CN113049706A - Method for analyzing and measuring chloride ions in process refrigerant - Google Patents
Method for analyzing and measuring chloride ions in process refrigerant Download PDFInfo
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Abstract
The invention discloses a method for analyzing and measuring chloride ions in a process refrigerant, which can realize accurate analysis of impurity chloride ions in the refrigerant and has higher accuracy and precision. The method comprises the steps of burning a refrigerant sample at a high temperature, boiling, dissolving and fixing the volume, and measuring a sample solution by adopting an ion chromatograph. The method comprises the following steps: (1) firing a refrigerant; (2) setting ion chromatography operating conditions; (3) drawing a standard working curve; (4) measuring the peak area of the sample solution; (5) and calculating the content of the chloride ions in the sample according to the peak area value of the solution and the working curve. Under the optimized experimental conditions, the mass concentration of the chloride ions is in a good linear relation with the peak area within the range of 0.00-1.20 mg/L, and the correlation coefficient is 0.99991. The detection limit of the chlorine method is 0.008mg/L, the quantification limit is 0.08mg/L, the relative standard deviation of the measurement result is 1.7-2.9% (n is 6), the sample standard addition recovery rate is 90.0-96.7%, and the method can be used for measuring the content of chloride ions in the refrigerant.
Description
Technical Field
The invention belongs to the field of analysis and detection, and particularly relates to an analysis and determination method for chloride ions in an industrial refrigerant.
Background
The refrigerant of the inlet air cooler of the gas turbine and air compressor takes 25% glycol solution as a medium, and various impurities including corrosive chloride ions can be brought into the refrigerant in the operation process. The chloride ions have the characteristics of small ionic radius, strong penetrating power and strong adsorption by the metal surface, so that the higher the chloride ion concentration is, the higher the conductivity of the aqueous solution becomes, the lower the resistance of the electrolyte is, the easier the chloride ions reach the metal surface, a chloride salt layer can be formed on the metal surface in an acid environment to replace an oxide film with a protective property, and the high pitting rate is caused. In order to prevent the impurity chlorine in the refrigerant from corroding the stainless steel equipment, the content of the chloride ions in the refrigerant is required to be measured, so that the refrigerant can be replaced in time when the content of the chloride ions is more than 50mg/L, and the corrosion of the equipment is avoided.
The current analytical methods for measuring chloride ions in industrial ethylene glycol comprise ion chromatography used in GB/T14571.5 and a turbidimetric method used in GB/T4649-2018. The ion chromatography directly enters the industrial ethylene glycol with the purity of more than 99.0 percent into the ion chromatography for analysis; the turbidimetric method is a method in which chloride ions in a sample are directly reacted with silver nitrate to produce a white silver chloride precipitate, and then turbidimetric reaction is performed with a standard solution. Because the content of ethylene glycol in the refrigerant is only 25 percent and various impurities are brought in during the operation process, a plurality of impurity peaks appear after the refrigerant is directly subjected to ion chromatographic analysis, and the concentration of chloride ions in the refrigerant is difficult to accurately determine; the concentration of the chloride ions in the ethylene glycol can only be roughly measured by adopting a turbidimetric method, and the accurate content cannot be obtained.
Disclosure of Invention
The invention aims to provide an analysis and determination method for chloride ions in a process refrigerant, which has high accuracy and good reproducibility, adopts a high-temperature digestion method to prepare samples, and adopts an ion chromatography method to determine the content of the chloride ions in the samples, thereby realizing the accurate analysis of the chloride ions as impurities in the refrigerant.
