CN206020441U - The measurement apparatus measured using standard addition method - Google Patents
The measurement apparatus measured using standard addition method Download PDFInfo
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- CN206020441U CN206020441U CN201620818228.6U CN201620818228U CN206020441U CN 206020441 U CN206020441 U CN 206020441U CN 201620818228 U CN201620818228 U CN 201620818228U CN 206020441 U CN206020441 U CN 206020441U
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Abstract
The measurement apparatus that utilization standard addition method of the present utility model is measured, including:Container, sampling pump;Mixed block, is connected by pipeline with sampling pump;Detector, is connected by pipeline with mixed block, and the first valve, the second valve, the 3rd valve are respectively used to the standard solution in control addition container, diluent, the amount of testing sample.The technical solution of the utility model enormously simplify the test process of standard addition method, shorten detection time, reduce reagent consumption, can apply to the conventional sense of batch samples.
Description
Technical field
This utility model is related to analytical chemistry field, the measurement that more particularly to a kind of utilization standard addition method is measured
Device.
Background technology
In modern chemical analysis, especially in atomic spectroscopic analysis, commonly used is standard curve method.Standard is bent
Suitable for the matrix of the standard sample situation roughly the same with the matrix of sample, advantage is that speed is fast to collimation method, has the disadvantage to work as sample
Matrix is difficult to obtain accurate result when complicated, because determining the content of unknown sample with standard curve method, calibration trace
Quality will directly affect the accuracy of unknown sample measurement result;An and good calibration trace will be prepared, with the proviso that mark
Quasi- series has to accurately be mated with the matrix of unknown sample, and precision of analysis depends directly on standard sample
Similarity with unknown sample physicochemical properties.However, in actual measurement process, the matrix of unknown sample, composition and dense
Degree is ever-changing, find completely extremely difficult with the unknown sample standard substance that matches of composition, especially to those complicated bases
Body sample.In addition, standard curve method also requires that unknown sample and standard sample are measured under " similarity condition ", but in actual survey
In amount, particularly in the test process of batch samples, with test carrying out, the drift of light source, peristaltic pump pump line tired
The many factors such as labor, the change of ambient temperature are actual all in change, it is difficult to accomplish real " similarity condition ".Therefore bent in standard
Due to the impact of these factors above-mentioned under collimation method, the increase of evaluated error is result in.
And Standard entertion rule can carry out Matrix Match automatically, the physics and chemical interference of sample matrices are compensated;While by
In unknown sample and standard sample be " while " detection, that is, unknown sample and standard sample is truly realized at " under similarity condition "
Detect, therefore impact very little of the change of above-mentioned many factors to measurement result, so as to improve the accuracy of measurement result.
Traditional standard addition method needs a series of difference of (generally 5 parts) additions equivalent analyte sample fluids of human configuration
The standard solution of concentration, then tests this serial solution respectively one by one, with concentration as abscissa, corresponding intensity (or extinction
Degree) standard curve is drawn out for vertical coordinate, the content of component to be measured is finally extrapolated from the cross point of standard curve and abscissa.
Now by taking the atomic fluorescence test in atomic spectrum as an example, the operation for sketching standard addition method is as follows:Divide and take 4~5 parts
Volume identical tested sample solution, be separately added into from second part same concentration, the tested component of different volumes standard molten
Liquid, is then diluted to same volume with blank solution, measures the fluorescence intensity of each test solution under identical experiment condition successively,
Fluorescence intensity is drawn out to adding the calibration trace (see Fig. 2) of concentration, correction extra curvature is prolonged and is intersected with abscissa, origin best friend
The distance (corresponding concentration when i.e. fluorescence intensity is 0) of point, content Cx of tested element as in tested sample.
Can be seen that from above-mentioned test process and a unknown sample is tested with standard addition method, will first configure 4 to 5 and add
Enter the standard solution of a certain amount of unknown sample, then another one is detected these samples, finally again by drafting curve meter
The content of the unknown sample is calculated, therefore whole process is very loaded down with trivial details time-consuming.Compared with standard curve method, the sample of complexity should not be said
Product are configured, and light sample detection is accomplished by spending more 4 to 5 times of time, and detection speed is very slow, and required reagent dosage is also very big.Cause
This, although standard addition method compared with standard curve method with lot of advantages, in the detection of actual batch samples, typically adopt
Standard addition method is seldom adopted with standard curve method.Standard addition method is general only few in sample size and matrix is more complicated
In the case of just use.
Utility model content
The technical problems to be solved in the utility model is to provide that a kind of efficiency is higher, reagent consume significantly reduced using mark
The measurement apparatus that quasi- addition is measured.
The measurement apparatus that utilization standard addition method of the present utility model is measured, including:
For accommodating the container of solution to be checked, the import of the container is defeated with the first of standard solution by the first valve respectively
Enter pipe connection, connected with the second input pipe of diluent by the second valve, by the 3rd valve and the 3rd input pipe of testing sample
Connection;
Sampling pump, is connected by pipeline with the container;
Mixed block, is connected by pipeline with the sampling pump, and the sampling pump is used for entering the liquid pump in the container
Mixed block, and mix in mixed block;
For detecting the detector of solution in mixed block, it is connected by pipeline with the mixed block,
First valve, the second valve, the 3rd valve be respectively used to control to add standard solution in the container, diluent,
The amount of testing sample.
