CN104865114B - A kind of sodium standard solution preparation method - Google Patents
A kind of sodium standard solution preparation method Download PDFInfo
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- CN104865114B CN104865114B CN201510270956.8A CN201510270956A CN104865114B CN 104865114 B CN104865114 B CN 104865114B CN 201510270956 A CN201510270956 A CN 201510270956A CN 104865114 B CN104865114 B CN 104865114B
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Abstract
The present invention relates to a kind of sodium standard solution preparation method, using brand-new design thinking, for sodium at high concentration standard liquid, design introduces strong electrolyte, constitute sodium solution to be mixed, mix acquisition mixing sodium solution with through the water to be mixed of demineralizer again, using sodium solution middle and high concentration sodium standard solution to be mixed and the ratio of strong electrolyte, and the characteristic of strong electrolyte, by measurement and calculating for mixed sodium electrical conductivity of solution value, obtain mixed sodium sodium ion in liquor concentration, take this as a foundation, dynamic adjusts the mixed proportion of sodium solution to be mixed and water to be mixed, realize obtaining the mixing sodium solution for specifying Na ion concentration.
Description
Technical field
The present invention relates to a kind of sodium standard solution preparation method, it is related to solution mixing system for technical field.
Background technology
Power plant therrmodynamic system due to anti-corrosion anti-scale, using online sodium analyzer in water sample remain sodium ion
Concentration is continuously detected.To ensure the accuracy of online sodium analyzer, it is necessary to the sodium standard solution of dynamic flowing enters to instrument
Performing check and calibration.The Na ion concentration of power plant therrmodynamic system water sample is typically smaller than 5 μ g/L, belongs to low concentration；Therefore, it is intended that system
Standby sodium standard solution concentration is approached with the Na ion concentration of power plant therrmodynamic system water sample, also belongs to low strength range.
In the prior art, the preparation of low concentration sodium standard solution, generally by the way of static state is prepared, will high concentration
Sodium standard solution, be added in demineralized water by a certain percentage with micro-reservoirs such as pipettors, the sodium standard for being mixed into low concentration is molten
Liquid.The compound method of this low concentration standard liquid, due to the reason such as pollution, the pollution of vessel of dust in air, can cause
Certain error；And because the sodium standard solution concentration prepared is very low, usually below 10 μ g/L, therefore, small is absolute
Error may be amplified as very big relative error, therefore use the uncertainty of the method preparation low concentration sodium standard solution very
Greatly.And, the low concentration sodium standard solution that static state is prepared is tested and is dynamically added when calibrating in online sodium analyzer,
Needing certain device could realize, this also brings some inconvenience to actually used.
In the prior art, also there is a kind of method that dynamic continuously prepares low concentration sodium standard solution：Will using micro pump
High standard solution is added continuously in the demineralized water of flowing, is diluted to the standard liquid of low concentration；Removed by measuring respectively
The flowmeter of brine flow and micro pump calculates thinner ratio, and then calculates the concentration of the low concentration standard liquid after dilution.Adopt
In this way, it is necessary to accurately measure the flow of demineralized water and the flow of micro pump, complex in structure, practical operation is not square
Just；And the flow of micro pump is generally in below 2mL/min, accurate measurement is difficult, low concentration concentration of standard solution value can be caused
Larger uncertainty.
The content of the invention
For above-mentioned technical problem, the technical problems to be solved by the invention are to provide a kind of sodium standard solution preparation side
Method, based on brand-new design thinking, design introduces strong electrolyte, and combines the detection of electrical conductivity, can accurately, easily prepare and obtain
Obtain sodium standard solution.
In order to solve the above-mentioned technical problem the present invention uses following technical scheme：The present invention devises a kind of sodium standard solution
Preparation method, comprises the following steps：
Be added to for the strong electrolyte of sodium at high concentration standard liquid and preset kind by preset ratio first and removed by step 001.
