CN104634707A - Method for detecting forms of trace metal particles in smoke based on plasma inductively-coupled atomic absorption spectrum - Google Patents
Method for detecting forms of trace metal particles in smoke based on plasma inductively-coupled atomic absorption spectrum Download PDFInfo
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- CN104634707A CN104634707A CN201510076553.XA CN201510076553A CN104634707A CN 104634707 A CN104634707 A CN 104634707A CN 201510076553 A CN201510076553 A CN 201510076553A CN 104634707 A CN104634707 A CN 104634707A
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Abstract
The invention discloses a method for detecting forms of trace metal particles in smoke based on a plasma inductively-coupled atomic absorption spectrum. The method comprises the following steps: carrying out ionization on a standard solution through inductively coupled plasma (ICP), and then continuously acquiring a single signal of a to-be-detected metal element by virtue of a direct-reading spectrometer (OES); calculating to obtain the quality, corresponding to the unit signal strength of the to-be-detected metal element, of to-be-detected metal ions; collecting smoke through a solvent, thereby obtaining a to-be-detected solution containing metal particles, and obtaining a signal of the to-be-detected metal element in the to-be-detected solution; and performing signal analysis to obtain a form distribution diagram of sizes and number of the metal particles in the to-be-detected solution. The method is capable of enduring interference of a complicated background, and is high in detection efficiency and low in lower detection limit; and the form distribution data about the sizes, the number and the like of the metal particles in the smoke can be accurately obtained.
Description
Technical field
The present invention relates to a kind of method detecting trace-metal particle shape in flue gas based on plasma inductance linking atom absorption spectrum, belong to particle shape metal detection technical field.
Background technology
Heavy metal substance in environment may be detrimental to health, and at koniology, may be distributed with some heavy metal substance in water body and soil.In the development that modern industry is produced, heavy metal substance is extracted from ore, is carried by air, water body flow, and the transportation of the mankind, progressively spread in the environment of ours, eventually through air, potable water and food enter human body, cause negative impact to health.As everyone knows, the heavy metal of different shape has different toxicity.The heavy metal of ionic forms is easy to migration, often strong toxicity.The heavy metal of particle shape, migration performance is weaker than ion, and toxicity is also more weak.Be both particle shape, negative ion is different, and the toxicity of heavy metal is also different.Such as cadmium carbonate, the physiological-toxicity of cadmium oxide and cadmium sulfide just weakens successively.
Current Heavy Metals research adopts sequential extraction procedures usually, the three step extraction methods (being called for short BCR method) of wherein most importantly European Union's proposition.The method adopts the solvent of different solubility property to extract testing sample successively, detects the concentration of heavy metal ion in supernatant liquor after centrifuging, obtains the content of beary metal of different dissolving power.The method is applicable to detection level at ten thousand/several sample to a few percent.If the content of heavy metal is low to moderate parts per million (ppm) in sample, due to operation and the error brought of slightly solubility sample diffusion can be serious the accuracy affecting result.
Liquid chromatography ICP coupling can detect the heavy metal of pole low content in sample.But be only limitted to the heavy metal ion that can be separated by liquid chromatography and the heavy metal organically combining state.Its chemical constitution is determined by the appearance time that this kind of material is different in liquid chromatography.Heavy metal particles can not be separated by liquid chromatography qualitative, also just can not adopt the heavy metal particles of liquid chromatography research pole low content.The electron microscope being furnished with energy depressive spectroscopy can observe small-sized heavy metal particles, is obtained the element composition information of particle by energy-spectrum scanning.But content of beary metal is low in fume sample, the organism containing a large amount of high concentration in sample, Electronic Speculum can not tell the little heavy metal particles of small-sized quantity from organism background.Dynamic light scattering can obtain the size of particle and the information of number in sample, but in fume sample, be easily subject to the interference of other materials, and this technology also cannot obtain the element composition signal in particle simultaneously.
Summary of the invention
For in prior art to the defect that the method for various detection solid metallic ion exists, the object of the invention is the method being to provide traces of solids metallic particles form in a kind of simple and quick detection flue gas, the method can the interference of resistance to complex background, detection efficiency high, Monitoring lower-cut is low, can obtain the fractions distribution data such as size and number of metallic particles form in flue gas.
