CN101813704A - Automatic and quick measurement method and device of high-concentration silicate - Google Patents
Automatic and quick measurement method and device of high-concentration silicate Download PDFInfo
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Abstract
The invention discloses automatic and quick measurement method and device of high-concentration silicate, belonging to the technical field of chemical analysis and quantification and used for water quality analysis and monitoring. The method comprises the following steps of: enabling a water sample and a polymeric silicon conversation liquid to enter a premixing coil pipe in a thermostatic system under the action of a pump to convert inert silicon in the water sample into active silicon, and then entering a first sample quantifying ring; enabling a color developing agent to enter a first color developing agent quantifying ring; simultaneously, pushing the water sample in a second sample quantifying ring and the reagent in a second color developing agent quantifying ring into a reaction coil pipe respectively by two carrying currents to react, measuring the absorbency value of the product by a circulating photometric detector, and processing the actual measurement result by a recording instrument or a computer. The collection, the quantification and the measurement of the sample and the color developing agent are carried out synchronously.
Description
Technical field
The present invention relates to automatic and quick measurement method and realize the determinator of this method, belong to chemical analysis and quantitative technical field.Be applicable to the fast measuring of water mesosilicic acid salt.
Background technology
GEOTHERMAL WATER or geothermal steam are after geothermal power plant uses, waste water generally recharges underground through inverted well, owing to contain high-concentration silicate in the GEOTHERMAL WATER, in the process of recharging, along with temperature and pressure descend, liquid evaporation, cause silicate contained in the water to reach hypersaturated state, cause the silicon dirt to be separated out, and attached to recharging the borehole wall.And along with the inverted well degree of depth increases, the also increase gradually of silicon dirt thickness finally causes recharging decrease in efficiency or pipeline is scrapped, and causes enormous economic loss thus.Separate out in order to reduce the silicon dirt, method commonly used at present is the solubleness that adds alkali in the ground thermal wastewater, increase silicate, or adds acid in the ground thermal wastewater, controls its acidity (about pH 4.0) and prolongs separating out the time of silicate.Because it is cheap to add acid, the general a kind of method in back that adopts.Therefore,,, realize the accurate control of acidity, can reach the purpose that prevents that silicate from separating out on the inverted well pipeline according to the addition of silicate concentration Signal Regulation acid by measuring GEOTHERMAL WATER mesosilicic acid salt.
In addition, along with requirements of green environmental protection, country supports to develop clean energy resource energetically, and GEOTHERMAL WATER is as a kind of resource of Sustainable Development and Utilization, in industries such as generating, heating, medical treatment more and more widely application prospect is arranged.Since GEOTHERMAL WATER mesosilicic acid salinity generally at 300～700mg/L (with SiO
2Meter) (Geothermics, 2005,34:320～329), the assay method of silicate has much at present, but all is the silicate at constant in the surface water or trace, measures the upper limit less than 100mg L
-1SiO
2, far below the concentration of GEOTHERMAL WATER mesosilicic acid salt, so all can not be directly used in the on-line monitoring of GEOTHERMAL WATER mesosilicic acid salt.
There is a kind of assay method (Bunseki Kagaku, 1991,40:425～427) of total silicon in the GEOTHERMAL WATER of reporting to see Fig. 2.This system is by a ultrapure water current-carrying, a developer (R
1) stream, a triple channel synchronous valve, a sample quantitatively encircle (C
2) and two alkaline solutions quantitatively encircle (C
1), condensate decomposes coil pipe (C
3), reaction coil pipe (C
4), back pressure pipe (C
5) and spectrophotometer (D) composition.Sample quantitatively encircles (C
2) be positioned at two alkaline solutions and quantitatively encircle (C
1) the centre.When the triple channel synchronous valve is in " sampling " position, sample (S) and NaOH solution (R
2) be filled into sample respectively and quantitatively encircle (C
2) and the interior (C of the quantitative ring of alkaline solution
1), ultrapure water current-carrying and developer converge liquid as the blank value of measuring (baseline).When sample quantitatively encircles (C
2) and alkaline solution quantitatively encircle (C
1) when being full of, valve goes to " injection " position, current-carrying promotes to be entered polymer unwinds coil pipe (C by the sample plug that two alkaline solution plugs are clipped in the middle simultaneously
3) in react, colloid silicon is changed into activated silica; And then with developer (R
1) converge, reaction generates molybdenum yellow, measures the product absorbance at last at the 400nm place.
