CN112098350A - Method for detecting concentration of soluble sulfate ions in sanitary ceramic slurry - Google Patents
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Abstract
The invention discloses a method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry, which comprises the following steps: taking sanitary ceramic slurry, carrying out high-pressure filtration on the sanitary ceramic slurry, and collecting filtrate to obtain high-pressure filtrate; preparing a barium sulfate standard curve solution; detecting the absorbance of the solution of the standard curve by using a spectrophotometer, and drawing a barium sulfate standard curve; filtering the high-pressure filtrate, removing solid impurities in the high-pressure filtrate, sucking the filtered high-pressure filtrate into a volumetric flask, adding a hydrochloric acid solution and a glycerol solution, fixing the volume by using distilled water, adding a barium chloride solid after shaking up, and fully shaking until the barium chloride solid in the solution is completely dissolved to obtain a solution to be detected; and detecting the absorbance of the solution to be detected by using a spectrophotometer, and calculating the concentration of soluble sulfate ions in the sanitary ceramic slurry according to the drawn standard sulfate curve. The detection method has the characteristics of simple operation, time saving, accuracy, good stability and wide linear range.
Description
Technical Field
The invention relates to a detection method of sanitary ceramic slurry, in particular to a method for detecting the concentration of soluble sulfate ions in the sanitary ceramic slurry.
Background
The sanitary ceramic slurry usually contains sulfate ions, and the concentration of the sulfate ions influences the fluidity of the sanitary ceramic slurry; if the concentration of sulfate ions in the sanitary ceramic slurry is high, the fluidity of the sanitary ceramic slurry is reduced, and pores on the glaze surface of a product are increased. In the production process of sanitary ceramics, the concentration of sulfate ions is reduced mainly by adjusting the adding amount of electrolyte in the sanitary ceramics slurry. However, the method for rapidly detecting the concentration of soluble sulfate ions in the sanitary ceramic slurry is lacked at present, and the addition of electrolyte in the sanitary ceramic slurry is difficult to adjust through the concentration of the sulfate ions.
Disclosure of Invention
The invention aims to provide a method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry, which solves the problem that the concentration of the soluble sulfate ions in the sanitary ceramic slurry is difficult to detect quickly.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry, which comprises the following steps:
step 1: taking sanitary ceramic slurry, carrying out high-pressure filtration on the sanitary ceramic slurry, and collecting filtrate to obtain high-pressure filtrate;
step 2: preparing a barium sulfate standard curve solution;
and step 3: detecting the absorbance of the standard curve solution in the step 2 by using a spectrophotometer, and drawing a barium sulfate standard curve;
and 4, step 4: filtering the high-pressure filtrate, removing solid impurities in the high-pressure filtrate, sucking the filtered high-pressure filtrate into a volumetric flask, adding a hydrochloric acid solution and a glycerol solution, fixing the volume by using distilled water, adding a barium chloride solid after shaking up, and fully shaking until the barium chloride solid in the solution is completely dissolved to obtain a solution to be detected;
and 5: and (4) detecting the absorbance of the solution to be detected in the step (4) by using a spectrophotometer, and calculating the concentration of soluble sulfate ions in the sanitary ceramic slurry according to the standard sulfate curve drawn in the step (3).
In the method for detecting the concentration of the soluble sulfate ions in the sanitary ceramic slurry, the detection wavelength of the spectrophotometer is 550 nm.
In the method for detecting the concentration of soluble sulfate ions in the sanitary ceramic slurry, the concentration calculation formula of the sulfate ions in the sanitary ceramic slurry is as follows:
sulfate ion concentration (ppm) of sanitary ceramic slurry (Cx 10 x sulfate factor)
Wherein c is the concentration of sulfate ions in the solution to be detected;
the sulfate factor is the ratio of the water content to the solid content in the sanitary ceramic slurry.
In the method for detecting the concentration of the soluble sulfate ions in the sanitary ceramic slurry, in the step 1, the pressure of high-pressure filtration is 0.3MPa, and the time of the high-pressure filtration is 2-5 h.