The invention provides a kind of method detecting trace-metal particle shape in flue gas based on plasma inductance linking atom absorption spectrum, it is characterized in that, comprise the following steps:
Step one: the standard solution containing metallic ion to be measured of concentration known is continuously pumped in ICP and carries out plasma, with each individual signals of OES detecting device continuous acquisition metallic element to be measured, according to the concentration of metallic ion to be measured in standard solution and the volume of standard solution and the total signal strength of metallic element to be measured that pump into ICP, calculate the quality of metallic ion to be measured corresponding to the unit signal intensity of metallic element to be measured;
Step 2: the solution to be measured being obtained containing metal particle by solvent collection flue gas, by the individual signals of metallic element to be measured in the method continuous acquisition liquid to be measured of step one, the size of GOLD FROM PLATING SOLUTION metal particles to be measured and the fractions distribution figure of number is obtained by each individual signals analysis, the number of the individual signals obtained equals the number of the metallic particles containing metallic element to be measured in solution to be measured, is calculated the quality of metallic element to be measured in each metallic particles by each individual signals intensity respectively.
Of the present inventionly detect the method for trace-metal particle shape in flue gas by plasma inductance linking atom absorption spectrum and also comprise following preferred version:
In preferred scheme, metallic ion to be measured is cadmium ion, lead ion, copper ion, ferric ion, zinc ion, chromium ion, magnesium ion, arsenic ion, gold ion, silver ion or tin ion.
Each individual signals intensitometer first by metallic element to be measured in step one in preferred scheme calculates the total signal intensity of this metallic element to be measured, go out the gross mass of the metallic ion to be measured in standard solution according to the concentration of metallic ion to be measured in standard solution and the volume computing of standard solution that pumps into ICP, then obtain the quality of metallic ion to be measured corresponding to this metallic ion unit signal intensity to be measured divided by the total signal strength of this metallic ion to be measured with the gross mass of metallic ion to be measured in standard solution.Wherein, the cumulative volume of standard solution of the standard solution cumulative volume=nebulization efficiency of ICP × for testing is pumped into; For the cumulative volume=pump into speed × detection time of the standard solution tested.
Individual signals intensity by metallic element to be measured in step 2 in preferred scheme is multiplied by the quality that correction coefficient obtains containing in single metal particle this metallic element to be measured, and correction coefficient equals the total signal strength of gross mass divided by this metallic ion to be measured of metallic ion to be measured in standard solution.Wherein, the signal intensity of the quality=correction coefficient × metallic element to be measured of metallic element to be measured in metallic particles; The total signal strength of metallic ion gross mass ÷ to be measured metallic ion to be measured in correction coefficient=standard solution.
In preferred scheme, the size of GOLD FROM PLATING SOLUTION metal particles to be measured is 1 nanometer ~ 500 nanometer.
Detecting analysis time section in preferred scheme is 10 seconds ~ 60 seconds.
In preferred scheme, sampling interval duration is the sampling interval of 0.1ms ~ 50ms, and gathering number is 10,000 ~ 200,000 continuous print individual signals.
In preferred scheme, in liquid to be measured, the concentration of metallic particles is 0.01 ~ 0.1 μ g/L.
In preferred scheme, solvent is at least one in water, methyl alcohol, ethanol, acetone.
By solvent collection flue gas in preferred scheme, then after being 0.01 ~ 0.1ug/L by the concentration that deionized water is diluted to metallic particles, ultrasonic disperse, obtains the finely dispersed solution to be measured of metallic particles.
In preferred scheme, solution to be measured pumps in ICP, metallic particles in ICP by plasma, generate the metallic ion of positively charged, OES detecting device is with high frequency collection metallic ion signal to be measured, the wavelength signals collected is collected, obtains the fractions distribution figure of metallic particles in sample solution.
The resultant signal number that in method of the present invention, OES detecting device collects equals the total number of the GOLD FROM PLATING SOLUTION metal particles entering ICP, and wherein, the signal order number containing metallic element to be measured, is the metallic particles number containing this kind of metallic element to be measured.The signal intensity of the individual signals of metallic element to be measured is multiplied by the quality that correction coefficient equals metallic element to be measured in this metallic particles; Can in the hope of the number of total GOLD FROM PLATING SOLUTION metal particles and size by the method.
