CN107389708B - Liquid sample introduction bottle and liquid sample introduction method for micro-area X-ray fluorescence spectrometer - Google Patents
Liquid sample introduction bottle and liquid sample introduction method for micro-area X-ray fluorescence spectrometer Download PDFInfo
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- CN107389708B CN107389708B CN201710500841.2A CN201710500841A CN107389708B CN 107389708 B CN107389708 B CN 107389708B CN 201710500841 A CN201710500841 A CN 201710500841A CN 107389708 B CN107389708 B CN 107389708B
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- 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
- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/20008—Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor
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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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- G01N23/20—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 using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
- G01N23/207—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions
- G01N23/2076—Diffractometry using detectors, e.g. using a probe in a central position and one or more displaceable detectors in circumferential positions for spectrometry, i.e. using an analysing crystal, e.g. for measuring X-ray fluorescence spectrum of a sample with wavelength-dispersion, i.e. WDXFS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a liquid sample introduction bottle for a micro-area X-ray fluorescence spectrometer, which comprises a bottle body and a bottle cap with a central hole, wherein a transparent film is clamped between the bottle cap and the bottle body, and the liquid sample introduction bottle and a liquid sample introduction method thereof can directly measure liquid, solve the problems of stability and focusing of a sample and reserve batch processing capacity, solve the problems of liquid surface tension, accurate focusing, batch focusing, helium interference and the like during measurement of the micro-area X-ray fluorescence spectrometer, can be directly suitable for detection of solid and liquid samples, enable the upper-irradiation micro-area X-ray fluorescence spectrometer to have the capacity of direct quantitative analysis and batch processing capacity of liquid (aqueous solution, emulsion and oil) on the basis of the original capacity of direct quantitative analysis and batch processing capacity of solid and other aqueous solutions, and enable the upper-irradiation micro-area X-ray fluorescence spectrometer to be suitable for detection and analysis of cosmetics or other aqueous solutions, greatly expands the application range of the micro-area X-ray fluorescence spectrometer.
Description
Technical Field
The invention relates to a sample introduction bottle and a sample introduction method, in particular to a liquid sample introduction bottle and a liquid sample introduction method for a micro-area X-ray fluorescence spectrometer.
Background
The micro-area X-ray fluorescence spectrometer is a special product in the field of X-ray fluorescence spectroscopy (XRF) analysis, obtains element components and distribution characteristics of a micro area of a sample through flexible structure and nondestructive detection, has application range including research fields of environment, archaeology, criminal investigation, materials, industrial quality control, biology and the like, and is a hotspot of the current international research in the field of X-ray spectroscopy.
At present, the application of X-ray fluorescence spectroscopy is mostly concentrated on solid samples. In addition to the direct measurement of oils in the field of petrochemical industry, the only reports have essentially changed from liquid samples to solid phase measurements. The XRF liquid analysis technology can be used, all the adopted instruments are lower irradiation instruments, and the sample cup support film has the risk of leakage and rupture when measuring liquid, so that the irradiation spectrum chamber is polluted and damaged; the X-fluorescence automatic sample feeding and discarding device is not suitable for micro-area X-fluorescence liquid sample feeding.
At present, the X fluorescent liquid sample analysis adopts a sample cup with a larger caliber. The sample cup instrument can focus on a membrane, but the liquid level cannot be kept consistent under the influence of the assembly of a clamping ring, the problem is that redundant liquid cannot be discharged in time, the conventional X fluorescence can be suitable, but the accuracy of the X fluorescence can be influenced when the X fluorescence is used for measuring the micro-area X fluorescence.
