CN105300900A - Liquid analysis method and device of spectrophotometry test with digestion - Google Patents
Liquid analysis method and device of spectrophotometry test with digestion Download PDFInfo
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- CN105300900A CN105300900A CN201510643117.6A CN201510643117A CN105300900A CN 105300900 A CN105300900 A CN 105300900A CN 201510643117 A CN201510643117 A CN 201510643117A CN 105300900 A CN105300900 A CN 105300900A
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Abstract
An embodiment of the invention relates to a liquid analysis method and device of a spectrophotometry test with digestion. The method comprises the following steps: adding a solution to be analyzed into an analyzer cup, and heating and digesting the solution to be analyzed; quantifying the digested solution, discharging residual parts, and causing a set quantity of solution to be analyzed to be left; after the solution to be analyzed stands, carrying out an absorbance test on the set quantity of solution within a specific wavelength range to obtain a first absorbance numerical value ABS1; adding a titration reagent corresponding to ions to be measured, and stirring; adding a color developing agent corresponding to the ions to be measured into the stirred solution to carry out color development on the solution; after the solution stands, carrying out the absorbance test on the evenly stirred solution within the specific wavelength range to obtain a second absorbance numerical value ABS2; calculating a difference value between the second absorbance numerical value ABS2 and the first absorbance numerical value ABS1; according to a preset corresponding relationship and the difference value between a absorbance variable quantity and ion concentration, determining the concentration of the ions to be measured in the solution to be analyzed.
Description
Technical field
The present invention relates to a kind of technical field of analytical chemistry, particularly relate to liquid analysis method and the device of the spectrophotometric method test that a kind of band is cleared up.
Background technology
Instrumental analysis (instrumentanalysis) and chemical analysis (chemicalanalysis) are two analytical approachs of analytical chemistry (analyticalchemistry).Wherein, the analysis based on the chemical reaction utilizing material, is called chemical analysis.Chemical analysis is with a long history, is the basis of analytical chemistry, is also called classical analysis.Chemical analysis is absolute quantitation, amount per sample, the amount of reaction product or consume the amount of reagent and the stoichiometric relationship of reaction, by calculating the amount of component to be measured.Instrumental analysis is an important branch of chemistry subject, and it is a kind of analytical approach set up based on the physics of material and physicochemical property.Utilize analytical instrument, qualitative analysis is carried out to material, quantitative test, morphological analysis.
Spectrophotometric method is absorbance by measuring measured matter light in certain wave strong point or a wavelength range or luminous intensity, this material is carried out to the method for qualitative and quantitative analysis.
Summary of the invention
The object of this invention is to provide liquid analysis method and the device of the spectrophotometric method test that a kind of band is cleared up, simple to operate, working stability, makes solution to be analyzed fully clear up by heating, carry out qualitative and quantitative analysis accurately to liquid again to measure, measuring accuracy is high, reproducible.
For achieving the above object, in first aspect, the invention provides the liquid analysis method of the spectrophotometric method test that a kind of band is cleared up, comprising:
Solution to be analyzed is added in analyzer cup;
Described solution to be analyzed is heated, described solution to be analyzed is fully cleared up;
Carry out quantitatively to the solution to be analyzed after clearing up, discharge redundance, the solution to be analyzed of residue set amount;
After leaving standstill, in particular range of wavelengths, absorbance test is carried out to the solution to be analyzed of described set amount, obtain the first absorption values ABS1;
In the solution to be analyzed of described set amount, add the titer reagent that a kind of ion pair to be determined is answered, and stir;
Add the developer that described ion pair to be determined is answered in solution after agitation, solution is developed the color;
After leaving standstill, in described particular range of wavelengths, absorbance test is carried out to the solution after stirring, obtain the second absorption values ABS2;
Calculate the difference of described second absorption values ABS2 and described first absorption values ABS1;
According to corresponding relation and the described difference of pre-set absorbance variable quantity and ion concentration, determine the concentration of ion to be determined described in described solution to be analyzed.
Preferably, analyze light source and send incident optical signal in particular range of wavelengths, through described analyzer cup and the solution be placed in described analyzer cup, form emergent light signal and received by photodetector;
The described emergent light signal received is converted to voltage signal by described photodetector, sends to processor;
Described processor determines corresponding absorbance parameter according to described voltage signal.
Preferred further, before described formation emergent light signal is received by photodetector, also comprise:
Optical filter is set between described analyzer cup and described photodetector, to make described incident optical signal through described analyzer cup and the solution be placed in described analyzer cup, then after described optical filter filters, forms emergent light signal and received by photodetector.
