CN104833711B - A kind of blood lead analyzer and its measurement blood lead method - Google Patents
A kind of blood lead analyzer and its measurement blood lead method Download PDFInfo
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- CN104833711B CN104833711B CN201510102387.6A CN201510102387A CN104833711B CN 104833711 B CN104833711 B CN 104833711B CN 201510102387 A CN201510102387 A CN 201510102387A CN 104833711 B CN104833711 B CN 104833711B
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Abstract
The invention discloses a kind of blood lead analyzer and its measurement blood lead methods, including cabinet, lifting electrolyser construction is provided in the cabinet, three electrode assemblies, circuit control component and data processor, circuit control component include water conservancy diversion dissolution control unit, water conservancy diversion dissolve out control unit control water conservancy diversion dissolution when, with to electrode it is in parallel with reference electrode after potentiometric stripping is generated between working electrode;For handling the data processor of test data, blood lead content is evaluated on the basis of cadmium internal standard compound.Present invention measurement is accurate, easy to operate, and the combination three-electrode module design of program-controlled mobile electrolytic cell is advantageously implemented the standardization and mass production of blood lead analyzer manufacture.
Description
Technical field
The present invention relates to a kind of blood lead analyzer of potentiometric stripping type and its measurement blood lead methods.
Background technique
Lead is toxic heavy metal, industrially widely used, especially the fast development of the Storage Battery Industry in China in recent years, so that
The probability that operating worker absorbs lead greatly increases.In process of production, lead and its compound are mainly with dust, smog or steam
Form enter human body through respiratory tract, cause the dysfunction of nearly all tract, especially blood and nervous system, make
At lead poisoning.
Blood lead concentration is the sensitive indicator for reflecting recent exposure, and blood lead analysis method is numerous, common are Atomic absorption
Spectroscopic methodology, isotope dilution mass spectrometry, atomic fluorescence spectrum, Atomic Emission Spectral Analysis and On Potentiometric Stripping Analysis.
For atomic absorption spectrography (AAS) since the atom rate of element is very low, the detection model of detection human body lead element is not achieved in its sensitivity
It encloses, false negative result often occurs, therefore eliminated.Isotope dilution mass spectrometry be blood lead analysis be it is most classical, most accurately, most reliably
Method.But it is time-consuming due to its measuring method complexity, and instrument price is expensive, this method has no value for clinical application.Atom is glimmering
Light spectrophotometry is a kind of atom vapor by measuring element to be measured, launches atom under the radiation excitation of certain wavelength
Fluorescence measures a kind of instrument analytical method of constituent content to be measured according to the intensity of fluorescent emission.This method high sensitivity, inspection
The lower limit 1-2 order of magnitude lower than atomic absorption method out, in analysis curve linear relationship, disturbing effect and multielement analysis ability
On be superior to atomic absorption method, but it is more serious by stray light effects, affects the universal and development of the method to a certain extent.
Atomic Emission Spectral Analysis is the spectrum generated after being stimulated according to the gaseous atom or ion of component and the analysis established
Method.But it is poor to high-content elemental analysis accuracy, a set of standard sample control is needed, practical operation is inconvenient, instrument valence
Costly, popularization and use are restricted lattice.On Potentiometric Stripping Analysis is a kind of emerging electrochemical analysis method, this method tool
There is high sensitivity, also there is very strong anti-interference ability, can effectively prevent the interference of organic impurities etc. in solution, so that
It when measuring the microelements such as lead in sample, can be measured without digestion, easy operation sequence.
Well known potentiometric stripping type blood lead analyzer measures blood lead concentration, is surveyed in dissolution time using three-electrode system
Determine the potentiometric stripping between working electrode and reference electrode, obtain current potential-dissolution time curve, peak is read using the direct method of measurement
High level causes the relative standard deviation RSD of measurement result big, and RSD value usually can all be greater than 10%, seriously affects analysis result
Accuracy.Deviation brought by RSD value is reduced, just has to improve relevant parameter and method, and it is related such
The related report of technology is not yet found so far.In addition the three-electrode system of common blood lead analyzer independently designs,
It is unfavorable for realizing the standardized production of blood lead analyzer.