In the method for detecting the concentration of the soluble sulfate ions in the sanitary ceramic slurry, the concentration of the hydrochloric acid solution in the step 4 is 1.000mol/L, and the using amount is 3 ml; the concentration of the glycerol is 50%, and the dosage is 5 ml; the purity of barium chloride was analytical grade, and the amount used was 0.3 g.
In the method for detecting the concentration of the soluble sulfate ions in the sanitary ceramic slurry, the absorption volume of the filtered solution to be detected in the step 4 is 5 ml; the capacity of the volumetric flask in step 3 was 50 ml.
In the method for detecting the concentration of the soluble sulfate ions in the sanitary ceramic slurry, the preparation of the barium sulfate standard curve solution in the step 2 comprises the following steps:
step 2.1: sequentially sucking 0.00 ml, 1.25 ml, 2.50 ml, 3.75 ml and 5.00ml of sulfate standard solution, and respectively placing the standard solution in 550 ml volumetric flasks;
step 2.2: respectively adding 3mL of 1.000mol/L hydrochloric acid solution and 5mL of 50% glycerol solution into the volumetric flask in the step 2.1, fixing the volume by using distilled water, and shaking up;
step 2.3: and (3) adding 0.3g of barium chloride into the volumetric flask with the constant volume in the step 2.2, and fully shaking until the barium chloride solid in the solution is completely dissolved.
In the method for detecting the concentration of the soluble sulfate ions in the sanitary ceramic slurry, distilled water is used for fixing the volume in the step 4 and the step 2.2, and the sanitary ceramic slurry needs to be kept stand at room temperature for 10-20 min after being shaken up.
In the method for detecting the concentration of soluble sulfate ions in the sanitary ceramic slurry, the concentration of sulfate ions in the standard sulfate solution is as follows: c (SO)4 2-)＝1.000g/L。
Has the advantages that:
(1) the detection method has the characteristics of simple operation, time saving, accuracy, good stability and wide linear range, and the solution medium is water, so that the determination of a spectrophotometer cannot be interfered;
(2) the detection method can simulate the sanitary ceramic high-pressure grouting forming process in a laboratory, judge the grouting efficiency of the high-pressure slurry through the filter pressing speed, and provide direction for parameter adjustment of the high-pressure slurry.
Drawings
The drawings are further illustrative of the invention and the content of the drawings does not constitute any limitation of the invention.
FIG. 1 is a standard curve of barium sulfate concentration plotted in example 1 of the present invention;
FIG. 2 is a standard curve of barium sulfate concentration plotted in example 2 of the present invention;
FIG. 3 is a standard curve of the barium sulfate concentration plotted in example 3 of the present invention.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The invention discloses a method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry, which comprises the following steps:
step 1: taking sanitary ceramic slurry, carrying out high-pressure filtration on the sanitary ceramic slurry, and collecting filtrate to obtain high-pressure filtrate;
step 2: preparing a barium sulfate standard curve solution;
and step 3: detecting the absorbance of the standard curve solution in the step 2 by using a spectrophotometer, and drawing a barium sulfate standard curve;
and 4, step 4: filtering the high-pressure filtrate, removing solid impurities in the high-pressure filtrate, sucking the filtered high-pressure filtrate into a volumetric flask, adding a hydrochloric acid solution and a glycerol solution, fixing the volume by using distilled water, adding a barium chloride solid after shaking up, and fully shaking until the barium chloride solid in the solution is completely dissolved to obtain a solution to be detected;
and 5: and (4) detecting the absorbance of the solution to be detected in the step (4) by using a spectrophotometer, and calculating the concentration of soluble sulfate ions in the sanitary ceramic slurry according to the standard sulfate curve drawn in the step (3).
In the method for detecting the concentration of the soluble sulfate ions in the sanitary ceramic slurry, the soluble sulfate ions are converted into barium sulfate, the concentration of the barium sulfate in the solution to be detected is measured by a spectrophotometry, and the concentration of the soluble sulfate ions in the sanitary ceramic slurry can be obtained by formula conversion. The detection method has the characteristics of simple operation, time saving, accuracy, good stability and wide linear range, and the solution medium is water, so that the determination of a spectrophotometer cannot be interfered.