Preferably, described in analyzer cup, add solution to be analyzed before, described method also comprises carries out prerinse to described analyzer cup.
Preferred further, described prerinse comprises:
Discharge opeing is carried out to described analyzer cup;
Use cleaning liquid to inject described analyzer cup, and stir;
Described cleaning liquid is discharged described analyzer cup;
Re-use cleaning liquid and inject described analyzer cup, and stir;
Again described cleaning liquid is discharged described analyzer cup.
Preferably, described in analyzer cup, add solution to be analyzed before, described method also comprises:
Utilize the solution of known ion concentration to test, set up the corresponding relation of described absorbance variable quantity and ion concentration.
Preferably, described described solution to be analyzed to be heated, described solution to be analyzed is fully cleared up and is specially:
Described solution to be analyzed is heated and stirred, makes described solution to be analyzed all gasify as gas to be cooled;
Described gas to be cooled is cooled, is again condensed into liquid backflow in analyzer cup.
In second aspect, embodiments provide a kind of liquid analysis device, in order to realize the liquid analysis method described in above-mentioned first aspect, comprising: analysis module and spiral condenser;
Described analysis module comprises fixed support, analyzer cup, porous plug and well heater; In described analyzer cup and the accommodating and described fixed support of described well heater, described porous plug is installed in the rim of a cup of described analyzer cup and is exposed by described support bracket fastened top, described well heater is arranged at the bottom of described analyzer cup, liquid to be analyzed in described analyzer cup is heated, make described liquid gasification to be analyzed become gas to be cooled, be expelled in spiral condenser by the venthole of described porous plug top center;
Bottom described spiral condenser, there is draft tube, be connected with described venthole is airtight, described gas to be cooled enters in described spiral condenser by described draft tube, heat interchange is carried out with cooling liquid in described spiral condenser, become the liquid to be analyzed after clearing up after described gas to be cooled being cooled reach condensing temperature, then be back in described analyzer cup by described spiral condenser;
Described analysis module also comprises analyzes light source and photodetector, and described analysis light source sends the incident light in a wavelength range, through in described analyzer cup and described analyzer cup accommodating clear up after liquid to be analyzed, become emergent light and received by photodetector; Described photodetector, according to the light intensity of described emergent light, determines the chemical substance contained by liquid accommodating in described analyzer cup and concentration.
The liquid analysis method of the spectrophotometric method test that the band that the embodiment of the present invention provides is cleared up, simple to operate, working stability, makes solution to be analyzed fully clear up by heating, carry out qualitative and quantitative analysis accurately to liquid again to measure, measuring accuracy is high, reproducible.
Accompanying drawing explanation
The process flow diagram of the liquid analysis method of the spectrophotometric method test that Fig. 1 clears up for the band that the embodiment of the present invention provides;
The schematic diagram of the liquid analysis device that Fig. 2 provides for the embodiment of the present invention;
The explosive view of the analysis module that Fig. 3 provides for the embodiment of the present invention;
The skeleton view of a kind of spiral condenser that Fig. 4 provides for the embodiment of the present invention;
The skeleton view of the another kind of spiral condenser that Fig. 5 provides for the embodiment of the present invention.
Embodiment
Below by drawings and Examples, technical scheme of the present invention is described in further detail.
The process flow diagram of the liquid analysis method of the spectrophotometric method test that Fig. 1 clears up for the band that the embodiment of the present invention provides.Below in conjunction with Fig. 1, the liquid analysis method that the present embodiment provides is described.
Described method comprises the steps:
Step 100, carries out prerinse to analyzer cup;
Concrete, before carrying out fluid analysis, first need to carry out emptying and cleaning to analyzer cup.Cleaning can adopt the cleaning liquids such as deionized water, and wash number is preferably twice.
Prewashed concrete steps can comprise:
Step 101, carries out discharge opeing to analyzer cup;
Step 102, uses cleaning liquid to inject analyzer cup, and stirs;
Step 103, discharges analyzer cup by cleaning liquid;
Step 104, re-uses cleaning liquid and injects analyzer cup, and stir;
Step 105, then cleaning liquid is discharged described analyzer cup.
Through above-mentioned pre-cleaning process, the remaining liq that in analyzer cup, possibility is remaining can be got rid of, avoid having an impact to current analytical test result.
