Method for determination of sulfuryl chloride by ion chromatography

Abstract

The present invention belongs to the technical field of chemical substance detection, and in particular to a method for determining sulfuryl chloride by ion chromatography. The method for determining sulfuryl chloride by ion chromatography of the present invention comprises the following steps: (1) sample pretreatment: adding water to a container, cooling to 1-5°C, introducing byproduct sulfuryl chloride to the bottom of the container, sealing the container, then heating up and maintaining temperature ultrasound, performing hydrolysis reaction, and obtaining a hydrolyzate; (2) preparing a standard curve concentration of chloride ions: using a standard substance of chloride ions for dilution of different gradients to obtain standard solutions of different concentrations; (3) using an ion chromatograph to prepare a standard curve of standard solutions of different concentrations, and then using the same ion chromatography parameters to determine the diluted hydrolyzate to obtain the concentration of chloride ions, and calculating the content of sulfuryl chloride. The present invention provides a method for determining sulfuryl chloride by ion chromatography, which has high accuracy, good precision, fast and accurate analysis, few required reagents and consumables, and low cost.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical substance detection, and particularly relates to a method for determining sulfuryl chloride by ion chromatography. Background Art

[0002] Sulfuryl chloride (SO2Cl2), also known as sulfur dioxide dichloride, is a colorless liquid with a strong pungent odor and strong corrosiveness. It has a melting point of -54.1°C and a boiling point of 69.1°C. It is soluble in glacial acetic acid, benzene, toluene, ether and other organic solvents. It decomposes slightly when left for a long time, producing sulfur dioxide and chlorine gas and turning yellow. Sulfuryl chloride decomposes slowly in water and produces sulfuric acid and hydrogen chloride. The decomposition speed is accelerated in hot water; in ice water, it produces SO2Cl2·15H2O, which looks similar to camphor; and in alkali, it reacts. Sulfuryl chloride is widely used as a chlorinating agent, sulfonating agent, chlorosulfonating agent, solvent and catalyst in organic synthesis. It is also used in the manufacture of drugs, dyes, plastics, etc.

[0003] There are two main methods for preparing sulfuryl chloride. One is to react sulfur dioxide with chlorine in the presence of a catalyst such as activated carbon, ferric chloride or camphor to produce sulfuryl chloride. The other is to heat and decompose chlorosulfonic acid in the presence of a catalyst such as mercuric sulfate or tin tetrachloride to produce sulfuryl chloride. At present, in the process of producing trifluoroacetyl chloride using raw materials trichlorotrifluoroethane (R113) and sulfur trioxide, sulfuryl chloride is the main by-product, and its purity is strictly controlled. In the by-product sulfuryl chloride, there are also small amounts of R113 and sulfur trioxide. There are few methods for direct detection of them.

[0004] At present, there is no systematic national standard or industry standard for the quality control of sulfuryl chloride. The industry mainly tests the content by boiling range method and gas chromatography analysis. However, the boiling range method has low accuracy, complicated operation and large error. In gas chromatography analysis, sulfuryl chloride is particularly corrosive and seriously corrodes the gas phase instrument system and chromatographic column. The analysis cost is high, which is not conducive to the analysis of the results and has weak qualitative analysis ability.

[0005] As a commonly used ion analysis instrument, ion chromatography analysis method usually analyzes samples with relatively stable ions. When sulfuryl chloride is analyzed by ion chromatography, it usually needs to be dissolved in water for detection. However, sulfuryl chloride is easily soluble in water and hydrolyzed. Therefore, the use of ion chromatography to analyze sulfuryl chloride will face more uncertainties and difficulties, resulting in poor accuracy and reliability. Summary of the invention

[0006] The technical problem to be solved by the present invention is to overcome the above-mentioned defects in the prior art and provide a method for determining sulfuryl chloride by ion chromatography, which has high accuracy, good precision, rapid and accurate analysis, few required reagents and consumables, and low cost.

[0007] The method for determining sulfuryl chloride by ion chromatography of the present invention comprises the following steps:

[0008] (1) Sample pretreatment: add water to the container, cool it to 1-5°C, introduce by-product sulfuryl chloride to the bottom of the container, seal the container, then heat it up and maintain the temperature under ultrasound to perform a hydrolysis reaction to obtain a hydrolyzate;

[0009] (2) Preparation of the standard curve concentration of chloride ion: Use the chloride ion standard substance to dilute it in different gradients to obtain standard solutions of different concentrations;

[0010] (3) Use an ion chromatograph to prepare a standard curve for standard solutions of different concentrations. Then use the same ion chromatographic parameters to measure the diluted hydrolyzate to obtain the concentration of chloride ions and calculate the content of sulfuryl chloride.

