CN113176286A - High-sensitivity X-ray fluorescence detection method for elements such as cadmium in water - Google Patents
High-sensitivity X-ray fluorescence detection method for elements such as cadmium in water Download PDFInfo
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- CN113176286A CN113176286A CN202110666288.6A CN202110666288A CN113176286A CN 113176286 A CN113176286 A CN 113176286A CN 202110666288 A CN202110666288 A CN 202110666288A CN 113176286 A CN113176286 A CN 113176286A
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Abstract
The invention relates to the technical field of analysis of trace heavy metals in water, in particular to a high-sensitivity X-ray fluorescence detection method for elements such as cadmium and the like in water, which is convenient to operate, high in detection accuracy and capable of reducing detection cost; the method comprises the following steps: s1, collecting a water sample to be detected, and filtering the water sample by using a 0.45um membrane for detection; s2, dropwise adding the water sample to be detected onto the adsorption material; s3, drying a water sample to be detected on an adsorbing material by using laser to dryness so as to enrich heavy metal elements in the water sample on the adsorbing material in the form of residual solid salt; s4, carrying out X-ray radiation on the residual solid salt on the adsorbing material, and receiving characteristic X-ray fluorescence released by the residual solid salt to obtain X-ray fluorescence spectrum data; and S5, performing qualitative and quantitative analysis on the heavy metals in the water sample to be detected according to the X-ray fluorescence spectrum data.
Description
Technical Field
The invention relates to the technical field of analysis of trace heavy metals in water, in particular to a high-sensitivity X-ray fluorescence detection method for elements such as cadmium in water.
Background
In the past, the portable field detection of heavy metals in water is generally carried out by adopting an anodic stripping voltammetry method in the industry, but the method is complex to operate, the types of test elements are limited, the interference by ions in samples is serious, and professional operators with consumable materials and chemical backgrounds are needed.
In recent years, a method for analyzing heavy metal elements in on-site water by combining a solid-phase microextraction enrichment technology with a monochromatic excitation X-ray fluorescence technology is developed, and compared with the traditional method, the method is improved in operation convenience, accuracy and the like, but has various influence factors such as ion exchange saturation upper limit, different ion adsorption efficiencies, enrichment of heavy metals in ionic states, inconsistent enrichment effects on different heavy metal elements, high price of enrichment materials, high long-term use cost and the like, so that the wide application of the method is limited. The laser evaporation enrichment technology is combined with the monochromatic excitation X-ray fluorescence technology, so that the rapid and effective analysis of the trace heavy metal elements in the water can be really realized.
Disclosure of Invention
In order to solve the technical problems, the invention provides the method and the device for analyzing the trace heavy metals in water by X-ray fluorescence, which have the advantages of convenient operation, high detection accuracy and detection cost reduction.
The invention relates to a high-sensitivity X-ray fluorescence detection method for elements such as cadmium in water, which comprises the following steps of:
s1, collecting a water sample to be detected, and filtering the water sample by using a 0.45um membrane for detection;
s2, dropwise adding the water sample to be detected onto the adsorption material;
s3, drying a water sample to be detected on an adsorbing material by using laser to dryness so as to enrich heavy metal elements in the water sample on the adsorbing material in the form of residual solid salt;
s4, carrying out X-ray radiation on the residual solid salt on the adsorbing material, and receiving characteristic X-ray fluorescence released by the residual solid salt to obtain X-ray fluorescence spectrum data;
and S5, performing qualitative and quantitative analysis on the heavy metals in the water sample to be detected according to the X-ray fluorescence spectrum data.
Further, the heavy metals detected by the method for analyzing the trace heavy metals in water by X-ray fluorescence comprise Mn, Fe, Ni, Cu, Zn, Pb, Cr, Cd and As.
Furthermore, the detection limit of the method to the trace heavy metals in water is in ug/L magnitude.
Further, the water sample dripped on the adsorbing material is 10-50mL, and the dripping speed is 0.05-0.2 mL/s.
Further, the adsorbent is a polymer adsorbent.
Further, the power of laser evaporation to dryness is 5-10 KW.
Further, the X-ray is a monochromated and focused X-ray.
