CN108008061B - Method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid by ion chromatography - Google Patents
Method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid by ion chromatography Download PDFInfo
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Abstract
The invention relates to a method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid in a process of preparing glycine by using a chloroacetic acid method through ion chromatography, which comprises the following specific steps: preparing a mixed standard solution of four anions of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical, selecting an AS19-HC analytical column and KOH eluent, and entering an ion chromatography detection system for gradient elution to obtain a linear equation of concentration and peak area. The content of each component in the chloroacetic acid is calculated by a linear equation. The whole analysis process is simple and rapid to operate, has small pollution and loss, has blank and sample standard addition recovery rates of 96-99.75%, and is suitable for detecting the contents of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radicals in chloroacetic acid.
Description
Technical Field
The invention relates to detection of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical, and belongs to the field of chemical analysis.
Background
Chloroacetic acid is an important intermediate for industrial production of glycine, and during the process of preparing glycine by using a chloroacetic acid method, due to the change of conditions, byproducts such as dichloroacetic acid, trichloroacetic acid, sulfate radicals and the like can be generated during the process of preparing chloroacetic acid in the industrial production process, and the purity of chloroacetic acid products directly influences the quality of glycine, so that during the process of producing chloroacetic acid, the detection of the concentrations of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radicals in chloroacetic acid is extremely important.
The existing commonly used method for detecting the content of chloroacetic acid is HG/T3271-2000 silver nitrate indirect titration method and gas chromatography, and the methods have complex pretreatment, need other chemical reagents in the process, are time-consuming and labor-consuming in the process, have great influence on human and environment and have poor reproducibility.
Disclosure of Invention
The present invention is directed to overcoming the above-mentioned drawbacks of the prior art and providing a method suitable for detecting the concentrations of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in the preparation process of glycine.
The purpose of the invention can be realized by the following technical scheme: a method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid by ion chromatography is characterized by comprising the following steps: diluting a sample to be detected by ten thousand times, analyzing the peak area of the sample diluent by adopting an ion chromatograph, and comparing the peak area with a standard calibration curve to obtain the concentrations of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radicals in the sample, thereby obtaining the concentrations of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radicals in the sample to be detected, wherein the detection conditions of the ion chromatograph are that an InPacAS19 analytical column is selected as a chromatographic column, an AG19 protective column is selected as an ASRS inhibitor, the sample injection amount is 20-30 mu L, the leacheate is KOH, and gradient leaching is carried out, wherein the time of 0-18min is 10 mmol/L; 35mmol/L for 18-25 min; 10mmol/L at 25-26min and 1.0mL/min flow rate.
The standard calibration curve is prepared by dissolving standard substances of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and anhydrous sodium sulfate in ultrapure water to prepare stock solutions of 10000ug/L, 1000ug/L, 1000ug/L and 1000ug/L respectively, storing at 4 ℃ in a dark place, diluting the standard solution of monochloroacetic acid to standard solutions of 500ug/mL, 600ug/mL, 700ug/mL, 800ug/mL, 900ug/mL and 1000ug/mL when in use, diluting the standard solution of dichloroacetic acid to standard solutions of 20ug/mL, 25ug/mL, 30ug/mL, 35ug/mL, 40ug/mL and 45ug/mL, diluting the standard solution of trichloroacetic acid to standard solutions of 15ug/mL, 20ug/mL, 25ug/mL, 30ug/mL and 35ug/mL, diluting the standard solution of sulfate radicals to 2ug/mL, 4ug/mL, 6ug/mL, 8ug/mL and 10ug/mL, performing ion chromatography on the mixed standard solution in an anion detection mode to obtain a standard spectrogram, and detecting mixed standard solutions with different concentrations to respectively obtain standard calibration curves of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radicals.
Compared with the prior art, the invention has the following advantages:
(1) the operation is simple, and the manual time is saved.
(2) The method is environment-friendly, economical and environment-friendly, and other reagents are not required to be added in the detection process.
(3) The ion chromatography has high detection sensitivity and high result reliability.
Drawings
FIG. 1 is a chromatogram of a standard under elution conditions 1.
FIG. 2 is a chromatogram of a standard under elution conditions 2.
FIG. 3 is an ion chromatogram of a standard.
FIG. 4 is an ion chromatogram for sample detection.
Detailed Description
The following examples are provided to further illustrate the present invention and are not intended to limit the scope of the invention.
The required devices are DIONEX ICS-2000 ion chromatograph, anion suppressor, conductivity detector, analytical column AS19-HC anion exchange column (4X 250mm), guard column AG19 (4X 50 mm).
Required reagents: the ultrapure water had a resistivity of 18.2 M.OMEGA.cm (25 deg.C), monochloroacetic Acid (AR), dichloroacetic Acid (AR), trichloroacetic Acid (AR), anhydrous sodium sulfate (AR), potassium hydroxide rinse (Thermo).
1. Preparation of standard solution: preparation of chloroacetic acid mixed standard solution: accurately weighing monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sodium sulfate standard substance, and respectively preparing into stock solutions with concentration of 10000ug/L, 1000ug/L, 1000ug/L and 1000ug/L with ultrapure water. Storing at 4 ℃ in the dark.