The micro-area X-ray fluorescence spectrometer is an instrument with an adjustable structure, can realize automatic sample introduction of multiple samples by adopting a moving platform, but errors generated by the movement of a three-dimensional platform and errors generated by naked eyes during focusing influence quantitative analysis of the micro-area X-ray fluorescence spectrometer. Therefore, two problems of accurate focusing and batch focusing are required to be overcome when a liquid sample needs to be directly fed, wherein the problem that the liquid cannot be focused due to double images, enlargement, disappearance and the like when laser irradiates on the liquid and the problem of liquid level vibration caused by protective gas are solved by the accurate focusing, and the problem of how to keep the liquid levels of all samples at one height is solved by the batch focusing.
The direct measurement of liquid samples by a micro-area X-ray fluorescence spectrometer has many problems, such as uneven liquid surface caused by the surface tension of the liquid, difficult focusing caused by too small or too large reflected light, and liquid surface fluctuation caused by protective gas. The liquid sample preparation technology of 'extraction', 'enrichment', 'filter paper' is a traditional XRF liquid analysis technology, RafalSitko, Shukuro Igarashi and the like apply the technology to the instruments, Thomasin C, Miller and the like propose an 'automatic printing' technology, KathrynG, Mclntosh and the like propose a 'microfluidic chip' technology and the like, and provide a new idea for quantitative batch detection of liquid samples, but the technologies do not directly measure liquid, or keep the idea that liquid is changed into solid and then detected.
Disclosure of Invention
The invention provides a liquid sample feeding bottle for a micro-area X-ray fluorescence spectrometer and a liquid sample feeding method thereof, which can be directly suitable for liquid samples, can adopt upper irradiation measurement, have high measurement precision and flat measurement liquid level and can feed samples continuously.
In order to achieve the purpose, the invention adopts the following technical scheme:
the utility model provides a liquid advances kind bottle for subregion X ray fluorescence spectrometer, liquid advances kind bottle includes bottle and the bottle lid of taking the centre of a circle hole, press from both sides between bottle lid and the bottle and establish transparent film.
In order to further optimize the technical scheme, the technical measures adopted by the invention are as follows:
preferably, the bottle body is cylindrical, and the bottle body and the bottle cap are provided with matched threaded parts;
preferably, the bottle cap is provided with a concave ring along a central hole; under the annular pressure of the concave ring downwards, the stretching range of the membrane is further reduced, and the membrane surface is more flat;
preferably, the micro-area X-ray fluorescence spectrometer is a focusing type small-focus X-ray fluorescence spectrometer;
preferably, the transparent film is a mylar film;
the invention also provides a liquid sample introduction method for the micro-area X-ray fluorescence spectrometer, which comprises the following specific steps:
the method comprises the following steps: pretreatment
When the sample liquid to be detected is an aqueous agent or an emulsion, checking whether bubbles or liquid stratification exists, and defoaming and homogenizing by using an ultrasonic cleaning machine if the bubbles or liquid stratification exists;
step two: sample loading
Filling the sample liquid processed in the step one into the liquid sample injection bottle, filling the liquid sample injection bottle with the sample liquid, making the liquid surface be a convex liquid surface and slightly higher than the bottle opening by utilizing the liquid surface tension, smoothly screwing the bottle cap after the transparent film is covered on the liquid surface of the bottle opening of the liquid sample injection bottle, pulling the transparent film to be tightly attached to the liquid surface, keeping the film surface flat, and finishing sample loading;
step three: data acquisition
And (4) placing the liquid sample injection bottle processed in the step two on a sample table, focusing by laser, measuring a sample, and collecting data.
