CN1700012A - High performance liquid chromatography-hydride atomic absorption / fluorescence spectrum instruments interface - Google Patents
High performance liquid chromatography-hydride atomic absorption / fluorescence spectrum instruments interface Download PDFInfo
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- CN1700012A CN1700012A CN 200510011797 CN200510011797A CN1700012A CN 1700012 A CN1700012 A CN 1700012A CN 200510011797 CN200510011797 CN 200510011797 CN 200510011797 A CN200510011797 A CN 200510011797A CN 1700012 A CN1700012 A CN 1700012A
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Abstract
The invention relates to an effective liquid chromatograph-hydride atom absorption/ fluorescence spectrum instrument interface in the field of analytical chemistry joint instrument interface designing technique. It has the following characters: it contains connected slim inner diameter three-bit byte, slim quartz tube, four-way connection, reaction tube and big inner diameter three-bit byte, wherein first tube of slim inner diameter three-bit byte is connected with effluent liquid entrance of effective liquid chromatograph; second tube is connected with oxidant spread tube; the third tube in connected with one end of slim quartz tube which in near a UV lamp tube; the other end of slim quartz tube is connected with first tube of four-way connection, second tube of four-way connection is connected with acid solution spread tube, the third tube is connected with reducer spread tube, the forth tube is connected with one end of reaction tube, while the other end is connected with first tube of big inner diameter three-bit byte, second tube in connected with addendum, the third tube is connected with spread tube which is to gas-liquid divider.
Description
Technical field:
The present invention relates to analytical chemistry coupling instrument Interface design technical field, particularly the Interface design of chromatogram and Electrothermal Atomic Absorption/atomic fluorescence device coupling.
Background technology:
The toxicity of element, the biological form that can be decided by its existence to a great extent to property and animal migration etc., morphological analysis can provide more information than the analysis of element total concentration, it can not only reflect content of analyte, and can reflect the existence of analyte, all significant to researchs such as environmental science, life sciences, caused enough attention of people.Morphological analysis usually measure to as if biology or environmental sample, in general sample matrices is comparatively complicated, to survey constituent content be trace level to desire, adds also and each form will will be distinguished qualitative, quantitative, so its difficulty is more much bigger than measuring the element total amount.Common morphological analysis method mainly is with high efficiency separation system and the coupling of element wholesomeness detecting device.The key of development coupling technique is an interfacing.
Chromatographic technique and the coupling of element detecting device have been widely used in the morphological analysis of trace toxic metals and metalloid.High performance liquid chromatography is simple with its high separating efficiency, sample preparation, fast, favorable reproducibility, advantage such as the moving phase range of choice is wide has become a kind of morphological analysis instrument of brute force.High performance liquid chromatography and the coupling of element detecting device had both had good selectivity, can reach the desired high sensitivity requirement of morphological analysis again.At present, high performance liquid chromatography mainly concentrates on and inductivity coupled plasma mass spectrometry (ICP-MS, inductively coupled plasma atomic emission (ICP-AES) coupling.But these instruments cost an arm and a leg, and the operating cost height is difficult to the means as conventional sense.
Atomic absorption (AAS)/atomic fluorescence (AFS) instrument is common element wholesomeness detecting device, and price and operation cost are low, and favorable reproducibility is highly sensitive, is easy to be used for conventional analysis.But it can only be used for the analysis of element total amount, realize element morphological analysis must with the isolation technics coupling.
Hydride takes place to have avoided interference, and improved the transfer efficiency (100%) of analyte because it separates analyte with matrix, has high selectivity and sensitivity, thereby is widely used in the analysis of arsenic, mercury, antimony, selenium.Arsenic is example, and several simple shapes of arsenic (As (III), As (V), monomethyl arsenic (MMA), dimethyl arsenic (DMA)) can directly produce hydride.And more complicated organoarsenium compound such as arsenic betaine (AsB), arsenocholines (AsC) etc. must add the device of an in-line digestion, with the comparatively complicated organo-arsenic molecule of destruction structure, but make its micromolecule that changes the direct hydrogenation thing into, thereby detect.
The key of liquid chromatography and atomic absorption/atomic fluorescence spectrophotometry coupling technique is the high efficiency in-line digestion device of design, what generally use at present is the micro-wave digestion device, the outstanding advantage of this device is the purpose that can reach in-line digestion by the power that controlled microwave is cleared up, but owing to the overheated phenomenon of solution occurs in the process of micro-wave digestion, cause the integral pressure of stream to raise greatly, the phenomenon that pipeline bursts apart therefore occurs.So in actual measurement, usually cause unnecessary trouble.Another shortcoming is the micro-wave oven that micro-wave digestion needs a large volume, has therefore caused the instrument volume to increase and stream increases and the phenomenon of the bands of a spectrum broadening of generation.