[0011] Step (1) Raise the temperature to 35-45°C and maintain the temperature for 10-20 minutes.

[0012] The mass ratio of by-product sulfuryl chloride to water in the container of step (1) is 1:(30-50).

[0013] The hydrolyzate of step (1) is obtained by diluting 10,000 times with water and filtering through 0.22 μm.

[0014] The water in step (1) is ultrapure water with a resistivity of ≥18.2 MΩ.

[0015] The standard solutions of different concentrations in step (2) are 5 μg / mL, 10 μg / mL, 20 μg / mL, 40 μg / mL, and 80 μg / mL, respectively.

[0016] The chloride ion standard substance used in step (2) has a concentration of 1000 mg / L.

[0017] The parameters of the ion chromatography described in step (3) are:

[0018] Eluent: 0.015 mol / L potassium hydroxide;

[0019] Eluent flow rate: 1mL / min;

[0020] Column temperature: 35°C;

[0021] Conductivity cell temperature: 35°C;

[0022] Suppressor current: 60mA.

[0023] The calculation formula of the content W of sulfuryl chloride in step (3) is: , where c is the concentration of chloride ions in μg / mL, D is the dilution factor of the hydrolyzate, and m is the mass of the by-product sulfuryl chloride.

[0024] After the hydrolysis reaction in step (1) is completed, the pH is adjusted to 7, and the solution used for adjustment is potassium hydroxide solution.

[0025] Specifically, the method for determining sulfuryl chloride by ion chromatography comprises the following steps:

[0026] (1) Sample pretreatment: Add ultrapure water to the iodine volumetric flask, cool to 1-5°C, accurately weigh the by-product sulfuryl chloride liquid mass, pass the by-product sulfuryl chloride to the bottom of the container, cover the bottle stopper, heat to 35-45°C in a heatable ultrasonic cleaner, maintain the temperature, and ultrasonicate for 10-20 minutes to carry out hydrolysis reaction. After the reaction, adjust the pH to 7 with a 100g / L potassium hydroxide solution, transfer to a 100mL volumetric flask and rinse the iodine volumetric flask several times. Transfer to the volumetric flask and dilute 100 times with ultrapure water and filter with a 0.22μm filter to obtain the hydrolyzate, which is ready for the ion chromatograph; (The purpose of controlling the temperature at 1-5°C is that the density of sulfuryl chloride is greater than that of water. After addition, sulfuryl chloride is sealed at the bottom of the bottle. The low temperature prevents sulfuryl chloride from volatilizing during weighing and the hydrogen chloride generated by hydrolysis from overflowing).

[0027] (2) Preparation of the standard curve concentration of chloride ion: Using 1000 mg / L of chloride ion standard substance, use ultrapure water to dilute it in different gradients to obtain 5 μg / mL, 10 μg / mL, 20 μg / mL, 40 μg / mL, and 80 μg / mL standard solutions;

[0028] (3) Using the following parameters: eluent: 0.015 mol / L potassium hydroxide; eluent flow rate: 1 mL / min; column temperature: 35°C; conductivity cell temperature: 35°C; suppressor current: 60 mA, use an ion chromatograph to prepare a standard curve using standard solutions of different concentrations, and then use the same ion chromatographic parameters to measure the diluted and filtered hydrolyzate to obtain the concentration of chloride ions. According to the formula , calculate the content of sulfuryl chloride.

[0029] The present invention measures byproduct sulfuryl chloride with a purity of ≥97%. First, the byproduct sulfuryl chloride is subjected to ultrasonic hydrolysis reaction at a certain temperature to generate a SO2Cl2+2H2O=H2SO4+2HCl reaction. The generated HCl is absorbed by water. After adjusting the pH, the product is diluted, filtered, and tested on a machine. The hydrolysis products of sulfuryl chloride are sulfuric acid and hydrogen chloride. Sulfur trioxide reacts with water to generate sulfuric acid. R113 is insoluble in water. Chloride ions are detected by ion chromatography. Impurities in the product have no effect on the accuracy of the test result.