Although barium sulfate is almost insoluble in water, because the concentration of soluble sulfate ions in the solution to be detected is small, a large amount of precipitate cannot be formed immediately after barium chloride is added, and the precipitate is accumulated in a volumetric flask; but forms fine particles, so that the solution after constant volume becomes turbid; and is capable of absorbing a portion of the light source emitted by the spectrophotometer. And (3) obtaining a linear regression equation of the concentration and the absorbance of the barium sulfate standard curve solution by setting the barium sulfate standard curve solution, and calculating to obtain the concentration of barium sulfate in the solution to be detected.
Before the constant volume, the high-pressure filtrate needs to be filtered, so that the problem that the high-pressure filtrate contains other insoluble substances when no barium chloride solid is added is avoided, and the deviation of sulfate ion concentration caused by the fact that the absorbance of the solution to be measured is changed by the other insoluble substances is prevented. In a specific example, the high pressure filtrate was filtered by means of atmospheric filtration using filter paper.
Specifically, the detection wavelength of the spectrophotometer is 550 nm. When the wavelength is 550nm, the barium sulfate solution can selectively absorb the light with the wavelength; through the analysis of a spectrophotometer, the concentration of barium sulfate in the solution to be detected can be quantitatively analyzed when the wavelength is 550nm, so that the concentration of soluble sulfate ions in the solution to be detected is obtained.
Specifically, the calculation formula of the concentration of sulfate ions in the sanitary ceramic slurry is as follows:
sulfate ion concentration (ppm) of sanitary ceramic slurry (Cx 10 x sulfate factor)
Wherein c is the concentration of sulfate ions in the solution to be detected;
the sulfate factor is the ratio of the water content to the solid content in the sanitary ceramic slurry.
After the concentration of the sulfate ions in the solution to be detected is obtained by the detection method, the concentration of the sulfate ions in the solution to be detected is substituted into the concentration calculation formula, and the concentration of the soluble sulfate ions in the sanitary ceramic slurry can be obtained. Wherein, the coefficient "10" is the volume multiple of the solution to be measured.
Specifically, in the step 1, the pressure of the high-pressure filtration is 0.3MPa, and the time of the high-pressure filtration is 2-5 h. The sanitary ceramic slurry contains a large amount of components which are insoluble in water, so that the water in the sanitary ceramic slurry can be completely filtered out only by high-pressure filtration with the pressure of 0.3MPa, and the problem that the soluble sulfate ions in the sanitary ceramic slurry are not uniformly dissolved, so that part of filtrate containing the soluble sulfate ions is remained in filter residues to cause measurement errors.
Specifically, the concentration of the hydrochloric acid solution in the step 4 is 1.000mol/L, and the dosage is 3 ml; the concentration of the glycerol is 50%, and the dosage is 5 ml; the purity of barium chloride was analytical grade, and the amount used was 0.3 g.
Specifically, the suction volume of the filtered solution to be detected in the step 4 is 5 ml; the capacity of the volumetric flask in step 3 was 50 ml. Barium chloride reacts with soluble sulfate ions to produce barium sulfate. The hydrochloric acid plays a role in reducing the pH value of the solution to be detected, so that the solution to be detected is kept in an acidic state, and barium ions in the solution to be detected are prevented from reacting with hydroxyl to produce barium hydroxide. The glycerol plays a role in solubilizing and preventing the barium sulfate from forming a precipitate before measurement. In order to prevent the waste of the reagent and the absorbance of the solution to be tested from exceeding the test range of the spectrophotometer, only 5ml of filtered solution to be tested needs to be sucked and diluted by 10 times for the test of the spectrophotometer.
Specifically, the preparation of the barium sulfate standard curve solution in the step 2 comprises the following steps:
step 2.1: sequentially sucking 0.00 ml, 1.25 ml, 2.50 ml, 3.75 ml and 5.00ml of sulfate standard solution, and respectively placing the standard solution in 550 ml volumetric flasks;
step 2.2: respectively adding 3mL of hydrochloric acid solution with the concentration of 1.000mol/L and 5mL of glycerol solution with the concentration of 50% into the volumetric flask in the step 2.1, fixing the volume by using distilled water, and shaking up;
step 2.3: and (3) adding 0.3g of barium chloride into the volumetric flask with the constant volume in the step 2.2, and fully shaking until the barium chloride solid in the solution is completely dissolved.