The invention also provides a liquid sample introduction method for the micro-area X-ray fluorescence spectrometer, which comprises the following specific steps:
the method comprises the following steps: pretreatment
When the sample to be detected is solid, dissolving the sample in water or dissolving the sample in water after ashing, recording the specific gravity of the sample and the water, and then immediately using or transferring the sample to a glass bottle with a cover for later use;
step two: sample loading
Filling the sample liquid processed in the step one into the liquid sample injection bottle, filling the liquid sample injection bottle with the sample liquid, making the liquid surface be a convex liquid surface and slightly higher than the bottle opening by utilizing the liquid surface tension, smoothly screwing the bottle cap after the transparent film is covered on the liquid surface of the bottle opening of the liquid sample injection bottle, pulling the transparent film to be tightly attached to the liquid surface, keeping the film surface flat, and finishing sample loading;
step three: data acquisition
Placing the liquid sample introduction bottle processed in the second step on a sample table, focusing the laser of the micro-area X-ray fluorescence spectrometer, measuring the sample, and collecting data;
preferably, the sample measured in the third step is an upper irradiation measuring method;
preferably, the sample stage is provided with at least one sample inlet hole of a sample inlet bottle;
preferably, the micro-area X-ray fluorescence spectrometer in the third step can continuously acquire data of the sample bottle;
preferably, the micro-area X-ray fluorescence spectrometer is an MIDEX SD type focusing type small-focus X-ray fluorescence spectrometer;
preferably, the analysis range of the micro-area X-ray fluorescence spectrometer is Na-U, the upper irradiation structure, the Mo target X-ray tube, the maximum power of 30W, the maximum voltage of 48kV, the Si drift detector and the detection distance of 2 mm;
preferably, the micro-area X-ray fluorescence spectrometer is used for loading samples once, continuously feeding samples, starting a measurement program according to measurement conditions, and completing data acquisition and result calculation;
by adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the invention provides a new sample introduction method for a micro-area X-ray fluorescence spectrometer to measure a liquid sample, namely a bottle mouth sticking film method, wherein a sample bottle with a bottle cap with a central hole is used for filling the sample, and a Mylar film (Mylar film, a polyester film) is used for consolidating the liquid level; the concave ring is arranged at the position of the central hole of the bottle cap, so that the transparent film can be stressed evenly and is smoother; the invention solves the problems of liquid surface tension, accurate focusing, batch focusing, helium interference and the like when the micro-area X-ray fluorescence spectrometer is used for measurement, can be directly suitable for detection of solid and liquid samples, enables the upper-irradiation micro-area X-ray fluorescence spectrometer to have the capability and batch processing capability of direct quantitative analysis of liquid (aqueous solution, emulsion and oil) on the original capability and batch processing capability of direct quantitative analysis of solid, enables the upper-irradiation micro-area X-ray fluorescence spectrometer to be suitable for detection and analysis of cosmetics or other aqueous solutions, and greatly expands the application field and application range of the micro-area X-ray fluorescence spectrometer.
Drawings
FIG. 1 is a schematic diagram of a liquid sample bottle according to a preferred embodiment of the present invention;
FIG. 2 is a schematic diagram of a preferred embodiment of a liquid sample bottle with a recessed ring;
FIG. 3 is a perspective view of a liquid sample bottle in accordance with a preferred embodiment of the present invention;
FIG. 4 is a top view of a liquid sample bottle in accordance with a preferred embodiment of the present invention;
fig. 5 is a schematic structural view of a bottle cap with a female ring according to a preferred embodiment of the present invention;
wherein the reference numerals are:
1 bottle body; 2, bottle cap; 3 a transparent film; 4 a threaded part; 21 a central hole; 22 concave ring.
Detailed Description
The invention provides a liquid sample introduction bottle for a micro-area X-ray fluorescence spectrometer and a liquid sample introduction method thereof;
the present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example one
As shown in FIGS. 1 to 5, the present example utilizes the liquid sample injection bottle of the micro-area X-ray fluorescence spectrometer and the liquid sample injection method to perform the detection of the bath salt solid sample.
1. Instrument and measurement conditions
MIDEX SD type focusing type small focus X-ray fluorescence spectrometer (German Spikek analyzer), analysis range Na-U, upper irradiation structure, Mo target X-ray tube, maximum power 30W, maximum voltage 48kV, Si drift detector, detection distance 2 mm.
