CN104865114A - Preparation method of standard sodium solution - Google Patents
Preparation method of standard sodium solution Download PDFInfo
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- CN104865114A CN104865114A CN201510270956.8A CN201510270956A CN104865114A CN 104865114 A CN104865114 A CN 104865114A CN 201510270956 A CN201510270956 A CN 201510270956A CN 104865114 A CN104865114 A CN 104865114A
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Abstract
The invention relates to a preparation method of a standard sodium solution. According to the preparation method, a brand new design idea is adopted, that is, a strong electrolyte is introduced to form a to-be-mixed sodium solution together with a high-concentration standard sodium solution, the to-be-mixed sodium solution is mixed with to-be-mixed water treated through a desalting device to obtain a mixed sodium solution, the sodium ion concentration in the mixed sodium solution is obtained by measuring and calculating the electrical conductivity value of the mixed sodium solution through the ratio of the high-concentration standard sodium solution to the strong electrolyte in the to-be-mixed sodium solution and the characteristics of the strong electrolyte, and accordingly the mixing ratio of the to-be-mixed sodium solution to the to-be-mixed water is dynamically adjusted to obtain the mixed sodium solution with specific sodium ion concentration.
Description
Technical field
The present invention relates to a kind of sodium standard solution preparation method, relate to solution mixing system for technical field.
Background technology
Generating plant therrmodynamic system, due to anti-corrosion anti-scale, adopts online sodium analyser to carry out continuous detecting to Na ion concentration residual in water sample.For ensureing the accuracy of online sodium analyser, the sodium standard solution of dynamic flow is needed to test to instrument and calibrate.The Na ion concentration of generating plant therrmodynamic system water sample is less than 5 μ g/L usually, belongs to low concentration; Therefore, wish that the Na ion concentration of sodium standard solution concentration and the generating plant therrmodynamic system water sample prepared is close, also belong to low strength range.
In the prior art, the preparation of low concentration sodium standard solution, usually adopts the mode of static preparation, by the sodium standard solution of high concentration, is added to by a certain percentage in demineralized water with micro-reservoir such as pipettors, is mixed into the sodium standard solution of low concentration.The compound method of this low concentration standard solution, due to reasons such as the pollution of dust in air, the pollutions of vessel, can cause certain error; And due to the sodium standard solution concentration of preparation very low, be generally 10 below μ g/L, therefore, small absolute error may be exaggerated into very large relative error, therefore adopts the uncertainty of the method preparation low concentration sodium standard solution very large.And the low concentration sodium standard solution of static preparation, dynamically joins when testing and calibrate in online sodium analyser, need certain device to realize, this brings some inconvenience also to actual use.
In the prior art, also there is a kind of method of dynamic continuous production low concentration sodium standard solution: adopt micro pump to be joined continuously in the demineralized water of flowing by high standard solution, dilute the standard solution for low concentration; Calculate dilution ratio by the flowmeter measuring demineralized water flow and micro pump respectively, and then calculate the concentration of the low concentration standard solution after dilution.Adopt in this way, need the flow of Measurement accuracy demineralized water and the flow of micro pump, comparatively complicated in structure, practical operation is inconvenient; And the flow of micro pump is usually at below 2mL/min, not easily Measurement accuracy, can cause the uncertainty that low concentration concentration of standard solution value is larger.
Summary of the invention
For above-mentioned technical matters, technical matters to be solved by this invention is to provide a kind of sodium standard solution preparation method, and based on brand-new design thinking, strong electrolyte is introduced in design, and in conjunction with the detection of conductivity, accurately, easily can prepare sodium standard solution.