Step 110, adds solution to be analyzed in analyzer cup;
Concrete, first, use solution to be analyzed to clean analyzer cup, make the environment facies of environment and solution to be analyzed in analyzer cup seemingly, get rid of test interference further;
Subsequently, then with adding solution to be analyzed, with to be detected.
Step 120, treats analytical solution and heats, and solution to be analyzed is fully cleared up;
Concrete, first, treat analytical solution and carry out heating and stirring, make solution to be analyzed all gasify as gas to be cooled; Wherein, heating-up temperature can set according to the character of solution to be analyzed.
Subsequently, described gas to be cooled is cooled, make gas to be cooled again be condensed into liquid backflow in analyzer cup.
The process of above-mentioned heating and gasifying and condensation can repeatedly, to ensure that all solution to be analyzed is all cleared up completely.
Step 130, treats the analytical solution after clearing up and carries out quantitatively, discharges redundance, the solution to be analyzed of residue set amount;
Concrete, carry out quantitatively according to the capacity of setting to the solution to be analyzed in analyzer cup, the part exceeding set amount is discharged analyzer cup, all identical with the amount of the solution to be analyzed ensureing each test, make test result more accurately and reliably.
Step 140, after leaving standstill, carries out absorbance test to the solution to be analyzed of set amount, obtains the first absorption values ABS1 in particular range of wavelengths;
Concrete, after the standing, sent the incident optical signal in particular range of wavelengths by analysis light source, through analyzer cup and the solution be placed in analyzer cup, form emergent light signal and received by photodetector.
Can also optical filter be had between photodetector and analyzer cup, make the wavelength of outgoing light signal for setting wavelength.The emergent light signal received is converted to voltage signal by photodetector, sends to processor; The wherein size of voltage signal, has funtcional relationship with the intensity of emergent light signal.
Processor is first converted into digital signal according to voltage signal, is corresponded to the numerical value of corresponding absorbance subsequently again by digital signal, is the first absorption values ABS1.The test of the first absorption values ABS1 can be carried out repeatedly, obtains the numerical value of multiple absorbance, chooses one of them as the first absorption values ABS1.
Such as 3 times be can testing, testing in 3 numerical value obtained, maximal value and minimum value got rid of, using the numerical value of centre as the first absorption values ABS1.
What analysis light source was commonly used can have wavelength coverage at the white light source of 380-1100nm, and wavelength coverage is at the purple light light source of 250-400nm.
It should be noted that, in some cases, quantitatively, remaining amount of liquid is less, need the amount adding titer reagent more, amount of liquid quantitatively can not meet the requirement of absorbance test, therefore after step 120, first can perform above-mentioned steps 140 and carry out absorbance test, then perform step 130 and carry out quantitatively.
Step 150, adds the titer reagent that a kind of ion pair to be determined is answered, and stirs in the solution to be analyzed of set amount;
Concrete, test for different elements, the titer reagent adopted is different.Such as, test fluorine ion adopts ferrous sulphate ammonia, and test cadmium ion adopts six methine four ammonium mixed solutions.
Step 160, adds the developer that ion pair to be determined is answered, develops the color to solution in solution after agitation;
Same, test for different elements, the developer adopted is also different.Such as, developer sulfosalicylic acid is adopted for fluorine ion, developer xylenol orange is adopted for cadmium ion.
Step 170, after leaving standstill, carries out absorbance test to the solution after stirring, obtains the second absorption values ABS2 in particular range of wavelengths;
Test process is identical with above-mentioned steps 140.The test of the second absorption values ABS2 can be carried out repeatedly, obtains the numerical value of multiple absorbance, chooses one of them as the second absorption values ABS2.
Such as 3 times be can testing, testing in 3 numerical value obtained, maximal value and minimum value got rid of, using the numerical value of centre as the second absorption values ABS2.
Concrete, for the concentration determination of fluorine ion, add titer reagent ferrous sulphate ammonia as complexing agent, form analysis environments, then with Fe
3+for in the water sample of complexing agent, adding sulfosalicylic acid is developer, can generate aubergine complex compound with the fluorine ion in water quality, measures respectively under 510nm light source to the absorption values added before and after developer, thus calculates the concentration of fluorine ion.
For the concentration determination of cadmium ion, when adding six methine four ammonium system of titer reagent summary acid, the cadmium in sample and xylenol orange is made to form stable complex system as buffer solvent, then measure the absorption values added before and after developer xylenol orange in wavelength 578nm place respectively, calculate the concentration of cadmium ion.
