CN-121978147-A - Method for rapidly detecting arsenic content in chemical wastewater

Abstract

The invention relates to a method for rapidly detecting arsenic content in chemical wastewater, which comprises the following steps of S1 sample pretreatment optimization, S2 energy dispersion X-ray fluorescence instrument parameter debugging, setting an energy detection interval of an instrument according to the characteristic X-ray energy range of arsenic elements, S3 standard curve establishment, collection of a plurality of groups of chemical wastewater standard samples with known arsenic content, detection by adopting an energy dispersion X-ray fluorescence instrument, drawing and fitting to obtain a standard curve, S4 actual sample detection, putting the sample to be detected into the energy dispersion X-ray fluorescence instrument after debugging to obtain the characteristic X-ray intensity of arsenic elements of the sample to be detected, and substituting the intensity value into the standard curve to calculate and obtain the arsenic content in the sample to be detected. The invention simplifies the operation flow, reduces the labor cost and the error risk, and realizes the high-efficiency and accurate detection of the arsenic content in the chemical wastewater.

Inventors

• ZHAO DEGANG
• WANG PENGYE
• JIANG XIN
• CHEN WEICHUAN
• FANG PEIJIN
• FENG LIMING

Assignees

• 金川集团永昌铜业有限公司
• 金川集团铜贵股份有限公司

Dates

Publication Date

20260505

Application Date

20260127

Claims (6)

1. 1. A method for rapidly detecting arsenic content in chemical wastewater comprises the following steps: s1, pretreatment optimization of a sample: taking a chemical wastewater vulcanized liquid sample, and filtering by adopting a filter membrane with the aperture of 0.45-0.8 mu m to obtain a sample to be detected; s2, parameter debugging of the energy dispersion X-ray fluorescence instrument: Setting an energy detection interval of the instrument according to the characteristic X-ray energy range of the arsenic element, and adjusting the detection time of the instrument to determine the optimal detection time parameter on the premise of ensuring that the detection sensitivity can accurately identify small changes of 0.01mg/L and below of the arsenic content; S3, establishing a standard curve: Collecting a plurality of groups of chemical wastewater standard samples with known arsenic content, carrying out 3 times of parallel detection on each group of standard samples by adopting the energy dispersion X-ray fluorescence instrument debugged in the step S2, recording corresponding characteristic X-ray intensity data, taking the average value of the characteristic X-ray intensity as the corresponding intensity data of the group of standard samples, and then drawing and fitting by using a linear regression method to obtain a standard curve by taking the arsenic content of the standard samples as an abscissa and the average value of the corresponding characteristic X-ray intensity as an ordinate; s4, detection of actual samples: And (3) placing the sample to be detected obtained in the step (S1) into a debugged energy dispersion X-ray fluorescence instrument, detecting according to an optimal detection time parameter to obtain the arsenic element characteristic X-ray intensity of the sample to be detected, substituting the intensity value into the standard curve established in the step (S3), and calculating to obtain the arsenic content in the sample to be detected.
2. 2. The method for rapidly detecting arsenic content in chemical wastewater according to claim 1, wherein the characteristic X-ray energy range of the arsenic element in the step S2 is set to be 10.5-11.5 keV.
3. 3. The method for rapidly detecting arsenic content in chemical wastewater according to claim 1, wherein the optimal detection time parameter in the step S2 is determined to be 3-5 minutes.
4. 4. The method for rapidly detecting arsenic content in chemical wastewater according to claim 1, wherein the standard samples of the chemical wastewater with known arsenic content in the step S3 are set to be 5-8 groups, and each group of standard samples has arsenic content covering 0.01-10 mg/L and uniform concentration gradient.
5. 5. The method for rapidly detecting arsenic content in chemical wastewater according to claim 1, wherein the linear correlation coefficient R 2 of the standard curve in the step S3 is more than or equal to 0.999.
6. 6. The method for rapidly detecting arsenic content in chemical wastewater according to claim 1, wherein the step S4 further comprises a detection result verification step of performing parallel detection on the same sample to be detected by adopting a traditional method of nitric acid acidification pretreatment and spectrometer analysis, comparing detection results of the two methods, and judging that the detection result of the method is effective if the deviation is less than 5%.

