CN112461817A - Method for measuring concentration of heavy metal in electroplating waste liquid by ICP (inductively coupled plasma) - Google Patents
Method for measuring concentration of heavy metal in electroplating waste liquid by ICP (inductively coupled plasma) Download PDFInfo
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- CN112461817A CN112461817A CN202011569931.5A CN202011569931A CN112461817A CN 112461817 A CN112461817 A CN 112461817A CN 202011569931 A CN202011569931 A CN 202011569931A CN 112461817 A CN112461817 A CN 112461817A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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Abstract
The invention discloses a method for measuring the concentration of heavy metal in electroplating waste liquid by ICP (inductively coupled plasma), belonging to the technical field of ICP (inductively coupled plasma) detection. The method comprises the following steps: firstly, sampling from the electroplating waste liquid treated by the sequencing batch treatment tank; filtering the liquid, taking 50ml in a 100ml conical flask, heating and evaporating to 10 ml; adding 10ml of concentrated nitric acid, heating and digesting until water is dry, and cooling; adding 5ml of nitric acid and 20ml of deionized water, carrying out ultrasonic treatment in ultrasonic waves for about 30min, dissolving residues and filtering; transferring the filtrate into a 50ml volumetric flask, adding water to a constant volume to a scale, and shaking up; finally, measuring the filtrate by adopting an ICP inductively coupled plasma spectrometer; the method adopts a certain nitric acid system and ultrasonic treatment to eliminate interference factors in the waste liquid sample, keeps the stability of heavy metal ions in the sample liquid, and can efficiently, quickly and accurately measure and analyze various heavy metal elements in the waste liquid.
Description
Technical Field
The invention belongs to the technical field of ICP (inductively coupled plasma) detection, and particularly relates to a method for measuring the concentration of heavy metal in electroplating waste liquid by ICP (inductively coupled plasma).
Background
The electroplating production wastewater has various types, complex components and different treatment modes, so the wastewater is reduced and reduced in the aspect of preventing and treating water pollution, and belongs to the tail end treatment of wastewater. Since the electroplating wastewater contains a complexing agent and a chelating component, the treatment is difficult to remove heavy metals.
Contain multiple high concentration's heavy metal in the electroplating effluent, it is main to have chromium, nickel etc. pollute extremely serious, should collect alone, for the overall management, collect the waste liquid back, the pumping goes into the preface batch type and handles the pond and carry out abundant processing, need survey liquid wherein each heavy metal concentration is up to standard after the processing, the corresponding sewage treatment system of re-pumping income or advance desliming system and handle.
At present, methods for measuring heavy metals in industrial wastewater mainly comprise an atomic absorption spectrometry and a colorimetric method, and the methods are single-element analysis, long in multi-element detection time and complex in operation. The ICP inductively coupled plasma atomic emission spectrometer can simultaneously measure a plurality of heavy metal elements in industrial wastewater, but a plurality of interference factors exist in the measurement, and the measurement result is influenced.
Disclosure of Invention
Aiming at the problems of defects and deficiencies in the prior art, the invention provides a method for measuring the concentration of heavy metal in electroplating waste liquid by ICP (inductively coupled plasma), which adopts a certain nitric acid system to be matched with ultrasonic treatment to eliminate interference factors in a waste liquid sample, keeps the stability of heavy metal ions in the sample liquid, and can efficiently, quickly and accurately measure and analyze various heavy metal elements in the waste liquid.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for measuring the concentration of heavy metal in electroplating waste liquid by ICP comprises the following steps:
the method comprises the following steps: sampling, namely collecting liquid from the electroplating waste liquid treated by the sequencing batch treatment tank through a sampler;
step two: filtering the liquid, putting 50ml into a 100ml conical flask, heating and evaporating to 10ml on an electric heating plate;
step three: adding 10ml of concentrated nitric acid into the conical flask, then placing the conical flask on an electric hot plate for heating and digesting, and cooling after water is dried;
step four: adding 5ml of nitric acid and 20ml of deionized water, carrying out ultrasonic treatment in ultrasonic waves for about 30min, dissolving residues and filtering;
step five: transferring the filtrate into a 50ml volumetric flask, adding water to a constant volume to a scale, and shaking up;
step six: and (3) measuring the filtrate by adopting an ICP (inductively coupled plasma) atomic emission spectrometer.