In order to achieve the purpose, the technical scheme of the invention is as follows: the method for analyzing and measuring chloride ions in a process refrigerant comprises the following steps:
s1, burning the refrigerant
Respectively weighing samples, burning at 450-550 ℃, slightly boiling for dissolution after burning, and fixing the volume to a 100mL volumetric flask;
s2 setting the running conditions of the ion chromatography
A Wantong anion column Metrosep A Supp 4250/4.06.1006.430, a protection column Metrosep A Supp4/5 Guard; column temperature: 35 ℃; and (3) quantitative ring: 10 mu L of the solution; flow rate: 0.8 ml/min;
s3, drawing of standard working curve
S3-1, respectively transferring the chloride ion standard solution into a volumetric flask with the volume of 1000mL, diluting with high-purity water and fixing the volume to prepare chloride ion standard working solutions with corresponding concentrations of 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L and 1.2 mg/L;
s3-2, taking high-purity water as a reference, and determining a series of chloride ion standard working solutions; performing linear regression by taking the mass concentration of the chloride ions as an independent variable and the absorbance as a dependent variable, and calculating to obtain Cl < - > and a standard curve K and a value B;
s4 measurement of sample solution peak area
And (4) analyzing the sample solution obtained in the step S1 by ion chromatography, using high-purity water as a blank, measuring the peak area of the sample solution under the chromatographic condition of the step S2, and obtaining the mass of the chloride ions in the sample solution according to the working curve drawn in the step S3.
Further, in step S1, the weight of the sample is measured to be 0.5 to 1.0 g.
Further, in step S1, the weight of the sample was weighed to 1.0 g.
Further, in step S1, the burning temperature is 550 ℃.
Further, in step S1, the burning time is 1-2 h.
Further, in step S1, the burning time is 2 h.
Further, in step S1, the solution was burned and dissolved for 10 min.
Further, in step S3-1, 0.20mL, 0.4mL, 0.6mL, 0.8mL and 1.2mL of 1000mg/L chloride ion standard solution were transferred to a 1000mL volumetric flask, respectively.
Further, in step S4, the content of chloride ions in the sample is calculated according to the peak area value of the sample solution and the working curve, and the calculation formula of the content of Cl < - > (mg/L) is as follows:
in the formula:
a-the peak area of the corresponding ion, (upsilons/cm) min;
V1-volume of volumetric flask, mL;
V2volume of sample, mL, generally considered a volume of 1mL of 1g of sample.
Compared with the prior art, the method for analyzing and measuring chloride ions in the process refrigerant has the following beneficial effects:
1. the method adopts a high-temperature digestion method to process the sample, completely burns off organic matters and impurities in the sample at the parameters of 550 ℃ of ignition temperature, 2h of ignition time, 10min of dissolution time, 1g of sample amount and the like, and then dissolves and fixes the volume to enter the ion chromatography for analysis, thereby improving the measurement accuracy and precision;
2. the ion chromatography condition is optimized, under the optimized experimental condition, the mass concentration of the chloride ion standard working solution is in a good linear relation with the peak area within the range of 0.00-1.20 mg/L, and the correlation coefficient is 0.99991. The detection limit of the chlorine method is 0.008mg/L, and the quantification limit is 0.08 mg/L;
3. the relative standard deviation of the measurement result of the method is 1.7-2.9% (n is 6), and the sample standard adding recovery rate is 90.0-96.7%. Compared with the analysis result of the dissolving dilution method in GB/T14571.5, the method can eliminate the impurity ions in the refrigerant, converts the organic chlorine into the chloride ions, has higher accuracy of the analysis result, and can be used for measuring the content of the chloride ions in the refrigerant.
4. The method has the advantages of high accuracy, good reproducibility and strong operability.
Drawings
FIG. 1 is a schematic diagram illustrating the influence of the temperature of refrigerant ignition on absorbance in the present invention;
FIG. 2 is a schematic diagram showing the influence of the ignition time of the refrigerant on the absorbance in the present invention;
FIG. 3 is a schematic diagram showing the influence of the dissolution time of a refrigerant after ignition on absorbance in the present invention;
FIG. 4 is a schematic diagram showing the influence of the sample amount of refrigerant on the concentration of chloride ions in the present invention;
FIG. 5 is a comparison of spectra before and after ignition of a refrigerant in the present invention;
Detailed Description
The following is a detailed description of the embodiments of the present invention, which is implemented on the premise of the technical solution of the present invention, and the detailed implementation and specific operation procedures are given, but the protection scope of the present invention is not limited to the following embodiments.