There is following shortcoming in this method: 1) be limited to 100mg L on maximum the mensuration
-1, can not be directly used in the quantitative of underground heat water sample middle and high concentration silicate, after can only diluting in advance sample, could measure; 2) be provided with the developer pipeline of a special use in the system, the reagent in this pipeline is in flow state always, and the result causes the developer consumption of this method big, has also increased the waste discharge of instrument thus, has polluted environment; 3) current-carrying liquid and reagent all will outgas in advance, have increased the system complex degree; 4) analysis speed is slow, only is 30 sample h
-15) used air bath (Ab) and water-bath (Wb) device in the system, temperature is respectively 145 ℃ and 90 ℃, causes being easy to generate bubble in the pipeline, influences the precision and the accuracy of measurement result; 6) system's internal pressure reaches 8-10kg/cm
2, must use ram pump could pump into current-carrying and reagent smoothly, instrument cost improves greatly.7) this system is to the yellow ability of not sheltering or eliminating of disturbing of phosphorus molybdenum.
Summary of the invention
The objective of the invention is to develop a kind of device that is used for the method for automatic fast measuring high-concentration silicate and realizes this method; solve the subject matter of present stage technology existence; simplify the operation course; save the reagent consumption; improve economy, be beneficial to environmental protection, accelerate analysis speed and automatization level, improve precision and accuracy; develop a kind of novel full-automatic high-concentration silicate analytical equipment on this basis, this device will be used for the water analysis and the monitoring of geothermal power plant effectively.
Technical scheme of the present invention is made up of assay method and determinator.
Measuring principle of the present invention: water sample and polymerization silicon conversion fluid at first react in the premixed coil pipe in a constant temperature system, make inertia silicon be transformed into activated silica; Then, pretreated water sample reacts with developer under acid condition again, generates molybdenum yellow; Chaff interference in the molybdenum yellow is eliminated it with oxalic acid in sheltering coil pipe, detects its absorbance with a flow type photometric detector at last, is worth the concentration of quantitative silicate according to this.
Mensuration process of the present invention: under the dynamic action of pump A, water sample by sample flow pump line, sample flow path, enter a threeway in the constant temperature system; Polymerization silicon conversion fluid converges by polymerization silicon conversion fluid pump line, polymerization silicon conversion fluid stream, the threeway and the water sample that enter in the constant temperature system, reacts in the premixed coil pipe in constant temperature system, makes inertia silicon be transformed into activated silica; Then, pretreated water sample flows into first sample from the outlet of premixed coil pipe and quantitatively encircles, and fills, quantitatively, and unnecessary water sample is discharged by the second waste discharge mouth; Simultaneously, developer by developer pump line, developer stream, enter first developer and quantitatively encircle, fill, quantitatively, unnecessary developer flows out through the second waste discharge mouth; Under the dynamic action of pump B, first via ultrapure water current-carrying by the first current-carrying liquid pump pipe, the first current-carrying liquid stream, with second sample quantitatively the water sample in the ring, through first connecting pipe, push the point a of multi-functional combination block; Another road ultrapure water current-carrying by the second current-carrying liquid pump pipe, the second current-carrying liquid stream, with second developer quantitatively the developer in the ring, through second connecting pipe, push the point a of multi-functional combination block, " sample plug " and " reagent plug " converged; Both react in the reaction coil pipe of multi-functional combination block, generate product, and the screening agent under promoting with pump B, and by screening agent pump line, screening agent stream, b converges at point, and the chaff interference in the product is sheltered in the coil pipe in interference and eliminated; At last, shelter the coil pipe outlet formula photometric detector that circulates through interference, detect the absorbance of product, the product after detected flows out from the 3rd waste discharge mouth; Measured result is by registering instrument or Computer Processing.The operation of the rotation of valve and pump, thermostat among the present invention, all available computers is controlled or is manually carried out.
