CN205263037U - Element form on -line measuring device - Google Patents

Element form on -line measuring device Download PDF

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Publication number
CN205263037U
CN205263037U CN201521101454.4U CN201521101454U CN205263037U CN 205263037 U CN205263037 U CN 205263037U CN 201521101454 U CN201521101454 U CN 201521101454U CN 205263037 U CN205263037 U CN 205263037U
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China
Prior art keywords
unit
measuring device
line measuring
enrichment
sample
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CN201521101454.4U
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Chinese (zh)
Inventor
张卫宏
秦德元
郑逢喜
叶建平
裴晓华
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BEIJING JITIAN INSTRUMENT Co Ltd
Beijing Titan Instruments Co Ltd
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BEIJING JITIAN INSTRUMENT Co Ltd
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Abstract

The utility model relates to an element form on -line measuring device, including detecting element, element form on -line measuring device further includes: the enrichment unit, the enrichment unit is used for need checking sample's enrichment, advance a kind unit, through the switching of advancing kind unit makes the enrichment unit selectively communicates sample unit or separating element, the sample unit, the sample unit includes reservoir, switches over parts and first transfer unit, the separating element, need checking sample after the separating element is used for the elution and separates the enrichment. The utility model has the advantages of simple structure, the enrichment is efficient, and detectivity is high, collects enrichment, analysis in an organic whole.