[0030] Compared with the prior art, the present invention has the following beneficial effects:

[0031] (1) The method for determining sulfuryl chloride by ion chromatography of the present invention is non-corrosive to equipment compared with the conventional boiling range method.

[0032] (2) Compared with the conventional gas chromatography, the ion chromatography method of the present invention has high analysis accuracy, good precision, fast and accurate analysis, less reagents and consumables, and low cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 This is the standard curve diagram of Example 1.

[0034] Figure 2 This is the standard curve diagram of Example 2.

[0035] Figure 3 This is the standard curve diagram of Example 3.

[0036] Figure 4 The linearity plot of sulfuryl chloride in the linearity experiment for the method verification experiment.

[0037] Figure 5 This is the ion chromatography spectrum of sulfuryl chloride detected in Example 1.

[0038] Figure 6 This is the ion chromatography spectrum of sulfuryl chloride detected in Example 2.

[0039] Figure 7 This is the ion chromatography spectrum of sulfuryl chloride detected in Example 3.

[0040] Figure 8 The gas chromatography spectrum of sulfuryl chloride was detected for Comparative Example 1.

[0041] Fig. 9 To verify the accuracy of the method in the experiment, the ion chromatogram was obtained.

[0042] Fig.10 Ion chromatograms were obtained to verify the robustness of the method. DETAILED DESCRIPTION

[0043] The present invention will be further described below in conjunction with specific embodiments.

[0044] The raw materials and reagents used in the following examples and comparative examples are all normal commercially available products.

[0045] The potassium hydroxide used as the eluent is a high-grade pure reagent, and the resistivity of the ultrapure water used is ≥18.2MΩ. The standard substance of chloride ion used is Tanmo Quality Inspection GBW (E) 082683 B23050079. The ion chromatograph used is Qingdao Shenghan CIC-D120.

[0046] The by-product sulfuryl chloride liquid used in the following examples and comparative examples is a by-product produced in the process of producing trifluoroacetyl chloride by Zibo Feiyuan Chemical Co., Ltd. using raw materials trichlorotrifluoroethane (R113) and sulfur trioxide.

[0047] Example 1

[0048] The method for determining sulfuryl chloride by ion chromatography comprises the following steps:

[0049] (1) Sample pretreatment: add 40g of ultrapure water to the iodine volumetric flask, cool to 2°C, accurately weigh 1.0165g of by-product sulfuryl chloride (1# finished product tank) liquid mass m, pass the by-product sulfuryl chloride to the bottom of the container, cover the bottle stopper, heat to 40°C in a heatable ultrasonic cleaner and maintain the temperature, ultrasonicate for 15min, and hydrolyze. After the reaction, adjust the pH to 7 with a 100g / L potassium hydroxide solution, transfer to a 100mL volumetric flask and rinse the iodine volumetric flask several times, transfer to a volumetric flask to make up the volume, dilute 100 times with ultrapure water, and filter with a 0.22μm filter to obtain the hydrolyzate, which is ready for the ion chromatograph;

[0050] (2) Preparation of the standard curve concentration of chloride ion: Use 1000 mg / L of chloride ion standard substance and use ultrapure water to dilute it in different gradients to obtain 5 μg / mL, 10 μg / mL, 20 μg / mL, 40 μg / mL, and 80 μg / mL standard solutions. The standard curve is Y=-2.561×10 7 +1.948×10 7 X, R=0.999922, the ordinate Y is the peak area, the abscissa X is the concentration of chloride ions, the unit is μg / mL, the standard curve is as follows Figure 1 As shown;

[0051] (3) The following parameters were used: eluent: 0.015 mol / L potassium hydroxide; eluent flow rate: 1 mL / min; column temperature: 35°C; conductivity cell temperature: 35°C; suppressor current: 60 mA. Standard solutions of different concentrations were used to prepare a standard curve using an ion chromatograph. The diluted and filtered hydrolyzate was then measured using the same ion chromatographic parameters. The dilution factor D was 10,000. The chloride ion concentration c was 52.54 μg / mL and the retention time was 6.172 min. According to the formula , the content of sulfuryl chloride was calculated to be 98.39%. The ion chromatography spectrum of sulfuryl chloride is as follows Figure 5 shown.