Summary of the invention
In order to solve the problems in the prior art, the object of the present invention is to provide a kind of blood lead analyzer and its measurement blood leads
Method, effectively improve blood lead measurement accuracy, blood lead analyzer of the invention is with the combination three of program-controlled mobile electrolytic cell
Electrode mould group, it is easy to operate, it is more advantageous to the standardization and mass production for realizing the manufacture of blood lead analyzer.
To achieve the above object, the invention adopts the following technical scheme: a kind of blood lead analyzer, including cabinet, it is described
Lifting electrolyser construction, three electrode assemblies, circuit control component and data processor, three electrodes are provided in cabinet
Component includes to electrode, reference electrode and working electrode, which is characterized in that the circuit control component includes water conservancy diversion dissolution control
Component processed, the mode of the water conservancy diversion dissolution control unit control water conservancy diversion dissolution, the water conservancy diversion dissolution mode is pair
Potentiometric stripping is generated between working electrode after electrode is in parallel with reference electrode;The data processor is surveyed for handling
Try data.
Wherein, the lifting electrolyser construction includes pop-up, undercarriage column, undercarriage, undercarriage gasket and electric pushrod, institute
The pop-up stated is fixedly connected on enclosure top, and the undercarriage column is fixed on chassis backplane, is arranged on the undercarriage column
There is undercarriage gasket, the undercarriage gasket corresponding position is provided with undercarriage, and described electric pushrod one end is connected to pop-up, another
End is connect across undercarriage and undercarriage gasket with lifter plate, and the lifter plate is fixedly connected by lifting fixing axle with sliding curtain, institute
The lifter plate stated is also connected with lifting shaft, electrolytic cell seat is provided on the lifting shaft, the electrolytic cell, which is taken, to be placed with
Electrolytic cell.
Wherein, the electrolytic cell, which is sat, is fixedly connected by electrolytic cell seat bolt with lifting shaft, and the electrolytic cell is sat straight
Diameter is adjustable.
Preferably, the electric pushrod is H-type 50mm electric pushrod.
Preferably, three electrode assemblies further include sitting to electrode, described to be fixed on to electrode and reference electrode
Electrode is taken, the three electrode assembly test leads enter electrolytic cell, make three-dimensional direction moving relative to electrolytic cell.
Preferably, described is Pt piece to electrode.
Preferably, the reference electrode is 232 saturated calomel electrodes.
Preferably, the working electrode is glass-carbon electrode, and the glass-carbon electrode outer tube uses Peek material.
Preferably, the circuit control component further includes lifting electrolytic cell control unit, controls electrolytic cell movement side
To.
Preferably, the cabinet is additionally provided with dust-proof upper layer shutter.
A method of measurement blood lead, which comprises the following steps:
Step 1 is added blood lead reagent into blood sample to be measured and cadmium ion internal standard compound prepares solution to be measured, by solution to be measured
It is placed in electrolytic cell;
Step 2 carries out enrichment procedure to the solution in electrolytic cell using blood lead analyzer, after being enriched with a period of time, disconnects
Power supply is dissolved out, potentiometric stripping will be generated between working electrode after in parallel with reference electrode to electrode in blood lead analyzer;
Step 3, the discrete signal of current potential and dissolution time point in obtaining step two;
Step 4 carries out 2 subdifferentials to discrete signal point in step 3 and Gauss normal distribution calculates, is sequentially connected these
Discrete signal point obtains full curve, calculates the peak height and corresponding spike potential of whole components in full curve;
Step 5 calculates correction coefficient K according to the cadmium ion internal standard compound peak height in step 4, wherein in the cadmium ion of K=10/
Mark object peak height;
The product of discrete signal point and K in step 4 is formed one group of new discrete signal point by step 6, and connection is all
Discrete signal point obtain a new full curve, calculate the peak height of whole components and corresponding peak electricity in full curve
Position obtains opposite peak height;
Step 7 is calculated with the opposite peak height in step 6, obtains blood lead content in solution to be measured.
