CN105954075A - Method for preparing series of micro-dust standard samples for XRF and TXRF analysis - Google Patents
Method for preparing series of micro-dust standard samples for XRF and TXRF analysis Download PDFInfo
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- CN105954075A CN105954075A CN201610273807.1A CN201610273807A CN105954075A CN 105954075 A CN105954075 A CN 105954075A CN 201610273807 A CN201610273807 A CN 201610273807A CN 105954075 A CN105954075 A CN 105954075A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
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- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of analytical chemistry, discloses a method for preparing a series of micro-dust standard samples for the XRF and TXRF analysis. According to the method, atmospheric dusts are analyzed by using a suspended atomizer and a soil standard sample. The method comprises the steps of (1) drying a polycarbonate film at 60 DEG C for 2 hours till the weight of the film is constant, and placing the polycarbonate film at a sampling position at the upper end of the suspended atomizer; (2) weighing a certain amount of a soil sample that meets the requirements of the national standard; (3) adjusting the sampling flow rate of the suspended atomizer, and setting the initial sampling flow rate thereof to be 18L/min; when the sampling flow rate of the suspended atomizer reaches 14L/min, stopping the sampling process and sampling the soil sample onto the polycarbonate film; (4) drying the soil sample obtained in the step (3) at 60 DEG for 2 hours till the weight of the soil sample is constant so as to obtain a film micro-dust standard sample; (5) sequentially selecting other types of soil samples contained in the series of micro-dust standard samples and repeating the above steps (1)-(4). The composition of the method is close to an atmospheric dust sample. Meanwhile, the method is simple in operation.
Description
Technical field
The invention belongs to technical field of analytical chemistry, be specifically related to a kind of XRF of being suitable to and TXRF analysis is
The preparation method of row micronic dust standard sample.
Background technology
The ultimate principle of total reflection X ray fluorescence (TXRF) is that the X-ray that light source produces is reflected body generation entirely
Get to after reflection on sample, make the element to be measured in sample produce characteristic x-ray fluorescence, according to tested element
Functional relationship between signal intensity and sample concentration, obtains the concentration of element to be measured in sample.
TXRF can be used for measuring atmospheric fallout sample, and traditional method typically uses nitrification process to be dissolved by sample,
Being subsequently adding internal standard, dripped by solution and dry measurement on specimen disc, this method has does not destroys sample, measurement time
The advantage that matrix will not be impacted by polycarbonate film short, sampling, but owing to lacking series standard sample
Product, it is impossible to instrument is carried out scale, it is impossible to provide the measured value of element in testing sample.It is presently available for X
The commercial standard (CS) film sample of ray fluorescence (XRF), great majority are single-element, and minority is that multielement mixes
Close, all use standard solution to make, differ bigger with atmospheric fallout sample matrices.Therefore it is badly in need of developing one
For measuring the standard sample of atmospheric fallout sample.
Summary of the invention
(1) goal of the invention
According to the problem existing for prior art, this application provides a kind of sample composition close to atmospheric fallout sample,
Simple to operate and be suitable to the preparation method of serial micronic dust standard sample that XRF and TXRF analyzes.
(2) technical scheme
In order to solve the problem existing for prior art, the present invention is achieved by the following technical solutions:
Be suitable to the preparation method of the serial micronic dust standard sample that XRF and TXRF analyzes, it is critical that the party
Method utilizes suspension nebulizer and soil changes to be analyzed atmospheric fallout, and it comprises the following steps:
(1) polycarbonate membrane is dried 2 hours at 60 DEG C until constant weight, and this polycarbonate membrane is placed in
The sample position, upper end of suspension nebulizer；
(2) weighing a certain amount of pedotheque, described pedotheque is series standard pedotheque；Choose and be
In a kind of injection port being placed in suspension nebulizer in row standard soil sample；Described standard soil sample is satisfied
The GBW07402 of Standard, GBW07403, GBW07404, GBW07405, GBW07406,
GBW07407、GBW07409、GBW07423、GBW07424、GBW07425、GBW07426、
GBW07427, GBW07428, GBW07429, GBW07430 pedotheque；
(3) adjusting the sampling velocity of suspension nebulizer, initial sample flow velocity is 18L/min, works as sampling velocity
Reach 14L/min and stop sampling, by pedotheque sampling to polycarbonate membrane；
(4) pedotheque that step (3) obtains is dried 2 hours at 60 DEG C, until constant weight, to obtain final product
To thin film micronic dust standard sample；
(5) choose other kinds in series standard pedotheque successively, and repeat step (1)～(4).
