CN103487427A - Method for detecting metallic elements in atmospheric exhaust gas particulates - Google Patents
Method for detecting metallic elements in atmospheric exhaust gas particulates Download PDFInfo
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- CN103487427A CN103487427A CN201310450385.7A CN201310450385A CN103487427A CN 103487427 A CN103487427 A CN 103487427A CN 201310450385 A CN201310450385 A CN 201310450385A CN 103487427 A CN103487427 A CN 103487427A
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Abstract
The invention provides a method for detecting metallic elements in atmospheric exhaust gas particulates. The method comprises the steps as follows: sample preprocessing is performed by using a microwave digestion technology firstly; after a sample is preprocessed, to-be-detected metallic elements are detected by default optimum spectral lines of an inductively coupled plasma radiating spectrograph; the to-be-detected metallic elements comprise one or more of aluminum, barium, cadmium, chromium, copper, manganese, molybdenum, nickel, lead, strontium, tin and zinc; a detection limit of the method is measured, and detection limits of the to-be-detected metallic elements are all 0.04 mg/L below; the precision of the method is measured, the relative standard deviation of the to-be-detected metallic elements is 2.36%-7.03%; and the accuracy of the method is measured, and the recovery rate of the to-be-detected metallic elements is 89.6%-119%. The method is high in sensitivity and accuracy and good in precision and can be applied to simultaneous detection of various metallic elements in an actual sample; and the detection result is better.
Description
Technical field
The present invention relates to the exhaust gas particle object detecting method, in particular to a kind of method that detects metallic element in atmosphere exhaust gas particle thing.
Background technology
Along with developing rapidly of industry, various pollutants also enter into environment thereupon, wherein the metallic pollution air quality that has been the serious impact of metal pollutant in a class, the especially Atmospheric particulates that the proportion that accounts in pollutant is larger.So, departments of government has strengthened the monitoring dynamics to Metals in Atmospheric Particulates, at present common assay method mainly contains: atomic absorption spectrophotometry, inductively coupled plasma mass spectrometry, inductively coupled plasma emission spectrography, wherein inductively coupled plasma emission spectrography because of its have highly sensitive, disturb less, the range of linearity is wide and the advantage that can simultaneously measure Determination of multiple metal elements is widely used.But, when being detected, the pretreatment condition of sample and analysis condition also may affect the result of detection, therefore, to be optimized sample pretreatment and analysis condition, could obtain the detection method that clever lightness is high, accuracy is high, precision is good, obtain satisfied result in actual sample detects.
Summary of the invention
The invention solves deficiency of the prior art, the method for metallic element in a kind of highly sensitive, accuracy is high, precision is good detection atmosphere exhaust gas particle thing is provided.
Technical scheme of the present invention is: a kind of method that detects metallic element in atmosphere exhaust gas particle thing, at first the method adopts microwave digestion technology to carry out sample pretreatment, sample metallic element to be measured after pre-service is used the best spectral line of induction coupled plasma radiating light spectrometer acquiescence to be measured, described metallic element to be measured comprises one or more in aluminium, barium, cadmium, chromium, copper, manganese, molybdenum, nickel, lead, strontium, tin and zinc, it is characterized in that, to the detection limit of the method measure draw described metallic element to be measured detection limit all lower than 0.04mg/L; It is 2.36～7.03% that the precision of the method is measured to the relative standard deviation that draws described metallic element to be measured; It is 89.6～119% that the accuracy of the method is measured to the recovery that draws described metallic element to be measured.
In a preferred embodiment of the present invention, further comprise, the condition of work that described use induction coupled plasma radiating light spectrometer is measured through the metallic element to be measured in pretreated sample is: radio-frequency power is 1300W, carrier gas flux 15L/min, and the assisted gas flow is 0.2L/min.
In a preferred embodiment of the present invention, further comprise, the step of described microwave digestion technology sample pretreatment is as follows:
(1) get appropriate filter membrane sample and filter membrane is shredded into to fritter and be placed in counteracting tank, add 10ml to clear up acid, make the sample submergence, add a cover, be placed in the counteracting tank assembly, be put on the microwave turntable mounting, start to clear up;
(2) digestion condition in step (1) is made as to 200 ℃, clears up 20 minutes, cooling after clearing up end;
(3) take out counteracting tank, with deionized water drip washing counteracting tank inwall, add the 10ml deionized water, carry out lixiviate standing half an hour, after filtration, is settled to 50ml, makes testing sample.
In a preferred embodiment of the present invention, further comprise, clear up nitric acid that acid is 5.55% and the potpourri of 16.75% hydrochloric acid described in step (1).
In a preferred embodiment of the present invention, further comprise, the filter membrane described in step (1) is the quartz fibre filter membrane.