Beneficial effect of the present invention: the present invention first using plasma inductive coupling atomic absorption spectrum detects trace-metal particle shape in flue gas, effectively can obtain the fractions distribution data such as size and number of metallic particles in flue gas, quantitative test goes out various metal, the method is simple to operate, detection efficiency is high, can restrain oneself the interference of complex background, Monitoring lower-cut is extremely low.
Accompanying drawing explanation
[Fig. 1] is the ICP-OES collection of illustrative plates of the cadmium nitrate aqueous solution of 50ppb in embodiment 1;
[Fig. 2] is the ICP-OES collection of illustrative plates of cadmium element in cigarette smoke in embodiment 1;
[Fig. 3] is the ICP-OES collection of illustrative plates of the plumbi nitras aqueous solution of 10ppb in embodiment 2;
[Fig. 4] is the ICP-OES collection of illustrative plates of lead element in cigarette smoke in embodiment 2.
Embodiment
Following examples are intended to content of the present invention is described, instead of the further restriction to scope.Embodiment 1
Be configured with the cadmium nitrate solution of 50ppb concentration, adopt ICP-OES to detect, testing conditions is as follows: cadmium atom wavelength is: 214nm; Get peak mode: single-point gets peak; Interval time 0.1ms; Reading times: 10000; Repeat 5 times; Total sampling time 30s; Detecting pattern: mode standard; Fig. 1 is shown in by collection of illustrative plates after collection.
Experimentally condition, peristaltic pump flow velocity is: 0.18mL min
-1, analysis time is 40s, and calculating known total liquid inlet volume is thus 0.12mL, and nebulization efficiency is 6%, and calculating the known liquor capacity entering plasma is 7.2 μ L.By signal plus all in Fig. 1, obtaining resultant signal is 712052.By concentration and the sampling volume of cadmium in solution, the total mass number calculating known cadmium ion is: 0.72*10
-10g.According to formula, calculating correction coefficient is: 0.6552*10
-15g count
-1.
Main flume is collected and is dissolved in methanol solution.With deionized water, flue gas methanol solution is diluted.Analyze the cadmium element in this mixed solution with ICP-OES, adopt the analysis condition that Fig. 1 is same, Fig. 2 is shown in by the collection of illustrative plates after collection.
According to same experiment condition, peristaltic pump flow velocity is: 0.18mL min
-1, analysis time is 40s, and calculating known total liquid inlet volume is thus 0.12mL, and nebulization efficiency is 6%, and calculating the known liquor capacity entering plasma is 7.2 μ L.The signal collected adds up to 272838, this value is multiplied with correction coefficient, and acquisition total mass number is 1.78*10
-10g.According to Fig. 1, total particle number is 27878, and averaged count is: 9.094, and average weight is 6.52*10
-9ng.
Embodiment 2
Be configured with the lead nitrate solution of 25ppb concentration, adopt ICP-OES to detect, testing conditions is as follows: lead element wavelength 220.35nm; Get peak mode: single-point gets peak; Interval time 0.1ms; Reading times: 10000; Repeat 5 times; Total sampling time 30s; Detecting pattern: mode standard; Fig. 3 is shown in by collection of illustrative plates after collection.
Experimentally condition, peristaltic pump flow velocity is: 0.18mL min
-1, analysis time is 24s, and calculating known total liquid inlet volume is thus 0.072mL, and nebulization efficiency is 6%, and calculating the known liquor capacity entering plasma is 4.32 μ L.By signal plus all in Fig. 3, obtaining resultant signal is 313347.By concentration plumbous in solution and sampling volume, the total mass number calculating known lead ion is: 0.75*10
-10g.According to formula, calculating correction coefficient is: 2.39*10
-16g count
-1.
According to same experiment condition, the main flume of cigarette is collected and is dissolved in methanol solution.Dilute with deionized water.Analyze the lead element in this mixed solution with ICP-OES, adopt the analysis condition that Fig. 3 is same, Fig. 4 is shown in by the collection of illustrative plates after collection.