Determinator of the present invention is by pump A, pump B, ultrapure water, the sample flow pump line, sample flow path, polymerization silicon conversion fluid pump line, polymerization silicon conversion fluid stream, the developer pump line, the developer stream, the first current-carrying liquid pump pipe, the first current-carrying liquid stream, the second current-carrying liquid pump pipe, the second current-carrying liquid stream, the screening agent pump line, the screening agent stream, water sample, polymerization silicon conversion fluid, developer, screening agent, constant temperature system, threeway, the premixed coil pipe, the outlet of premixed coil pipe, the first waste discharge mouth, first developer quantitatively encircles, second sample quantitatively encircles, first sample quantitatively encircles, second developer quantitatively encircles, the second waste discharge mouth, multifunction valve, first connecting pipe, second connecting pipe, point a, the reaction coil pipe, point b, coil pipe is sheltered in interference, multi-functional combination block, the coil pipe outlet is sheltered in interference, the flow type photometric detector, the 3rd waste discharge mouth, registering instrument or computing machine are formed.In the present invention, the sample flow pump line is connected with threeway in the constant temperature system by sample flow path; Polymerization silicon conversion fluid pump line is connected with threeway in the constant temperature system by polymerization silicon conversion fluid stream; Premixed coil pipe in the constant temperature system quantitatively encircles with first sample of multifunction valve by the outlet of premixed coil pipe and is connected; Another road developer pump line quantitatively encircles with first developer of multifunction valve by the developer stream and is connected; The first current-carrying liquid pump pipe quantitatively encircles by the first current-carrying liquid stream and second sample on the multifunction valve and is connected, and its outlet is connected with the reaction tray manifold chalaza a of multi-functional combination block by first connecting pipe; The second current-carrying liquid pump pipe quantitatively encircles with second developer of multifunction valve by the second current-carrying liquid stream and is connected, and its outlet is connected with the reaction tray manifold chalaza a of multi-functional combination block by second connecting pipe; The screening agent pump line passes through the screening agent stream, is connected with the outlet of reaction coil pipe at the point b of multi-functional combination block, and its outlet is sheltered coil pipe with interference and is connected; Interference is sheltered the coil pipe outlet and is connected with the flow type photometric detector; Measured result is by registering instrument or Computer Processing, the operation of the rotation of valve and pump, thermostat among the present invention, available computers control.
In the determinator of the present invention, each ingredient architectural feature is as follows:
Sample and developer are injected in the current-carrying simultaneously in the mode of " sample plug " and " developer plug " respectively, enter pipeline point b then, react in the reaction coil pipe.When second sample quantitatively ring and second developer when quantitatively ring is positioned at " injections " state, simultaneously, first sample quantitatively ring and first developer quantitatively ring be in " filling quantitative " state, realization samples, adopt developer and water determination carries out synchronously.
At a certain temperature, in the premixed coil pipe, water sample continuously converges, react with polymerization silicon conversion fluid, makes inertia silicon wherein be transformed into activated silica, realization high concentration total silicon quantitative.
The flow type photometric detector can carry out the mensuration of high-concentration silicate in the 350nm-450nm wavelength coverage.
Screening agent in the stream replaces with the mixed liquor of screening agent and reductive agent, in the 650nm-820nm wavelength coverage, adopts the blue method of molybdenum can carry out the mensuration of low silicon hydrochlorate.Polymerization silicon conversion fluid is a strong alkali solution, and screening agent is the reagent that is used for sheltering the water sample interfering material, and reductive agent is meant the reducing substances that can be mixed with screening agent.