The invention relates to a high-sensitivity X-ray fluorescence detection method for elements such as cadmium in water, which comprises the following steps:
the dropwise adding component is used for dropwise adding the water sample to be detected onto the adsorbing material;
the laser evaporation-to-dryness component is used for evaporating and drying a water sample to be detected on the adsorbing material so as to enrich heavy metal elements in the water sample on the adsorbing material in the form of residual solid salt;
the X-ray transmitting and receiving assembly is used for carrying out X-ray radiation on the residual solid salt on the adsorbing material and receiving characteristic X-ray fluorescence released by the residual solid salt to obtain X-ray fluorescence spectrum data;
and the analysis component is used for qualitatively and quantitatively analyzing the heavy metal in the water sample to be detected according to the X-ray fluorescence spectrum data.
Further, the device also comprises a test platform for placing the adsorption material;
further, the adsorbent is a polymer adsorbent.
Compared with the prior art, the invention has the beneficial effects that: the enrichment upper limit can be increased by 3 orders of magnitude, and the method is suitable for various water samples and sewage; the enrichment effect on different heavy metal elements is consistent, the efficiency of exchanging different elements by anions and cations is greatly different, and the accuracy in the actual test process is higher; the enrichment exchange material with high cost is not needed, and the use cost is greatly reduced; the analysis result is the full analysis of the heavy metal elements, not the ionic sample in the ion exchange method, and has high comparability with the current laboratory standard method; the use and the operation are more convenient.
Drawings
FIG. 1 is a flow chart of the steps of a method for analyzing trace heavy metals in water by X-ray fluorescence according to the present invention;
FIG. 2 is a schematic structural diagram of a high-sensitivity X-ray fluorescence detection method for elements such as cadmium in water according to an embodiment of the present invention;
in the drawings, the reference numbers: 1. laser evaporation to dryness of the components; 2. a test platform; 3. a dropping component; 4. an X-ray transmitting and receiving assembly; 5. and analyzing the component.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
In the description of the present invention, it should be noted that the orientations or positional relationships indicated by the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like are based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
Example 1
The embodiment provides a high-sensitivity X-ray fluorescence detection method for elements such as cadmium in water, and as shown in figure 2, the device comprises:
the dripping component 3 is used for dripping the water sample to be detected on the adsorbing material drop by drop;
the laser evaporation-to-dryness component 1 is used for carrying out evaporation-to-dryness treatment on a water sample to be detected on the adsorption material so as to enrich heavy metal elements in the water sample on the adsorption material in the form of residual solid salt;
the X-ray transmitting and receiving assembly 4 is used for carrying out X-ray radiation on the residual solid salt on the adsorption material and receiving characteristic X-ray fluorescence released by the residual solid salt to obtain X-ray fluorescence spectrum data;
and the analysis component 5 is used for qualitatively and quantitatively analyzing the heavy metals in the water sample to be detected according to the X-ray fluorescence spectrum data.
In the embodiment of the present invention, the dripping module 3 employs a peristaltic pump capable of controlling the dripping speed, and the laser evaporation module 1 employs a solid laser emitter (please note whether this is feasible or not). In practical application, firstly, a water sample to be detected is dripped onto an adsorption material, then, the water sample is subjected to evaporation by using a laser evaporation component 1, heavy metals in the water sample are enriched on the adsorption material in the form of residual solid salt, then, an X-ray emission and receiving component 4 is used for generating X-ray radiation to the residual solid salt and receiving characteristic X-ray fluorescence released by the residual solid salt to obtain X-ray fluorescence spectrum data, and finally, an analysis component 5 is used for carrying out qualitative and quantitative analysis on the X-ray fluorescence spectrum data to obtain the type and the content of the heavy metals in the water sample.
As shown in fig. 2, as a preferred embodiment of the present invention, the apparatus further comprises:
and the test platform 2 is used for placing the adsorption material.
Specifically, the test platform 2 needs to be able to withstand the temperature of the laser emitted by the laser evaporation component 1, and the test platform 2 needs to have no influence on normal radiation of the X-rays onto the residual solid salt and normal reception of the characteristic X-ray fluorescence by the X-ray emission and reception component 4.
In a preferred embodiment of the present invention, the adsorbent is a polymer adsorbent.