For the ion that other are different, only corresponding titer reagent and developer need be selected to test accordingly.
Step 180, calculates the difference of the second absorption values ABS2 and the first absorption values ABS1;
Step 190, according to corresponding relation and this difference of pre-set absorbance variable quantity and ion concentration, determines the concentration of ion to be determined in solution to be analyzed.
Concrete, the corresponding relation of absorbance variable quantity and ion concentration is before fluid analysis, utilizes the solution of known ion concentration to carry out testing and obtain.By testing the liquid of known ion concentration, obtaining the absorbance before and after titration colour developing, and calculating the variable quantity of absorbance, thus setting up the corresponding relation of described absorbance variable quantity and ion concentration.
The liquid analysis method that the embodiment of the present invention provides, simple to operate, working stability, makes solution to be analyzed fully clear up by heating, then can carry out qualitative and quantitative analysis measurement accurately to liquid.Adopt the variable quantity determination ion concentration of absorbance, make to further reduce test error, measuring accuracy is high, reproducible.
Accordingly, the embodiment of the present invention additionally provides a kind of liquid analysis device in order to realize aforesaid liquid analytical approach, specifically can as shown in Figure 2, comprise: analysis module 1 and spiral condenser 2;
Analysis module 1 can specifically shown in composition graphs 3.Described analysis module 1 comprises fixed support 13, analyzer cup 11, porous plug 12 and well heater (not shown); Analyzer cup 11 and well heater accommodating with in fixed support 13, porous plug 12 is installed in the rim of a cup of analyzer cup 11 and is exposed by the top of fixed support 13, well heater is arranged at the below of analyzer cup 11, liquid to be analyzed in analyzer cup 11 is heated, make liquid gasification to be analyzed become gas to be cooled, be expelled in spiral condenser 2 by the venthole 124 of porous plug 12 top center;
Spiral condenser 2 can specifically shown in composition graphs 4 or Fig. 5, there is bottom spiral condenser 2 draft tube 20, be connected with venthole 124 is airtight, gas to be cooled enters in spiral condenser 2 by draft tube 20, heat interchange is carried out with cooling liquid in spiral condenser 2, become the liquid to be analyzed after clearing up after gas to be cooled being cooled reach condensing temperature, then be back in analyzer cup 11 by spiral condenser 2;
Again shown in composition graphs 3, analysis module 1 also comprises analyzes light source 14 and photodetector 15, analyze light source 14 and send incident light in a wavelength range, through in analyzer cup 11 and analyzer cup 11 accommodating clear up after liquid to be analyzed, become emergent light and received by photodetector 15; Photodetector 15, according to the light intensity of emergent light, determines the chemical substance contained by liquid accommodating in analyzer cup 11 and concentration.
Except analyzer cup 11, porous plug 12, fixed support 13, analysis light source 14 and photodetector 15 and well heater (not shown), analysis module 1 also comprises stirring motor 16, magnet 17, magnet rotor (not shown) and optical filter 18.
Concrete, analyzer cup 11, is made up of corrosion-resistant and high-temperature resistant glass, has bulge loop structure 11 at the rim of a cup of analyzer cup 11; Well heater can be looped around the bottom of analyzer cup 11, heats the liquid in analyzer cup 11.
Porous plug 12 is many mill dells body structure, and centre is porous plug cavity; The end face and individual side of porous plug 12 all has a circular hole 121, in order to insert different liquid lines; Bottom surface is loop configuration 122, matches respectively with the internal diameter of bulge loop structure 111 and external diameter; The loop configuration 122 of porous plug 12 bottom surface is installed on bulge loop structure 111, and porous plug cavity is connected with the inside of analyzer cup 11, and liquid line inserts in analyzer cup 11 through porous plug 12.
In order to accurate positioning, loop configuration 122 has a gulde edge 1221 in edge, loop configuration 122 is socketed in porous plug locating ring 123, is blocked and establishes, fixed by the setting angle of porous plug 12 by the locating slot 1231 in gulde edge 1221 and porous plug locating ring 123.
Liquid line at least can comprise: these are several for titration liquid feed tube, liquid feed tube to be analyzed, cleaning liquid feed tube, quantity tube and discharging tube.