It is the in-line digestion means of a kind of simple and effective of growing up gradually in recent years that ultraviolet is cleared up.It is by the degradation of radical pair organic macromolecule under the strong UV-irradiation, the big molecule that being difficult to of making that chromatogram flows out forms hydride is converted into the micromolecule that is easy to form hydride, thereby makes the compound of hydride generation-atomic absorption/atom fluorimetry different shape become possibility.In order to reach the high-level efficiency of in-line digestion, generally adopted the in-line digestion pipeline that reaches 5 meters, but, therefore reduced the efficient of chromatographic resolution widely because the longer pipe road causes broadening behind the serious post.
High performance liquid chromatography and atomic absorption coupling can be become the strong analysis tool of morphological analysis, but realize that the key of this coupling technique is interface arrangement and in-line digestion device.In Interface design, how to realize that chromatogram effluent and digestion solution are mixed and under UV-irradiation, complicated ingredient is cleared up; How to make to improve and clear up efficient, produce hydride and do not cause the chromatogram broadening; Become high performance liquid chromatography-on-line ultraviolet to clear up-hydride generation-atomic absorption/key technical problem of atomic fluorescence spectrophotometry coupling.
Summary of the invention:
The objective of the invention is to solve the above-mentioned key issue in high performance liquid chromatography and the atomic absorption/atomic fluorescence device coupling technique, development high performance liquid chromatography and electrothermal quartz tube atomic absorption/atomic fluorescence combined apparatus, be arsenic, mercury, antimony, the morphological analysis of selenium etc. are set up simply fast, the technology platform of economic and reliable.
High performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface proposed by the invention is characterised in that it contains the fine inner diameter threeway (2) that connects successively, thin quartz ampoule (4), four-way (6), reaction tube (9), large diameter threeway (12); First arm of described fine inner diameter threeway (2) connects high performance liquid chromatography effluent inlet (1), second arm connects oxidizing agent solution transfer tube (3), the 3rd arm connects an end of described thin quartz ampoule (4), and described thin quartz ampoule (4) is close to a ultraviolet lamp tube (5); The other end of described thin quartz ampoule (4) connects first arm of described four-way, second arm of described four-way (6) connects acid solution transfer tube (7), its the 3rd arm connects reductant solution transfer tube (8), its the 4th arm connects an end of described reaction tube (9), the other end of described reaction tube (9) connects first arm of large diameter threeway (12), second arm of described large diameter threeway (12) connects carrier gas transfer tube (10), and its 3rd arm connects the delivery tube (11) of leading to gas-liquid separator.
Its feature is that also described thin quartz ampoule (4) also connects another thin quartz ampoule (4) by connecting pipe, and these two thin quartz ampoules are adjacent on ultraviolet lamp tube.
The internal diameter of described fine inner diameter threeway (2) is 0.5～1.2mm.The internal diameter of described four-way (6) is 1～2mm.The internal diameter of described large diameter threeway (12) is 1.5～2.5mm.The internal diameter of described reaction tube (9) is 0.5-2mm, and length is 30～60cm.The internal diameter of described thin quartz ampoule (4) is 0.5～2mm, and length is 10～40cm.The power of described uviol lamp is 5-15W.
The described flow that pumps into that pumps into oxidizing agent solution in the pipe (3) is that the flow that pumps into that 0.5-2ml/min pumps into the middle acid solution of pipe (7) is 0.5-2.5ml/min; The flow that pumps into that pumps into reductant solution in the pipe (8) is 0.5-2.5ml/min.Described oxygenant is K
2S
2O
3Solution, described acid solution are to connect hydrochloric acid solution, and described reductive agent is KBH
4Or NaBH
4Solution.
Experimental results show that: the present invention can realize complicated organo-arsenic, and mercury in the time of antimony, the in-line digestion of compounds such as selenium, has solved the problem of peak broadening again, has been dealt into its intended purposes.
Description of drawings:
Fig. 1 is the high performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface synoptic diagram;
Fig. 2 is four kinds of chromatograms that arsenium morphological analysis obtains.