Preferably, the thickness of described polycarbonate membrane is 47mm, and aperture is 0.4 μm.
Preferably, the model of described suspension nebulizer is SSPD3433.
(3) beneficial effect
The preparation method using the present invention to provide has two main beneficial effects:
1. owing to meeting the matrix of the soil changes of Standard with atmospheric fallout closely, and soil mark
The composition of quasi-sample is known with content.The application utilizes soil changes to prepare atmospheric fallout sample standard sample
So that element contained in atmospheric fallout is analyzed, with high accuracy and workable.
2. the serial atmospheric fallout standard sample being suitable to XRF and TXRF analysis is usually film sample.This Shen
Please by soil changes being passed through commercial suspension nebulizer under certain sampling velocity controls by Soil standard
Sample, on polycarbonate membrane, is suitable for XRF and TXRF and analyzes, simple to operate.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further elaborated.
(1) polycarbonate membrane is dried 2 hours at 60 DEG C, until constant weight this polycarbonate membrane is placed in
The sample position, upper end of suspension nebulizer；
(2) weighing a certain amount of pedotheque, described pedotheque is series standard pedotheque；To choose
In a kind of injection port being placed in suspension nebulizer in series standard pedotheque；Described standard soil sample is full
Foot the GBW07402 of Standard, GBW07403, GBW07404, GBW07405, GBW07406,
GBW07407、GBW07409、GBW07423、GBW07424、GBW07425、GBW07426、
GBW07427, GBW07428, GBW07429, GBW07430 pedotheque；
(3) adjusting the sampling velocity of suspension nebulizer, initial sample flow velocity is 18L/min, when sampling velocity reaches
Sampling is stopped, by pedotheque sampling to polycarbonate membrane to 14L/min；
(4) pedotheque that step (3) obtains is dried 2 hours at 60 DEG C, until constant weight, to obtain final product
To thin film micronic dust standard sample；
(5) choose other kinds in series standard pedotheque successively, and repeat step (1)～(4).
The thickness of described polycarbonate membrane is 47mm, and aperture is 0.4 μm.The model of described suspension nebulizer is
SSPD3433。
As a example by the element of Cu and Zn in atmospheric fallout, said method is utilized to be prepared as meeting the thin of XRF analysis
Membrane sample.The concentration that peak intensity according to Cu with Zn element is corresponding, draws Cu and Zn element (μ g/g)
Working curve, and preserve work.
The concentration (μ g/g) of table 1 Cu/Zn element and the corresponding relation of peak intensity
When measuring unknown atmospheric fallout sample, calling in working curve and measure, measurement terminates, and can automatically be given
The concentration of Cu and Zn.The intensity of such as Cu is 500, then concentration is 17.295 μ g/g；Zn intensity is 480,
Then concentration is 6 μ g/g.