Furthermore, the pH value of the sample solution sampled in the step one is less than or equal to 7, and the concentration of hydrochloric acid or nitric acid is less than or equal to 10%.
Further, the content of the matrix element in the sample solution sampled in the first step must not exceed ten thousand times of the heavy metal element to be detected.
Furthermore, the incident power of the ICP instrument is 900-1300W during measurement.
Further, the atomizer of the ICP instrument works at an atomization pressure of 2.02 multiplied by 105Pa。
The invention has the following beneficial effects: the incident power and the physicochemical pressure of the ICP instrument are optimally selected, so that the stability and the signal-to-back ratio of the measurement are facilitated; a certain nitric acid system is adopted to be matched with ultrasonic treatment to eliminate interference factors in the waste liquid sample and keep the stability of heavy metal ions in the sample liquid; the method has the advantages of high sensitivity, good safety and accurate measurement result, and can be used for efficiently, quickly and accurately measuring and analyzing various heavy metal elements in the waste liquid.
Detailed Description
The following examples are provided to illustrate specific embodiments of the present invention.
The first embodiment is as follows:
a method for measuring the concentration of heavy metal in electroplating waste liquid by ICP comprises the following steps:
the method comprises the following steps: sampling, namely collecting liquid from the electroplating waste liquid treated by the sequencing batch treatment tank through a sampler, wherein the sample amount is 100-200 ml;
step two: filtering the liquid, putting 50ml into a 100ml conical flask, heating and evaporating to 10ml on an electric heating plate;
step three: adding 10ml of concentrated nitric acid into the conical flask, then placing the conical flask on an electric hot plate for heating and digesting, and cooling after water is dried;
step four: adding 5ml of nitric acid and 20ml of deionized water, carrying out ultrasonic treatment in ultrasonic waves for about 30min, dissolving residues and filtering;
step five: transferring the filtrate into a 50ml volumetric flask, adding water to a constant volume to a scale, and shaking up;
step six: and (3) measuring the filtrate by adopting an ICP (inductively coupled plasma) atomic emission spectrometer.
The pH value of the test solution sampled in the step one is less than or equal to 7, and the concentration of hydrochloric acid or nitric acid is less than or equal to 10%.
The content of the matrix elements of the test solution sampled in the step one cannot exceed ten thousand times of the heavy metal elements to be detected.
The working power of the ICP instrument during measurement is 900-1300W, and the proper power is beneficial to measuring the stability and the signal-to-back ratio of element spectral lines.
When the atomizer of the ICP instrument works, the atomization pressure is 2.02 multiplied by 105Pa, at which the intensity of heavy metals in the test solution is reduced.
Specifically, the filtrate is delivered into an atomizer through a peristaltic pump to form fine and even spray, and is loaded into a plasma torch flame with the high temperature of 8000 ℃ generated by high-frequency current together with inert gas argon, and the incandescent plasma is used as an excitation light source to ionize and excite various elements in the test solution. The characteristic radiation spectral line generated in the process of excitation is decomposed into monochromatic spectrums representing all elements by a grating light splitting system, the energy of the spectrums is detected by a semiconductor detector, and the content of the heavy metal element to be detected in the test solution is calculated by referring to a standard solution measured at the same time.
The method is adopted to determine heavy metal elements in the electroplating waste liquid, and an atomic absorption method is used for comparison analysis, so that whether the concentration of each heavy metal in the electroplating waste liquid treated by the sequencing batch type treatment tank reaches the standard is judged, and the electroplating waste liquid is treated in the next step.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. The present invention is not limited to the above-described embodiments, which are described in the specification and illustrated only for illustrating the principle of the present invention, but various changes and modifications may be made within the scope of the present invention as claimed without departing from the spirit and scope of the present invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. An ICP method for measuring the concentration of heavy metal in electroplating waste liquid is characterized by comprising the following steps:
the method comprises the following steps: sampling, namely collecting liquid from the electroplating waste liquid treated by the sequencing batch treatment tank through a sampler;
step two: filtering the liquid, putting 50ml into a 100ml conical flask, heating and evaporating to 10ml on an electric heating plate;
step three: adding 10ml of concentrated nitric acid into the conical flask, then placing the conical flask on an electric hot plate for heating and digesting, and cooling after water is dried;
step four: adding 5ml of nitric acid and 20ml of deionized water, carrying out ultrasonic treatment in ultrasonic waves for about 30min, dissolving residues and filtering;
step five: transferring the filtrate into a 50ml volumetric flask, adding water to a constant volume to a scale, and shaking up;
step six: and (3) measuring the filtrate by adopting an ICP (inductively coupled plasma) atomic emission spectrometer.
