阅读说明：本技术 一种烯丙基磺酸钠的高效液相色谱检测方法 (High performance liquid chromatography detection method of sodium allylsulfonate ) 是由 李化平 周通 卢晓锋 张四增 李改变 丁丰荣 宛顺磊 李亦婧 郭勇 王立成 于 2021-05-31 设计创作，主要内容包括：本发明提供了一种烯丙基磺酸钠的高效液相色谱检测方法,是将含有烯丙基磺酸钠的样品进行高效液相色谱检测,得到烯丙基磺酸钠的色谱峰面积,色谱条件为：所用色谱柱为C18色谱柱；所用流动相A为甲醇,流动相B为乙酸铵溶液；蒸发光检测器漂移管75～100℃,载气流速3.0～3.5L/min；柱温为20～40℃；流速为0.5～1.5mL/min；进样量为5～20μL；根据烯丙基磺酸钠的标准曲线,结合烯丙基磺酸钠的色谱峰面积,得到烯丙基磺酸钠的含量。本发明的烯丙基磺酸钠的检测方法简便易行,可快速测定烯丙基磺酸钠含量,具有较高的准确性、稳定性和分离度。(The invention provides a high performance liquid chromatography detection method of sodium allylsulfonate, which is characterized in that a sample containing sodium allylsulfonate is subjected to high performance liquid chromatography detection to obtain the chromatographic peak area of the sodium allylsulfonate, and the chromatographic conditions are as follows: the chromatographic column is C18 chromatographic column; the mobile phase A is methanol, and the mobile phase B is ammonium acetate solution; the drift tube of the evaporation light detector is 75-100 ℃, and the flow rate of carrier gas is 3.0-3.5L/min; the column temperature is 20-40 ℃; the flow rate is 0.5-1.5 mL/min; the sample injection amount is 5-20 mu L; and (3) according to a standard curve of the sodium allylsulfonate, combining the chromatographic peak area of the sodium allylsulfonate to obtain the content of the sodium allylsulfonate. The detection method of sodium allylsulfonate is simple and easy to implement, can quickly detect the content of sodium allylsulfonate, and has higher accuracy, stability and separation degree.)

1. A high performance liquid chromatography detection method of sodium allylsulfonate comprises the following steps:

(1) performing high performance liquid chromatography detection on a water sample to be detected containing sodium allylsulfonate to obtain the chromatographic peak area of the sodium allylsulfonate; the chromatographic conditions were as follows:

the chromatographic column is C18 chromatographic column; the mobile phase A is methanol, and the mobile phase B is ammonium acetate solution; the drift tube of the evaporation light detector is 75-100 ℃, and the flow rate of carrier gas is 3.0-3.5L/min; the column temperature is 20-40 ℃; the flow rate is 0.5-1.5 mL/min; the sample injection amount is 5-20 mu L;

(2) according to a standard curve of the sodium allylsulfonate, combining the chromatographic peak area of the sodium allylsulfonate to obtain the content of the sodium allylsulfonate;

the linear equation of the sodium allylsulfonate standard curve is as follows: y =2.1394x-3.8556, correlation coefficient R²= 0.9927; wherein x is the mass concentration of sodium allylsulfonate, unit: mg/L, y is the chromatographic peak area of sodium allylsulfonate, unit: intens.

2. The high performance liquid chromatography detection method of sodium allylsulfonate as claimed in claim 1, wherein: in the step (1), the molar concentration of the ammonium acetate solution is 0.005-0.05 mol/L.

3. The high performance liquid chromatography detection method of sodium allylsulfonate as claimed in claim 1, wherein: in the step (1), the volume ratio of the mobile phase A to the mobile phase B is 5: 95-15: 85.

Technical Field

The invention relates to a high performance liquid chromatography detection method of sodium allylsulfonate, belonging to the technical field of analytical chemistry.

Background

The sodium allylsulfonate product is prepared by the reaction of 3-chloropropene and sodium sulfite, is a nickel electroplating brightener and can improve the metal distribution capacity and ductility; the third monomer of the acrylic fiber can improve the dyeing property of the fiber and ensure firm coloring; in addition, sodium allylsulfonate is also used as an anionic surfactant, a water quality treating agent, an oil field drilling mud additive and a cement water reducing agent for construction. When the brightener is used as a nickel electroplating brightener, the brightener is often compounded with other brighteners to form a composite brightener which is added into an electrolyte. The content of sodium allylsulfonate in the composite brightener is an index which is more concerned by technical personnel in the electroplating field, so that the development of a detection method of sodium allylsulfonate is urgently needed.

The titration of anionic active matter in national standard adopts direct two-phase titration method, but the method is only suitable for anionic active matter with carbon chain length above C8, and sodium allylsulfonate can not react with color developing agent. The potentiometric titration method can detect the mutation potential when the concentration of the surfactant is below the critical micelle concentration by using the surfactant ion selective electrode, so that the detection of the concentration of the anionic surfactant in a sample is realized, but the quantitative detection of the sodium allylsulfonate is greatly interfered because various anionic surfactants can be added into a composite brightener system. The liquid chromatography has higher accuracy and separation degree, simple method and good universality, and is suitable for being used as a detection method of sodium allylsulfonate.

Disclosure of Invention

The invention aims to provide a high performance liquid chromatography detection method for sodium allylsulfonate, which is simple to operate, can quickly determine the content of sodium allylsulfonate and has higher accuracy, stability and separation degree.