The quantitative ring of first sample and first developer are quantitatively encircled with two identical physical dimension tubules replacements, become second sample quantitatively ring and the quantitative shunt valve that encircles of second developer, again first connecting pipe and second connecting pipe are changed into the tubule of two samples different in size, make the reagent of injected system arrive pipeline point a earlier, form the pattern of " developer " parcel " sample "; When " the alkaline sample plug " of small size by " the acid developer plug " of large volume when wrapping up fully, sample and developer could mix well, reaction product just can reach at most, the influence of the acidity gradient at reaction zone band two ends just can drop to minimum.
After polymerization silicon conversion fluid pump line, polymerization silicon conversion fluid stream and the removal of premixed coil pipe, do not use polymerization silicon conversion fluid, the direct sample liquid stream is quantitatively encircled with first sample of multifunction valve is connected, and is used for the direct quantitative of high concentration activated silica.
Flow cell light path in the flow type photometric detector is 0.5cm-2cm; When if the phosphatic concentration of chaff interference is less than 10mg/L in the water sample, pump line in screening agent, the screening agent stream and interference can be sheltered the coil pipe removal, directly measure.
The sample quantitatively volume of ring is that the volume that 10-100 μ L, developer quantitatively encircle is 100-600 μ L, all can realize the mensuration of high concentration total silicon.
Basic fundamental parameter of the present invention is: measurement range: 20～800mg/L SiO
2Relative standard deviation RSD＜1.5%; Linearly dependent coefficient r＞0.9990; Analysis speed 60 samples/h.
Advantage of the present invention and good effect are: the range of linearity is wide, easy and simple to handle, finding speed fast, favorable reproducibility; After device energising of the present invention is stable, directly the sample ingress pipe is inserted in the water sample, need not any other operation, just can be implemented in the line monitoring.Quantitative and the injection of sample, the quantitative and injection of developer, the conversion of inertia silicon, the reaction of molybdenum yellow, the elimination of interference, the cleaning of stream, the mensuration of product etc. is to carry out automatically entirely.Thus, the present invention is a kind of new assay method, full-automatic high-concentration silicate analytical approach and device fast of comprising.Of the present inventionly specificly be:
A) direct-on-line of high-concentration silicate is monitored automatically, has eliminated the prediluted step of sample, has reduced manual steps;
B) with polymerization silicon conversion fluid sample is carried out online treatment in advance, avoided separating out of silicon dirt in the mensuration system;
C) the online activated silica that is converted into of inertia silicon in the water sample has been realized total silicon mensuration;
D) design interference and sheltered pipeline, realized the online elimination of disturbing;
E) fast (60-180 sample/h), favorable reproducibility (RSD＜1.5%) of analysis speed of the present invention.
F) reagent consumption of the present invention only is 120 μ L/ time, and current-carrying flow also little (only being 2.0ml/min) greatly reduces testing cost, helps environmental protection.
G) wide (20～800mg/L SiO of the range of linearity
2), can be used for the quantitative of the interior water sample mesosilicic acid salt of variable concentrations scope.
The present invention is applicable to the mensuration of all aqueous phase silicate; Related scientific domain has multiple subjects such as chemical instruments, analytical chemistry, is the synthetic study achievement of cross discipline, has very important use meaning and social value.