In salt solution, constitute sodium solution to be mixed, and in sodium solution to be mixed strong electrolyte 100 times of concentration more than Na ion concentration；
Then according to the preset ratio, the concentration for obtaining sodium ion in sodium solution to be mixed is CA, the concentration of strong electrolyte is MA；
Meanwhile, the electrical conductivity of water sample is down to below default water sample conductivity value, obtain water to be mixed；
The mixed proportion of sodium solution to be mixed and water to be mixed is initialized, into step 002；
Step 002. according to sodium solution to be mixed and the mixed proportion of water to be mixed, by treating for sodium solution to be mixed and flowing
Mixing water is mixed, and mixing sodium solution is obtained, into step 003；
Step 003. obtains the conductivity value D of mixing sodium solution, and according to the strong electrolyte zwitterion unlimited dilute
Molar conductivity sum when releasingThe concentration for obtaining strong electrolyte in mixing sodium solution as follows is MB, into step
004；
Concentration M of the step 004. according to strong electrolyte in mixing sodium solutionB, sodium in mixing sodium solution is obtained as follows
The concentration of ion is CB, into step 005；
Step 005. judges whether the concentration of mixed sodium sodium ion in liquor reaches the default Na ion concentration specified, and is then
The mixing sodium solution for obtaining and specifying Na ion concentration is represented, compounding method terminates, otherwise according to the current mixing sodium solution for obtaining
The concentration C of middle sodium ionB, adjust the mixed proportion of sodium solution to be mixed and water to be mixed, return to step 002.
As a preferred technical solution of the present invention：The strong electrolyte is cesium bromide.
As a preferred technical solution of the present invention：In the step 001, filled by desalination by by the water sample
Put so that the electrical conductivity of water sample is down to below default water sample conductivity value, obtain the water to be mixed.
As a preferred technical solution of the present invention：The demineralizer is mixed resin column.
As a preferred technical solution of the present invention：It is using micro pump that the sodium to be mixed is molten in the step 002
Liquid is added into the water to be mixed of the flowing and mixed, and obtains the mixing sodium solution.
As a preferred technical solution of the present invention：In the step 005, the dense of mixed sodium sodium ion in liquor is judged
Whether degree reaches the default Na ion concentration specified, and is then to represent the mixing sodium solution for obtaining and specifying Na ion concentration, system formula
Method terminates, otherwise according to the concentration C of the current mixed sodium sodium ion in liquor for obtainingB, adjust to be mixed by the micro pump
The mixed proportion of sodium solution and water to be mixed, return to step 002.
As a preferred technical solution of the present invention：In the step 002, after mixing sodium solution is obtained, statistics
The flow of mixing sodium solution is obtained, step 003 is entered back into.
As a preferred technical solution of the present invention：In the step 002, the mixing is obtained using flowmeter statistics
The flow of sodium solution.
As a preferred technical solution of the present invention：In the step 003, using online conductivity meter for described mixed
Closing sodium solution carries out conductivity measurement, obtains the conductivity value D of mixing sodium solution.
A kind of sodium standard solution preparation method of the present invention using above technical scheme compared with prior art, with
Lower technique effect：The sodium standard solution preparation method of present invention design, it is molten for sodium at high concentration standard using brand-new design thinking
Liquid, design introduces strong electrolyte, constitutes sodium solution to be mixed, then molten with acquisition mixed sodium is mixed through the water to be mixed of demineralizer
Liquid, using sodium solution middle and high concentration sodium standard solution to be mixed and the ratio of strong electrolyte, and strong electrolyte characteristic, pass through
For the measurement and calculating of mixed sodium electrical conductivity of solution value, mixed sodium sodium ion in liquor concentration is obtained, taken this as a foundation, dynamic
The mixed proportion of sodium solution to be mixed and water to be mixed is adjusted, realizes obtaining the mixing sodium solution for specifying Na ion concentration；Entirely
Preparation method, not only solves the complicated and uncertain big defect of prior art construction, and being capable of convenient, accurate acquisition
The mixing sodium solution of Na ion concentration is specified, the reliability of the inspection of online sodium analyzer and calibration and accurate can be greatly improved
Property.
Brief description of the drawings
Fig. 1 is the hardware schematic of the sodium standard solution preparation method for present invention design.
Specific embodiment
Specific embodiment of the invention is described in further detail with reference to Figure of description.