In a preferred embodiment of the present invention, further comprise, the amount of the filter membrane sample described in step (1) is that whole little filter membrane or 1/8th magnifies filter membrane.
The defect that solves prior art of the present invention has following beneficial effect:
The present invention is optimized with the sample detection analysis condition and is optimized by the condition of clearing up to the sample microwave digestion technology, to the detection limit of the method measure draw metallic element to be measured detection limit all lower than 0.04mg/L; It is 2.36～7.03% that the precision of the method is measured to the relative standard deviation that draws metallic element to be measured; It is 89.6～119% that the accuracy of the method is measured to the recovery that draws metallic element to be measured, and the method is highly sensitive, accuracy is high, precision is good, and can be used in Determination of multiple metal elements in actual sample and measure simultaneously, and the result of measuring is better.
Embodiment
In order to make those skilled in the art person understand better the present invention, and above-mentioned advantage of the present invention can be become apparent more, below in conjunction with specific embodiment, the present invention is further detailed explanation.
Embodiment
(1) sample pretreatment
Get one whole little round filter membrane (if large filter membrane is desirable, getting 1/8th), being cut into fractionlet is placed in counteracting tank, add 10ml to clear up acid (potpourri of 5.55% nitric acid and 16.75% hydrochloric acid), make the complete submergence of sample, add a cover, be placed in the counteracting tank assembly, be put on the microwave turntable mounting, start to clear up; Digestion condition is made as 200 ℃, clears up 20 minutes, cooling after clearing up end; Then take out counteracting tank, with deionized water drip washing counteracting tank inwall, add the 10ml deionized water, carry out lixiviate standing half an hour, after filtration, is settled to 50ml, makes testing sample.
(2) sample detection
By the good sample of pre-service in step (1), use the best spectral line of induction coupled plasma radiating light spectrometer acquiescence to be measured, metallic element to be measured comprises aluminium, barium, cadmium, chromium, copper, manganese, molybdenum, nickel, lead, strontium, tin and zinc.
Condition of work is: radio-frequency power is 1300W, carrier gas flux 15L/min, and the assisted gas flow is 0.2L/min.
Carrier gas is argon gas, and purity reaches 99.99%, the steel gas cylinder.
Wherein, the model of microwave dissolver is MLS1200, inductive coupling plasma emission spectrograph (PE, 7300DV), what filter membrane adopted is the quartz fibre filter membrane, and this filter membrane inclusion-free pollutes, remaining reagent of using is that top grade is pure, and experimental water is deionized water.
The mensuration of method detection limit
Consistent with the step in the embodiment of the present invention, do 7 blank tests, then according to the standard deviation of these 7 parallel experiments, calculate the detection limit of each metallic element that will measure in the present invention, result is as shown in table 1.
Table 1 method detection limit result
| Element | Method detection limit (mg/L) |
| Aluminium | 0.04 |
| Barium | 0.006 |
| Cadmium | 0.001 |
| Chromium | 0.01 |
| Copper | 0.005 |
| Manganese | 0.004 |
| Molybdenum | 0.01 |
| Nickel | 0.03 |
| Plumbous | 0.02 |
| Strontium | 0.01 |
| Tin | 0.005 |
| Zinc | 0.02 |
The mensuration of method precision
Get large filter membrane of an actual sample, filter membrane is divided into to 8 parts, equalled into mensuration for 6 parts that get wherein, consistent as in embodiment of the pre-service of this sample and sample determination step, acquired results is as shown in table 2.The scope of the relative standard deviation of each metal element content that the present invention measures is between 2.36～7.03%, illustrates that the precision of the method the present invention relates to is good.
The precision result that table 2 actual sample is measured
The mensuration of method accuracy
Use the method in the embodiment of the present invention to measure each metallic element in the Quality Control filter membrane, measurement result is as shown in table 3, and in the Quality Control filter membrane, the recovery of each metallic element is between 89.6～119%, and detection method accuracy of the present invention is high.
The detected value of each metallic element in table 3 Quality Control filter membrane
| Element | Reference value (μ g) | Measured value (μ g) | The recovery (%) |
| Aluminium | 110 | 98.6 | 89.6 |
| Barium | 18.4 | 17.9 | 97.2 |
| Cadmium | 7.35 | 7.64 | 104 |
| Chromium | 23.5 | 23.9 | 102 |
| Copper | 36.9 | 40.1 | 109 |
| Manganese | 73.6 | 72.9 | 99 |
| Molybdenum | 15.9 | 15.1 | 95 |
| Nickel | 29.7 | 35.2 | 119 |
| Plumbous | 18.2 | 19.3 | 106 |
| Strontium | 17.3 | 16.8 | 97.1 |
| Tin | 18.6 | 19.7 | 106 |
| Zinc | 111 | 124 | 112 |
The above; be only the specific embodiment of the present invention, protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement, within all should being encompassed in protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claim was defined.