Description of drawings
The automatic fast measuring device of Fig. 1 high-concentration silicate synoptic diagram
(1) pump A among the figure, (2) pump B, (3) ultrapure water, (4) sample flow pump line, (4a) sample flow path, (5) polymerization silicon conversion fluid pump line, (5a) polymerization silicon conversion fluid stream, (6) developer pump line, (6a) developer stream, (7) first current-carrying liquid pump pipes, (7a) the first current-carrying liquid stream, (8) second current-carrying liquid pump pipes, (8a) the second current-carrying liquid stream, (9) screening agent pump line, (9a) screening agent stream, (10) water sample, (11) polymerization silicon conversion fluid, (12) developer, (13) screening agent, (14) constant temperature system, (15) threeway, (16) premixed coil pipe, (17) premixed coil pipe outlet, (18) first waste discharge mouths, (19) first developers quantitatively encircle, (20) second samples quantitatively encircle, (21) first samples quantitatively encircle, (22) second developers quantitatively encircle, (23) second waste discharge mouths, (24) multifunction valve, (25) first connecting pipes, (26) second connecting pipes, (27) point a, (28) reaction coil pipe, (29) point b, (30) coil pipe is sheltered in interference, (31) multi-functional combination block, (32) the coil pipe outlet is sheltered in interference, (33) flow type photometric detector, (34) registering instrument, (35) the 3rd waste discharge mouths, (36) computing machine.
Total silicon device synoptic diagram in Fig. 2 flow injection spectrophotometry GEOTHERMAL WATER
P among the figure
1Pump, P
2Pump, R
1Developer, R
2NaOH solution, S sample, Ab air bath, Wb water-bath, C
1Alkaline solution quantitatively encircles, C
2Sample quantitatively encircles, C
3Condensate decomposes coil pipe, C
4Reaction coil pipe, D detecting device, C
5Back pressure pipe, W waste discharge mouth.
Fig. 3 embodiment 1 high-concentration silicate canonical plotting
Fig. 4 embodiment 1 high-concentration silicate physical record curve map
Fig. 5 embodiment 2 developer volumes are to the curve map of sensitivity influence
Fig. 6 embodiment 3 chromogenic agents are to the curve map of sensitivity influence
Fig. 7 embodiment 4 developer acidity are to the curve map of sensitivity influence
Fig. 8 embodiment 5 premixed coil lengths are to the curve map of sensitivity influence
Fig. 9 embodiment 6 disturbs the curve map of masking disk length of tube to the sensitivity influence
Figure 10 embodiment 7 screening agent concentration are disturbed the curve map of removing influence to phosphate
Embodiment
In conjunction with the accompanying drawings embodiments of the invention are further described:
Embodiment 1
Utilize method of the present invention and device (see figure 1) that six GEOTHERMAL WATER mesosilicic acid salt are measured.Experiment condition: polymerization silicon conversion fluid (11) is that 0.1mol/L NaOH, developer (12) are that 2% ammonium molybdate (w/v) (containing the 10ml/L concentrated sulphuric acid), screening agent (13) are that 1% oxalic acid (w/v) (containing the 2ml/L concentrated sulphuric acid), current-carrying liquid (3) are pure water; Premixed coil pipe (16) has used long 350cm, the polyfluortetraethylene pipe of internal diameter 0.5mm; Reaction coil pipe (28) has used long 160cm, the polyfluortetraethylene pipe of internal diameter 0.5mm; Interference is sheltered coil pipe (30) and has been used long 300cm, the polyfluortetraethylene pipe of internal diameter 0.5mm; Function combinations piece (31) has used the organic glass material to make; Flow type photometric detector (33) is a spectrophotometer; Registering instrument (34) is KH 200 type recording instrument without paper.
The silicate typical curve that the obtains (range of linearity: 25～800mg/L SiO
2) as shown in Figure 3, wherein the measured curve of silicon titer as shown in Figure 4.Determination data and recovery of standard addition experiment to six GEOTHERMAL WATER mesosilicic acid salt are as shown in table 1.As can be seen, relative standard deviation (RSD)＜1.5%; The recovery is between 88.9-109.2%; As seen the present invention's requirement of hot water middle and high concentration silicate mensuration fully contentedly.