Description

Element morphology on-line measuring device
Technical field
The utility model relates to element detection field, the element morphology on-line measuring device of the particularly automatic enrichment of a kind of trace heavy metals, sample introduction.
Background technology
Heavy metal pollution refers to the environmental pollution being caused by heavy metal or its compound, its extent of injury depends on concentration and the chemical form of metallic element, different heavy metal pollution has directly endangered health, as the minamata disease that mercury pollution causes, contains arsenic poison can etc. At present, generally use atomic fluorescence method to carry out heavy metal element determination, but can only measure total amount. But most of heavy metal elements have variform, and different shape toxicity difference is larger, for example, concerning mercury, methyl mercury toxicity maximum, the limit value of GB3838-2002 " water environment quality standard " regulation is 1ppt, and the limit value of inorganic mercury is approximately 1000 times of methyl mercury, the heavy metal element of different shape can only detect in conjunction with atomic fluorescence or other atom spectrum by morphological analysis instrument. But for the morphological analysis of some trace heavy metals, the form of some low concentrations cannot detect at all, therefore need to carry out enrichment processing to trace heavy metals.
At present, the enrichment of trace heavy metals is carried out off-line enrichment by SPE manually or automatically conventionally, eluent after enrichment is only got wherein seldom part and is measured, eluent belongs to waste greatly, and institute's sample thief volume is more, as GB/T17132-1997 " the mensuration gas chromatography of environment methyl mercury " the about 1000mL of required sample volume, both reduced analysis efficiency, again for sampling work has brought inconvenience, in agent transfer process, easily cause loss, cause the rate of recovery to reduce simultaneously.
Utility model content
In order to solve the deficiency in above-mentioned prior art scheme, it is a kind of simple in structure that the utility model provides, and bioaccumulation efficiency is high, and detection sensitivity is high, the element morphology on-line measuring device of integrate enrichment, analyzing.
The purpose of this utility model is achieved through the following technical solutions:
A kind of element morphology on-line measuring device, comprises detecting unit, and described element morphology on-line measuring device further comprises:
Enrichment unit, described enrichment unit is for the enrichment of testing sample;
Sample injection unit, by the switching of described sample injection unit, makes described enrichment unit selectively be communicated with sample unit or separative element;
Sample unit, described sample unit comprises reservoir vessel, switching part and the first transfer unit, for the material and the testing sample that provide the pretreatment of described enrichment unit to need;
Separative element, described separative element is used for the testing sample after wash-out separation and concentration.
According to above-mentioned element morphology on-line measuring device, alternatively, described enrichment unit is enriching column.
According to above-mentioned element morphology on-line measuring device, preferably, described enrichment unit is universal enriching column.
According to above-mentioned element morphology on-line measuring device, alternatively, described switching part is transfer valve, and described transfer valve comprises at least two imports and an outlet.
According to above-mentioned element morphology on-line measuring device, preferably, described the first transfer unit is liquid phase pump.
According to above-mentioned element morphology on-line measuring device, alternatively, described sample injection unit is multiposition valve.
According to above-mentioned element morphology on-line measuring device, preferably, described sample injection unit is six valves.
According to above-mentioned element morphology on-line measuring device, preferably, described separative element comprises the second transfer unit and chromatographic column.
According to above-mentioned element morphology on-line measuring device, preferably, on described the second transfer unit, be provided with gradient elution program.
According to above-mentioned element morphology on-line measuring device, preferably, described chromatographic column is integral post.
According to above-mentioned element morphology on-line measuring device, alternatively, described detecting unit is atomic fluorescence detector.
Compared with prior art, the beneficial effect the utlity model has is:
1, the utility model collection enriching column pretreatment, example enrichment, separate, be detected on one, whole-process automatic control, realizes real unmanned, detection efficiency is high, concentration effect good, and has avoided the sample loss occurring in offline inspection and the operate miss that may occur.
2, the whole sample detection of testing sample after the utility model enrichment, greatly reduce the sampling amount of testing sample, have improved detection sensitivity.
3, the utility model adopts multiposition valve to realize sample feeding, and described multiposition valve leaves interface simultaneously, can directly be connected with separation, detecting unit, convenient and swift.
4, the solid-phase extraction column that the enriching column volume ratio off-line enrichment that the utility model adopts is used is little a lot, and post inner stuffing plasmid footpath is little, density is high, thereby elute effect is good.
5, the utility model adopts universal enriching column to carry out example enrichment, and integral post is carried out eluent separation, makes package unit can realize on-line preconcentration and the detection of multiple element, without changing pillar.
Brief description of the drawings
With reference to accompanying drawing, disclosure of the present utility model will be easier to understand. Those skilled in the art hold intelligible: these accompanying drawings are only for illustrating the technical solution of the utility model, and are not intended to protection domain of the present utility model to be construed as limiting. In figure:
Fig. 1 is the structural representation of the element morphology on-line measuring device of embodiment 1;
Fig. 2 is the structure diagram of the element morphology on-line measuring device of embodiment 2.
Detailed description of the invention
Fig. 1-2 and following declarative description optional embodiment of the present utility model how to implement and to reproduce the utility model with instruction those skilled in the art. In order to instruct technical solutions of the utility model, simplify or omitted some conventional aspects. Those skilled in the art should understand that be derived from these embodiments modification or replace will be in scope of the present utility model. Those skilled in the art should understand that following characteristics can combine to form multiple modification of the present utility model in every way. Thus, the utility model is not limited to following embodiment, and is only limited by claim and their equivalent.
Embodiment 1
Fig. 1 has schematically provided the structure diagram of the element morphology on-line measuring device of the present embodiment, and as shown in Figure 1, described element morphology on-line measuring device comprises:
Enrichment unit, described enrichment unit is enriching column, for the enrichment of testing sample;
Sample injection unit, by the switching of described sample injection unit, makes described enrichment unit selectively be communicated with sample unit or separative element;
Sample unit, described sample unit comprises reservoir vessel, switching part and the first transfer unit, for the material and the testing sample that provide the pretreatment of described enrichment unit to need;
Separative element, described separative element is used for the testing sample after wash-out separation and concentration;
Detecting unit, described detecting unit is communicated with described separative element.
In order to improve the elute effect of enriching column, widen the scope of application of described element morphology on-line measuring device, therefore:
Further, described enriching column is universal enriching column, and the solid-phase extraction column that the enrichment of described universal enriching column volume ratio off-line is used is little a lot, and post inner stuffing plasmid footpath is little, density is high, thereby has enrichment well and elute effect.
Before testing sample enrichment, enrichment unit need carry out pretreatment, needs therefore sample unit must provide the various reagent used in preprocessing process, therefore:
Further, described switching part is transfer valve, and described transfer valve comprises at least two imports and an outlet, by the switching of transfer valve, provides enriching column pretreating reagent or testing sample to enrichment unit.
In the universal enriching column that the present embodiment adopts, particle diameter is little, density is large, directly makes enriching column internal pressure higher, therefore:
Further, described the first transfer unit is liquid phase pump.
For simplification device structure, optimal design stream, therefore:
Further, described sample injection unit is multiposition valve.
As preferably, described sample injection unit is six valves.
For to the separation that realizes testing sample after enrichment, therefore:
Further, described separative element comprises the second transfer unit and chromatographic column, and mobile phase is wash-out enriching column under the pumping of described the second transfer unit, and eluent enters chromatographic column and separates.
Embodiment 2
Application examples in detecting according to the element morphology on-line measuring device of embodiment 1 mercury element form in water sample. Fig. 2 has schematically provided the structure diagram of the element morphology on-line measuring device of the present embodiment, and as shown in Figure 2, in this application examples, element morphology on-line measuring device specifically comprises:
Reservoir vessel, described reservoir vessel comprises container 11, container 12, container 13 and container 14;
Switching part, described switching part is low pressure transfer valve 2, described low pressure transfer valve 2 comprises four imports and an outlet;
The first transfer unit, described the first transfer unit is liquid phase pump 3;
Enrichment unit, described enrichment unit is universal enriching column 4;
Sample injection unit, described sample injection unit is six valves 5, comprises sample inlet a, sample export b, waste liquid entrance e, waste liquid outlet f, mobile phase entrance c and mobile phase outlet d;
Separative element, described separative element comprises the second transfer unit and chromatographic column, and described the second transfer unit is low pressure liquid phase pump 61, and chromatographic column is integral post 62; Using integral post as splitter, it is large that post inner pore becomes, pressure significantly reduces, can be by current gradient being set on low pressure liquid phase pump 61, enriching column is carried out to gradient elution, can be by more different shapes of more element and element of the same race, the strong reservation form of element separates better even, and analysis time is short, peak shape and detection limit all have clear improvement;
Detecting unit, described detecting unit is atomic fluorescence detector 7, and the mercury element form after separating is detected.
The workflow of the element morphology on-line measuring device of the present embodiment is as follows:
S1. six valves 5 are adjusted to connection status as described in Figure 2, start liquid phase pump 3, by the switching of low pressure transfer valve 2, successively the water of the methanol solution of container 11 interior storages and container 12 interior storages is pumped into universal enriching column 4 and carry out post activation, the sodium diethyldithiocarbamate of container 13 interior storages is pumped into and in enriching column, carries out post modification; Efflux after enriching column is discharged through waste liquid entrance e, the waste liquid outlet f of six valves 5;
S2. regulate low pressure transfer valve 2, the water sample to be measured in container 14 is pumped into enrichment on-line enrichment;
S3. the connection status that changes six valves 5 (is adjusted to the b mouth connection c mouth of six valves, d mouth connects e mouth, f mouth connects the state of a mouth), make universal enriching column 4 be communicated with separative element, mobile phase is wash-out enriching column under the effect of described low pressure liquid phase pump 61, eluent enters integral post 62 and separates, and enters afterwards atomic fluorescence detector 7 and carries out the detection of mercury element form.
Above-mentioned embodiment should not be construed as the restriction to the utility model protection domain. Key of the present utility model is: realize the automatic on-line detection that collects enriching column pretreatment, example enrichment, separates, is detected on the speciation of heavy metal element of one. In the situation that not departing from the utility model spirit, within any type of change that utility model is made all should fall into protection domain of the present utility model.