Specifically, the adsorbing material can be at least one of polysulfone membrane, terpropylene vinyl acetate membrane, tetrapropylene vinyl acetate membrane, cellulose acetate membrane, aromatic polyhydrazide membrane and aromatic polyamide membrane; the adsorption material has high adsorption efficiency on heavy metal elements in water, is low in cost and is easy to obtain.
Example 2
The embodiment provides a method for analyzing trace heavy metals in water by X-ray fluorescence, which comprises the following steps as shown in the attached figure 1:
a clean sample cup is used for collecting a certain water sample, and secondary pollution of the collected water sample is avoided in the collecting process; the collected water samples can be a series of water samples such as surface water, underground water, domestic water, industrial wastewater and the like; preparing a 30mL water sample for later use;
placing an adsorption material on the test platform, wherein the adsorption material is a macromolecular adsorption material; dropwise adding the prepared water sample onto the adsorbing material by using a dropper at the speed of 0.05-0.1 mL/s;
emitting laser by a laser generator to enable the generated laser to irradiate on the adsorbing material; the laser power emitted by the laser is 5 KW;
when the water sample in the adsorption material is evaporated to dryness by laser and heavy metal elements in the water sample are enriched on the adsorption material in the form of residual solid salt, closing the laser generator;
generating X rays by using an X-ray fluorescence spectrometer, and radiating the X rays onto the adsorbing material after monochromatization and focusing; different element atoms in the residual solid salt on the adsorbing material release characteristic X-ray fluorescence, and the characteristic X-ray fluorescence is received by the X-ray fluorescence spectrometer to generate X-ray fluorescence spectrum data;
and qualitatively and quantitatively processing the X-ray fluorescence spectrum data to obtain the types and the contents of the heavy metals in the water sample.
By the embodiment, the optimal power range of the laser used when the laser evaporates to enrich is determined.
Example 3
This example provides a method for the fluorescent analysis of trace heavy metals in water by X-ray, which is carried out in the same manner as in example 2, except that the laser power emitted by the laser is 10 KW.
By the embodiment, the optimal power range of the laser used when the laser evaporates to enrich is determined.
Example 4
This example provides a method for the fluorescent analysis of trace heavy metals in water by X-ray, which is carried out in the same manner as in example 2, except that the laser power emitted by the laser is 8 KW.
By the embodiment, the optimal power of the laser used when the laser evaporates to enrich is determined.
Example 5
This example provides a method for the fluorescent analysis of trace heavy metals in water by X-ray, which is carried out in the same manner as in example 2, except that the laser power emitted by the laser is 11 KW.
According to the embodiment, when the power of the laser used in the laser evaporation enrichment exceeds 10KW, the efficiency of the laser evaporation enrichment is greatly reduced.
Example 6
This example provides a method for analyzing trace heavy metals in water by X-ray fluorescence, which is carried out in the same manner as in example 2, except that the laser power emitted by the laser is 4 KW.
According to the embodiment, when the power of the laser used for the laser evaporation enrichment is lower than 5KW, the efficiency of the laser evaporation enrichment is greatly reduced.
Example 7
This example provides a method for the X-ray fluorescence analysis of trace heavy metals in water, which was carried out in the same manner as in example 4, except that 15mL of the water sample was prepared.
This example was used to determine the optimal volume range of the water sample used when the enrichment was laser evaporated.
Example 8
This example provides a method for the X-ray fluorescence analysis of trace heavy metals in water, which was carried out in the same manner as in example 4, except that 50mL of the water sample was prepared.
This example was used to determine the optimal volume range of the water sample used when the enrichment was laser evaporated.
Example 9
This example provides a method for the X-ray fluorescence analysis of trace heavy metals in water, which was carried out in the same manner as in example 4, except that 51mL of the water sample was prepared.
According to the embodiment, when the volume of the water sample used in the laser evaporation enrichment exceeds 50mL, the efficiency of the laser evaporation enrichment is greatly reduced.
Example 10
This example provides a method for the X-ray fluorescence analysis of trace heavy metals in water, which was carried out in the same manner as in example 4, except that 14mL of the water sample was prepared.