Table 1 underground heat water sample mesosilicic acid salt measurement result and standard are added recovery experiment *
* recovery experiment is that isopyknic water sample and silicon titer are mixed
When the a:FIA standard addition method was measured, water sample adopted in advance and contains 0.1M Na
2CO
3Handle at 1: 1 with the mixed liquor of 0.5mol/L NaOH, remove portion C a
2+, Mg
2+, preventing to add timestamp has precipitation to generate
Present embodiment is at room temperature to investigate with the Standard Solution of Silicate of variable concentrations respectively to adopt the influence of reagent volume to sensitivity.As can be seen from Figure 5, along with the increase of adopting reagent volume, sensitivity increases gradually; When sampling volume during greater than 115 μ L, the increase of absorbance tends to be steady.
Embodiment 3
Present embodiment is at room temperature to investigate the influence of chromogenic agent to sensitivity.As can be seen from Figure 6, along with the increase of ammonium molybdate concentration, the absorbance of variable concentrations silicon mark liquid increases gradually; When ammonium molybdate concentration greater than 2% the time, absorbance changes slowly.
Present embodiment is at room temperature to investigate the influence of developer acidity to sensitivity.As can be seen from Figure 7, along with the increase of sulfuric acid content in the developer, absorbance increases afterwards earlier and reduces, and contains 10ml L in ammonium molybdate reagent
-1During the concentrated sulphuric acid, the absorbance maximum.
Present embodiment is to investigate the premixed coil lengths is converted into activated silica to inertia silicon influence.As can be seen from Figure 8, along with RC
1The increase of length, the absorbance of actual water sample also increase gradually, work as RC
1Length is during greater than 350cm, and the absorbance of water sample tends towards stability.That is, show that abundant reaction has taken place for polymerization silicate contained in NaOH solution and the GEOTHERMAL WATER or non-solubility silicate, generated molybdenum yellow reactive activity silicon can take place.
Present embodiment is to investigate to disturb the influence of masking disk length of tube to the phosphate interference eliminated.As can be seen from Figure 9, when disturbing the masking disk length of tube greater than 300cm, the phosphate of 100mg/L can well be eliminated.
Embodiment 7
Present embodiment is to investigate the influence of concentration of oxalic acid to the phosphate interference eliminated.As can be seen from Figure 10, along with the increase of concentration of oxalic acid, the absorbance that contains the phosphatic silicon standard solution of 100mg/L reduces gradually, when concentration of oxalic acid greater than 0.5% the time, absorbance tends to be steady, and can reach to eliminate the purpose that phosphate disturbs fully.
Claims (10)
1. automatic and quick measurement method is characterized in that: under the dynamic action of pump A (1), water sample (10) by sample flow pump line (4), sample flow path (4a), enter the threeway (15) in the constant temperature system (14); Polymerization silicon conversion fluid (11) by polymerization silicon conversion fluid pump line (5), polymerization silicon conversion fluid stream (5a), enter the threeway (15) in the constant temperature system (14), after water sample and polymerization silicon conversion fluid (11) converge, fully react premixed coil pipe (16) lining in constant temperature system (14), enters through premixed coil pipe outlet (17) that first sample quantitatively encircles (21), unnecessary pre-service water sample is flowed out by the second waste discharge mouth (23); Developer (12) by developer pump line (6), developer stream (6a), enter first developer and quantitatively encircle (19), unnecessary developer flows out through the first waste discharge mouth (18); Simultaneously, under the dynamic action of pump B (2), one road ultrapure water (3) by the first current-carrying liquid pump pipe (7), the first current-carrying liquid stream (7a), with second sample quantitatively encircle sample in (20), through first connecting pipe (25), push the pipeline point a (27) of multi-functional combination block (31); Another road ultrapure water (3) is by the second current-carrying liquid pump pipe (8), the second current-carrying liquid stream (8a), second developer is quantitatively encircled developer in (22), through second connecting pipe (26), push the pipeline point a (27) of multi-functional combination block (31), after " sample plug " and " reagent plug " converges, in the reaction coil pipe (28) of multi-functional combination block (31), react, generate the screening agent (13) under product and pump B (2) promotion, by screening agent pump line (9), screening agent stream (9a), converge at pipeline point b (29), interference is sheltered in the coil pipe (30) in interference and is eliminated, at last, shelter coil pipe outlet (32) the formula photometric detector (33) that circulates through interference, measure the product absorbance, measured curve is by registering instrument (34) record, computing machine (36) is according to the linear equation that stores, the output measurement result, and the rotation of autocontrol valve and pump, the operation of constant temperature system is flowed out from the 3rd waste discharge mouth (35) at last.