The beneficial effect that the present invention realizes is, the present invention by the way of water conservancy diversion dissolution control unit control water conservancy diversion dissolution,
To compose in parallel the Low ESR reference electrode that can conduct electric current to electrode and reference electrode, it is molten that current potential is generated between working electrode
Out, Low ESR reference electrode current potential is stablized, so that the measurement of working electrode is more accurate;The present invention uses cadmium internal standard compound for base
Standard is reduced the influence of operating condition and solution dilution to peak height, is reduced existing with lead content in opposite peak height evaluation blood
The relative deviation RSD value of blood lead analyzer;The present invention uses the combination three-electrode mould group of program-controlled mobile electrolytic cell, easy to operate,
Be conducive to the standardization and mass production of the manufacture of blood lead analyzer.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, present invention be described in more detail:
Fig. 1 is the three-dimensional structure diagram of blood lead analyzer cabinet of the present invention;
Fig. 2 is the main view of blood lead analyzer of the present invention;
Fig. 3 is the left view of blood lead analyzer of the present invention;
Fig. 4 is the lifting electrolyser construction left view of blood lead analyzer of the present invention;
Fig. 5 is the partial enlarged view to electrode assembly and reference electrode component of blood lead analyzer of the present invention;
Fig. 6 is the partial enlarged view of the working electrode component of blood lead analyzer of the present invention;
Fig. 7 is the circuit diagram that blood lead analyzer water conservancy diversion of the present invention dissolves out mode;
Fig. 8 is the blood lead measuring method block diagram of blood lead analyzer of the present invention.
In diagram: 1, cabinet, 2, lifting electrolyser construction, 3, three electrode assemblies, 4, to electrode, 5, reference electrode, 6, work
Make electrode, 7, pop-up, 8, undercarriage column, 9, undercarriage, 10, undercarriage gasket, 11, electric pushrod, 12, lifter plate, 13, lifting fixation
Axis, 14, sliding curtain, 15, lifting shaft, 16, electrolytic cell sit, 17, electrolytic cell, 18, electrolytic cell sit bolt, 19, electrode is sat, 20, to electricity
Polar cap, 21, to electrode stem, 22, reference anchorage clip, 23, reference rotating clamp, 24, reference upright bar, 25, rotation electrode motor, 26,
Electrode shaft coupling, 27, Z motor rack.
Specific embodiment
Such as Fig. 1, shown in 2,3,4,5,6, a kind of blood lead analyzer, including cabinet 1 is provided with lifting in the cabinet 1
Electrolyser construction 2, three electrode assemblies 3, circuit control component and data processor, the lifting electrolyser construction 2 include
Pop-up 7, undercarriage column 8, undercarriage 9, undercarriage gasket 10 and electric pushrod 11, the pop-up 7 are fixedly connected on 1 top of cabinet,
The undercarriage column 8 is fixed on 1 bottom plate of cabinet, and undercarriage gasket 10, the undercarriage pad are provided on the undercarriage column 8
10 corresponding position of piece is provided with undercarriage 9, and described 11 one end of electric pushrod is connected to pop-up 7, and the other end passes through undercarriage 9 and undercarriage
Gasket 10 is connect with lifter plate 12, and the lifter plate 12 is fixedly connected by lifting fixing axle 13 with sliding curtain 14, the liter
Drop plate 12 is also connected with lifting shaft 15, and electrolytic cell is provided on the lifting shaft 15 and sits 16, the electrolytic cell, which is sat on 16, to be put
It is equipped with electrolytic cell 17.Dust-proof upper layer shutter is additionally provided on the cabinet 1.
Such as Fig. 1, shown in 5,6, three electrode assemblies 3 include to electrode assembly, reference electrode component and working electrode
Component, described includes, to electrode stem 21, sitting 19 to electrode cap 20 to electrode and to electrode 4, sitting 19 to electrode to electrode assembly
With to electrode stem 21 connect, on electrode stem 21 by being connected with electrode fastening screw to electrode cap 20, to electrode 4 along right
It is mobile that electrode stem 21 does Z-direction.Reference electrode component includes reference anchorage clip 22, reference rotating clamp 23 and reference electrode 5, ginseng
Reference anchorage clip 22 is fixed in reference upright bar 24 than fastening screw, reference anchorage clip 22 is removable in Z-direction, can also do circle
Arc is mobile, and reference rotating clamp 23 clamps reference electrode 5, is fixed on reference anchorage clip 22, reference electrode 5 is done relative to electrolytic cell
Three-dimensional direction moving, reference electrode 5 and to electrode 4 be all fixed on to electrode sit 19 on, realize the whole design of three-electrode system.