In a specific embodiment, the barium sulfate standard curve solution settings set five different concentrations, including 0ppm, 25ppm, 50ppm, 75ppm, and 100 ppm; and measuring by a spectrophotometer to obtain respective absorbance, and drawing a barium sulfate standard curve. From lambert beer's law, a linear regression equation can be derived (C ═ K × a + B, where C is concentration, K is slope, a is absorbance, and B is intercept). And obtaining the concentration of barium sulfate in the solution to be detected through the absorbance of the solution to be detected, so as to obtain the concentration of soluble sulfate ions in the solution to be detected.
According to a single variable method, in order to avoid errors caused by reagents such as hydrochloric acid, glycerol and barium chloride on the test of a spectrophotometer, the dosage and concentration of hydrochloric acid, the dosage and concentration of glycerol and the dosage and purity of barium chloride need to be consistent with those of a solution to be tested. It should be noted that when a standard curve is formulated, the r value of the standard curve should be between 0.999 and 1.000; the r value is a correlation coefficient of a standard curve and represents the amount of linear correlation degree between absorbance and concentration, and when the r value is closer to 1, the relationship between the absorbance and the concentration is closer to the linear relationship, the higher the coincidence degree is, and the more accurate the detection result is; the closer the r value is to 0, the lower the coincidence degree between the absorbance and the concentration is, which proves that the standard curve is interfered by other reasons and is inaccurate, so that the detection result is inaccurate.
The calculation formula of the r value is as follows:
wherein: e (X), E (Y) are the average values of X, Y respectively; d (x), D (y) are the variances of X, Y, respectively.
Specifically, in the step 4 and the step 2.2, the volume is determined by distilled water, and after shaking up, the mixture needs to be kept stand at room temperature for 10-20 min. After the volume is fixed, the volumetric flask needs to be shaken and kept stand at room temperature for 10-20 min, so that the barium chloride and the soluble sulfate ions are fully reacted.
Specifically, the sulfate radical concentration in the sulfate standard solution is as follows: c (SO)4 2-)＝1.000g/L。
For convenience of calculation, the concentration of the sulfate standard solution was 1.000 g/L. The preparation method of the 1.000g/L sulfate standard solution comprises the following steps: drying potassium sulfate at 110 ℃ for 2h, accurately weighing 1.8141g of potassium sulfate, and dissolving in 1000ml of water.
Example 1
Step 1: taking sanitary ceramic slurry, detecting that the slurry specific gravity of the sanitary ceramic slurry is 1.770, pouring 1000ml of the sanitary ceramic slurry into a filter pressing device, filtering for 3 hours under high pressure at the pressure of 0.3MPa, and collecting 100ml of filtrate.
Step 2: sequentially sucking 0.00 ml, 1.25 ml, 2.50 ml, 3.75 ml and 5.00ml of sulfate standard solution, and respectively placing the standard solution in 550 ml volumetric flasks;
respectively adding 3mL of hydrochloric acid solution with the concentration of 1.000mol/L and 5mL of glycerol solution with the concentration of 50% into a volumetric flask, fixing the volume to a scale with distilled water, and shaking up;
and adding 0.3g of barium chloride into the volumetric flask after constant volume, fully shaking until the barium chloride solid in the solution is completely dissolved, and standing for 10min at room temperature.
And step 3: and (3) detecting the absorbance of the sample solution by using a spectrophotometer, wherein the detection wavelength is 550nm, the absorbance obtained by detection is shown in table 1, drawing a standard curve according to the absorbance obtained by detection and the corresponding concentration of barium sulfate in the sample solution, and obtaining a linear regression equation according to the Lambert beer law: c ═ 202.8 × a +13.97, where a is absorbance and C is the concentration of barium sulfate in the sample solution (in ppm).