Liquid feed tube to be analyzed is inserted into the bottom of analyzer cup 11, in analyzer cup 11, carry liquid to be analyzed;
Titration liquid feed tube is inserted into the top of analyzer cup 11, quantitatively instills the titration liquid carrying out with liquid to be analyzed reacting;
Quantity tube is inserted into the middle and upper part of analyzer cup 11 with fixed position, is discharged by the liquid exceeding this position, makes residual liquid quantity in analyzer cup 11 be fixed amount;
Cleaning liquid feed tube injects cleaning liquid in analyzer cup 11, as deionized water;
Discharging tube is inserted into the bottom of analyzer cup 11, is all discharged by the liquid in analyzer cup 11.
Fixed support 13, specifically comprises fixed support body 131, upper cover 132 and bottom 133;
Fixed support body 131 inside is cylindrical cavity, and outside is rectangular parallelepiped, and relative two sides have been opened two accommodating windows 1311 of photo-detector; Analyzer cup 11 is placed in cylindrical cavity, and the diameter of bulge loop structure 111 is greater than the diameter of cylindrical cavity, thus is stuck on the upper surface of fixed support body 131;
Preferably, view window 1312 has been opened in the front of fixed support body 131, for user through the working condition in view window 1312 observation analysis cup 11.
The liquid carrying out analyzing under lucifuge state for satisfying the demand, to the requirement of equipment, can also install lucifuge plug 1313 outside view window 1312; Lucifuge plug 1313 and the mating shapes of view window 1312, be fastened on view window 1312, and the lucifuge in fixed support body 131 of the liquid in analyzer cup 11 is placed.
Upper cover 132, is fastened on porous plug 12, establishes be connected with the upper surface spiral shell of fixed support body 131; The top of upper cover 132 has ring structure 1321, after assembling, the side of porous plug 12 and end face expose by the middle of ring structure 1321, the loop configuration 122 of bottom surface is crimped in bulge loop structure 111 by ring structure 1321, have packing ring 120 between loop configuration 122 and bulge loop structure 111, loop configuration 122, packing ring 120, bulge loop structure 111 are crimped on the upper surface of fixed support body 131 by the ring structure 1321 of upper cover 132 together.
Magnet 17 is fixed in the rotating shaft of stirring motor 16, is with moving magnet 17 to rotate by stirring motor 16.Stirring motor 16 and magnet 17 are fixed on the below of fixed support body 131 by base 133, and at the bottom of the cup of magnet 17 and analyzer cup 11 between very little gap, an interval.
Be equipped with magnet rotor (not shown) in analyzer cup 11, drive the magnet rotor in analyzer cup 11 to rotate with magnet 17 by the magnetic force of magnet 17, thus liquid accommodating in analyzer cup 11 is stirred.
Analyze light source 14, be arranged in an accommodating window 1311 of institute's detector, be installed on cover plate 135 by web member 1351, and be fastened on fixed support body 131 by cover plate 135, send the incident light in a wavelength range to cylindrical cavity direction.What analysis light source 14 was conventional can have wavelength coverage at the white light source of 380-1100nm, and wavelength coverage is at the purple light light source of 250-400nm.
Photodetector 15, be arranged in the accommodating window 1311 of photo-detector described in another, be installed on cover plate 135 by web member 1351, and be fastened on fixed support body 131 by cover plate 135, the incident light that analysis light source 14 sends, through liquid accommodating in analyzer cup 11 and analyzer cup 11, becomes emergent light and is received by photodetector 15.Photodetector 15, according to the light intensity of incident light and emergent light and variable quantity, determines the chemical substance contained by liquid accommodating in analyzer cup 11 and concentration.
When analyzing certain element-specific, the analysis module that the present embodiment provides also includes optical filter 18, light path along emergent light is arranged between analyzer cup 11 and photodetector 15, by the light filtering of other wavelength in emergent light except required particular range of wavelengths, and make the light therethrough optical filter 18 in emergent light in particular range of wavelengths arrive photodetector 15, in order to according to set optical filter and the light light intensity arriving photodetector 15, determine the concentration of this kind of element-specific in liquid.
Such as test the Fe element in liquid, the wavelength of required light is 510nm, can arrange corresponding optical filter, by the light filtering of other wavelength, only leaves the light in 510 ± 2nm wavelength coverage, for the content analysis of Fe element in liquid.
In the present embodiment, the test of analysis module 1 carries out for the liquid to be analyzed after clearing up.That is first by modes such as heating, stirrings, liquid to be analyzed is fully cleared up, by the conversion realizing fluid-gas-liquid that coordinates with spiral condenser 2, complete digestion process.And then carry out measuring process by analysis light source 14 and photodetector 15.