Embodiment:
Embodiment one
As shown in Figure 1, the present invention mainly comprises: fine inner diameter threeway (2), thin quartz ampoule (4), uviol lamp (5), four-way (6), reaction tube (9), large diameter threeway (12) and connecting pipe.Its connected mode is: fine inner diameter threeway (2) successively with thin quartz ampoule (4), four-way (6), reaction tube (9), large diameter threeway (12) connects.Fine inner diameter threeway (2) arm connects high performance liquid chromatography effluent inlet (1) and K
2S
2O
3(1.5%) the solution transfer tube (3) that (, can also adopt other persulfate) as oxygenant.Two thin quartz ampoules (4) (internal diameter: 0.5mm, length: connect with connecting line (14) 20cm), be close proximity to ultraviolet lamp tube (5) (uviol lamp power: 5W) outer wall.Four-way connects hydrochloric acid solution (30%) (acid solution produces active hydrogen with the reductive agent reaction, and reduction arsenic is hydride) transfer tube (7) and KBH
4(1.5%) (reductive agent is generally used KBH
4Or NaBH
4) solution transfer tube (8).Reaction tube (9) internal diameter 1.5mm, length 30cm.The connecting line that need to prove interface selects for use different inner diameters how logical, fine inner diameter threeway (2): 0.5mm, and four-way (6): 1mm, large diameter threeway (12): 1.5mm couples together each parts with connecting pipe.Three pumps are connected to the K that is connected with fine inner diameter threeway (2)
2S
2O
3Solution pumps into pipe (3), and (pump into flow: 1ml/min), the hydrochloric acid solution that is connected with four-way (6) pumps into pipe (7) and (pumps into flow: 1ml/min) and KBH
4Solution pump into pipe (8) go up (pump into flow: 1ml/min), in order to pump into required reaction solution.Large diameter threeway (12) one arms are connected the gas delivery tube (10) that connects the argon gas steel cylinder, and argon gas is as the carrier gas of gas transmission.Another arm of large diameter threeway (12) connects the delivery tube (11) of leading to gas-liquid separator.During use, analyte separates after fine inner diameter threeway (2) and K through high performance liquid chromatography
2S
2O
3The mixed ultraviolet that enters of solution is cleared up part (thin quartz ampoule (4)), clears up to produce the micromolecule that is easy to hydride under action of ultraviolet ray.Product after clearing up with hydrochloric acid solution and KBH
4The mixed back of solution forms hydride, enters gas-liquid separator under the carrying secretly of argon gas.Gas through gas-liquid separator carries out atomization towards atomizing apparatus, detects with atomic absorption or atomic fluorescence device then.Fig. 2 has provided four kinds of chromatograms that arsenium morphological analysis obtains, and as can be seen from the figure, several arsenic morphologies have obtained baseline separation, and have kept good peak shape, has solved the problem of peak broadening, has effectively realized the coupling of HPLC and atomic absorption/atomic absorption.
Embodiment two
Connected mode is with embodiment 1,
Two thin quartz ampoules (4), internal diameter: 1.5mm, length: 40cm;
Uviol lamp power: 15W;
Reaction tube (9): internal diameter 0.5mm, length 60cm;
Fine inner diameter threeway (2): internal diameter 1.2mm;
Four-way (6): internal diameter 1.5mm;
Large diameter threeway (12): internal diameter 2.5mm;
K
2S
2O
3Solution pump inbound traffics: 0.5ml/min;
Hydrochloric acid solution pumps into flow: 0.5ml/min;
KBH
4Solution pump inbound traffics: 0.5ml/min.
Analyte separates after fine inner diameter threeway (2) and K through high performance liquid chromatography
2S
2O
3The mixed ultraviolet that enters of solution is cleared up part (thin quartz ampoule (4)), clears up to produce the micromolecule that is easy to hydride under action of ultraviolet ray.Product after clearing up with hydrochloric acid solution and KBH
4The mixed back of solution forms hydride, enters gas-liquid separator under the carrying secretly of argon gas.Gas through gas-liquid separator carries out atomization towards atomizing apparatus, detects with atomic absorption or atomic fluorescence device then, and (DMA, arsenobetaine arsenocholine) have obtained good separation to several arsenic morphologies, and peak shape is good.
Embodiment three
Connected mode is with embodiment 1,
Two thin quartz ampoules (4), internal diameter: 2mm, length: 10cm;
Uviol lamp power: 8W;
Reaction tube (9): 2mm, length 40cm;
Fine inner diameter threeway (2): internal diameter 1mm;
Four-way (6): internal diameter 2mm;
Large diameter threeway (12): internal diameter 2mm;
K
2S
2O
3Solution pump inbound traffics: 2ml/min;
Hydrochloric acid solution pumps into flow: 2.5ml/min;
KBH
4Solution pump inbound traffics: 2.5ml/min.
Analyte separates after fine inner diameter threeway (2) and K through high performance liquid chromatography
2S
2O
3The mixed ultraviolet that enters of solution is cleared up part (thin quartz ampoule (4)), clears up to produce the micromolecule that is easy to hydride under action of ultraviolet ray.Product after clearing up with hydrochloric acid solution and KBH
4The mixed back of solution forms hydride, enters gas-liquid separator under the carrying secretly of argon gas.The atomizing apparatus that the gas of process gas-liquid separator leads to carries out atomization, detects with atomic absorption or atomic fluorescence device then, and several arsenic morphologies (Asbetaine, As (III), MMA, As (V)) have all obtained good separation, and peak shape is good.