2. the automatic fast measuring device of high-concentration silicate is characterized in that: by pump A (1), pump B (2), ultrapure water (3), sample flow pump line (4), sample flow path (4a), polymerization silicon conversion fluid pump line (5), polymerization silicon conversion fluid stream (5a), developer pump line (6), developer stream (6a), the first current-carrying liquid pump pipe (7), the first current-carrying liquid stream (7a), the second current-carrying liquid pump pipe (8), the second current-carrying liquid stream (8a), screening agent pump line (9), screening agent stream (9a), water sample (10), polymerization silicon conversion fluid (11), developer (12), screening agent (13), constant temperature system (14), threeway (15), premixed coil pipe (16), premixed coil pipe outlet (17), the first waste discharge mouth (18), first developer quantitatively encircles (19), second sample quantitatively encircles (20), first sample quantitatively encircles (21), second developer quantitatively encircles (22), the second waste discharge mouth (23), multifunction valve (24), first connecting pipe (25), second connecting pipe (26), pipeline point a (27), reaction coil pipe (28), pipeline point b (29), coil pipe (30) is sheltered in interference, multi-functional combination block (31), coil pipe outlet (32) is sheltered in interference, flow type photometric detector (33), registering instrument (34), the 3rd waste discharge mouth (35), computing machine (36) is formed.
In the present invention, sample flow pump line (4) is connected with threeway (15) in the constant temperature system (14) by sample flow path (4a); Polymerization silicon conversion fluid pump line (5) is connected with threeway (15) in the constant temperature system (14) by polymerization silicon conversion fluid stream (5a); Premixed coil pipe (16) in the constant temperature system (14) quantitatively encircles (21) by premixed coil pipe outlet (17) with first sample of multifunction valve (24) and is connected; Another road developer pump line (6) quantitatively encircles (19) by developer stream (6a) with first developer of multifunction valve (24) and is connected; The first current-carrying liquid pump pipe (7) quantitatively encircles (20) by the first current-carrying liquid stream (7a) and second sample on the multifunction valve (24) and is connected, and its outlet is connected with reaction coil pipe (28) the point a (27) of multi-functional combination block (31) by first connecting pipe (25); The second current-carrying liquid pump pipe (8) quantitatively encircles (22) by the second current-carrying liquid stream (8a) with second developer of multifunction valve (24) and is connected, and its outlet is connected with reaction coil pipe (28) the point a (27) of multi-functional combination block (31) by second connecting pipe (26); Screening agent pump line (9) passes through screening agent stream (9a), is connected with the outlet of reaction coil pipe (28) at the point b (29) of multi-functional combination block (31), and its outlet is sheltered coil pipe (30) with interference and is connected; Interference is sheltered coil pipe outlet (32) and is connected with flow type photometric detector (33); Measured result is handled by registering instrument (34) or computing machine (36), the operation of the rotation of valve and pump, thermostat among the present invention, available computers (36) control.
3. automatic and quick measurement method as claimed in claim 1, it is characterized in that: sample and reagent inject current-carrying simultaneously in the mode of " sample plug " and " reagent plug " respectively, enter pipeline point b then, in the reaction coil pipe, react.When a pair of sample quantitatively encircles (20) and developer when quantitatively encircling (22) and being positioned at " injection " state, simultaneously, another quantitatively encircles (21) to sample and developer quantitatively encircles (19) and is in " fill quantitatively " state, realizes sampling, adopts reagent and water determination carries out synchronously.