In a concrete example, spiral condenser 2 can specifically as shown in Figure 4.
Spiral condenser 2 comprises: cooling tube 21 and recirculatory pipe 22.
Cooling tube 21 is in cylindric, and cooling tube 21 is inner for surround by tube wall 211 the columned cooling cavities 212 formed; The tube wall 211 of side, cooling tube 21 top has liquid coolant water delivering orifice 213, the tube wall 211 of side, bottom has liquid coolant water inlet 214, liquid coolant enters cooling cavities 212 by liquid coolant water delivering orifice 213, then flows out cooling cavities 212 by liquid coolant water inlet 214;
Recirculatory pipe 22 in the shape of a spiral, is contained in cooling cavities 212; The bottom of recirculatory pipe 22 has draft tube 20, the bottom of cooling tube 21 is connected at draft tube 20 place with the bottom of recirculatory pipe 22, make the bottom of cooling cavities 212 form closed structure, and recirculatory pipe 22 inside is by the ft connection of draft tube 20 with spiral condenser; The top of recirculatory pipe 22 has escape pipe 222, the outer wall of escape pipe 222 penetrates the outside of cooling tube 21 to spiral condenser, make recirculatory pipe 22 at the ft connection of top and spiral condenser, and the sidewall of the outer wall of escape pipe 222 and cooling tube 21 is tightly connected; Gas to be cooled enters in recirculatory pipe 22 by draft tube 20, heat interchange is carried out by the liquid coolant in the tube wall of recirculatory pipe 22 and cooling cavities 212, become liquid after gas to be cooled being cooled reach condensing temperature, flow out spiral condenser 2 by draft tube 20 and be back in analyzer cup.
In liquid circulation process, liquid coolant in cooling cavities 212 contacts with the outer wall of recirculatory pipe 22, carry out heat interchange by the gas to be cooled in the spiral fashion tube wall of recirculatory pipe 22 and recirculatory pipe 22, thus the gas to be cooled in recirculatory pipe 22 is cooled; After gas to be cooled reaches condensing temperature, become liquid, condense on the inwall of recirculatory pipe 22, under gravity along the spiral inner wall of recirculatory pipe 22 to downstream to draft tube 20.
In order to ensure that spiral condenser can trouble free service, avoid causing the problems such as explosion because internal gas pressure is excessive, the escape pipe 222 at recirculatory pipe 22 top and ft connection, when gas to be cooled enters recirculatory pipe 22 inside, the inner original air of recirculatory pipe 22 can be discharged from escape pipe 222.
Analysis module 1 in spiral condenser in this example and Fig. 1 with the use of time, the draft tube 20 of spiral condenser 2 is mated with venthole 124 and is linked together, the gas volatilized in analyzer cup 1 enters cooling in recirculatory pipe 22, liquefaction, when can not gas to be cooled be made in recirculatory pipe 22 to liquefy completely, the pipeline that the gas to be cooled arriving recirculatory pipe 22 top can be connected by escape pipe 222 arrives emission-control equipment and processes.
Cooling tube 21 and recirculatory pipe 22 all can adopt the glass of fire resistant anticorrosive to make, to produce chemical reaction between the gas avoided and carry out condensation.
In the example that another is concrete, spiral condenser 2 can specifically as shown in Figure 5.
Spiral condenser comprises: cooling tube 31, recirculatory pipe 32 and condenser pipe 33.
The tube wall 311 of cooling tube 31 is in cylindric, and inner encirclement by tube wall 11 forms columned cooling cavities 312; The tube wall 311 of side, cooling tube 31 top have liquid coolant water delivering orifice 313 and liquid coolant water inlet 314;
The tube wall 321 of recirculatory pipe 32 is in cylindric, and inner encirclement by tube wall 321 forms columned backflow cavity 322; Recirculatory pipe 32 is placed in cooling cavities 312, connects in bottom with cooling tube 31; The bottom of recirculatory pipe 32 has draft tube 20, the bottom of cooling tube 31 is connected at draft tube 20 place with the bottom of recirculatory pipe 32, the bottom of cooling cavities 312 is made to form closed structure, and backflow cavity 322 is communicated with analyzer cup by draft tube 20, thus make gas to be cooled can enter in backflow cavity 322 by draft tube 20;
Condenser pipe 33, in the shape of a spiral, be contained in backflow cavity 322, the inwall of condenser pipe 33 one end connects with the outer wall of recirculatory pipe 32, the outer wall of this end of condenser pipe 33 connects with the inwall of recirculatory pipe 32 simultaneously, and the inside of condenser pipe 33 is connected with the cooling cavities 312 outside recirculatory pipe 32; The sidewall of sidewall and cooling tube 31 that the other end of condenser pipe 33 penetrates recirculatory pipe 32 is connected with liquid coolant water inlet 314, and to connect respectively formation closed structure with the sidewall of recirculatory pipe 32 and the sidewall of cooling tube 31, make the liquid coolant entered by liquid coolant water inlet 314, be introduced in condenser pipe 33, enter in cooling cavities 312 by condenser pipe 3 again, finally discharged outside spiral condenser by liquid coolant water delivering orifice 313.