The measurement apparatus that utilization standard addition method of the present utility model is measured, wherein, also include controller, the control
Device processed is connected with first valve, the second valve, the 3rd valve respectively, and the controller is used for controlling the first valve, the second valve, the 3rd valve
Opening time, control to add the amount of standard solution in the container, diluent, testing sample with this.
The measurement apparatus that utilization standard addition method of the present utility model is measured, wherein, first valve, the second valve,
3rd valve is electromagnetic valve or dilution proportion valve.
The measurement apparatus that utilization standard addition method of the present utility model is measured, wherein, the sampling pump is peristaltic pump
Or syringe pump or plunger displacement pump or liquid chromatography pump.
The measurement apparatus that utilization standard addition method of the present utility model is measured, wherein, the mixed block is capillary tube
Or mixing reactor.
The measurement apparatus that utilization standard addition method of the present utility model is measured, wherein, the detector is atom light
Spectrometer, molecular spectrum instrument or ion-selective electrode.
The technical solution of the utility model eliminates traditional standard addition method needs variable concentrations of the human configuration containing sample
Series standard solution and detect the loaded down with trivial details time consuming process of the series standard solution one by one, it is only necessary to single-point standard solution, detection
Once (less than 1 minute) can be automatically performed the detection of whole standard addition method, enormously simplify the test of standard addition method
Journey, shortens detection time, reduces reagent consumption, makes this method have the conventional sense that can apply to batch samples.
Description of the drawings
Fig. 1 is the structural representation of the measurement apparatus that utilization standard addition method of the present utility model is measured;
Fig. 2 is the calibration trace for carrying out atomic fluorescence test using standard addition method;
Fig. 3 is being embodied as the workflow of the measurement apparatus that utilization standard addition method of the present utility model is measured
Injection valve control pulse sequence figure in example;
Fig. 4 is being embodied as the workflow of the measurement apparatus that utilization standard addition method of the present utility model is measured
The signal and calibration trace schematic diagram of example.
Specific embodiment
As shown in figure 1, the measurement apparatus that utilization standard addition method of the present utility model is measured, including:
For accommodating the container 1 of solution to be checked, the import of container 1 is defeated with the first of standard solution by the first valve 11 respectively
Enter pipe 21 to connect, connected with the second input pipe 22 of diluent by the second valve 12, by the of the 3rd valve 13 and testing sample
Three input pipes 23 are connected;
Sampling pump 2, is connected by pipeline with container 1;
Mixed block 3, is connected by pipeline with sampling pump 2, and sampling pump is used for for the liquid pump in container entering mixed block, and
Mix in mixed block;
For detecting the detector 4 of solution in mixed block, it is connected by pipeline with mixed block 3,
First valve 11, the second valve 12, the 3rd valve 13 are respectively used to control to add standard solution in container 1, diluent, treat
The amount of test sample product.
Full-automatic online fast standard addition method of the present utility model and device, wherein, also include controller 5, controller 5
It is connected with the first valve 11, the second valve 12, the 3rd valve 13 respectively, controller 5 is used for controlling the first valve 11, the second valve 12, the 3rd valve
13 opening time, with this control add container 1 in standard solution, diluent, testing sample amount.
Full-automatic online fast standard addition method of the present utility model and device, wherein, the first valve 11, the second valve 12, the
Three valves 13 are electromagnetic valve or dilution proportion valve.First valve 11, the second valve 12, the 3rd valve 13 are referred to as injection valve.
Full-automatic online fast standard addition method of the present utility model and device, wherein, sampling pump 2 is peristaltic pump or injection
Pump or plunger displacement pump or liquid chromatography pump.
Full-automatic online fast standard addition method of the present utility model and device, wherein, mixed block 3 is capillary tube or mixing
Reactor.
Full-automatic online fast standard addition method of the present utility model and device, wherein, detector 4 be atomic spectrograph,
Molecular spectrum instrument or ion-selective electrode.
Full-automatic online fast standard addition method of the present utility model and device, wherein, controller 5 can be computer or
PLC, you can programmed logic controller.
The workflow of the measurement apparatus that utilization standard addition method of the present utility model is measured is embodied as example
Under:
The mouth of pipe of the first input pipe is placed in standard solution, the mouth of pipe of the second input pipe is placed in diluent,
The mouth of pipe of the 3rd input pipe is placed in testing sample;
Sampling pump is adjusted, the aggregate sample flow rate kept constant for exporting sampling pump;
Using the standard solution in the first valve, the second valve, the 3rd valve control addition container, diluent, testing sample
Amount, make to respectively obtain multiple variable concentrations in the container but solution of the volume identical containing equivalent testing sample;
By multiple variable concentrations but volume identical containing the solution of equivalent testing sample, pump enters mixed block respectively;
It is utilized respectively detector and detects multiple variable concentrations but solution of the volume identical containing equivalent testing sample, paints
System is with concentration as abscissa, standard curve of the Testing index as vertical coordinate, extrapolates from cross point of the standard curve with abscissa
The content of testing sample.