Example 1
The invention relates to an analytical determination method for chloride ions in a process refrigerant, which comprises the following steps:
s1, burning the refrigerant
Respectively weighing 0.5g of sample, burning at 450 ℃, slightly boiling and dissolving for 10min after burning for 1h, and fixing the volume to a 100mL volumetric flask;
s2 setting the running conditions of the ion chromatography
A Wantong anion column Metrosep A Supp 4250/4.06.1006.430, a protection column Metrosep A Supp4/5 Guard; column temperature: 35 ℃; and (3) quantitative ring: 10 mu L of the solution; flow rate: 0.8 ml/min;
s3, drawing of standard working curve
S3-1, respectively transferring 0.20mL, 0.4mL, 0.6mL, 0.8mL and 1.2mL of 1000mg/L chloride ion standard solutions into a 1000mL volumetric flask by using a pipette, diluting with high-purity water and fixing the volume to prepare chloride ion standard working solutions with corresponding concentrations of 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L and 1.2 mg/L;
s3-2, taking high-purity water as a reference, and determining a series of chloride ion standard working solutions; performing linear regression by taking the mass concentration of the chloride ions as an independent variable and the absorbance as a dependent variable, and calculating to obtain Cl < - > and a standard curve K and a value B;
s4 measurement of sample solution peak area
And (4) analyzing the sample solution obtained in the step S1 by ion chromatography, using high-purity water as a blank, measuring the peak area of the sample solution under the chromatographic condition of the step S2, and obtaining the mass of the chloride ions in the sample solution according to the working curve drawn in the step S3.
Calculating the content of chloride ions in the sample according to the peak area value of the sample solution and the working curve, wherein the content of Cl < - > (mg/L) is calculated according to the following formula:
in the formula:
a-the peak area of the corresponding ion, (upsilons/cm) min;
V1-volume of volumetric flask, mL;
V2volume of sample, mL, generally considered a volume of 1mL of 1g of sample.
Example 2
The invention relates to an analytical determination method for chloride ions in a process refrigerant, which comprises the following steps:
s1, burning the refrigerant
Respectively weighing 1g of sample, burning at 550 ℃, slightly boiling for dissolving for 10min after burning for 2h, and fixing the volume to a 100mL volumetric flask;
s2 setting the running conditions of the ion chromatography
A Wantong anion column Metrosep A Supp 4250/4.06.1006.430, a protection column Metrosep A Supp4/5 Guard; column temperature: 35 ℃; and (3) quantitative ring: 10 mu L of the solution; flow rate: 0.8 ml/min;
s3, drawing of standard working curve
S3-1, respectively transferring 0.20mL, 0.4mL, 0.6mL, 0.8mL and 1.2mL of 1000mg/L chloride ion standard solutions into a 1000mL volumetric flask by using a pipette, diluting with high-purity water and fixing the volume to prepare chloride ion standard working solutions with corresponding concentrations of 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L and 1.2 mg/L;
s3-2, taking high-purity water as a reference, and determining a series of chloride ion standard working solutions; performing linear regression by taking the mass concentration of the chloride ions as an independent variable and the absorbance as a dependent variable, and calculating to obtain Cl < - > and a standard curve K and a value B;
s4 measurement of sample solution peak area
And (4) analyzing the sample solution obtained in the step S1 by ion chromatography, using high-purity water as a blank, measuring the peak area of the sample solution under the chromatographic condition of the step S2, and obtaining the mass of the chloride ions in the sample solution according to the working curve drawn in the step S3.
Calculating the content of chloride ions in the sample according to the peak area value of the sample solution and the working curve, wherein the content of Cl < - > (mg/L) is calculated according to the following formula:
in the formula:
a-the peak area of the corresponding ion, (upsilons/cm) min;
V1-volume of volumetric flask, mL;
V2volume of sample, mL, generally considered a volume of 1mL of 1g of sample.