2. Solid sample detection
The solid sample detection process of the X-ray fluorescence spectrometer comprises the following steps:
the method comprises the following steps: pretreatment
Dissolving a bath salt sample in water, recording the specific gravity of the sample and the water, and standing for later use;
step two: sample loading
Filling the sample liquid processed in the step one into the liquid sample inlet bottle, filling the liquid sample inlet bottle with the sample liquid, enabling the liquid surface to be a convex liquid surface and to be slightly higher than the bottle opening by utilizing the liquid surface tension, after the transparent film 3 covers the liquid surface of the bottle opening of the liquid sample inlet bottle, smoothly screwing the bottle cover 2, pulling the transparent film 3 to be tightly attached to the liquid surface, keeping the film surface flat, and finishing sample filling; ensuring that the liquid level in the film is bubble-free and the film surface is flat.
Step three: data acquisition
Placing the liquid sample introduction bottle processed in the second step on a sample table, focusing the laser of the micro-area X-ray fluorescence spectrometer, measuring the sample, and collecting data;
4 bath salt samples were taken and compared with the standard method GB/T13025.5 and the solid sample injection method of the example, 3 replicates were taken and the average value was taken and the data is shown in Table 1. The comparison shows that the detection requirements of common constants are met.
TABLE 1 bath salt Standard method and example comparison of the results
Example two
As shown in fig. 1 to 5, in this embodiment, the content of Pb and As in the aqueous solution and emulsion sample is detected by using the liquid sample injection bottle of the micro-area X-ray fluorescence spectrometer and the liquid sample injection method.
1. Instrument and measurement conditions
MIDEX SD type focusing type small focus X-ray fluorescence spectrometer (German Spikek analyzer), analysis range Na-U, upper irradiation structure, Mo target X-ray tube, maximum power 30W, maximum voltage 48kV, Si drift detector, detection distance 2 mm.
2. Liquid sample detection
The liquid sample detection process of the X-ray fluorescence spectrometer of the present embodiment:
the method comprises the following steps:
checking whether the sample to be detected has bubbles or liquid stratification, and defoaming and homogenizing by using an ultrasonic cleaning machine if the sample to be detected has bubbles or liquid stratification;
step two:
filling the sample liquid processed in the step one into the liquid sampling bottle, filling the liquid sampling bottle with the sample liquid, making the liquid surface be a convex liquid surface and slightly higher than the bottle opening by utilizing the liquid surface tension, after the transparent film 3 covers the liquid surface of the bottle opening of the liquid sampling bottle, smoothly screwing the bottle cover 2, pulling the transparent film 3 to be tightly attached to the liquid surface, keeping the film surface flat, and finishing sample filling;
step three:
and (4) placing the liquid sample injection bottle processed in the step two on a sample table, focusing by laser, measuring a sample, and collecting data.
5 samples of water aqua and emulsion (S5-S9) are selected, and a standard method (ICP-MS method) in chapter 1.6 of chapter IV of technical Specification for safety of cosmetics is adopted to compare with the liquid sample detection method of the second embodiment, the data is shown in Table 2, and the data display is basically consistent with the standard method.
TABLE 2 comparison of liquid cosmetic standards and method A results
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (10)
1. A liquid sample introduction bottle for a micro-area X-ray fluorescence spectrometer is characterized in that: the liquid sample introduction bottle comprises a bottle body (1) and a bottle cap (2) with a central hole (21), wherein a transparent film (3) is clamped between the bottle cap (2) and the bottle body (1), and the transparent film (3) is a Mylar film; the bottle cap (2) is provided with a concave ring (22) along the central hole (21).
2. The liquid sample bottle according to claim 1, wherein: the bottle body (1) is cylindrical, and the bottle body (1) and the bottle cap (2) are provided with matched threaded parts (4).
3. The liquid sample bottle according to claim 1, wherein: the micro-area X-ray fluorescence spectrometer is a focusing type small-focus X-ray fluorescence spectrometer.