The present invention is in order to solve the problems of the technologies described above by the following technical solutions: the present invention devises a kind of sodium standard solution preparation method, comprises the steps:
First the strong electrolyte of sodium at high concentration standard solution and preset kind joins in demineralized water by preset ratio by step 001., forms sodium solution to be mixed, and in sodium solution to be mixed, the concentration of strong electrolyte is greater than 100 times of Na ion concentration; Then according to this preset ratio, the concentration obtaining sodion in sodium solution to be mixed is C
a, the concentration of strong electrolyte is M
a;
Meanwhile, the conductivity of water sample is down to below default water sample conductivity value, obtains water to be mixed;
The blending ratio of initialization sodium solution to be mixed and water to be mixed, enters step 002;
The water to be mixed of sodium solution to be mixed and flowing, according to the blending ratio of sodium solution to be mixed and water to be mixed, mixes by step 002., obtains mixed sodium solution, enters step 003;
Step 003. obtains the conductivity value D of mixed sodium solution, and according to the molar conductivity sum of described strong electrolyte zwitterion when infinite dilution
the concentration obtaining strong electrolyte in mixed sodium solution by following formula is M
b, enter step 004;
Step 004. is according to the concentration M of strong electrolyte in mixed sodium solution
b, the concentration obtaining mixed sodium sodium ion in liquor by following formula is C
b, enter step 005;
Step 005. judges whether the concentration of mixed sodium sodium ion in liquor reaches the Na ion concentration preset and specify, represent the mixed sodium solution obtaining and specify Na ion concentration, compounding method terminates, otherwise the concentration C of mixed sodium sodium ion in liquor according to current acquisition
b, adjust the blending ratio of sodium solution to be mixed and water to be mixed, return step 002.
As a preferred technical solution of the present invention: described strong electrolyte is cesium bromide.
As a preferred technical solution of the present invention: in described step 001, by by described water sample through demineralizer, make the conductivity of water sample be down to below default water sample conductivity value, obtain described water to be mixed.
As a preferred technical solution of the present invention: described demineralizer is mixed resin column.
As a preferred technical solution of the present invention: in described step 002, adopt micro pump to be added to by described sodium solution to be mixed in the water to be mixed of described flowing and mix, obtain described mixed sodium solution.
As a preferred technical solution of the present invention: in described step 005, judge whether the concentration of mixed sodium sodium ion in liquor reaches the Na ion concentration preset and specify, represent the mixed sodium solution obtaining and specify Na ion concentration, compounding method terminates, otherwise the concentration C of mixed sodium sodium ion in liquor according to current acquisition
b, adjusted the blending ratio of sodium solution to be mixed and water to be mixed by described micro pump, return step 002.
As a preferred technical solution of the present invention: in described step 002, after acquisition mixed sodium solution, statistics obtains the flow of mixed sodium solution, then enters step 003.
As a preferred technical solution of the present invention: in described step 002, flowmeter statistics is adopted to obtain the flow of described mixed sodium solution.
As a preferred technical solution of the present invention: in described step 003, adopt online conductivity meter to carry out conductivity measurement for described mixed sodium solution, obtain the conductivity value D of mixed sodium solution.
A kind of sodium standard solution preparation method of the present invention adopts above technical scheme compared with prior art, there is following technique effect: the sodium standard solution preparation method of the present invention's design, adopt brand-new design thinking, for sodium at high concentration standard solution, strong electrolyte is introduced in design, form sodium solution to be mixed, mix with the water to be mixed through demineralizer again and obtain mixed sodium solution, utilize the ratio of sodium solution middle and high concentration sodium standard solution to be mixed and strong electrolyte, and the characteristic of strong electrolyte, by the measurements and calculations for mixed sodium electrical conductivity of solution value, obtain mixed sodium sodium ion in liquor concentration, take this as a foundation, the blending ratio of dynamic conditioning sodium solution to be mixed and water to be mixed, realize obtaining the mixed sodium solution of specifying Na ion concentration, whole preparation method, not only solve prior art complex structure and the large defect of uncertainty, and can obtain convenient, accurately and specify the mixed sodium solution of Na ion concentration, greatly can improve reliability and the accuracy of the inspection of online sodium analyser and calibration.
Accompanying drawing explanation
Fig. 1 is the hardware schematic diagram of the sodium standard solution preparation method for the present invention's design.
Embodiment
Below in conjunction with Figure of description, the specific embodiment of the present invention is described in further detail.