The verification process of the invention is as follows:
firstly, selecting the burning temperature of the invention. The main component of the refrigerant is organic matter glycol, the boiling point of the glycol is 197.4 ℃, the burning point is 418 ℃, and therefore, the burning temperature is set to be 150 ℃, 250 ℃, 350 ℃, 450 ℃ and 550 ℃. The sample amount is set to be 1.0g, the ignition time is set to be 2h, and the dissolution time is set to be 10 min. It can be seen from fig. 1 that the absorbance does not change substantially when the burning temperature is more than 450 ℃, and all the organic substances can be burned off at 550 ℃, and the burning temperature is preferably 550 ℃.
Secondly, selecting the burning time. Weighing 1.0g of refrigerant sample in a clean porcelain crucible, respectively burning for 0.5h, 1h, 1.5h, 2.0h and 2.5h in a muffle furnace at 550 ℃, dissolving for 10min, and fixing the volume in a 100mL volumetric flask. FIG. 2 shows the peak areas of chloride ions for different burning times. As can be seen from FIG. 2, the peak area of the sample at 1 hour of burning tends to be stable. Indicating that the chloride ions in the sample have been completely digested. The burning time is preferably 2h, considering that different batches of samples may have different types of impurities.
And thirdly, selecting the dissolving time. Since a yellowish brown deposit is formed on the surface of the crucible after the sample is burned, the crucible is placed on an electric furnace and heated to a slight boiling state so as to dissolve the deposit on the surface of the crucible in order to completely dissolve the burned product in the high purity water after the burning. The micro-boiling dissolution time is set to be 0min, 10min, 20min, 30min and 40min respectively. As can be seen from fig. 3, the sample had dissolved completely after the sample was slightly boiled on the electric furnace for 10 min. Therefore, the time for the sample to be dissolved by boiling is preferably 10 min.
And fourthly, selecting the sample amount. As the main component of the refrigerant sample is the ethylene glycol aqueous solution, the ethylene glycol undergoes a boiling point and a burning point in the burning process at 550 ℃, and the selection of the proper sample amount is important in order to prevent the loss of the sample in the burning process. In the experiment, 0.5g, 1.0g, 1.5g, 2.0g and 2.5g of samples are respectively weighed and burned at 550 ℃, slightly boiled and dissolved for 10min after burning, and the volume is determined to be 100mL of volumetric flask, as can be seen from figure 4, the concentration of chlorine reaches the maximum value when the sample amount is 1.0g, and the concentration of chlorine tends to decrease along with the increase of the sample amount. This may be due to the sample splattering or deflagration that occurs during the burning process as the sample size increases. Therefore, the amount of the sample is preferably 1.0 g.
And fifthly, comparing spectrograms before and after burning. As can be seen from the spectrogram 5, compared with direct dilution sampling, the spectrogram of the refrigerant subjected to burning digestion does not have an impurity peak, and the separation degree can meet the analysis requirement.
Sixthly, the invention optimizes the chromatographic condition. The linear equation, the detection limit and the quantitative limit draw a standard curve according to the method of step S2. The linear equation is Y ═ 11.68A +0.007, and the correlation coefficient is 0.99991. For Cl with the mass concentration of 0.010mg/L-The standard solution is repeatedly injected for 10 times, and the average value of peak area is [ mu.s/cm) & min]It was 0.009, and the standard deviation was 0.00254. The detection limit refers to the concentration of elements with the ultimate noise standard deviation value of 3 times, and the detection limit is calculated to be 0.008mg/L according to the formula LOD (LOD-3 sigma C/X); the limit of quantitation was 10 times the detection limit, which was 0.08 mg/L.
And seventhly, checking the analysis result.
(1) Precision. The refrigerant sample is diluted into three samples with different concentrations, and the measurement is repeated for 6 times under the specified instrument working conditions, and the measurement results are shown in table 1. As can be seen from Table 1, the relative standard deviation of the measurement results is 1.7-2.9%, which is less than 3%, indicating that the method of the present invention has high precision.