For reaching better cooling effect, one end that condenser pipe 33 is communicated with cooling cavities 312 is arranged on the bottom near recirculatory pipe 32, and liquid coolant water inlet 314 is arranged on the tip position near recirculatory pipe 32.Like this, when liquid coolant is introduced in condenser pipe 33, temperature is minimum, liquefy after making first to carry out heat interchange rapidly by the area of dissipation of the tube wall of screw type condenser pipe 33 and the minimum liquid coolant of temperature by the gas to be cooled in recirculatory pipe 32, condense on the outer wall of condenser pipe 33, under gravity along the outer wall of outer wall screw downstream to condenser pipe 33 and the inwall joint of recirculatory pipe 32 of condenser pipe 33, then along the inwall of recirculatory pipe 32 to downstream to draft tube 20.Less gas to be cooled is only had to continue to rise to the position at recirculatory pipe 32 top, and the liquid coolant that can continue through in uphill process in cooling cavities 312 contacts with the outer wall of recirculatory pipe 32, carry out heat interchange by the gas to be cooled in the tube wall of recirculatory pipe 32 and recirculatory pipe 32, thus the gas to be cooled in recirculatory pipe 32 is cooled; After gas to be cooled reaches condensing temperature, become liquid, condense on the inwall of recirculatory pipe 32, under gravity along the inwall of recirculatory pipe 32 to downstream to draft tube 20.
In order to ensure that spiral condenser can trouble free service, avoid causing the problems such as explosion because internal gas pressure is excessive, the top of recirculatory pipe 32 also has escape pipe 324.The outer wall of escape pipe 324 penetrates the outside of cooling tube 31 to spiral condenser, makes recirculatory pipe 32 at the ft connection of top and spiral condenser.When gas to be cooled enters recirculatory pipe 32 inside, the inner original air of recirculatory pipe 32 can be discharged from escape pipe 324.In addition, in digestion process, when not needing to carry out circulating collection to the residual gas to be cooled of not cooled backflow, can directly the pipeline that escape pipe 24 connects be connected in waste gas collection device, carry out nontoxic process.
The draft tube 20 of spiral condenser 2 is mated with the venthole 124 of analysis module 1 and is linked together, and the gas volatilized in analyzer cup enters in recirculatory pipe 32 and carries out cooling, liquefying, and is back to clear up in cup clears up further by draft tube 20.When can not gas to be cooled be made in recirculatory pipe 32 to liquefy completely, the pipeline that the gas to be cooled arriving recirculatory pipe 32 top can be connected by escape pipe 324 be discharged in waste gas collection device.
The analytical equipment that the embodiment of the present invention provides, structure is simple, and working stability, can make testing liquid fully clear up, and is applicable to light splitting spectrophotometric method and carries out analysis to measure accurately to testing liquid.
Professional should recognize further, in conjunction with unit and the algorithm steps of each example of embodiment disclosed herein description, can realize with electronic hardware, computer software or the combination of the two, in order to the interchangeability of hardware and software is clearly described, generally describe composition and the step of each example in the above description according to function.These functions perform with hardware or software mode actually, depend on application-specific and the design constraint of technical scheme.Professional and technical personnel can use distinct methods to realize described function to each specifically should being used for, but this realization should not thought and exceeds scope of the present invention.
The software module that the method described in conjunction with embodiment disclosed herein or the step of algorithm can use hardware, processor to perform, or the combination of the two is implemented.Software module can be placed in the storage medium of other form any known in random access memory (RAM), internal memory, ROM (read-only memory) (ROM), electrically programmable ROM, electrically erasable ROM, register, hard disk, moveable magnetic disc, CD-ROM or technical field.