4. A liquid sample introduction method for a micro-area X-ray fluorescence spectrometer is characterized by comprising the following steps: the liquid sampling method comprises the following specific steps:
the method comprises the following steps: pretreatment
When the sample liquid to be detected is an aqueous agent or an emulsion, checking whether bubbles or liquid stratification exists, and defoaming and homogenizing by using an ultrasonic cleaning machine if the bubbles or liquid stratification exists;
step two: sample loading
Filling the sample liquid processed in the step one into the liquid sampling bottle of any one of claims 1-2, filling the liquid sampling bottle with the sample liquid, making the liquid surface be a convex liquid surface which is slightly higher than the bottle mouth by using the liquid surface tension, smoothly screwing the bottle cap (2) after the transparent film (3) covers the liquid surface of the bottle mouth of the liquid sampling bottle, pulling the transparent film (3) to be tightly attached to the liquid surface, keeping the film surface flat, and finishing sample loading;
step three: data acquisition
And (4) placing the liquid sample injection bottle processed in the step two on a sample table, focusing by laser, measuring a sample, and collecting data.
5. The liquid sample introduction method according to claim 4, characterized in that: and in the third step, the sample is measured by upper irradiation measurement, and the upper irradiation measurement is performed above the liquid sampling bottle.
6. The liquid sample introduction method according to claim 4, characterized in that: the sample platform is provided with at least one liquid sample inlet bottle sample inlet hole.
7. A liquid sample introduction method for a micro-area X-ray fluorescence spectrometer is characterized by comprising the following steps: the liquid sampling method comprises the following specific steps:
the method comprises the following steps: pretreatment
When the sample to be detected is solid, dissolving the sample in water or dissolving the sample in water after ashing, recording the specific gravity of the sample and the water, and then immediately using or transferring the sample to a glass bottle with a cover for later use;
step two: sample loading
Filling the sample liquid processed in the step one into the liquid sampling bottle of any one of claims 1-2, filling the liquid sampling bottle with the sample liquid, making the liquid surface be a convex liquid surface which is slightly higher than the bottle mouth by using the liquid surface tension, smoothly screwing the bottle cap (2) after the transparent film (3) covers the liquid surface of the bottle mouth of the liquid sampling bottle, pulling the transparent film (3) to be tightly attached to the liquid surface, keeping the film surface flat, and finishing sample loading;
step three: data acquisition
And (4) placing the liquid sample injection bottle processed in the step two on a sample table, focusing the laser of the micro-area X-ray fluorescence spectrometer, measuring the sample, and collecting data.
8. The liquid sample introduction method according to claim 7, characterized in that: and in the third step, the sample is measured by upper irradiation measurement, and the upper irradiation measurement is performed above the liquid sampling bottle.
9. The liquid sample introduction method according to claim 7, characterized in that: the sample platform is provided with at least one liquid sample inlet bottle sample inlet hole.
10. The liquid sample introduction method according to claim 9, characterized in that: the micro-area X-ray fluorescence spectrometer in the third step can continuously acquire data of the liquid sampling bottle.
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| CN203385655U (en) * | 2013-07-04 | 2014-01-08 | 浙江福立分析仪器有限公司 | Water seal device in atomic absorption spectrometer |
| CN203405430U (en) * | 2013-08-15 | 2014-01-22 | 浙江工业大学 | Portable microbeam X-ray fluorescence spectrometer |
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| CN203385655U (en) * | 2013-07-04 | 2014-01-08 | 浙江福立分析仪器有限公司 | Water seal device in atomic absorption spectrometer |
| CN203405430U (en) * | 2013-08-15 | 2014-01-22 | 浙江工业大学 | Portable microbeam X-ray fluorescence spectrometer |
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| 《直接进样X 射线荧光光谱法测定汽油中痕量锰和铁》;邬蓓蕾等;《理化检验-化学分册》;20041130;第40卷(第11期);全文 * |
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