Claims (6)
1. a method that detects metallic element in atmosphere exhaust gas particle thing, at first the method adopts microwave digestion technology to carry out sample pretreatment, sample metallic element to be measured after pre-service is used the best spectral line of induction coupled plasma radiating light spectrometer acquiescence to be measured, described metallic element to be measured comprises one or more in aluminium, barium, cadmium, chromium, copper, manganese, molybdenum, nickel, lead, strontium, tin and zinc, it is characterized in that, to the detection limit of the method measure draw described metallic element to be measured detection limit all lower than 0.04mg/L; It is 2.36～7.03% that the precision of the method is measured to the relative standard deviation that draws described metallic element to be measured; It is 89.6～119% that the accuracy of the method is measured to the recovery that draws described metallic element to be measured.
2. the method for metallic element in detection atmosphere exhaust gas particle thing according to claim 1, it is characterized in that, the condition of work that described use induction coupled plasma radiating light spectrometer is measured through the metallic element to be measured in pretreated sample is: radio-frequency power is 1300W, carrier gas flux 15L/min, the assisted gas flow is 0.2 L/min.
3. the method for metallic element in detection atmosphere exhaust gas particle thing according to claim 1, is characterized in that, the step of described microwave digestion technology sample pretreatment is as follows:
(1) get appropriate filter membrane sample and filter membrane is shredded into to fritter and be placed in counteracting tank, add 10ml to clear up acid, make the sample submergence, add a cover, be placed in the counteracting tank assembly, be put on the microwave turntable mounting, start to clear up;
(2) digestion condition in step (1) is made as to 200 ℃, clears up 20 minutes, cooling after clearing up end;
(3) take out counteracting tank, with deionized water drip washing counteracting tank inwall, add the 10ml deionized water, carry out lixiviate standing half an hour, after filtration, is settled to 50ml, makes testing sample.
4. the method for metallic element in detection atmosphere exhaust gas particle thing according to claim 3, is characterized in that, described in step (1), clears up nitric acid that acid is 5.55% and the potpourri of 16.75% hydrochloric acid.
5. the method for metallic element in detection atmosphere exhaust gas particle thing according to claim 3, is characterized in that, the filter membrane described in step (1) is the quartz fibre filter membrane.
6. the method for metallic element in detection atmosphere exhaust gas particle thing according to claim 3, is characterized in that, the amount of the filter membrane sample described in step (1) is that whole little filter membrane or 1/8th magnifies filter membrane.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105067537A (en) * | 2015-07-15 | 2015-11-18 | 南京理工大学 | Method for detecting trace lead in particulate matters |
| CN105319202A (en) * | 2015-07-10 | 2016-02-10 | 贵州航天精工制造有限公司 | Method for measuring indissolvable nickel-base superalloy multielement content with microwave digestion ICP method |
| CN107727642A (en) * | 2017-09-26 | 2018-02-23 | 苏州莱铯科技有限公司 | A kind of laser detecting method of Atmospheric particulates heavy metal element |
| CN109883971A (en) * | 2019-03-20 | 2019-06-14 | 兰州金川新材料科技股份有限公司 | Trace meter copper, Direct spectrophotometry method in a kind of nickel and cobalt solution |
| CN116046879A (en) * | 2023-02-17 | 2023-05-02 | 山东省产品质量检验研究院 | Method for detecting heavy metal elements in air or waste gas particulate matters |
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2013
- 2013-09-27 CN CN201310450385.7A patent/CN103487427A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105319202A (en) * | 2015-07-10 | 2016-02-10 | 贵州航天精工制造有限公司 | Method for measuring indissolvable nickel-base superalloy multielement content with microwave digestion ICP method |
| CN105067537A (en) * | 2015-07-15 | 2015-11-18 | 南京理工大学 | Method for detecting trace lead in particulate matters |
| CN107727642A (en) * | 2017-09-26 | 2018-02-23 | 苏州莱铯科技有限公司 | A kind of laser detecting method of Atmospheric particulates heavy metal element |
| CN107727642B (en) * | 2017-09-26 | 2020-07-10 | 苏州莱铯科技有限公司 | Laser detection method for heavy metal elements in atmospheric particulates |
| CN109883971A (en) * | 2019-03-20 | 2019-06-14 | 兰州金川新材料科技股份有限公司 | Trace meter copper, Direct spectrophotometry method in a kind of nickel and cobalt solution |
| CN109883971B (en) * | 2019-03-20 | 2021-11-02 | 兰州金川新材料科技股份有限公司 | Method for measuring trace metal copper and zinc in nickel-cobalt solution |
| CN116046879A (en) * | 2023-02-17 | 2023-05-02 | 山东省产品质量检验研究院 | Method for detecting heavy metal elements in air or waste gas particulate matters |
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Application publication date: 20140101 |