Specifically, by controlling the length of the first valve, the second valve, the 3rd valve opening time controlling the mixed of three kinds of reagents
Composition and division in a proportion example.Its control mode adopts Pulse Width Control, pulse sequence to see Fig. 3.
Wherein:TA is the first valve opening time, and TB is the second valve opening time, and TC is the 3rd valve opening time, and T is three
The startup cycle of valve, the length in cycle embody the uniformity of sample mixing.On the premise of each valve minimum starting time is ensured, T gets over
The uniformity of little sample mixing is better.
TA+TB+TC=T,
TA:TB:The amount of TC=standard solution:The amount of diluent:The amount of testing sample.
The workflow of the measurement apparatus that utilization standard addition method of the present utility model is measured is embodied as example
Under:First input pipe 21 (sample introduction capillary tube) of the first valve is placed in standard solution always, the second of the second valve is input into
Pipe 22 (sample introduction capillary tube) is placed in blank solution (diluent) always, by 23 (the sample introduction capillary of the 3rd input pipe of the 3rd valve
Pipe) it is placed in unknown sample to be measured.In the case of the output aggregate sample flow rate kept constant of sampling pump 2, the opening of three valves
Time is than being the mixed proportion of three kinds of reagents.
Assume the first valve, the second valve, the 3rd three valves of valve opening time ratio as shown in the table:
Under the parameter of upper table, it is assumed that the solution concentration of the first input pipe 21 (sample introduction capillary tube) is 100 μ g/L, then corresponding
TA accounts for the mixed liquid concentration that sample injection time ratio (%) is 0,5,10,20,40 and is respectively 0,5 μ g/L, 10 μ g/L, 20 μ g/L, 40 μ
g/L.The continuous signal and calibration trace schematic diagram that measure are shown in a and b of Fig. 4 respectively.The concentration of unknown sample to be measured is 2CX.
In sum as can be seen that the technical solution of the utility model eliminates traditional standard addition method needs human configuration
The series standard solution for containing the variable concentrations of sample and the loaded down with trivial details time consuming process for detecting the series standard solution one by one, it is only necessary to single
Put standard solution, detect that once (less than 1 minute) can be automatically performed the detection of whole standard addition method, enormously simplify standard
The test process of addition method, shortens detection time, reduces reagent consumption, makes this method can apply to high-volume sample
The conventional sense of product.
The technical solution of the utility model can contain the series standard solution of the variable concentrations of sample with rapid configuration, can be with side
Configuration frontier inspection is surveyed, so as to greatly reduce the detection time and reagent consumption of sample.
The above is only preferred implementation of the present utility model, it is noted that for the ordinary skill people of the art
For member, on the premise of without departing from this utility model principle, some improvements and modifications can also be made, these improvements and modifications
Also of the present utility model protection domain should be regarded as.
Claims (6)
1. the measurement apparatus that a kind of utilization standard addition method is measured, it is characterised in that include:
For accommodating the container of solution to be checked, the import of the container is respectively by the first valve and the first input pipe of standard solution
Connection, is connected with the second input pipe of diluent by the second valve, is connected with the 3rd input pipe of testing sample by the 3rd valve;
Sampling pump, is connected by pipeline with the container;
Mixed block, is connected by pipeline with the sampling pump, and the sampling pump is used for for the liquid pump in the container entering mixing
Block, and mix in mixed block;
For detecting the detector of solution in mixed block, it is connected by pipeline with the mixed block,
First valve, the second valve, the 3rd valve are respectively used to control to add standard solution in the container, diluent, to be measured
The amount of sample.
2. the measurement apparatus that utilization standard addition method as claimed in claim 1 is measured, it is characterised in that also include controlling
Device, the controller are connected with first valve, the second valve, the 3rd valve respectively, the controller be used for control the first valve, second
Valve, the opening time of the 3rd valve, control to add the amount of standard solution in the container, diluent, testing sample with this.
3. the measurement apparatus that utilization standard addition method as claimed in claim 2 is measured, it is characterised in that described first
Valve, the second valve, the 3rd valve are electromagnetic valve or dilution proportion valve.
4. the measurement apparatus that utilization standard addition method as claimed in claim 2 is measured, it is characterised in that the sampling pump
For peristaltic pump or syringe pump or plunger displacement pump or liquid chromatography pump.
5. the measurement apparatus that utilization standard addition method as claimed in claim 2 is measured, it is characterised in that the mixed block
For capillary tube or mixing reactor.
6. the measurement apparatus that utilization standard addition method as claimed in claim 2 is measured, it is characterised in that the detector
For atomic spectrograph, molecular spectrum instrument or ion-selective electrode.
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CN106018863A (en) * | 2016-07-29 | 2016-10-12 | 北京宝德仪器有限公司 | Measuring device and process for measuring by virtue of standard addition method |
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CN106018863A (en) * | 2016-07-29 | 2016-10-12 | 北京宝德仪器有限公司 | Measuring device and process for measuring by virtue of standard addition method |
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