Working electrode component is by rotation electrode motor 25, electrode shaft coupling 26, working electrode 6, Z motor rack 27, gyro double carbon contacts, GC
Contact conductor composition, the double carbon contacts of gyro have well conducting, low noise, low linear velocity and wear-resisting advantage.Working electrode 6 is
Glass-carbon electrode, the effective Peek material manufacture of the housing of glass-carbon electrode, therefore there is good inertia and rigidity.
If Fig. 7 is that conductor dissolves out mode circuit diagram, R1=R2=100 Ω, R3=500 Ω.When enriched lead, K1, K2 are logical, K3,
K4, K5 are disconnected;When lead dissolves out, K1, K2 are disconnected, and K3, K4, K5 are logical.When dissolution, pass through, reference electricity in parallel to electrode 4 and reference electrode 5
The current potential of pole 5 is more stable, so that the data that working electrode 6 is tested are more acurrate.
Such as the method block diagram that Fig. 8 is blood lead analysis-e/or determining blood lead of the invention, include the following steps:
Step 1 is added blood lead reagent into blood sample to be measured and cadmium ion internal standard compound prepares solution to be measured, by solution to be measured
It is placed in electrolytic cell;
Step 2 carries out enrichment procedure to the solution in electrolytic cell using blood lead analyzer, after being enriched with a period of time, disconnects
Power supply is dissolved out, potentiometric stripping will be generated between working electrode after in parallel with reference electrode to electrode in blood lead analyzer;
Step 3, the discrete signal of current potential and dissolution time point in obtaining step two;
Step 4 carries out 2 subdifferentials to discrete signal point in step 3 and Gauss normal distribution calculates, is sequentially connected these
Discrete signal point obtains full curve, calculates the peak height and corresponding spike potential of whole components in full curve;
Step 5 calculates correction coefficient K according to the cadmium ion internal standard compound peak height in step 4, wherein in the cadmium ion of K=10/
Mark object peak height;
The product of discrete signal point and K in step 4 is formed one group of new discrete signal point by step 6, and connection is all
Discrete signal point obtain a new full curve, calculate the peak height of whole components and corresponding peak electricity in full curve
Position obtains opposite peak height;
Step 7 is calculated with the opposite peak height in step 6, obtains blood lead content in solution to be measured.
Blood lead reagent is added in blood sample to be measured and cadmium ion internal standard compound prepares solution to be measured, is placed in electrolytic cell 17, opens
Blood lead analyzer will be put into electrolytic cell 17 electrode 4, reference electrode 5 and working electrode 6, be adjusted by circuit control component
The position of electrolytic cell 17 and three electrodes, is measured after suitable position, carries out lead in blood using flow controlling component and is working
Enrichment and dissolution operation on electrode, are recorded the discrete signal point of current potential and dissolution time, are counted using data processor
According to processing, lead content in blood is obtained.
The present invention is by the way of water conservancy diversion dissolution control unit control water conservancy diversion dissolution, in parallel with reference electrode group of electrode
At the Low ESR reference electrode that can conduct electric current, potentiometric stripping is generated between working electrode, Low ESR reference electrode current potential is steady
It is fixed, so that the measurement of working electrode is more accurate;On the basis of the present invention uses cadmium internal standard compound, contained with lead in opposite peak height evaluation blood
Amount, reduces the influence of operating condition and solution dilution to peak height, reduces the relative deviation RSD of existing blood lead analyzer
Value;The present invention uses the combination three-electrode mould group of program-controlled mobile electrolytic cell, easy to operate, is conducive to the mark of blood lead analyzer manufacture
Standardization and mass production.