The technical problem to be solved by the invention can be realized by the following technical scheme:

(1) determination of chromatographic conditions

Preparing standard sodium allylsulfonate into standard solution with sodium allylsulfonate concentration of 100mg/L by using deionized water to constant volume, analyzing by using a liquid chromatograph, and obtaining corresponding retention time (3.028 min, 4.245 min) as shown in figure 1, and determining chromatographic conditions as follows:

the chromatographic column is C18 chromatographic column; the mobile phase A is methanol, and the mobile phase B is ammonium acetate solution; the drift tube of the evaporation light detector is 75-100 ℃, and the flow rate of carrier gas is 3.0-3.5L/min; the column temperature is 20-40 ℃; the flow rate is 0.5-1.5 mL/min; the sample injection amount is 5-20 mu L; the molar concentration of the ammonium acetate solution is 0.005-0.05 mol/L; the volume ratio of the mobile phase A to the mobile phase B is 5: 95-15: 85.

(2) Preparation of Standard solutions

And (2) fixing the volume of the sodium allylsulfonate standard substance by using deionized water to obtain a standard solution with the concentration of 1mg/mL, and preparing a standard working solution with a concentration gradient, wherein the sodium allylsulfonate in the standard working solution is in a gradient series of 10mg/L, 20mg/L, 50mg/L, 80mg/L and 100 mg/L.

(3) Drawing of standard curve

Performing detection analysis on the standard working solution under the chromatographic condition in the step (2), and performing linear regression by using the peak area of the sodium allylsulfonate and the corresponding mass concentration of the sodium allylsulfonate to obtain a linear regression equation, namely a standard curve of the sodium allylsulfonate, wherein the linear equation and the detection limit are shown in table 1:

the detection accuracy, precision and recovery rate were verified by the following methods: the standard solution is continuously diluted until the signal-to-noise ratio S/N is 3, the injection concentration is taken as the detection Limit (LOD), and the concentration corresponding to 10 times of the signal-to-noise ratio is taken as the lower limit of quantification (LOQ). Taking a standard solution of 50mg/L sodium allylsulfonate as a standard adding recovery experiment, calculating the accuracy of a recovery rate investigation method, investigating the precision of the recovery rate Relative Standard Deviation (RSD) investigation method, adding 1mg/ml standard solution into the standard solution of 50mg/L sodium allylsulfonate, wherein the standard adding levels are 5mg/L, 20mg/L and 40 mg/L respectively, measuring 6 times in parallel at each adding level, and calculating the standard adding recovery rate by using the following formula;

C₁is the sample concentration, C₂For adding the concentration of the sample, C₃Is an addition scalar quantity.

The recovery and precision of the added standard are shown in Table 2:

(4) sample detection

And (2) fixing the volume of the water sample to be detected containing the sodium allylsulfonate by using deionized water, and performing liquid chromatography detection under the chromatographic condition of the step (1) to obtain the chromatographic peak area of the sodium allylsulfonate.

(5) Sample content calculation

And (4) calculating the content of the sodium allylsulfonate according to the standard curve of the sodium allylsulfonate in the step (3) and the chromatographic peak area of the sodium allylsulfonate in the step (4).

The invention has the beneficial effects that: the method adopts chromatographic column separation of octadecyl bonding phase and detection by an evaporative light detector, has simple and easy detection method, can quickly determine the content of sodium allylsulfonate, and has higher accuracy, stability and separation degree.

Drawings

FIG. 1 is an HPLC chromatogram of a standard solution of sodium allylsulfonate.

Detailed Description

The technical means of the present invention will be described in detail below with reference to examples.

Instruments and reagents used in the invention

High performance liquid chromatography (Agilent 1100, Agilent corporation, usa); evaporative light detector (UM5800 Plus, by micronaire).

Sodium allylsulfonate is an analytical reagent; ammonium acetate and methanol are chromatographic grade reagents.

Example 1

(1) Fixing the volume of a water sample to be detected containing sodium allylsulfonate by using deionized water, and then carrying out high performance liquid chromatography detection to obtain the chromatographic peak area of the sodium allylsulfonate; the chromatographic conditions were as follows:

a chromatographic column: c18(4.6 mm. times.300 mm,5 μm); column temperature: 25 ℃; sample introduction amount: 20 mu L of the solution; flow rate: 1.0 mL/min; mobile phase: a is methanol, B is 0.02mol/L ammonium acetate solution, A: B =2: 98; the evaporation light detector drift tube is at 95 ℃, and the flow rate of the carrier gas is 3.5L/min.

(2) According to a standard curve y =2.1394x-3.8556 of sodium allylsulfonate (x is the mass concentration of sodium allylsulfonate, and y is the chromatographic peak area of sodium allylsulfonate), the content of sodium allylsulfonate is obtained by combining the chromatographic peak area of sodium allylsulfonate, and the content of sodium allylsulfonate in the sample is 58.50 mg/L.

Example 2

Except that the water sample to be tested containing sodium allylsulfonate is different, the other steps are the same as the example 1, and the content of sodium allylsulfonate in the sample is 72.63mg/L through HPLC determination and analysis.

Example 3

Except that the water sample to be tested containing sodium allylsulfonate is different, the other steps are the same as the example 1, and the content of sodium allylsulfonate in the sample is 32.60mg/L by HPLC determination and analysis.