CN104655597A - Hydride generation and sample introduction method of seleninic acid radical ions - Google Patents
Hydride generation and sample introduction method of seleninic acid radical ions Download PDFInfo
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- CN104655597A CN104655597A CN201310601226.2A CN201310601226A CN104655597A CN 104655597 A CN104655597 A CN 104655597A CN 201310601226 A CN201310601226 A CN 201310601226A CN 104655597 A CN104655597 A CN 104655597A
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Abstract
The invention discloses a hydride generation and sample introduction method of seleninic acid radical ions. The method comprises the following steps: inorganically digesting a to-be-detected sample, and reducing selenate radical ions into seleninic acid radical ions to obtain a digested solution; adding solid acid and soluble salt containing chloride ions or iodide ions into the digested solution, and fixing the volume with pure water to obtain a to-be-detected sample solution; respectively extracting the to-be-detected sample solution and an alkaline potassium borohydride solution by virtue of a sampling pump, and mixing; reacting the seleninic acid radical ions in the to-be-detected sample solution with potassium borohydride under an acidic condition to generate hydrogen selenide and hydrogen after the to-be-detected sample solution and the alkaline potassium borohydride solution are mixed; separating liquid-state components of the generated hydrogen selenide and hydrogen in a gas-liquid separator, and feeding into an atomizer of atomic fluorescence so as to complete the hydride generation and sample introduction processes of atomic fluorescence detection. Compared with the method only using sulfamic acid, the method has the advantages that 90 percent of reagent consumption is reduced, and the problem that detection is influenced by easily crystallized high-concentration sulfamic acid is solved. The method has excellent popularization and application values.
Description
Technical field
The present invention relates to atomic spectroscopic analysis field, in particular to a kind of hydride generation sample injection method of selenite radical ion.
Background technology
In atomic spectroscopic analysis field, hydride generation/steam generation sampling technique is because have higher sample introduction efficiency relative to the nebulization sampling of routine, one of sample introduction means being always used as atomic spectrum instrument, to obtain higher sensitivity for analysis, make Matrix effects greatly reduce simultaneously.
The hydride generation sampling technique of selenite radical ion is widely used in atomic spectrum alanysis instrument at present, as atomic absorption spectrophotometer (AAS), atomic fluorescence spectrometer, inductively coupled plasma-emission spectrometer and sense coupled plasma-mass spectrum etc.
Application number is 201210238016.7, name is called that a kind of sulfaminic acid that uses that patent discloses of " solid acid compressing tablet of portable atomic fluorescence field quick detection and its preparation method and application " substitutes concentrated acid as solid acid, when solving atomic fluorescence field quick detection, concentrated acid is difficult to carry, potential danger is large and field environment is changeable, quantitatively pipettes the problem of comparatively difficulty.But, above-mentioned patent is when being applied to the hydride generation sampling technique of selenite radical ion, if only need the mass concentration of sulfaminic acid just can reach the sensitivity close with 20% hydrochloric acid more than 20%, therefore very big to the consumption of sulfaminic acid, analysis cost is higher, and the sulfaminic acid of higher concentration very easily crystallization, affect the mensuration of selenite radical ion.Patent also not relevant at present or document propose the method solved to the problems referred to above.
Summary of the invention
The invention provides a kind of hydride generation sample injection method of selenite radical ion, the hydrogen ion needed for hydride generation is provided by solid acid, soluble-salt containing chlorion or iodide ion provides selenite radical ion to generate anionic atmosphere required for hydrogen selenide, relative to the reagent consumption only using the method for 20% sulfaminic acid to save 90%, and there is not the problem of high concentration sulfaminic acid easy crystallization impact mensuration, there are preferably promotion and application and be worth.
For achieving the above object, the invention provides a kind of hydride generation sample injection method of selenite radical ion, comprising the following steps:
Clear up at testing sample through inorganization and after being selenite radical ion by selenate radical ion reduction, obtain digestion solution;
In digestion solution, add solid acid and the soluble-salt containing chlorion or iodide ion, obtain testing sample solution with after pure water constant volume;
Extract testing sample solution respectively by sampling pump and alkaline solution of potassium borohydride mixes, the selenite radical ion after the two mixing in testing sample solution reacts with potassium borohydride in acid condition and generates hydrogen selenide and hydrogen;
The hydrogen selenide generated and hydrogen enter the atomizer of atomic fluorescence in gas-liquid separator after separation of liquid component, complete the hydride generation sample introduction process that atomic fluorescence detects.