Claims (6)
1. a kind of blood lead analyzer, including cabinet (1), the cabinet (1) is interior to be provided with lifting electrolyser construction (2), three electricity
Pole component (3), circuit control component and data processor, three electrode assemblies (3) include to electrode (4), reference electricity
Pole (5) and working electrode (6), which is characterized in that
The circuit control component includes water conservancy diversion dissolution control unit, the water conservancy diversion dissolution control unit control water conservancy diversion dissolution
Mode, the described water conservancy diversion dissolution mode is, it is described it is in parallel with reference electrode (5) to electrode (4) after with working electrode (6) it
Between generate potentiometric stripping;
The data processor, for handling test data;
The lifting electrolyser construction (2) includes pop-up (7), undercarriage column (8), undercarriage (9), undercarriage gasket (10) and electronic
Push rod (11), the pop-up (7) are fixedly connected at the top of cabinet (1), and the undercarriage column (8) is fixed on cabinet (1) bottom
Plate is provided with undercarriage gasket (10) on the undercarriage column (8), and described undercarriage gasket (10) corresponding position is provided with undercarriage
(9), the electric pushrod (11) one end is connected to pop-up (7), and the other end passes through undercarriage (9) and undercarriage gasket (10) and lifting
Plate (12) connection, the lifter plate (12) are fixedly connected by lifting fixing axle (13) with sliding curtain (14), the lifter plate
(12) it is also connected with lifting shaft (15), electrolytic cell is provided on the lifting shaft (15) and sits (16), the electrolytic cell is sat
(16) it is placed on electrolytic cell (17), the diameter that the electrolytic cell sits (16) is adjustable;
Three electrode assemblies (3) further include sitting (19) to electrode, described to be fixed on to electrode (4) and reference electrode (5)
Electrode is sat on (19), the three electrode assembly test leads enter electrolytic cell (17), make three-dimensional side relative to electrolytic cell (17)
To movement;
Described is Pt piece to electrode (4), and the reference electrode (5) is 232 saturated calomel electrodes, the working electrode
It (6) is glass-carbon electrode.
2. blood lead analyzer as described in claim 1, which is characterized in that the electric pushrod (11) is that H-type 50mm is electronic
Push rod, the electrolytic cell are sat (16) and are fixedly connected by electrolytic cell seat bolt (18) with lifting shaft (15).
3. blood lead analyzer as described in claim 1, which is characterized in that the glass-carbon electrode outer tube uses Peek material
Material.
4. blood lead analyzer as described in claim 1, which is characterized in that the circuit control component further includes lifting electrolysis
Pond control unit controls electrolytic cell moving direction.
5. blood lead analyzer as described in claim 1, which is characterized in that the cabinet is additionally provided with dust-proof upper layer and blocks
Plate.
6. a kind of blood lead measuring method, which is characterized in that use blood lead analyzer as described in any one in claim 1-5, packet
Include following steps:
Step 1 is added blood lead reagent into blood sample to be measured and cadmium ion internal standard compound prepares solution to be measured, solution to be measured is placed in
Electrolytic cell;
Step 2 carries out enrichment procedure to the solution in electrolytic cell using blood lead analyzer, after being enriched with a period of time, disconnects dissolution
Power supply will generate potentiometric stripping after in parallel with reference electrode to electrode in blood lead analyzer between working electrode;
Step 3, the discrete signal of current potential and dissolution time point in obtaining step two;
Step 4 carries out 2 subdifferentials to discrete signal point in step 3 and Gauss normal distribution calculates, it is discrete to be sequentially connected these
Signaling point obtains full curve, calculates the peak height and corresponding spike potential of whole components in full curve;
Step 5 calculates correction coefficient K according to the cadmium ion internal standard compound peak height in step 4, wherein K=10/ cadmium ion internal standard compound
Peak height;
The product of discrete signal point and K in step 4 is formed one group of new discrete signal point by step 6, connect it is all from
Scattered signal point obtains a new full curve, calculates the peak height and corresponding spike potential of whole components in full curve, obtains
Obtain opposite peak height;
Step 7 is calculated with the opposite peak height in step 6, obtains blood lead content in solution to be measured.
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US4090926A (en) * | 1974-09-11 | 1978-05-23 | Environmental Sciences, Inc. | Testing product |
CN2548158Y (en) * | 2002-06-20 | 2003-04-30 | 复旦大学 | Disposable electrochemical sensor for measuring blood lend concentration |
CN101424693A (en) * | 2008-12-08 | 2009-05-06 | 盛青松 | Portable plumbum ion concentration analyzer using disposable sensor |
CN201340408Y (en) * | 2008-12-12 | 2009-11-04 | 鹤壁电子研究所有限公司 | High-efficient energy-saving full automatic sulphur determinator |
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