According to the embodiment, when the volume of the water sample used in the laser evaporation enrichment is less than 15mL, the efficiency of the laser evaporation enrichment is greatly reduced.
Comparative example 1
The comparative example provides a method for analyzing trace heavy metals in water by adopting a solid-phase microextraction enrichment technology, which comprises the following steps:
a clean sample cup is used for collecting a certain water sample, and secondary pollution of the collected water sample is avoided in the collecting process; the collected water samples can be a series of water samples such as surface water, underground water, domestic water, industrial wastewater and the like; preparing a 30mL water sample for later use;
transferring the water sample into an enrichment pipe of a solid phase microextraction enrichment device, wherein a solid phase microextraction membrane is connected in the enrichment pipe; pumping the water sample by a vacuum pump, and allowing the water sample to pass through a solid phase micro-extraction membrane for 10 min;
taking out the solid phase micro-extraction membrane; generating X rays by using an X-ray fluorescence spectrometer, and radiating the X rays onto the solid-phase micro-extraction membrane after monochromatization and focusing; the metal elements on the solid phase micro-extraction membrane release characteristic X-ray fluorescence, and the characteristic X-ray fluorescence is received by an X-ray fluorescence spectrometer to generate X-ray fluorescence spectrum data;
and qualitatively and quantitatively processing the X-ray fluorescence spectrum data to obtain the types and the contents of the heavy metals in the water sample.
Two groups of same water samples are prepared, the detection limits of four heavy metals of Cr, As, Cd and Pb in the two groups of water samples are respectively detected by the method in the embodiment 2 and the method in the comparative example 1, and the detection results are shown in the attached table 1: when the method in the embodiment 2 is adopted, the detection limits of the four heavy metals of Cr, As, Cd and Pb in the water sample are respectively 0.002mg/L, 0.001mg/L and 0.001 mg/L; when the method of comparative example 1 was used, the detection limits of the four heavy metals Cr, As, Cd, Pb in the water sample were 1mg/L, 0.5mg/L, respectively. It can be seen that the detection limit of the heavy metals in the water sample is obviously improved after the laser evaporation enrichment method is adopted.
TABLE 1
| Unit mg/L | Cr | As | Cd | Pb |
| Detection limit of solid phase micro-extraction technology | 1 | 0.5 | 0.5 | 0.5 |
| Detection limit after laser evaporation to dryness enrichment | 0.002 | 0.001 | 0.001 | 0.001 |
According to the comparison example, the detection limit of the heavy metal in the water sample is obviously improved by adopting the laser evaporation enrichment method compared with the solid-phase micro-extraction technical method.
Comparative example 2
This comparative example provides a method for analyzing trace amounts of heavy metals in water using a solid phase microextraction enrichment technique, which was carried out in the same manner as in comparative example 1, except that 15mL of the prepared water sample was used.
According to the comparative example, the detection limit of the laser evaporation enrichment method is always higher than that of the solid phase micro-extraction technology method in the volume range of the optimal water sample of the laser evaporation enrichment method.
Comparative example 3
This comparative example provides a method for analyzing trace amounts of heavy metals in water using a solid phase microextraction enrichment technique, which was carried out in the same manner as in comparative example 1, except that a 50mL sample of water was prepared.
According to the comparative example, the detection limit of the laser evaporation enrichment method is always higher than that of the solid phase micro-extraction technology method in the volume range of the optimal water sample of the laser evaporation enrichment method.
Comparative example 4
This comparative example provides a method for analyzing trace amounts of heavy metals in water using a solid phase microextraction enrichment technique, which was carried out in the same manner as in comparative example 1, except that a 51mL sample of water was prepared.
According to the comparative example, even if the volume range of the optimal water sample of the laser evaporation enrichment method is not within, the detection limit of the laser evaporation enrichment method is higher than that of the solid phase micro-extraction technical method.
Comparative example 5
This comparative example provides a method for analyzing trace amounts of heavy metals in water using a solid phase microextraction enrichment technique, which was carried out in the same manner as in comparative example 1, except that 14mL of the prepared water sample was used.
According to the comparative example, even if the volume range of the optimal water sample of the laser evaporation enrichment method is not within, the detection limit of the laser evaporation enrichment method is higher than that of the solid phase micro-extraction technical method.