Optionally, extract testing sample solution and alkaline solution of potassium borohydride respectively by sampling pump to carry out blend step and comprise:
Be kept in accessing ring by the first peristaltic pump pumps testing sample solution;
The alkaline solution of potassium borohydride synchronously extracted by the testing sample solution in the first peristaltic pump promotion accessing ring and the second peristaltic pump is mixed in threeway mixing module.
Optionally, the atomizer step that the hydrogen selenide generated and hydrogen enter atomic fluorescence in gas-liquid separator after separation of liquid component comprises:
The hydrogen selenide generated and hydrogen and reacted mixed liquor are sent into gas-liquid separator by threeway mixing module and are carried out gas-liquid separation, hydrogen selenide after separation and hydrogen enter the atomizer of atomic fluorescence, wherein the top of gas-liquid separator is communicated with the atomizer of atomic fluorescence, the bottom of gas-liquid separator is communicated with waste liquid cup, and the upper portion side wall of gas-liquid separator is communicated with argon gas source.
Optionally, solid acid is at least one in trichloroacetic acid, sulfaminic acid, oxalic acid and tartrate.
Optionally, the soluble-salt containing chlorion is LiCl, NaCl, KCl, MgCl
2, CaCl
2and FeCl
3in at least one.
Optionally, the soluble-salt containing iodide ion is NaI and/or KI.
Optionally, the mass concentration of solid acid in testing sample solution is 0.5% ~ 10%.
Optionally, the mass concentration of soluble-salt in testing sample solution is 0.2% ~ 20%.
In the present invention, solid acid provides the hydrogen ion needed for hydride generation, and the soluble-salt containing chlorion or iodide ion is then to provide selenite radical ion and generates anionic atmosphere required for hydrogen selenide; Because reagent used in the present invention is solid, there is no volatility, environmental pollution is little, little to human injury, and simple to operate, solve the consumption of sulfaminic acid greatly, the higher and sulfaminic acid of higher concentration of analysis cost is very easily because temperature variation crystallization affects the problem of the mensuration of selenite radical ion; Relative to the reagent consumption only using the method for 20% sulfaminic acid to save 90%, and there is not the problem of high concentration sulfaminic acid easy crystallization impact mensuration, there are preferably promotion and application and be worth.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the hydride generation sampling device structural representation of the selenite radical ion of one embodiment of the invention;
Fig. 2 is the hydride generation sample injection method process flow diagram of the selenite radical ion of one embodiment of the invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not paying the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Fig. 1 is the hydride generation sampling device structural representation of the selenite radical ion of one embodiment of the invention; As shown in the figure, this device comprises: 1-testing sample solution; 2-first peristaltic pump; 3-accessing ring; 4-threeway mixing module; 5-gas-liquid separator; 6-argon gas source of the gas; 7-waste liquid cup; 8-second peristaltic pump; 9-solution of potassium borohydride.
Fig. 2 is the hydride generation sample injection method process flow diagram of the selenite radical ion of one embodiment of the invention.As shown in the figure, this hydride generation sample injection method comprises the following steps:
S110, clears up at testing sample through inorganization and after being selenite radical ion by selenate radical ion reduction, obtain digestion solution;
S120, adds solid acid and the soluble-salt containing chlorion or iodide ion, obtains testing sample solution with after pure water constant volume in digestion solution;
Wherein, solid acid provides the hydrogen ion needed for hydride generation, and the soluble-salt containing chlorion or iodide ion is then to provide selenite radical ion and generates anionic atmosphere required for hydrogen selenide.The mass concentration of solid acid in testing sample solution is 0.5% ~ 10%.Solid acid can be at least one in trichloroacetic acid, sulfaminic acid, oxalic acid and tartrate.The mass concentration of soluble-salt in testing sample solution is 0.2% ~ 20%.Soluble-salt containing chlorion can be LiCl, NaCl, KCl, MgCl
2, CaCl
2and FeCl
3in at least one.Soluble-salt containing iodide ion can be NaI and/or KI.
