.
And (3) performing a sample blank test and a reagent blank test, and measuring the content of chloride ions at a wavelength of 420nm by using a TU-1950 double-beam ultraviolet-visible spectrophotometer in a 3cm quartz cuvette and taking a reagent blank sample as a reference. And automatically obtaining the corresponding mass concentration of the chloride ions in the cobaltosic oxide to be detected from the working curve according to the standard working curve value, wherein the detection result is shown in a table 2. The sample blank test comprises the following steps: transferring 20.0mL of the filtrate into a 50mL colorimetric tube, adding 5.0mL of nitric acid solution and 5.0mL of glycerol solution into the filtrate, and fixing the volume with water. The reagent blank test is carried out as follows: transferring 20.0mL of the filtrate into a 50mL colorimetric tube, adding 5.0mL of nitric acid solution, 5.0mL of glycerol solution and 2.0mL of silver nitrate solution with the concentration of 17g/L into the filtrate, fixing the volume with water, shaking uniformly, and standing in a dark place for 20min.
The chloride ion content of the sample was calculated as follows:
in the formula: m is 1 -the amount of chloride ions, μ g, found from the working curve;
m 0 -amount of test material, g.
Table 2 test results of example 2 repeated 6 times
In the embodiment 1, 2g/L silver nitrate is adopted to perform experiment comparison with the embodiment 2, 17g/L silver nitrate is adopted, the content of chloride ions is basically consistent, and the content is shown in tables 1 and 2, so that the detection result is not influenced by the concentration of the silver nitrate.
Example 3
Weighing 8 parts of a test material (cobaltosic oxide batch number KL 2010050), placing the test material into 250mL beakers with the numbers of 1#, 2#, 3#, 4#, 5#, 6#, 7#, and 8#, respectively adding 50mL of water, sequentially adding 5.0mL of chloride ion standard solution into the 3#, 4#, and 5# beakers, sequentially adding 20.0mL of chloride ion standard solution into the 6#, 7# and 8# beakers, placing 8 beakers on an electric heating plate, heating to boil, dissolving at a low temperature for 20 minutes, taking down, slightly cooling, adding 10mL of nitric acid (1 + 1), and cooling. The resulting solution together with the precipitate was transferred to a 100mL volumetric flask, made up to volume with water and filtered in the original beaker with filter paper.
Transferring 20.0mL of filtrate into a 50mL colorimetric tube, adding 5.0mL of nitric acid, adding 5.0mL of glycerol solution, adding 2.0mL of silver nitrate solution, fixing the volume with water, shaking uniformly, placing in a dark place for 20min, and measuring the content of chloride ions in a position with a wavelength of 420nm by using a reagent blank as a reference in a 3cm cuvette by using a TU-1950 double-beam ultraviolet-visible spectrophotometer. The mass concentration of the corresponding chloride ions was automatically obtained from the working curve in example 1, and the recovery rate of the chloride ions was calculated from the concentration of the added chloride ions and is shown in Table 3, and the results in Table 3 show that the recovery rate is within the acceptable range.
TABLE 3 tagged recovery measured data
| Standard addition of chloride ion mg/L | +0.00 | +40.00 | 160.00 |
| Measurement value mg/L (average value) | 100.89 | 42.96 | 155.28 |
| The recovery rate is high | - | 107.40 | 97.05 |
Example 4
Weighing 11 parts of a sample (cobaltosic oxide batch number KL 2010050), respectively placing the sample in 250mL beakers, respectively adding 50mL of water, placing the beakers on an electric hot plate, heating the beakers to boil, dissolving the beakers at a low temperature for 20 minutes, taking down the beakers, slightly cooling the beakers, adding 10.0mL of nitric acid (1 + 1), and cooling the beakers. The resulting solution was transferred into a 100mL volumetric flask together with the precipitate, made up to volume with water and filtered in the original beaker with filter paper.
Transferring 20.0mL of the filtered filtrate into a 50mL colorimetric tube, adding 5.0mL of nitric acid (1 + 1), adding 5.0mL of glycerol solution, adding 2.0mL of silver nitrate solution, fixing the volume with water, shaking uniformly, placing in a dark place for 20min, taking a reagent blank as a reference in a 3cm cuvette, and measuring the content of chloride ions at a wavelength of 420nm by using a TU-1950 double-beam ultraviolet-visible spectrophotometer. The corresponding mass concentration of the chloride ions was automatically obtained from the working curve in example 1, and statistics of the content measurement results of the chloride ions calculated from the mass concentration of the chloride ions are shown in Table 4. The relative standard deviation of the 11 detection results is 2.61%, which is shown in Table 4 and meets the precision requirement.
TABLE 4 summary of precision testing statistics and measurements
Claims (3)
1. A method for measuring the content of chloride ions in cobaltosic oxide by using a two-beam turbidimetry method, which is characterized by comprising the following steps:
(1) Adding cobaltosic oxide to be detected into deionized water, stirring uniformly, heating to boil, dissolving at 95-100 ℃ for 20-30 min, and cooling to room temperature to obtain a mixed solution; the solid-liquid ratio of cobaltosic oxide to deionized water to be detected is 1 (20-25);
(2) Adding a nitric acid solution into the mixed solution, shaking uniformly, standing for 20-30 min, and filtering to obtain a filtrate; the volume ratio of the mixed solution to the nitric acid solution is (10-15): 1;
(3) Adding a nitric acid solution, a glycerol solution and a silver nitrate solution into the filtrate, and standing for 20-30 min in the shade to obtain a sample to be detected; the volume ratio of the filtrate to the nitric acid solution to the glycerol solution to the silver nitrate solution is (10-15): 2.5-3): 1; the concentration of the silver nitrate solution is 2g/L-6g/L;
(4) Transferring the filtrate obtained in the step (2) into a colorimetric tube, adding a chloride ion working standard solution into the colorimetric tube containing the filtrate, and then performing the step (3) to obtain a filtrate containing the chloride ion working standard solution; drawing a standard working curve by taking the chloride ion content in the filtrate containing the chloride ion working standard solution as an abscissa and the absorbance as an ordinate;
(5) Carrying out color comparison on a sample to be detected on an ultraviolet spectrophotometer at a wavelength of 420nm, simultaneously carrying out a sample blank test and a reagent blank test, and calculating to obtain the content of chloride ions in cobaltosic oxide to be detected according to a standard working curve value; the reagent blank test comprises the following steps: adding a nitric acid solution, a glycerol solution and a silver nitrate solution into the filtrate, uniformly mixing, placing the mixture in the shade, and standing for 20-30 min to obtain a reagent blank sample; the volume ratio of the filtrate to the nitric acid solution to the glycerol solution to the silver nitrate solution is (10-15): 2.5-3): 1.
2. The method for determining the chloride ion content of cobaltosic oxide by using the two-beam turbidimetry as claimed in claim 1, wherein the nitric acid solution in the step (2) and the nitric acid solution in the step (3) are both prepared from concentrated nitric acid and water in a volume ratio of 1; the glycerol solution in the step (3) is prepared by glycerol and water with the volume ratio of 1.
3. The method for determining the chloride ion content of cobaltosic oxide by two-beam turbidimetry according to claim 1, wherein the concentration of the chloride ion working standard solution in step (4) is from 0.04mg/mL to 0.2mg/mL.
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