In sodium standard solution preparation process, obtain in water to be mixed hardly containing any impurity through demineralizer, the concentration of the strong electrolyte added in sodium at high concentration standard solution is much larger than the concentration of wherein sodion, here design in sodium standard solution preparation method in the present invention, the concentration designing the strong electrolyte added in sodium at high concentration standard solution is greater than 100 times of wherein Na ion concentration, therefore, the conductivity mixing through water to be mixed the low concentration standard solution obtained almost derives from the contribution of the ion after wherein strong electrolyte ionization; Further, in low concentration standard solution, in this low ionic strength environment, the conductivity contribution of ion is in close proximity to molar conductivity during its infinite dilution.Therefore, the conductivity of low concentration standard solution is in close proximity to the conductivity sum of each ion of the strong electrolyte added, the Their unit conductance rate of each ion of strong electrolyte is in close proximity to molar conductivity during its infinite dilution, and the molar conductivity of ion when infinite dilution can be found in reference book, therefore by measure obtain the conductivity value of low concentration standard solution, namely the concentration of strong electrolyte in obtained low concentration standard solution can be calculated, contrast strong electrolyte concentration known in sodium at high concentration standard solution and the concentration of sodion again, namely the dilution ratio of obtained low concentration standard solution can be calculated, and then calculate the concentration of the low concentration standard solution after mixed diluting, and take this as a foundation, dynamic conditioning mixed diluting ratio, thus the mixed sodium solution of specifying Na ion concentration can be obtained.
Based on above-mentioned mentality of designing and design concept with as shown in Figure 1 for designing the hardware schematic diagram of sodium standard solution preparation method, the following sodium standard solution preparation method of specific design of the present invention, in the middle of the application process of reality, specifically comprises the steps:
First sodium at high concentration standard solution and cesium bromide (CsBr) strong electrolyte join in demineralized water by preset ratio by step 001., form sodium solution to be mixed, and in sodium solution to be mixed, the concentration of cesium bromide (CsBr) strong electrolyte is greater than 100 times of Na ion concentration; Then according to this preset ratio, the concentration obtaining sodion in sodium solution to be mixed is C
a(μ g/L), the concentration of cesium bromide (CsBr) strong electrolyte is M
a(mol/L).
Meanwhile, by described water sample through demineralizer (mixed resin column), the conductivity of water sample is made to be down to default water sample conductivity value 0.1 μ S*cm
-1below, described water to be mixed is obtained.
The blending ratio of initialization sodium solution to be mixed and water to be mixed, enters step 002.
Step 002. is according to the blending ratio of sodium solution to be mixed and water to be mixed, adopt micro pump to be added to by described sodium solution to be mixed in the water to be mixed of described flowing to mix, obtain described mixed sodium solution, and adopt flowmeter to add up the flow obtaining mixed sodium solution, enter step 003.
Step 003. adopts online conductivity meter to carry out conductivity measurement for described mixed sodium solution, obtains conductivity value D (the μ S*cm of mixed sodium solution
-1), and according to the molar conductivity sum of described cesium bromide (CsBr) strong electrolyte zwitterion when infinite dilution
the concentration obtaining cesium bromide (CsBr) strong electrolyte in mixed sodium solution by following formula is M
b(mol/L), step 004 is entered;
Wherein, Cs
+infinite dilution time molar conductivity be 77300 μ S*cm
-1/ [mol/L], Br
-infinite dilution time molar conductivity be 78100 μ S*cm
-1/ [mol/L], both sums are 155400 μ S*cm
-1/ [mol/L]; Further, online conductivity meter be a kind of easy, reliably, measurement instrument accurately, its accuracy can reach ± 0.5%FS within.
Step 004. is according to the concentration M of cesium bromide (CsBr) strong electrolyte in mixed sodium solution
b(mol/L) concentration, obtaining mixed sodium sodium ion in liquor by following formula is C
b(μ g/L), enters step 005.
Step 005. judges whether the concentration of mixed sodium sodium ion in liquor reaches the Na ion concentration preset and specify, represent the mixed sodium solution obtaining and specify Na ion concentration, compounding method terminates, otherwise the concentration C of mixed sodium sodium ion in liquor according to current acquisition
b(μ g/L), is adjusted the blending ratio of sodium solution to be mixed and water to be mixed, returns step 002 by micro pump.
The sodium standard solution preparation method of technique scheme design, adopt brand-new design thinking, for sodium at high concentration standard solution, strong electrolyte is introduced in design, form sodium solution to be mixed, mix with the water to be mixed through demineralizer again and obtain mixed sodium solution, utilize the ratio of sodium solution middle and high concentration sodium standard solution to be mixed and strong electrolyte, and the characteristic of strong electrolyte, by the measurements and calculations for mixed sodium electrical conductivity of solution value, obtain mixed sodium sodium ion in liquor concentration, take this as a foundation, the blending ratio of dynamic conditioning sodium solution to be mixed and water to be mixed, realize obtaining the mixed sodium solution of specifying Na ion concentration, whole preparation method, not only solve prior art complex structure and the large defect of uncertainty, and can obtain convenient, accurately and specify the mixed sodium solution of Na ion concentration, greatly can improve reliability and the accuracy of the inspection of online sodium analyser and calibration, and then can the low concentration standard solution that is close of convenient, accurate acquisition and online sodium analyser actual measurement concentration, its concentration error < ± 2%FS.