Claims (10)

1. an element morphology on-line measuring device, comprises detecting unit, it is characterized in that: described element shapeState on-line measuring device further comprises:
Enrichment unit, described enrichment unit is for the enrichment of testing sample;
Sample injection unit, by the switching of described sample injection unit, makes described enrichment unit selectively be communicated with sampleUnit or separative element;
Sample unit, described sample unit comprises reservoir vessel, switching part and the first transfer unit;
Separative element, described separative element is used for the testing sample after wash-out separation and concentration.
2. element morphology on-line measuring device according to claim 1, is characterized in that: described enrichmentUnit is enriching column.
3. element morphology on-line measuring device according to claim 1, is characterized in that: described switchingParts are transfer valve, and described transfer valve comprises at least two imports and an outlet.
4. element morphology on-line measuring device according to claim 1, is characterized in that: described firstTransfer unit is liquid phase pump.
5. element morphology on-line measuring device according to claim 1, is characterized in that: described sample introductionUnit is multiposition valve.
6. element morphology on-line measuring device according to claim 5, is characterized in that: described sample introductionUnit is six valves.
7. element morphology on-line measuring device according to claim 1, is characterized in that: described separationUnit comprises the second transfer unit and chromatographic column.
8. element morphology on-line measuring device according to claim 7, is characterized in that: described secondOn transfer unit, be provided with gradient elution program.
9. element morphology on-line measuring device according to claim 7, is characterized in that: described chromatogramPost is integral post.
10. element morphology on-line measuring device according to claim 1, is characterized in that: described inspectionMeasurement unit is atomic fluorescence detector.
CN201521101454.4U 2015-12-25 2015-12-25 Element form on -line measuring device Active CN205263037U (en)

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Application Number Priority Date Filing Date Title
CN201521101454.4U CN205263037U (en) 2015-12-25 2015-12-25 Element form on -line measuring device

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CN205263037U true CN205263037U (en) 2016-05-25

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108871915A (en) * 2018-04-26 2018-11-23 南京新循环保科技有限公司 Heavy metal ion device for fast detecting
CN111380977A (en) * 2020-03-16 2020-07-07 东华理工大学 Sequential ionization analysis method for rare earth samples

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108871915A (en) * 2018-04-26 2018-11-23 南京新循环保科技有限公司 Heavy metal ion device for fast detecting
CN111380977A (en) * 2020-03-16 2020-07-07 东华理工大学 Sequential ionization analysis method for rare earth samples

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