TABLE 1 precision test results
(2) And (4) standard addition recovery test. Weighing 1g of sample in a porcelain crucible, and adding 100.0mg/L Cl-The standard solution is 0.00mL, 0.10mL, 0.20mL, 0.30mL, and is dissolved to a constant volume in a 100mL volumetric flask after being burned at 550 ℃, the sample is subjected to a standard addition recovery test, and the test results are listed in Table 2. As can be seen from Table 2, the recovery rate of the sample from the addition of the standard is 90.0% to 96.7%, which indicates that the accuracy of the method of the present invention can meet the analysis requirements.
TABLE 2 test results of recovery with addition of a standard
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the scope of the present invention, therefore, the present invention is not limited by the appended claims.
Claims (9)
1. The method for analyzing and measuring chloride ions in the process refrigerant is characterized by comprising the following steps of:
s1, burning the refrigerant
Respectively weighing samples, burning at 450-550 ℃, slightly boiling for dissolution after burning, and fixing the volume to a 100mL volumetric flask;
s2 setting the running conditions of the ion chromatography
A Wantong anion column Metrosep A Supp 4250/4.06.1006.430, a protection column Metrosep A Supp4/5 Guard; column temperature: 35 ℃; and (3) quantitative ring: 10 mu L of the solution; flow rate: 0.8 ml/min;
s3, drawing of standard working curve
S3-1, respectively transferring the chloride ion standard solution into a volumetric flask with the volume of 1000mL, diluting with high-purity water and fixing the volume to prepare chloride ion standard working solutions with corresponding concentrations of 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L and 1.2 mg/L;
s3-2, taking high-purity water as a reference, and determining a series of chloride ion standard working solutions; performing linear regression by taking the mass concentration of the chloride ions as an independent variable and the absorbance as a dependent variable, and calculating to obtain Cl < - > and a standard curve K and a value B;
s4 measurement of sample solution peak area
And (4) analyzing the sample solution obtained in the step S1 by ion chromatography, using high-purity water as a blank, measuring the peak area of the sample solution under the chromatographic condition of the step S2, and obtaining the mass of the chloride ions in the sample solution according to the working curve drawn in the step S3.
2. The method for analyzing and measuring chloride ions in a process refrigerant as claimed in claim 1, wherein: in step S1, the weight of the sample is weighed to be 0.5-1.0 g.
3. The method for analyzing and measuring chloride ions in a process refrigerant as claimed in claim 2, wherein: in step S1, the weight of the sample was weighed to 1.0 g.
4. The method for analyzing and measuring chloride ions in a process refrigerant as claimed in claim 1, wherein: in step S1, the burning temperature is 550 ℃.
5. The method for analyzing and measuring chloride ions in a process refrigerant as claimed in claim 1, wherein: in step S1, the burning time is 1-2 h.
6. The method for analyzing and measuring chloride ions in a process refrigerant as claimed in claim 5, wherein: in step S1, the burning time is 2 h.
7. The method for analyzing and measuring chloride ions in a process refrigerant as claimed in claim 1, wherein: in step S1, the solution is burned and dissolved for 10 min.
8. The method for analyzing and measuring chloride ions in a process refrigerant as claimed in claim 1, wherein: in step S3-1, 0.20mL, 0.4mL, 0.6mL, 0.8mL and 1.2mL of 1000mg/L chloride ion standard solution were transferred to a 1000mL volumetric flask, respectively.
9. The method for analyzing and measuring chloride ions in a process refrigerant as claimed in claim 1, wherein: in step S4, the content of chloride ions in the sample is calculated according to the peak area value of the sample solution and the working curve, and the calculation formula of the content of Cl < - > (mg/L) is as follows:
in the formula:
a-the peak area of the corresponding ion, (upsilons/cm) min;
V1-volume of volumetric flask, mL;
V2volume of sample, mL, generally considered a volume of 1mL of 1g of sample.
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| CN115598280A (en) * | 2022-10-20 | 2023-01-13 | 国网黑龙江省电力有限公司电力科学研究院（Cn） | Method for detecting content of chloride ions in cooling water in converter valve of convertor station in low-temperature region |
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