[0052] Example 2

[0053] The method for determining sulfuryl chloride by ion chromatography comprises the following steps:

[0054] (1) Sample pretreatment: add 43g of ultrapure water to the iodine volumetric flask, cool to 1°C, accurately weigh 1.0910g of by-product sulfuryl chloride (3# finished product tank) liquid mass m, pass the by-product sulfuryl chloride to the bottom of the container, cover the bottle stopper, heat to 35°C in a heatable ultrasonic cleaner and maintain the temperature, ultrasonicate for 20min, and hydrolyze. After the reaction, adjust the pH to 7 with a 100g / L potassium hydroxide solution, transfer to a 100mL volumetric flask and rinse the iodine volumetric flask several times, transfer to a volumetric flask to make up the volume, dilute 100 times with ultrapure water, and filter with a 0.22μm filter to obtain the hydrolyzate, which is ready for the ion chromatograph;

[0055] (2) Preparation of the standard curve concentration of chloride ion: Use 1000 mg / L of chloride ion standard substance and use ultrapure water to dilute it in different gradients to obtain 5 μg / mL, 10 μg / mL, 20 μg / mL, 40 μg / mL, and 80 μg / mL standard solutions. The standard curve is Y=-2.34×10 7 +1.923×10 7 X, R=0.999944, the standard curve is as follows Figure 2 As shown;

[0056] (3) The following parameters were used: eluent: 0.015 mol / L potassium hydroxide; eluent flow rate: 1 mL / min; column temperature: 35°C; conductivity cell temperature: 35°C; suppressor current: 60 mA. Standard solutions of different concentrations were used to prepare a standard curve using an ion chromatograph. The diluted and filtered hydrolyzate was then measured using the same ion chromatographic parameters. The dilution factor D was 10,000. The chloride ion concentration c was 56.28 μg / mL and the retention time was 6.188 min. According to the formula , the content of sulfuryl chloride was calculated to be 98.20%. The ion chromatography spectrum of sulfuryl chloride is as follows Figure 6 shown.

[0057] Example 3

[0058] The method for determining sulfuryl chloride by ion chromatography comprises the following steps:

[0059] (1) Sample pretreatment: add 40g of ultrapure water to the iodine volumetric flask, cool to 5°C, accurately weigh 1.0786g of by-product sulfuryl chloride (4# finished product tank) liquid mass m, pass the by-product sulfuryl chloride to the bottom of the container, cover the bottle stopper, heat to 45°C in a heatable ultrasonic cleaner and maintain the temperature, ultrasonicate for 10min, and hydrolyze. After the reaction, adjust the pH to 7 with a 100g / L potassium hydroxide solution, transfer to a 100mL volumetric flask and rinse the iodine volumetric flask several times, transfer to a volumetric flask to make up the volume, dilute 100 times with ultrapure water, and filter with a 0.22μm filter to obtain the hydrolyzate, which is ready for the ion chromatograph;

[0060] (2) Preparation of the standard curve concentration of chloride ion: Use 1000 mg / L of chloride ion standard substance and use ultrapure water to dilute it in different gradients to obtain 5 μg / mL, 10 μg / mL, 20 μg / mL, 40 μg / mL, and 80 μg / mL standard solutions. The standard curve is Y=-2.705×10 7 +1.967×10 7 X, R=0.999932, the standard curve is as follows Figure 3 As shown;

[0061] (3) The following parameters were used: eluent: 0.015 mol / L potassium hydroxide; eluent flow rate: 1 mL / min; column temperature: 35°C; conductivity cell temperature: 35°C; suppressor current: 60 mA. Standard solutions of different concentrations were used to prepare a standard curve using an ion chromatograph. The diluted and filtered hydrolyzate was then measured using the same ion chromatographic parameters. The dilution factor D was 10,000. The chloride ion concentration c was 53.82 μg / mL and the retention time was 6.182 min. According to the formula , the content of sulfuryl chloride was calculated to be 98.16%. The ion chromatography spectrum of sulfuryl chloride is as follows Figure 7 shown.