TABLE 1 results of absorbance test at wavelength 550nm for each barium sulfate concentration
According to the results of the absorbance test in table 1, a standard curve of the barium sulfate concentration is drawn, please refer to fig. 1.
And 4, step 4: filtering the high-pressure filtrate by using medium-speed qualitative filter paper to remove solid impurities in the solution. Accurately sucking 5.0ml of filtered high-pressure filtrate into a 50ml volumetric flask, washing the flask wall with a little water, adding 3ml of hydrochloric acid solution and 5ml of glycerol solution, diluting with water to a scale, shaking uniformly, carefully adding 0.3g of barium chloride into the solution, fully shaking until the barium chloride solid in the solution is completely dissolved, and standing at room temperature for 10 min.
And 5: and (3) detecting the absorbance of the solution to be detected by using a spectrophotometer, wherein the detection wavelength is 550nm, the absorbance value is 0.272, and the barium sulfate concentration of the filtrate to be detected is 69.1ppm by calculating a linear regression equation in the step 3.
Calculation of analysis results: substituting the calculated barium sulfate concentration of the filtrate to be measured of 69.1ppm into the following formula:
sulfate ion concentration (ppm) in the slurry c × 10 × sulfate factor
The specific gravity of the sanitary ceramic slurry is 1.770, and the formula is calculated according to the solid content in the slurry:
the solid content in the mud of the sanitary ceramic mud can be obtained, wherein S is the mud proportion;
wherein the water content in the slurry is 1-the solid content in the slurry
By calculation, the sulphate factor was 0.4146, giving a concentration of 286.62ppm soluble sulphate calculated.
The filtrate collected in step 1 of this example was analyzed by ion mass spectrometry, and the result showed that the concentration of sulfate in the filtrate was 287.86ppm, which is close to the analysis result of this example, and the relative error of the analysis result was < 1%, thus, the analysis result of this example is accurate and reliable, the method has less investment and low analysis cost.
Example 2
Step 1: taking sanitary ceramic slurry, detecting that the slurry specific gravity of the sanitary ceramic slurry is 1.770, pouring 1000ml of the sanitary ceramic slurry into a filter pressing device, filtering for 2 hours under high pressure at 0.3MPa, and collecting 100ml of filtrate.
Step 2: sequentially sucking 0.00 ml, 1.25 ml, 2.50 ml, 3.75 ml and 5.00ml of sulfate standard solution, and respectively placing the standard solution in 550 ml volumetric flasks;
respectively adding 3mL of hydrochloric acid solution with the concentration of 1.000mol/L and 5mL of glycerol solution with the concentration of 50% into a volumetric flask, fixing the volume to a scale with distilled water, and shaking up;
and adding 0.3g of barium chloride into the volumetric flask after constant volume, fully shaking until the barium chloride solid in the solution is completely dissolved, and standing for 10min at room temperature.
And step 3: and (3) detecting the absorbance of the sample solution by using a spectrophotometer, wherein the detection wavelength is 550nm, the absorbance obtained by detection is shown in table 1, drawing a standard curve according to the absorbance obtained by detection and the corresponding concentration of barium sulfate in the sample solution, and obtaining a linear regression equation according to the Lambert beer law: c ═ 202.8 × a +13.88, where a is absorbance and C is the concentration of barium sulfate in the sample solution (in ppm).
TABLE 2 Absorbance test results at wavelength 550nm for each barium sulfate concentration
According to the results of the absorbance test in table 2, a standard curve of the barium sulfate concentration is drawn, please refer to fig. 2.
And 4, step 4: filtering the high-pressure filtrate by using medium-speed qualitative filter paper to remove solid impurities in the solution. Accurately sucking 5.0ml of filtered high-pressure filtrate into a 50ml volumetric flask, washing the flask wall with a little water, adding 3ml of hydrochloric acid solution and 5ml of glycerol solution, diluting with water to a scale, shaking uniformly, carefully adding 0.3g of barium chloride into the solution, fully shaking until the barium chloride solid in the solution is completely dissolved, and standing at room temperature for 10 min.