Above-described embodiment; object of the present invention, technical scheme and beneficial effect are further described; be understood that; the foregoing is only the specific embodiment of the present invention; the protection domain be not intended to limit the present invention; within the spirit and principles in the present invention all, any amendment made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. the liquid analysis method that the spectrophotometric method that band is cleared up is tested, it is characterized in that, the liquid analysis method of described employing spectrophotometric method comprises:
Solution to be analyzed is added in analyzer cup;
Described solution to be analyzed is heated, described solution to be analyzed is fully cleared up;
Carry out quantitatively to the solution to be analyzed after clearing up, discharge redundance, the solution to be analyzed of residue set amount;
After leaving standstill, in particular range of wavelengths, absorbance test is carried out to the solution to be analyzed of described set amount, obtain the first absorption values ABS1;
In the solution to be analyzed of described set amount, add the titer reagent that a kind of ion pair to be determined is answered, and stir;
Add the developer that described ion pair to be determined is answered in solution after agitation, solution is developed the color;
After leaving standstill, in described particular range of wavelengths, absorbance test is carried out to the solution after stirring, obtain the second absorption values ABS2;
Calculate the difference of described second absorption values ABS2 and described first absorption values ABS1;
According to corresponding relation and the described difference of pre-set absorbance variable quantity and ion concentration, determine the concentration of ion to be determined described in described solution to be analyzed.
2. liquid analysis method according to claim 1, is characterized in that, described absorbance test comprises:
Analyze light source and send incident optical signal in particular range of wavelengths, through described analyzer cup and the solution be placed in described analyzer cup, form emergent light signal and received by photodetector;
The described emergent light signal received is converted to voltage signal by described photodetector, sends to processor;
Described processor determines corresponding absorbance parameter according to described voltage signal.
3. liquid analysis method according to claim 2, is characterized in that, before described formation emergent light signal is received by photodetector, also comprises:
Optical filter is set between described analyzer cup and described photodetector, to make described incident optical signal through described analyzer cup and the solution be placed in described analyzer cup, then after described optical filter filters, forms emergent light signal and received by photodetector.
4. liquid analysis method according to claim 1, is characterized in that, described in analyzer cup, add solution to be analyzed before, described method also comprises carries out prerinse to described analyzer cup.
5. liquid analysis method according to claim 4, is characterized in that, described prerinse comprises:
Discharge opeing is carried out to described analyzer cup;
Use cleaning liquid to inject described analyzer cup, and stir;
Described cleaning liquid is discharged described analyzer cup;
Re-use cleaning liquid and inject described analyzer cup, and stir;
Again described cleaning liquid is discharged described analyzer cup.
6. liquid analysis method according to claim 1, is characterized in that, described in analyzer cup, add solution to be analyzed before, described method also comprises:
Utilize the solution of known ion concentration to test, set up the corresponding relation of described absorbance variable quantity and ion concentration.
7. liquid analysis method according to claim 1, is characterized in that, describedly heats described solution to be analyzed, described solution to be analyzed is fully cleared up and is specially:
Described solution to be analyzed is heated and stirred, makes described solution to be analyzed all gasify as gas to be cooled;
Described gas to be cooled is cooled, is again condensed into liquid backflow in analyzer cup.
8. a liquid analysis device, in order to realize the liquid analysis method described in the claims 1, is characterized in that, described liquid analysis device comprises: analysis module and spiral condenser;
Described analysis module comprises fixed support, analyzer cup, porous plug and well heater; In described analyzer cup and the accommodating and described fixed support of described well heater, described porous plug is installed in the rim of a cup of described analyzer cup and is exposed by described support bracket fastened top, described well heater is arranged at the bottom of described analyzer cup, liquid to be analyzed in described analyzer cup is heated, make described liquid gasification to be analyzed become gas to be cooled, be expelled in spiral condenser by the venthole of described porous plug top center;
Bottom described spiral condenser, there is draft tube, be connected with described venthole is airtight, described gas to be cooled enters in described spiral condenser by described draft tube, heat interchange is carried out with cooling liquid in described spiral condenser, become the liquid to be analyzed after clearing up after described gas to be cooled being cooled reach condensing temperature, then be back in described analyzer cup by described spiral condenser;
Described analysis module also comprises analyzes light source and photodetector, and described analysis light source sends the incident light in a wavelength range, through in described analyzer cup and described analyzer cup accommodating clear up after liquid to be analyzed, become emergent light and received by photodetector; Described photodetector, according to the light intensity of described emergent light, determines the chemical substance contained by liquid accommodating in described analyzer cup and concentration.
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