Description

Method for rapidly detecting arsenic content in chemical wastewater Technical Field The invention relates to the technical field of water quality detection, in particular to a method for rapidly detecting arsenic content in chemical wastewater. Background In the chemical production process, particularly in chemical branch factories related to copper industry production, sulfide-containing wastewater can be generated, and the arsenic content in the wastewater is an important process control and environment-friendly monitoring index. Arsenic is used as a toxic and harmful element, and the content of the arsenic is too high, so that the stability of a subsequent production process can be influenced, and serious pollution to the environment is possible, and the arsenic content in chemical wastewater needs to be accurately and timely detected. At present, a method of 'sample nitric acid pretreatment + spectrometer analysis' is commonly adopted for analysis of arsenic content in a vulcanized liquid sample of a chemical engineering branch factory. The specific flow of the method comprises the steps of filtering, acidifying, separating, detecting, uploading data and the like, and the analysis time of a single sample is up to 2 hours. In actual production, the process control needs to adjust parameters in time according to the arsenic content detection result so as to ensure stable production and avoid waste, and the detection period of 2 hours is difficult to meet the requirement of the process control on timeliness, which may cause process deviation in the production process due to incapability of timely acquiring arsenic content data, and increase production waste and environmental protection risks. Meanwhile, the nitric acid acidification pretreatment step in the traditional method is time-consuming, has the problems of complex operation and easiness in introducing human errors, and the use of nitric acid can increase the detection cost and the environment-friendly treatment pressure. Therefore, development of a method for detecting arsenic content in chemical wastewater, which can shorten the detection time and simplify the operation flow and ensure the detection accuracy, is needed. Disclosure of Invention The invention aims to provide a simple, accurate and rapid method for detecting arsenic content in chemical wastewater. In order to solve the problems, the method for rapidly detecting the arsenic content in the chemical wastewater comprises the following steps: s1, pretreatment optimization of a sample: taking a chemical wastewater vulcanized liquid sample, and filtering by adopting a filter membrane with the aperture of 0.45-0.8 mu m to obtain a sample to be detected; s2, parameter debugging of the energy dispersion X-ray fluorescence instrument: Setting an energy detection interval of the instrument according to the characteristic X-ray energy range of the arsenic element, and adjusting the detection time of the instrument to determine the optimal detection time parameter on the premise of ensuring that the detection sensitivity can accurately identify small changes of 0.01mg/L and below of the arsenic content; S3, establishing a standard curve: Collecting a plurality of groups of chemical wastewater standard samples with known arsenic content, carrying out 3 times of parallel detection on each group of standard samples by adopting the energy dispersion X-ray fluorescence instrument debugged in the step S2, recording corresponding characteristic X-ray intensity data, taking the average value of the characteristic X-ray intensity as the corresponding intensity data of the group of standard samples, and then drawing and fitting by using a linear regression method to obtain a standard curve by taking the arsenic content of the standard samples as an abscissa and the average value of the corresponding characteristic X-ray intensity as an ordinate; s4, detection of actual samples: And (3) placing the sample to be detected obtained in the step (S1) into a debugged energy dispersion X-ray fluorescence instrument, detecting according to an optimal detection time parameter to obtain the arsenic element characteristic X-ray intensity of the sample to be detected, substituting the intensity value into the standard curve established in the step (S3), and calculating to obtain the arsenic content in the sample to be detected. The characteristic X-ray energy range of the arsenic element in the step S2 is set to be 10.5-11.5 keV. And in the step S2, the optimal detection time parameter is determined to be 3-5 minutes. And in the step S3, the standard samples of the chemical wastewater with known arsenic content are set into 5-8 groups, the arsenic content of each group of standard samples covers 0.01-10 mg/L, and the concentration gradient is uniform. And the linear correlation coefficient R 2 of the standard curve in the step S3 is more than or equal to 0.999. The step S4 also comprises a detection result verification