By reference to the accompanying drawings embodiments of the present invention are explained in detail above, but the present invention is not limited to above-mentioned embodiment, in the ken that those of ordinary skill in the art possess, can also makes a variety of changes under the prerequisite not departing from present inventive concept.
Claims (9)
1. a sodium standard solution preparation method, is characterized in that, comprises the steps:
First the strong electrolyte of sodium at high concentration standard solution and preset kind joins in demineralized water by preset ratio by step 001., forms sodium solution to be mixed, and in sodium solution to be mixed, the concentration of strong electrolyte is greater than 100 times of Na ion concentration; Then according to this preset ratio, the concentration obtaining sodion in sodium solution to be mixed is C
a, the concentration of strong electrolyte is M
a;
Meanwhile, the conductivity of water sample is down to below default water sample conductivity value, obtains water to be mixed;
The blending ratio of initialization sodium solution to be mixed and water to be mixed, enters step 002;
The water to be mixed of sodium solution to be mixed and flowing, according to the blending ratio of sodium solution to be mixed and water to be mixed, mixes by step 002., obtains mixed sodium solution, enters step 003;
Step 003. obtains the conductivity value D of mixed sodium solution, and according to the molar conductivity sum of described strong electrolyte zwitterion when infinite dilution
the concentration obtaining strong electrolyte in mixed sodium solution by following formula is M
b, enter step 004;
Step 004. is according to the concentration M of strong electrolyte in mixed sodium solution
b, the concentration obtaining mixed sodium sodium ion in liquor by following formula is C
b, enter step 005;
Step 005. judges whether the concentration of mixed sodium sodium ion in liquor reaches the Na ion concentration preset and specify, represent the mixed sodium solution obtaining and specify Na ion concentration, compounding method terminates, otherwise the concentration C of mixed sodium sodium ion in liquor according to current acquisition
b, adjust the blending ratio of sodium solution to be mixed and water to be mixed, return step 002.
2. a kind of sodium standard solution preparation method according to claim 1, is characterized in that: described strong electrolyte is cesium bromide.
3. a kind of sodium standard solution preparation method according to claim 1, is characterized in that: in described step 001, by by described water sample through demineralizer, make the conductivity of water sample be down to below default water sample conductivity value, obtain described water to be mixed.
4. a kind of sodium standard solution preparation method according to claim 3, is characterized in that: described demineralizer is mixed resin column.
5. a kind of sodium standard solution preparation method according to claim 1, is characterized in that: in described step 002, adopts micro pump to be added to by described sodium solution to be mixed in the water to be mixed of described flowing and mixes, obtain described mixed sodium solution.
6. a kind of sodium standard solution preparation method according to claim 5, it is characterized in that: in described step 005, judge whether the concentration of mixed sodium sodium ion in liquor reaches the Na ion concentration preset and specify, represent the mixed sodium solution obtaining and specify Na ion concentration, compounding method terminates, otherwise the concentration C of mixed sodium sodium ion in liquor according to current acquisition
b, adjusted the blending ratio of sodium solution to be mixed and water to be mixed by described micro pump, return step 002.
7. a kind of sodium standard solution preparation method according to claim 1, is characterized in that: in described step 002, and after acquisition mixed sodium solution, statistics obtains the flow of mixed sodium solution, then enters step 003.
8. a kind of sodium standard solution preparation method according to claim 7, is characterized in that: in described step 002, adopts flowmeter statistics to obtain the flow of described mixed sodium solution.
9. a kind of sodium standard solution preparation method according to claim 1, is characterized in that: in described step 003, adopts online conductivity meter to carry out conductivity measurement for described mixed sodium solution, obtains the conductivity value D of mixed sodium solution.
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| CN107957475A (en) * | 2017-11-17 | 2018-04-24 | 广西华银铝业有限公司 | A kind of method for improving backwater receipts rate in aluminium oxide backwater technique |
| CN112903759A (en) * | 2021-01-23 | 2021-06-04 | 西安热工研究院有限公司 | Online calibration system and method for silicon meter |
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