Of the present inventionly be skillfully constructed, simple for structure, novel in design, dead volume is little.This interface is being realized complicated organo-arsenic, and mercury in the time of antimony, the in-line digestion of compounds such as selenium, has solved the problem of peak broadening again.High performance liquid chromatography and atomic absorption/atomic fluorescence spectrometer device good binding are got up.The fine inner diameter threeway can effectively reduce the diffusion of high performance liquid chromatography effluent; The transmitance that thin quartz ampoule has increased ultraviolet light has realized complicated organo-arsenic preferably, mercury, and antimony, the in-line digestion of compounds such as selenium, digestion tube is short out, has improved peak broadening problem greatly.The four-way design has effectively realized clearing up afterproduct and hydride generation liquid is mixed, and mixed pipeline has guaranteed the efficient that hydride takes place; The large diameter threeway has solved hydride the hydrogen of generation and the line pressure problem of unstable that the carrier gas adding causes has taken place, and can realize the output of stable air-flow and liquid stream.The present invention combine high performance liquid chromatography high separating efficiency, sample consumption less, the advantage of strong, the low instrument price of favorable reproducibility and atomic absorption antijamming capability, low operation cost; Overcome the shortcoming that atomic absorption/atomic fluorescence spectrometer device only carries out the total quantitative determination of element simultaneously.Coupling technique provided by the invention can provide the information of abundant element, for morphological analysis provides a strong analysis tool.This interface is applicable to the analysis of steam generation element (arsenic, mercury, antimony, selenium) etc.
Claims (10)
1. high performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface is characterized in that: it contains the fine inner diameter threeway (2) that connects successively, thin quartz ampoule (4), four-way (6), reaction tube (9), large diameter threeway (12); First arm of described fine inner diameter threeway (2) connects high performance liquid chromatography effluent inlet (1), second arm connects oxidizing agent solution transfer tube (3), the 3rd arm connects an end of described thin quartz ampoule (4), and described thin quartz ampoule (4) is close to a ultraviolet lamp tube (5); The other end of described thin quartz ampoule (4) connects first arm of described four-way, second arm of described four-way (6) connects acid solution transfer tube (7), its the 3rd arm connects reductant solution transfer tube (8), its the 4th arm connects an end of described reaction tube (9), the other end of described reaction tube (9) connects first arm of large diameter threeway (12), second arm of described large diameter threeway (12) connects carrier gas transfer tube (10), and its 3rd arm connects the delivery tube (11) of leading to gas-liquid separator.
2. high performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface as claimed in claim 1 is characterized in that, described thin quartz ampoule (4) also connects another thin quartz ampoule (4) by connecting pipe, and these two thin quartz ampoules are adjacent on ultraviolet lamp tube.
3. high performance liquid chromatography one hydride atomic absorption/fluorescence spectrum instruments interface as claimed in claim 1 is characterized in that the internal diameter of described fine inner diameter threeway (2) is 0.5～1.2mm.
4. high performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface as claimed in claim 1 is characterized in that, the internal diameter of described four-way (6) is 1～2mm.
5. high performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface as claimed in claim 1 is characterized in that, the internal diameter of described large diameter threeway (12) is 1.5～2.5mm.
6. high performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface as claimed in claim 1 is characterized in that, the internal diameter of described reaction tube (9) is 0.5-2mm, and length is 30～60cm.
7. high performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface as claimed in claim 1 or 2 is characterized in that, the internal diameter of described thin quartz ampoule (4) is 0.5～2mm, and length is 10～40cm.
8. high performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface as claimed in claim 1 or 2 is characterized in that, the power of described uviol lamp is 5-15W.
9. the described high performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface of claim 1 is characterized in that, the flow that pumps into of oxidizing agent solution is 0.5-2ml/min in the described oxygenant transfer tube (3); The flow that pumps into of acid solution is 0.5-2.5ml/min in the acid solution transfer tube (7); The flow that pumps into of reductant solution is 0.5-2.5ml/min in the reductant solution transfer tube (8).
10. ask 1 described high performance liquid chromatography-hydride atomic absorption/fluorescence spectrum instruments interface as right, it is characterized in that, described oxygenant is K
2S
2O
3Solution, described acid solution are to connect hydrochloric acid solution, and described reductive agent is KBH
4Or NaBH
4Solution.
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| CN101358924B (en) * | 2007-08-03 | 2011-05-04 | 北京路捷仪器有限公司 | Morphological analysis apparatus for mercury element and analysis method thereof |
| CN101261258B (en) * | 2008-01-04 | 2011-05-18 | 中国水产科学研究院黄海水产研究所 | Aquatic product inorganic arsenic determination method |
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