Peristaltic pump flow velocity is: 0.18mL min
-1, analysis time is 24s, and calculating known total liquid inlet volume is thus 0.072mL, and nebulization efficiency is 6%, and calculating the known liquor capacity entering plasma is 4.32 μ L.The signal collected adds up to 42821, this value is multiplied with correction coefficient, and acquisition total mass number is 1.02*10
-11g.According to Fig. 4, total particle number is 5329, and averaged count is: 1.42, and average weight is 1.97*10
-9ng.
Claims (8)
1. detect a method for trace-metal particle shape in flue gas based on plasma inductance linking atom absorption spectrum, it is characterized in that, comprise the following steps:
Step one: the standard solution containing metallic ion to be measured of concentration known is continuously pumped in ICP and carries out plasma, with each individual signals of OES detecting device continuous acquisition metallic element to be measured, according to the concentration of metallic ion to be measured in standard solution and the volume of standard solution and the total signal strength of metallic element to be measured that pump into ICP, calculate the quality of metallic ion to be measured corresponding to the unit signal intensity of metallic element to be measured;
Step 2: the solution to be measured being obtained containing metal particle by solvent collection flue gas, by each individual signals of metallic element to be measured in the method continuous acquisition liquid to be measured of step one, the size of GOLD FROM PLATING SOLUTION metal particles to be measured and the fractions distribution figure of number is obtained by each individual signals analysis, the number of the individual signals obtained equals the number of the metallic particles containing metallic element to be measured in solution to be measured, is calculated the quality of metallic element to be measured in each metallic particles by each individual signals intensity respectively.
2. method according to claim 1, is characterized in that, described metallic ion to be measured is cadmium ion, lead ion, copper ion, ferric ion, zinc ion, chromium ion, magnesium ion, arsenic ion, gold ion, silver ion or tin ion.
3. method according to claim 1, it is characterized in that, each individual signals intensitometer first by metallic element to be measured in step one calculates the total signal intensity of this metallic element to be measured, go out the gross mass of the metallic ion to be measured in standard solution according to the concentration of metallic ion to be measured in standard solution and the volume computing of standard solution that pumps into ICP, then obtain the quality of metallic ion to be measured corresponding to this metallic ion unit signal intensity to be measured divided by the total signal strength of this metallic ion to be measured with the gross mass of metallic ion to be measured in standard solution.
4. method according to claim 1, it is characterized in that, be multiplied by by the individual signals intensity of metallic element to be measured the quality that correction coefficient obtains containing in single metal particle this metallic element to be measured in step 2, correction coefficient equals the total signal strength of gross mass divided by this metallic ion to be measured of metallic ion to be measured in standard solution.
5. method according to claim 1, is characterized in that, the size of GOLD FROM PLATING SOLUTION metal particles to be measured is 1 nanometer ~ 500 nanometer.
6. method according to claim 1, is characterized in that, detection section analysis time is 10 seconds ~ 60 seconds; Sampling interval duration is the sampling interval of 0.1ms ~ 50ms, and gathering number is 10,000 ~ 200,000 continuous print individual signals.
7. method according to claim 1, is characterized in that, in described liquid to be measured, the concentration of metallic particles is 0.01 ~ 0.1 μ g/L.
8. method according to claim 1, is characterized in that, described solvent is at least one in water, methyl alcohol, ethanol, acetone.
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| CN106872558A (en) * | 2017-03-01 | 2017-06-20 | 中国科学院南京土壤研究所 | A kind of method of Nano Silver and silver ion in measure plant |
| CN109682793A (en) * | 2019-01-22 | 2019-04-26 | 黄豪杰 | It is a kind of at the same measure lead in coupernick, cadmium content inductively coupled plasma emission spectrography rapid detection method |
| CN111105979A (en) * | 2018-10-26 | 2020-05-05 | 安捷伦科技有限公司 | Automatic detection of nanoparticles using single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) |
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| CN111105979A (en) * | 2018-10-26 | 2020-05-05 | 安捷伦科技有限公司 | Automatic detection of nanoparticles using single particle inductively coupled plasma mass spectrometry (SP-ICP-MS) |
| CN109682793A (en) * | 2019-01-22 | 2019-04-26 | 黄豪杰 | It is a kind of at the same measure lead in coupernick, cadmium content inductively coupled plasma emission spectrography rapid detection method |
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