Claims (3)
1. be suitable to the preparation method of the serial micronic dust standard sample that XRF and TXRF analyzes, it is characterised in that
The method utilizes suspension nebulizer and soil changes to be analyzed atmospheric fallout, and it comprises the following steps:
(1) polycarbonate membrane is dried 2 hours at 60 DEG C until constant weight, and this polycarbonate membrane is placed in
The sample position, upper end of suspension nebulizer；
(2) weighing a certain amount of pedotheque, described pedotheque is series standard pedotheque；Choose and be
In a kind of injection port being placed in suspension nebulizer in row standard soil sample；Described standard soil sample is satisfied
The GBW07402 of Standard, GBW07403, GBW07404, GBW07405, GBW07406,
GBW07407、GBW07409、GBW07423、GBW07424、GBW07425、GBW07426、
GBW07427, GBW07428, GBW07429, GBW07430 pedotheque；
(3) adjusting the sampling velocity of suspension nebulizer, initial sample flow velocity is 18L/min, works as sampling velocity
Reach 14L/min and stop sampling, by pedotheque sampling to polycarbonate membrane；
(4) pedotheque that step (3) obtains is dried 2 hours at 60 DEG C, until constant weight, to obtain final product
To thin film micronic dust standard sample；
(5) choose other kinds in series standard pedotheque successively, and repeat step (1)～(4).
The system being suitable to the serial micronic dust standard sample that XRF and TXRF analyzes the most according to claim 1
Preparation Method, it is characterised in that the thickness of described polycarbonate membrane is 47mm, aperture is 0.4 μm.
The system being suitable to the serial micronic dust standard sample that XRF and TXRF analyzes the most according to claim 1
Preparation Method, it is characterised in that the model of described suspension nebulizer is SSPD3433.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610273807.1A CN105954075A (en) | 2016-04-28 | 2016-04-28 | Method for preparing series of micro-dust standard samples for XRF and TXRF analysis |
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| CN201610273807.1A CN105954075A (en) | 2016-04-28 | 2016-04-28 | Method for preparing series of micro-dust standard samples for XRF and TXRF analysis |
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| CN201610273807.1A Pending CN105954075A (en) | 2016-04-28 | 2016-04-28 | Method for preparing series of micro-dust standard samples for XRF and TXRF analysis |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112730493A (en) * | 2020-12-21 | 2021-04-30 | 广东贝源检测技术股份有限公司 | On-site detection method for soil metal substances |
Citations (6)
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| CN103323319A (en) * | 2012-11-23 | 2013-09-25 | 江苏天瑞仪器股份有限公司 | Enriching and detecting equipment for particles |
| CN103983618A (en) * | 2014-05-14 | 2014-08-13 | 四川大学 | Pretreatment method of powder sample for laser induced breakdown spectrographic detection |
| US20140326802A1 (en) * | 2011-12-02 | 2014-11-06 | Braincon Handels-Gmbh | Atomization device |
| CN104251809A (en) * | 2014-09-15 | 2014-12-31 | 天津开发区合普工贸有限公司 | High-precision steady calibration device for tiny solid particle aerosol |
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| CN104819872A (en) * | 2015-05-09 | 2015-08-05 | 中国科学院地球环境研究所 | Filter membrane clamping and collecting method for falling dust of museum of ancient ruined site |
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2016
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Patent Citations (6)
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| US20140326802A1 (en) * | 2011-12-02 | 2014-11-06 | Braincon Handels-Gmbh | Atomization device |
| CN103323319A (en) * | 2012-11-23 | 2013-09-25 | 江苏天瑞仪器股份有限公司 | Enriching and detecting equipment for particles |
| CN103983618A (en) * | 2014-05-14 | 2014-08-13 | 四川大学 | Pretreatment method of powder sample for laser induced breakdown spectrographic detection |
| CN104251809A (en) * | 2014-09-15 | 2014-12-31 | 天津开发区合普工贸有限公司 | High-precision steady calibration device for tiny solid particle aerosol |
| CN204220333U (en) * | 2014-11-07 | 2015-03-25 | 河南省日立信股份有限公司 | Dust is quantitative aerosol device precisely |
| CN104819872A (en) * | 2015-05-09 | 2015-08-05 | 中国科学院地球环境研究所 | Filter membrane clamping and collecting method for falling dust of museum of ancient ruined site |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112730493A (en) * | 2020-12-21 | 2021-04-30 | 广东贝源检测技术股份有限公司 | On-site detection method for soil metal substances |
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Application publication date: 20160921 |