S130, extracts testing sample solution respectively by sampling pump and alkaline solution of potassium borohydride mixes, and the selenite radical ion after the two mixing in testing sample solution reacts with potassium borohydride in acid condition and generates hydrogen selenide and hydrogen;
Wherein, extract testing sample solution and alkaline solution of potassium borohydride respectively by sampling pump to carry out blend step and comprise: be kept in accessing ring by the first peristaltic pump pumps testing sample solution; The alkaline solution of potassium borohydride synchronously extracted by the testing sample solution in the first peristaltic pump promotion accessing ring and the second peristaltic pump is mixed in threeway mixing module.
S140, the hydrogen selenide generated and hydrogen enter the atomizer of atomic fluorescence in gas-liquid separator after separation of liquid component, complete the hydride generation sample introduction process that atomic fluorescence detects.
Wherein, the atomizer step that the hydrogen selenide generated and hydrogen enter atomic fluorescence in gas-liquid separator after separation of liquid component comprises: the hydrogen selenide generated and hydrogen and reacted mixed liquor are sent into gas-liquid separator by threeway mixing module and carried out gas-liquid separation, hydrogen selenide after separation and hydrogen enter the atomizer of atomic fluorescence, wherein the top of gas-liquid separator is communicated with the atomizer of atomic fluorescence, the bottom of gas-liquid separator is communicated with waste liquid cup, and the upper portion side wall of gas-liquid separator is communicated with argon gas source.
Be sulfaminic acid, soluble-salt below with solid acid be example for potassium chloride, illustrate the hydride generation sample introduction process of selenite radical ion:
(1) clear up at testing sample through inorganization and after being selenite radical ion by selenate radical ion reduction, obtain 2mL digestion solution;
(2) in digestion solution, add 0.20g sulfaminic acid and 0.5g potassium chloride, after also dissolving with pure water constant volume the material added, mix, obtain testing sample solution;
(3) first peristaltic pump pumps testing sample solutions are also kept in accessing ring;
The alkaline solution of potassium borohydride that testing sample solution in (4) first peristaltic pumps promotion accessing rings and the second peristaltic pump synchronously extract mixes in threeway mixing module;
(5) the selenite radical ion after the two mixing in sample solution reacts with potassium borohydride in acid condition and generates hydrogen selenide and hydrogen;
(6) hydrogen selenide and hydrogen enter the atomizer of atomic fluorescence in gas-liquid separator after separation of liquid component, namely complete the hydride generation sample introduction process that atomic fluorescence detects.
In above-described embodiment, solid acid provides the hydrogen ion needed for hydride generation, and the soluble-salt containing chlorion or iodide ion is then to provide selenite radical ion and generates anionic atmosphere required for hydrogen selenide; Because reagent used in the present invention is solid, there is no volatility, environmental pollution is little, little to human injury, and simple to operate, solve the consumption of sulfaminic acid greatly, the higher and sulfaminic acid of higher concentration of analysis cost is very easily because temperature variation crystallization affects the problem of the mensuration of selenite radical ion; Relative to the reagent consumption only using the method for 20% sulfaminic acid to save 90%, and there is not the problem of high concentration sulfaminic acid easy crystallization impact mensuration, there are preferably promotion and application and be worth.
One of ordinary skill in the art will appreciate that: accompanying drawing is the schematic diagram of an embodiment, the module in accompanying drawing or flow process might not be that enforcement the present invention is necessary.
One of ordinary skill in the art will appreciate that: the module in the device in embodiment can describe according to embodiment and be distributed in the device of embodiment, also can carry out respective change and be arranged in the one or more devices being different from the present embodiment.The module of above-described embodiment can merge into a module, also can split into multiple submodule further.
Last it is noted that above embodiment is only in order to illustrate technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in previous embodiment, or carries out equivalent replacement to wherein portion of techniques feature; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the spirit and scope of embodiment of the present invention technical scheme.