In sodium standard solution preparation process, any impurity is practically free of in obtaining water to be mixed through demineralizer, to
The concentration of the strong electrolyte added in sodium at high concentration standard liquid is designed in the present invention here much larger than the concentration of wherein sodium ion
In sodium standard solution preparation method, design concentration to the strong electrolyte added in sodium at high concentration standard liquid more than wherein sodium from
100 times of sub- concentration, therefore, mix the electrical conductivity of obtained low concentration standard liquid almost from wherein through water to be mixed
The contribution of the ion after strong electrolyte ionization；Also, in low concentration standard liquid, in this low ionic strength environment, ion
Molar conductivity of conductivity contribution when being in close proximity to its infinite dilution.Therefore, the electrical conductivity of low concentration standard liquid is non-
Very close in the electrical conductivity sum of each ion of strong electrolyte for adding, the Their unit conductance rate of each ion of strong electrolyte is in close proximity to
Molar conductivity during its infinite dilution, and molar conductivity of the ion in infinite dilution can be to find in reference book
, therefore the conductivity value of low concentration standard liquid is obtained by measurement, you can with calculating obtained low concentration standard liquid
The concentration of strong electrolyte, then contrast the concentration of known strong electrolyte concentration and sodium ion in sodium at high concentration standard liquid, you can
To calculate the thinner ratio of obtained low concentration standard liquid, and then calculate the dense of the low concentration standard liquid after mixed diluting
Degree, and take this as a foundation, dynamic adjustment mixed diluting ratio such that it is able to obtain the mixing sodium solution for specifying Na ion concentration.
Based on above-mentioned mentality of designing and design principle and the hardware for being used to design sodium standard solution preparation method as shown in Figure 1
Schematic diagram, the following sodium standard solution preparation method of specific design of the present invention in the middle of actual application process, is specifically included as follows
Step：
Be added to for sodium at high concentration standard liquid and cesium bromide (CsBr) strong electrolyte by preset ratio first by step 001.
In demineralized water, constitute sodium solution to be mixed, and in sodium solution to be mixed cesium bromide (CsBr) strong electrolyte concentration more than sodium from
100 times of sub- concentration；Then according to the preset ratio, the concentration for obtaining sodium ion in sodium solution to be mixed is CA(μ g/L), bromine
The concentration for changing caesium (CsBr) strong electrolyte is MA(mol/L)。
Meanwhile, by the water sample by demineralizer (mixed resin column) so that the electrical conductivity of water sample is down to default water sample electricity
The μ S*cm of conductivity value 0.1-1Hereinafter, the water to be mixed is obtained.
The mixed proportion of sodium solution to be mixed and water to be mixed is initialized, into step 002.
Step 002. according to sodium solution to be mixed and the mixed proportion of water to be mixed, using micro pump by the sodium to be mixed
Solution is added into the water to be mixed of the flowing and mixed, and obtains the mixing sodium solution, and obtain using flowmeter statistics
The flow of sodium solution must be mixed, into step 003.
Step 003. carries out conductivity measurement using online conductivity meter for the mixing sodium solution, obtains mixed sodium molten
Conductivity value D (the μ S*cm of liquid-1), and according to the cesium bromide (CsBr) strong electrolyte zwitterion rubbing in infinite dilution
That electrical conductivity sumCesium bromide (CsBr) forceful electric power solution in mixing sodium solution is obtained as follows
The concentration of matter is MB(mol/L), into step 004；
Wherein, Cs+Infinite dilution when molar conductivity be 77300 μ S*cm-1/ [mol/L], Br-Infinite dilution when
Molar conductivity be 78100 μ S*cm-1/ [mol/L], both sums are 155400 μ S*cm-1/[mol/L]；Also, online electricity
Electrical conductivity instrument is a kind of easy, reliable, accurate measuring instrumentss, and its accuracy can be reached within ± 0.5%FS.
Concentration M of the step 004. according to cesium bromide (CsBr) strong electrolyte in mixing sodium solutionB(mol/L), by following public affairs
The concentration that formula obtains mixed sodium sodium ion in liquor is CB(μ g/L), into step 005.
Step 005. judges whether the concentration of mixed sodium sodium ion in liquor reaches the default Na ion concentration specified, and is then
The mixing sodium solution for obtaining and specifying Na ion concentration is represented, compounding method terminates, otherwise according to the current mixing sodium solution for obtaining
The concentration C of middle sodium ionB(μ g/L), the mixed proportion of sodium solution to be mixed and water to be mixed is adjusted by micro pump, returns to step
Rapid 002.
The sodium standard solution preparation method of above-mentioned technical proposal design, using brand-new design thinking, for sodium at high concentration mark
Quasi- solution, design introduces strong electrolyte, constitutes sodium solution to be mixed, then mixed with the water to be mixed through demineralizer
Sodium solution, using sodium solution middle and high concentration sodium standard solution to be mixed and the ratio of strong electrolyte, and strong electrolyte characteristic,
By measurement and calculating for mixed sodium electrical conductivity of solution value, mixed sodium sodium ion in liquor concentration is obtained, taken this as a foundation,
Dynamic adjustment sodium solution to be mixed and the mixed proportion of water to be mixed, realize obtaining the mixing sodium solution for specifying Na ion concentration；
Whole preparation method, not only solves the complicated and uncertain big defect of prior art construction, and can be convenient, accurate
The mixing sodium solution for specifying Na ion concentration is obtained, the reliability and standard of online sodium analyzer inspection and calibration can be greatly improved
True property, and then the low concentration standard liquid that measurement concentration actual with online sodium analyzer is close convenient, accurate can be obtained, its is dense
Degree error ＜ ± 2%FS.