Comparative example 6
The comparative example provides a method for analyzing trace heavy metals in water by adopting a solid-phase microextraction enrichment technology, and the implementation steps of the method are the same as those of the comparative example 1, wherein the difference is that the suction filtration time is 5 min.
According to the comparative example, even in the optimal suction filtration range of the solid phase micro extraction enrichment technology, the detection limit of the laser evaporation enrichment technology is still higher than that of the solid phase micro extraction technology.
Comparative example 7
The comparative example provides a method for analyzing trace heavy metals in water by adopting a solid-phase microextraction enrichment technology, and the implementation steps of the method are the same as those of the comparative example 1, wherein the difference is that the suction filtration time is 15 min.
According to the comparative example, even in the optimal suction filtration range of the solid phase micro extraction enrichment technology, the detection limit of the laser evaporation enrichment technology is still higher than that of the solid phase micro extraction technology.
The high-sensitivity X-ray fluorescence detection method for elements such as cadmium in water is implemented in a common mechanical mode in an installation mode, a connection mode or a setting mode as long as the beneficial effects of the method can be achieved.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for analyzing trace heavy metals in water by X-ray fluorescence is characterized by comprising the following steps:
s1, collecting a water sample to be detected for detection;
s2, dropwise adding the water sample to be detected onto the adsorption material;
s3, drying a water sample to be detected on an adsorbing material by using laser to dryness so as to enrich heavy metal elements in the water sample on the adsorbing material in the form of residual solid salt;
s4, carrying out X-ray radiation on the residual solid salt on the adsorbing material, and receiving characteristic X-ray fluorescence released by the residual solid salt to obtain X-ray fluorescence spectrum data;
and S5, performing qualitative and quantitative analysis on the heavy metals in the water sample to be detected according to the X-ray fluorescence spectrum data.
2. The method for X-ray fluorescence analysis of trace heavy metals in water As claimed in claim 1, wherein the heavy metals detected by the method for X-ray fluorescence analysis of trace heavy metals in water include Mn, Fe, Ni, Cu, Zn, Pb, Cr, Cd and As.
3. The method for X-ray fluorescence analysis of trace heavy metals in water as claimed in claim 2, wherein the detection of trace heavy metals in water is limited to ug/L.
4. The method for X-ray fluorescence analysis of trace heavy metals in water of claim 1, wherein the water sample is dropped onto the adsorbent material at a rate of 10-50mL at a rate of 0.05-0.2 mL/s.
5. The method for X-ray fluorescence analysis of trace heavy metals in water according to claim 1, wherein the adsorbing material is a polymeric adsorbing material.
6. The method for analyzing trace heavy metals in water by X-ray fluorescence according to claim 1, wherein the power of laser evaporation to dryness is 5-10 KW.
7. The method for X-ray fluorescence analysis of trace heavy metals in water of claim 1, wherein the X-ray is a monochromated and focused X-ray.
8. A high-sensitivity X-ray fluorescence detection method for elements such as cadmium in water is characterized by comprising the following steps:
the dropwise adding component is used for dropwise adding the water sample to be detected onto the adsorbing material;
the laser evaporation-to-dryness component is used for evaporating and drying a water sample to be detected on the adsorbing material so as to enrich heavy metal elements in the water sample on the adsorbing material in the form of residual solid salt;
the X-ray transmitting and receiving assembly is used for carrying out X-ray radiation on the residual solid salt on the adsorbing material and receiving characteristic X-ray fluorescence released by the residual solid salt to obtain X-ray fluorescence spectrum data;
and the analysis component is used for qualitatively and quantitatively analyzing the heavy metal in the water sample to be detected according to the X-ray fluorescence spectrum data.
9. The method of claim 8, wherein the apparatus further comprises a testing platform for placing the adsorbing material.
10. The method of claim 8, wherein the adsorbent is a polymeric adsorbent.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114878617A (en) * | 2022-06-01 | 2022-08-09 | 苏州佳谱科技有限公司 | Enrichment detection method and device for trace heavy metal elements in liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114878617A (en) * | 2022-06-01 | 2022-08-09 | 苏州佳谱科技有限公司 | Enrichment detection method and device for trace heavy metal elements in liquid |
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