And 5: and (3) detecting the absorbance of the solution to be detected by using a spectrophotometer, wherein the detection wavelength is 550nm to obtain an absorbance value of 0.274, and calculating by using a linear regression equation in the step 3 to obtain the barium sulfate concentration of the filtrate to be detected of 69.4 ppm.
Calculation of analysis results: substituting the calculated barium sulfate concentration of the filtrate to be measured of 69.4ppm into the following sulfate ion concentration formula in the slurry:
sulfate ion concentration (ppm) in the slurry c × 10 × sulfate factor
The sanitary ceramic slurry has the same slurry specific gravity as that of the sanitary ceramic slurry in example 1, which is 1.770, so that the sulfate factor in example 2 is 0.4146; substituting into the sulfate ion concentration formula in the slurry to calculate the concentration of the soluble sulfate to 287.73 ppm.
The filtrate collected in step 1 of this example was analyzed by ion mass spectrometry, and the result showed that the concentration of sulfate in the filtrate was 287.86ppm, which is close to the analysis result of this example, and the relative error of the analysis result was < 1%, thus, the analysis result of this example is accurate and reliable, the method has less investment and low analysis cost.
Example 3
Step 1: taking the sanitary ceramic slurry, detecting that the slurry specific gravity of the sanitary ceramic slurry is 1.770, pouring 1000ml of the sanitary ceramic slurry into a filter pressing device, filtering for 5 hours under high pressure at the pressure of 0.3MPa, and collecting 100ml of filtrate.
Step 2: sequentially sucking 0.00 ml, 1.25 ml, 2.50 ml, 3.75 ml and 5.00ml of sulfate standard solution, and respectively placing the standard solution in 550 ml volumetric flasks;
respectively adding 3mL of hydrochloric acid solution with the concentration of 1.000mol/L and 5mL of glycerol solution with the concentration of 50% into a volumetric flask, fixing the volume to a scale with distilled water, and shaking up;
and adding 0.3g of barium chloride into the volumetric flask after constant volume, fully shaking until the barium chloride solid in the solution is completely dissolved, and standing for 20min at room temperature.
And step 3: and (3) detecting the absorbance of the sample solution by using a spectrophotometer, wherein the detection wavelength is 550nm, the absorbance obtained by detection is shown in table 1, drawing a standard curve according to the absorbance obtained by detection and the corresponding concentration of barium sulfate in the sample solution, and obtaining a linear regression equation according to the Lambert beer law: c ═ 202.8 × a +13.67, where a is absorbance and C is the concentration of barium sulfate in the sample solution (in ppm).
TABLE 3 Absorbance test results at wavelength 550nm for each barium sulfate concentration
According to the results of the absorbance test in Table 3, a standard curve of the barium sulfate concentration was plotted, please refer to FIG. 3.
And 4, step 4: filtering the high-pressure filtrate by using medium-speed qualitative filter paper to remove solid impurities in the solution. Accurately sucking 5.0ml of filtered high-pressure filtrate into a 50ml volumetric flask, washing the flask wall with a little water, adding 3ml of hydrochloric acid solution and 5ml of glycerol solution, diluting with water to a scale, shaking uniformly, carefully adding 0.3g of barium chloride into the solution, fully shaking until the barium chloride solid in the solution is completely dissolved, and standing at room temperature for 20 min.
And 5: and (3) detecting the absorbance of the solution to be detected by using a spectrophotometer, wherein the detection wavelength is 550nm to obtain an absorbance value of 0.277, and calculating by using a linear regression equation in the step 3 to obtain the barium sulfate concentration of the filtrate to be detected of 69.8 ppm.
Calculation of analysis results: substituting the barium sulfate concentration of the filtrate to be measured, which is obtained by the calculation, into the following sulfate ion concentration formula in the slurry, wherein the barium sulfate concentration is 69.8 ppm:
sulfate ion concentration (ppm) in the slurry c × 10 × sulfate factor
The sanitary ceramic slurry has the same slurry specific gravity as that of the sanitary ceramic slurry in example 1, which is 1.770, so that the sulfate factor in example 2 is 0.4146; substituting into the sulfate ion concentration formula in the slurry to calculate the concentration of the soluble sulfate to 289.39 ppm.