[0062] Comparative Example 1

[0063] Gas chromatography to detect sulfuryl chloride content

[0064] The by-product sulfuryl chloride sample of Example 1 was subjected to gas chromatography detection. The gas chromatography parameters are as follows: gas chromatograph Shimadzu GC-2014C; chromatographic column: Haohan Chromatography (Shandong) Company HH-SO2CL2 special column 30m (length) × 0.53mm (diameter) capillary column; SPL temperature 150°C; chromatographic column temperature: 100°C; detector: TCD detector; detector current 110mA; injection volume: 1μL; carrier gas: hydrogen flow rate 2mL / min. After setting the detection parameters, after the gas chromatograph is stabilized, the sulfuryl chloride sample is injected with a microinjection needle with an injection volume of 1μL, and gas chromatography detection is performed. The result is calculated by the area normalization method, and the by-product sulfuryl chloride content of this batch is measured to be: 98.307%. The RSD of this result and the ion chromatography detection result (98.39%) is: 0.06%, and the result has good precision. The gas chromatography detection sulfuryl chloride spectrum is as follows Figure 8 As shown, the peak of sulfuryl chloride is at a retention time of 1.508 min, the peak area is 2353851, and the area (content) is 98.307%.

[0065] Verification test of the method for determining sulfuryl chloride by ion chromatography of the present invention:

[0066] The method for determining sulfuryl chloride by ion chromatography comprises the following steps:

[0067] (1) Sample pretreatment: Add ultrapure water to the iodine volumetric flask, cool to 1°C, accurately weigh the mass m of sulfuryl chloride liquid, pass the by-product sulfuryl chloride to the bottom of the container, cover the bottle with a stopper, heat to 40°C in a heatable ultrasonic cleaner and maintain the temperature, ultrasonicate for 10 min, and hydrolyze. After the reaction, adjust the pH to 7 with 100 g / L potassium hydroxide solution, transfer to a 100 mL volumetric flask and rinse the iodine volumetric flask several times. Transfer to a volumetric flask to make up the volume, dilute 100 times with ultrapure water, and filter with a 0.22 μm filter to obtain the hydrolyzate, which is ready for the ion chromatograph.

[0068] (2) Preparation of the standard curve concentration of chloride ion: Using 1000 mg / L of chloride ion standard substance, use ultrapure water to dilute it in different gradients to obtain 5 μg / mL, 10 μg / mL, 20 μg / mL, 40 μg / mL, and 80 μg / mL standard solutions. The obtained standard curve is Y=-2.561×10 7 +1.948×10 7 X, R=0.999922, such as Figure 1 As shown; this standard curve was used in the following verification experiments.

[0069] (3) Using the following parameters: eluent: 0.015 mol / L potassium hydroxide; eluent flow rate: 1 mL / min; column temperature: 35°C; conductivity cell temperature: 35°C; suppressor current: 60 mA, standard solutions of different concentrations were used to prepare a standard curve using an ion chromatograph. The diluted and filtered hydrolyzate was then measured using the same ion chromatographic parameters to obtain the chloride ion concentration. According to the formula , calculate the content of sulfuryl chloride.

[0070] Verify the above method

[0071] ① Qualitative and quantitative repeatability (precision): Weigh 1.0750 g of sulfuryl chloride and perform hydrolysis treatment according to the above sample pretreatment procedure, then repeat the injection 5 times. The results are shown in Table 1. The sulfuryl chloride is analytical pure sulfuryl chloride with a content of more than 98%.

[0072] Table 1 Results of qualitative and quantitative repeatability experiments of sulfuryl chloride

[0073]

[0074] After calculation: Qualitative (retention time) repeatability RSD: 0.003%; according to the general rules for ion chromatography analysis methods JY / T0575-2020, the qualitative repeatability is ≤1.5%; quantitative (concentration) repeatability RSD: 0.035%; according to the general rules for ion chromatography analysis methods JY / T0575-2020, the quantitative repeatability is ≤3.0%.

[0075] ② Linearity: Weigh 2.0750g of sulfuryl chloride and perform hydrolysis treatment according to the above sample pretreatment procedure and then dilute it. The concentration of the sample solution is 104.4μg / mL. The sample solution is diluted 2 times, 5 times, 10 times, and 20 times for detection on the machine. The detection result is the concentration of chloride ions in sulfuryl chloride, which is the concentration y (μg / mL) in Table 2. The results are shown in Table 2. The linear graph of sulfuryl chloride is shown in Figure 4 As shown, the linear relationship is y=103.59x+0.6265, x is the dilution factor (with the sample solution as 1, the dilution factor of 2 times is 0.5, the dilution factor of 5 times is 0.2, the dilution factor of 10 times is 0.1, and the dilution factor of 20 times is 0.05), wherein the ordinate y is the content of chloride ions in sulfuryl chloride, in μg / mL, and the abscissa x is the correlation coefficient of sulfuryl chloride content R=0.9999. The sulfuryl chloride is analytical pure sulfuryl chloride, with a content of more than 98%.