2. Determination of optimal conditions: and (3) carrying out ion chromatography analysis on the standard solution in the step, wherein under the conditions that the sample injection amount is 25uL, the flow rate is 1.0mL/min, and the detection column temperature is 35 ℃, the conditions are as follows: carrying out equal-gradient leaching, wherein the concentration of leaching liquor is 25mol/L, and the time is 35 min; condition 2: gradient elution is carried out, the concentration of the eluent is 0-18min:10mmol/L, 18-25min:25mmol/L, 25-35min:10mmol/L, the optimal detection conditions are obtained by synthesizing detection conditions of symmetrical peak shape, high sensitivity, good reproducibility and the like, wherein the optimal detection conditions are that the sample size is 25 mu L, the concentration of the eluent is 0-18min:10mmol/L, 18-25min:35mmol/L, 25-26min:10mmol/L, flow rate 1.0 mL/min. And (4) analyzing the standard substance of the prepared mixed standard solution under the optimal detection condition.
3. Drawing a standard curve: diluting a standard stock solution of monochloroacetic acid to a standard solution of 500ug/mL, 600ug/mL, 700ug/mL, 800ug/mL, 900ug/mL, 1000ug/mL, diluting a standard stock solution of dichloroacetic acid to a standard solution of 20ug/mL, 25ug/mL, 30ug/mL, 35ug/mL, 40ug/mL, 45ug/mL, diluting a standard stock solution of trichloroacetic acid to a standard solution of 15ug/mL, 20ug/mL, 25ug/mL, 30ug/mL, 35ug/mL, diluting a standard stock solution of sulfate radical to a standard solution of 2ug/mL, 4ug/mL, 6ug/mL, 8ug/mL, 10ug/mL, performing ion chromatography on the series of standard solutions under the optimal detection conditions, and respectively drawing a correction curve by taking the concentration of monochloroacetic acid, the concentration of dichloroacetic acid, the concentration of trichloroacetic acid and the concentration of sulfate radical as abscissa and taking the peak area as ordinate, so as to obtain a correction curve equation, wherein linear correlation coefficients and linear ranges are shown in table 1.
Table 1: linear range and correlation coefficient of measured object
| Object to be measured | Linear Range (mg/L) | Linear equation of equations | Correlation coefficient |
| Monochloroacetic acid | 500-1000 | Y＝0.0818x+8.5168 | 0.9991 |
| Dichloroacetic acid | 20-45 | Y＝0.1876x-3.077 | 0.9996 |
| Trichloroacetic acid | 15-35 | Y＝0.1186x-1.3643 | 0.9996 |
| Sulfate radical | 2-10 | Y＝0.2025x+0.0396 | 0.9996 |
4. Reproducibility test: under the best detection condition, the repeatability of the sulfate detection of monochloroacetic acid, dichloroacetic acid and trichloroacetic acid in chloroacetic acid is examined, the experiment is carried out by repeating 6 times of parallel detection on the sample, and the obtained data are as follows:
table 2: standard deviation of repeated detection of analyte in sample
| 1 | 2 | 3 | 4 | 5 | 6 | X | RSD,％ | |
| Monochloroacetic acid | 0.7661 | 0.7663 | 0.7665 | 0.7664 | 0.7669 | 0.7664 | 0.7664 | 0.03 |
| Dichloroacetic acid | 0.0451 | 0.0453 | 0.0455 | 0.0457 | 0.0454 | 0.0451 | 0.0454 | 0.52 |
| Trichloroacetic acid | 0.0298 | 0.0301 | 0.0302 | 0.0296 | 0.0297 | 0.298 | 0.0299 | 0.78 |
| Sulfate radical | 0.0207 | 0.0206 | 0.0204 | 0.0205 | 0.0203 | 0.0206 | 0.0205 | 0.72 |
5. Detection of the actual sample:
(1) and (4) detecting the sample. Taking chloroacetic acid product in production, accurately weighing 1.0000g, dissolving with ultrapure water, diluting to 10000 times, directly injecting sample, and detecting under optimal detection condition.
(2) Preparing and detecting a standard substance: the data obtained are as follows
Table 3: recovery rate of standard substance after adding standard substance
Claims (1)
1. A method for detecting monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radical in chloroacetic acid by ion chromatography is characterized by comprising the following steps: diluting a sample to be detected ten thousand times, analyzing the peak area of a sample diluent by adopting an ion chromatograph, comparing the peak area with a standard correction curve, and obtaining the concentrations of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radicals in the diluent, thereby obtaining the concentrations of monochloroacetic acid, dichloroacetic acid, trichloroacetic acid and sulfate radicals in the sample to be detected, and the detection condition of the ion chromatograph: the chromatographic column is an AS19-HC analytical column, the protective column is AG19, the suppressor is an ASRS suppressor, the sample size is 20-30 mu L, the eluent is KOH, gradient elution is carried out, the detection is completed within 30min, and the gradient elution conditions are AS follows:
0-18min：10mmol/L；
18-25min：35mmol/L；
25-26min：10mmol/L。
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| CN110346503A (en) * | 2019-05-29 | 2019-10-18 | 北京市水文总站 | Detect the analysis method of dichloroacetic acid and trichloroacetic acid in water |
| CN112305144A (en) * | 2019-07-30 | 2021-02-02 | 游咏妍 | Method for measuring dichloroacetic acid and trichloroacetic acid in water by ion chromatography |
| CN110441464A (en) * | 2019-08-09 | 2019-11-12 | 南通化学环境监测站有限公司 | Monoxone method for measurement of concentration in a kind of workplace carboxylic acids |
| CN110632243B (en) * | 2019-10-23 | 2021-10-12 | 中国日用化学研究院有限公司 | Method for simultaneously determining contents of glycolic acid, monochloroacetic acid and dichloroacetic acid in alcohol ether carboxylate |
| CN113109462B (en) * | 2021-03-10 | 2022-12-20 | 南京海纳医药科技股份有限公司 | Method for detecting chloroacetic acid in lidocaine |
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