Claims (8)
1. a hydride generation sample injection method for selenite radical ion, is characterized in that, comprise the following steps:
Clear up at testing sample through inorganization and after being selenite radical ion by selenate radical ion reduction, obtain digestion solution;
In described digestion solution, add solid acid and the soluble-salt containing chlorion or iodide ion, obtain testing sample solution with after pure water constant volume;
Extract described testing sample solution respectively by sampling pump and alkaline solution of potassium borohydride mixes, the selenite radical ion after the two mixing in described testing sample solution reacts with potassium borohydride in acid condition and generates hydrogen selenide and hydrogen;
The hydrogen selenide generated and hydrogen enter the atomizer of atomic fluorescence in gas-liquid separator after separation of liquid component, complete the hydride generation sample introduction process that atomic fluorescence detects.
2. the method for claim 1, is characterized in that, describedly extracts described testing sample solution and alkaline solution of potassium borohydride respectively by sampling pump and carries out blend step and comprise:
Be kept in accessing ring by testing sample solution described in the first peristaltic pump pumps;
Promote by described first peristaltic pump the alkaline solution of potassium borohydride that testing sample solution in described accessing ring and the second peristaltic pump synchronously extract to mix in threeway mixing module.
3. method as claimed in claim 2, it is characterized in that, the atomizer step that described generated hydrogen selenide and hydrogen enter atomic fluorescence in gas-liquid separator after separation of liquid component comprises:
The hydrogen selenide generated and hydrogen and reacted mixed liquor are sent into gas-liquid separator by described threeway mixing module and are carried out gas-liquid separation, hydrogen selenide after separation and hydrogen enter the atomizer of atomic fluorescence, the top of wherein said gas-liquid separator is communicated with the atomizer of described atomic fluorescence, the bottom of described gas-liquid separator is communicated with waste liquid cup, and the upper portion side wall of described gas-liquid separator is communicated with argon gas source.
4. the method for claim 1, is characterized in that, described solid acid is at least one in trichloroacetic acid, sulfaminic acid, oxalic acid and tartrate.
5. the method for claim 1, is characterized in that, the described soluble-salt containing chlorion is LiCl, NaCl, KCl, MgCl
2, CaCl
2and FeCl
3in at least one.
6. the method for claim 1, is characterized in that, the described soluble-salt containing iodide ion is NaI and/or KI.
7. the method for claim 1, is characterized in that, the mass concentration of described solid acid in described testing sample solution is 0.5% ~ 10%.
8. the method for claim 1, is characterized in that, the mass concentration of described soluble-salt in described testing sample solution is 0.2% ~ 20%.
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| CN102305779A (en) * | 2011-07-04 | 2012-01-04 | 西北有色地质研究院 | Solid sampling-non-dispersion atomic fluorescence photometer collocating device and analyzing method |
| CN102721678A (en) * | 2012-07-09 | 2012-10-10 | 北京瑞利分析仪器有限公司 | Solid acid tablet for quick field detection of portable atomic fluorescence and preparation method and application thereof |
| CN103018227A (en) * | 2012-12-27 | 2013-04-03 | 江苏德林环保技术有限公司 | On-line in-water heavy metal monitor based on atomic fluorescence spectroscopy |
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2013
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| JP2004045123A (en) * | 2002-07-10 | 2004-02-12 | Tdk Corp | Element analysis method and element analysis device |
| CN102305779A (en) * | 2011-07-04 | 2012-01-04 | 西北有色地质研究院 | Solid sampling-non-dispersion atomic fluorescence photometer collocating device and analyzing method |
| CN102721678A (en) * | 2012-07-09 | 2012-10-10 | 北京瑞利分析仪器有限公司 | Solid acid tablet for quick field detection of portable atomic fluorescence and preparation method and application thereof |
| CN103018227A (en) * | 2012-12-27 | 2013-04-03 | 江苏德林环保技术有限公司 | On-line in-water heavy metal monitor based on atomic fluorescence spectroscopy |
Non-Patent Citations (3)
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| NOROOZ MALEKI等: "Determination of selenium in water and soil by hydride generation atomic absorption spectrometry using solid reagents", 《TALANTA》 * |
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Effective date of registration: 20230914 Address after: 100094 160 Beiqing Road, Haidian District, Beijing Patentee after: BEIJING BEIFEN-RUILI ANALYTICAL INSTRUMENT (Group) Co.,Ltd. Address before: 100016, A5 building, No. 9 East Jiuxianqiao Road, Beijing, Chaoyang District Patentee before: BEIJING RAYLEIGH ANALYTICAL INSTRUMENT CO.,LTD. |
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