[0076] Table 2 Sulfuryl chloride linear results

[0077]

[0078] ③ Accuracy: Weigh 1.0301g of sulfuryl chloride standard and dilute it according to the sulfuryl chloride pretreatment method, then perform ion chromatography detection. The chloride ion content is 53.34μg / mL, and the retention time is 6.172min. The sulfuryl chloride content is calculated to be 98.57%. Fig. 9 As shown in Figure a; accurately weigh 0.8318g of sulfuryl chloride standard again, hydrolyze and dilute it according to the sulfuryl chloride pretreatment method, and then perform ion chromatography detection. The chloride ion content is 43.03μg / mL, and the retention time is 6.152min. After calculation, the sulfuryl chloride content is: 98.47%, such as Fig. 9 As shown in Figure b, the sulfuryl chloride content of the standard is 98.5%, RSD: 0.051%.

[0079] ④ Durability: Weigh 0.2168g of sulfuryl chloride and perform hydrolysis treatment according to the sulfuryl chloride pretreatment method. Then dilute and inject the sample. The result shows that the chloride ion content is 11.18μg / mL, and the retention time is 6.143min. After calculation, the sulfuryl chloride content is 98.17%. Fig.10 As shown in Figure a; 0.4084g of sulfuryl chloride was weighed and hydrolyzed according to the sulfuryl chloride pretreatment method, and then diluted and injected. The result showed that the chloride ion content was 21.29μg / mL, and the retention time was 6.163min. After calculation, the sulfuryl chloride content was: 98.24%. Fig.10 As shown in Figure b; weigh 2.0688g of sulfuryl chloride, hydrolyze it according to the sulfuryl chloride pretreatment method, dilute it and inject it. The result is that the chloride ion content is 106.6μg / mL, and the retention time is 6.207min. After calculation, the sulfuryl chloride content is: 98.09%. Fig.10 As shown in Figure c;

[0080] The sample is a repeatability test sample with an average content of 98.37%. Since the ion chromatography parameters are generally fixed, the RSD of the test result after changing the sample mass is: 0.12%. According to the general rules for ion chromatography analysis methods JY / T0575-2020, the quantitative repeatability ≤3.0% meets the requirements. After method verification, the test method meets the test requirements.

Claims

1. A method for measuring sulfuryl chloride by ion chromatography, characterized in that: The following steps are involved: (1) Sample pretreatment: add ultrapure water with resistivity ≥18.2MΩ into the container, cool it to 1-5°C, introduce by-product sulfuryl chloride into the bottom of the container, seal the container, then heat it to 35-45°C and maintain the temperature for 10-20 min for ultrasonic hydrolysis. After the reaction, adjust the pH to 7 with potassium hydroxide solution to obtain a hydrolyzate. The mass ratio of by-product sulfuryl chloride to water is 1:(30-50). The hydrolyzate is diluted 100 times with water and filtered through 0.22μm. The by-product sulfuryl chloride is produced in the process of producing trifluoroacetyl chloride using raw materials trichlorotrifluoroethane and sulfur trioxide; (2) Preparation of the standard curve concentration of chloride ion: Use a 1000 mg / L chloride ion standard substance to perform different gradient dilutions to obtain standard solutions of different concentrations, namely 5 μg / mL, 10 μg / mL, 20 μg / mL, 40 μg / mL, and 80 μg / mL; (3) Using an ion chromatograph to prepare a standard curve for standard solutions of different concentrations, and then using the same ion chromatographic parameters to measure the diluted hydrolyzate to obtain the concentration of chloride ions and calculate the content of sulfuryl chloride; The parameters of the ion chromatography are: Eluent: 0.015 mol / L potassium hydroxide; Eluent flow rate: 1mL / min; Column temperature: 35°C; Conductivity cell temperature: 35°C; Suppressor current: 60mA; The calculation formula of sulfuryl chloride content W is: , where c is the concentration of chloride ions μg / mL, D is the dilution factor of the hydrolyzate, and m is the mass of by-product sulfuryl chloride in g.

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