2. An ICP method as recited in claim 1, wherein the method comprises the following steps: the pH value of the test solution sampled in the step one is less than or equal to 7, and the concentration of hydrochloric acid or nitric acid is less than or equal to 10%.
3. An ICP method as recited in claim 1, wherein the method comprises the following steps: the content of the matrix elements of the test solution sampled in the step one cannot exceed ten thousand times of the heavy metal elements to be detected.
4. An ICP method as recited in claim 1, wherein the method comprises the following steps: and the incident power is 900-1300W when the ICP instrument is used for measuring.
5. An ICP method as recited in claim 4, wherein the method comprises the following steps: when the atomizer of the ICP instrument works, the atomization pressure is 2.02 multiplied by 105Pa。
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4362629A (en) * | 1980-10-08 | 1982-12-07 | Murata Manufacturing Co., Ltd. | Method for processing solution including heavy metal |
| CN106399695A (en) * | 2016-10-09 | 2017-02-15 | 武汉华喻燃能工程技术有限公司 | Method for sequential extraction of heavy metal elements in petroleum coke |
| CN106769919A (en) * | 2016-11-25 | 2017-05-31 | 防城港市质量技术监督局 | A kind of assay method of heavy metal in waste water Cr |
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2020
- 2020-12-25 CN CN202011569931.5A patent/CN112461817A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4362629A (en) * | 1980-10-08 | 1982-12-07 | Murata Manufacturing Co., Ltd. | Method for processing solution including heavy metal |
| CN106399695A (en) * | 2016-10-09 | 2017-02-15 | 武汉华喻燃能工程技术有限公司 | Method for sequential extraction of heavy metal elements in petroleum coke |
| CN106769919A (en) * | 2016-11-25 | 2017-05-31 | 防城港市质量技术监督局 | A kind of assay method of heavy metal in waste water Cr |
Non-Patent Citations (8)
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| 严伟等: "超声波协助提取技术", 《化工进展》, vol. 21, no. 9, 31 December 2002 (2002-12-31), pages 649 - 651 * |
| 于瑞莲等: "超声辅助硝酸提取-冷原子吸收光谱法测定土壤/沉积物中汞", 《冶金分析》, vol. 30, no. 12, 31 December 2010 (2010-12-31), pages 56 - 59 * |
| 刘卫丽等: "电感耦合等离子体质谱仪测定水体中的12种元素", 《南方金属》, no. 05, 15 October 2016 (2016-10-15), pages 27 - 29 * |
| 周春艳等: "离子色谱-电感耦合等离子体质谱法测定野生食用菌中6种砷形态", 《中国卫生检验杂志》, vol. 27, no. 14, 25 July 2017 (2017-07-25), pages 1980 - 1982 * |
| 周雷等: "超声辅助酸提取-ICP-MS快速测定水产品中多种重金属", 《食品科技》, vol. 45, no. 08, 20 August 2020 (2020-08-20), pages 292 - 297 * |
| 李杨等: "电感耦合等离子体质谱仪测定水体中的23种元素", 《绿色科技》, no. 07, 25 July 2013 (2013-07-25), pages 219 - 220 * |
| 赵亚男等: "ICP-AES分析技术的应用研究进展", 《广东微量元素科学》, vol. 17, no. 05, 15 May 2010 (2010-05-15), pages 18 - 24 * |
| 鲁丹、阮毅: "电感耦合等离子体原子发射光谱法测定工业废水中铅、镉、铬和砷", 《理化检验-化学分册》, vol. 43, no. 12, 31 December 2007 (2007-12-31), pages 1023 * |
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