Embodiments of the present invention are explained in detail above in conjunction with accompanying drawing, but the present invention is not limited to above-mentioned implementation
Mode, in the ken that those of ordinary skill in the art possess, can also be on the premise of present inventive concept not be departed from
Make a variety of changes.
Claims (9)
1. a kind of sodium standard solution preparation method, prepares sodium solution to be mixed and water to be mixed, it is characterised in that including following step
Suddenly：
The strong electrolyte of sodium at high concentration standard liquid and preset kind is added to demineralized water by step 001. by preset ratio first
In, constitute sodium solution to be mixed, and in sodium solution to be mixed strong electrolyte 100 times of concentration more than Na ion concentration；Then
According to the preset ratio, the concentration for obtaining sodium ion in sodium solution to be mixed is CA, the concentration of strong electrolyte is MA；
Meanwhile, the electrical conductivity of water sample is down to below default water sample conductivity value, obtain water to be mixed；
The mixed proportion of sodium solution to be mixed and water to be mixed is initialized, into step 002；
Step 002. is to be mixed with flowing by sodium solution to be mixed according to sodium solution to be mixed and the mixed proportion of water to be mixed
Water is mixed, and mixing sodium solution is obtained, into step 003；
Step 003. obtains the conductivity value D of mixing sodium solution, and according to the strong electrolyte zwitterion in infinite dilution
Molar conductivity sumThe concentration for obtaining strong electrolyte in mixing sodium solution as follows is MB, into step 004；
Concentration M of the step 004. according to strong electrolyte in mixing sodium solutionB, mixed sodium sodium ion in liquor is obtained as follows
Concentration be CB, into step 005；
Step 005. judges whether the concentration of mixed sodium sodium ion in liquor reaches the default Na ion concentration specified, and is to represent
The mixing sodium solution for specifying Na ion concentration is obtained, compounding method terminates, otherwise according to sodium in the current mixing sodium solution for obtaining
The concentration C of ionB, adjust the mixed proportion of sodium solution to be mixed and water to be mixed, return to step 002.
2. a kind of sodium standard solution preparation method according to claim 1, it is characterised in that：The strong electrolyte is bromination
Caesium.
3. a kind of sodium standard solution preparation method according to claim 1, it is characterised in that：In the step 001, by inciting somebody to action
The water sample is by demineralizer so that the electrical conductivity of water sample is down to below default water sample conductivity value, obtains described to be mixed
Water.
4. a kind of sodium standard solution preparation method according to claim 3, it is characterised in that：The demineralizer is mixed resin
Post.
5. a kind of sodium standard solution preparation method according to claim 1, it is characterised in that：In the step 002, use
The sodium solution to be mixed is added into the water to be mixed of the flowing and mixed by micro pump, obtains the mixed sodium molten
Liquid.
6. a kind of sodium standard solution preparation method according to claim 5, it is characterised in that：In the step 005, judge mixed
Whether the concentration for closing sodium ion in sodium solution reaches the default Na ion concentration specified, and is then to represent to obtain to specify Na ion concentration
Mixing sodium solution, compounding method terminates, otherwise according to the concentration C of the current mixed sodium sodium ion in liquor for obtainingB, by institute
State the mixed proportion that micro pump adjusts sodium solution to be mixed and water to be mixed, return to step 002.
7. a kind of sodium standard solution preparation method according to claim 1, it is characterised in that：In the step 002, obtaining
After mixing sodium solution, statistics obtains the flow of mixing sodium solution, enters back into step 003.
8. a kind of sodium standard solution preparation method according to claim 7, it is characterised in that：In the step 002, using stream
Gauge statistics obtains the flow of the mixing sodium solution.
9. a kind of sodium standard solution preparation method according to claim 1, it is characterised in that：In the step 003, using
Line conductivity meter carries out conductivity measurement for the mixing sodium solution, obtains the conductivity value D of mixing sodium solution.
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