The filtrate collected in step 1 of this example was analyzed by ion mass spectrometry, and the result showed that the concentration of sulfate in the filtrate was 287.86ppm, which is close to the analysis result of this example, and the relative error of the analysis result was < 1%, thus, the analysis result of this example is accurate and reliable, the method has less investment and low analysis cost.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Other embodiments of the invention will occur to those skilled in the art without the exercise of inventive faculty based on the explanations herein, and such equivalent modifications or substitutions are intended to be included within the scope of the present invention as defined in the appended claims.
Claims (9)
1. A method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry is characterized by comprising the following steps: the method comprises the following steps:
step 1: taking sanitary ceramic slurry, carrying out high-pressure filtration on the sanitary ceramic slurry, and collecting filtrate to obtain high-pressure filtrate;
step 2: preparing a barium sulfate standard curve solution;
and step 3: detecting the absorbance of the standard curve solution in the step 2 by using a spectrophotometer, and drawing a barium sulfate standard curve;
and 4, step 4: filtering the high-pressure filtrate, removing solid impurities in the high-pressure filtrate, sucking the filtered high-pressure filtrate into a volumetric flask, adding a hydrochloric acid solution and a glycerol solution, fixing the volume by using distilled water, adding a barium chloride solid after shaking up, and fully shaking until the barium chloride solid in the solution is completely dissolved to obtain a solution to be detected;
and 5: and (4) detecting the absorbance of the solution to be detected in the step (4) by using a spectrophotometer, and calculating the concentration of soluble sulfate ions in the sanitary ceramic slurry according to the standard sulfate curve drawn in the step (3).
2. The method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry as claimed in claim 1, wherein: the detection wavelength of the spectrophotometer is 550 nm.
3. The method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry as claimed in claim 1, wherein: the concentration calculation formula of sulfate ions in the sanitary ceramic slurry is as follows:
sulfate ion concentration (ppm) of sanitary ceramic slurry (Cx 10 x sulfate factor)
Wherein c is the concentration of sulfate ions in the solution to be detected;
the sulfate factor is the ratio of the water content to the solid content in the sanitary ceramic slurry.
4. The method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry as claimed in claim 1, wherein: in the step 1, the pressure of the high-pressure filtration is 0.3MPa, and the time of the high-pressure filtration is 2-5 h.
5. The method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry as claimed in claim 1, wherein: in the step 4, the concentration of the hydrochloric acid solution is 1.000mol/L, and the dosage is 3 ml; the concentration of the glycerol is 50%, and the dosage is 5 ml; the purity of barium chloride was analytical grade, and the amount used was 0.3 g.
6. The method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry as claimed in claim 5, wherein: the suction volume of the filtered solution to be detected in the step 4 is 5 ml; the capacity of the volumetric flask in step 3 was 50 ml.
7. The method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry as claimed in claim 1, wherein: the preparation of the barium sulfate standard curve solution in the step 2 comprises the following steps:
step 2.1: sequentially sucking 0.00 ml, 1.25 ml, 2.50 ml, 3.75 ml and 5.00ml of sulfate standard solution, and respectively placing the standard solution in 550 ml volumetric flasks;
step 2.2: respectively adding 3mL of 1.000mol/L hydrochloric acid solution and 5mL of 50% glycerol solution into the volumetric flask in the step 2.1, fixing the volume by using distilled water, and shaking up;
step 2.3: and (3) adding 0.3g of barium chloride into the volumetric flask with the constant volume in the step 2.2, and fully shaking until the barium chloride solid in the solution is completely dissolved.
8. The method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry as claimed in claim 7, wherein: and in the step 4 and the step 2.2, the volume is determined by distilled water, and after shaking up, the mixture needs to be kept stand at room temperature for 10-20 min.
9. The method for detecting the concentration of soluble sulfate ions in sanitary ceramic slurry as claimed in claim 7, wherein: the sulfate radical concentration of the sulfate standard solution is as follows: c (SO)4 2-)＝1.000g/L。
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