4. automatic and quick measurement method as claimed in claim 1, it is characterized in that: under a constant temperature, in premixed coil pipe (16), water sample (10) continuously and polymerization silicon conversion fluid (11) converge, react, make inertia silicon wherein be transformed into activated silica, realize the quantitative of high concentration total silicon.
5. automatic and quick measurement method as claimed in claim 1 is characterized in that: the wavelength of flow type photometric detector (33) can carry out the mensuration of high-concentration silicate in the 350-450nm scope; Wavelength is in the 650nm-820nm scope, and the screening agent in the stream (13) replaces with the mixed liquor of screening agent and reductive agent, adopts the blue method of molybdenum can carry out the mensuration of low silicon hydrochlorate.
6. reagent as claimed in claim 5 is characterised in that: polymerization silicon conversion fluid is a strong alkali solution, and screening agent is the reagent that is used for sheltering the water sample interfering material, and reductive agent is meant the reducing substances that can be mixed with screening agent.
7. the automatic fast measuring device of high-concentration silicate as claimed in claim 2, it is characterized in that: first sample is quantitatively encircled (20) and first developer quantitatively encircle (22) and replace with two identical physical dimension tubules, become second sample and quantitatively encircle the shunt valve that (20) and second developer quantitatively encircle (22), again first connecting pipe (25) and second connecting pipe (26) are changed into the tubule of two samples different in size, make the reagent of injected system arrive pipeline point a (27) earlier, form the pattern of " reagent " parcel " sample ".
8. the automatic fast measuring device of high-concentration silicate as claimed in claim 2, it is characterized in that: after polymerization silicon conversion fluid pump line (5), polymerization silicon conversion fluid stream (5a) and premixed coil pipe (16) are removed, do not use polymerization silicon conversion fluid (11), directly sample liquid stream (4a) is quantitatively encircled (21) with first sample of multifunction valve (24) and be connected, be used for the direct quantitative of high concentration activated silica.
9. the automatic fast measuring device of high-concentration silicate as claimed in claim 2 is characterized in that: the light path of flow type cuvette is 0.5cm-2cm in the flow type photometric detector (33); When if the phosphatic concentration of chaff interference is less than 10mg/L in the water sample, pump line (9) in screening agent (13), the screening agent stream (9a) and interference can be sheltered coil pipe (30) removal, directly measure.
10. the automatic fast measuring device of high-concentration silicate as claimed in claim 2 is characterized in that: the sample quantitatively volume of ring is that the volume that 10-100 μ L, developer quantitatively encircle is 100-600 μ L.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN108802026A (en) * | 2018-06-19 | 2018-11-13 | 四川大学 | Peroxidase activity and ascorbic acid automatic measuring method and device simultaneously |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105041586A (en) * | 2015-07-23 | 2015-11-11 | 中国科学院广州能源研究所 | Geothermal power generation device and real-time monitoring system thereof |
| CN105041586B (en) * | 2015-07-23 | 2018-02-06 | 中国科学院广州能源研究所 | Geothermal power generation plant and its real-time monitoring system |
| CN110160962A (en) * | 2018-02-16 | 2019-08-23 | 恩德莱斯和豪瑟尔分析仪表两合公司 | Determine the analytical equipment for indicating the measured variable of silicate concentration in sample liquid |
| US11293874B2 (en) | 2018-02-16 | 2022-04-05 | Endress+Hauser Conducta Gmbh+Co. Kg | Analysis device for determining a measurand representing a silicate concentration in a sample liquid |
| CN110160962B (en) * | 2018-02-16 | 2022-10-25 | 恩德莱斯和豪瑟尔分析仪表两合公司 | Analysis device for determining a measured variable representing the concentration of silicate in a sample liquid |
| CN110294481A (en) * | 2018-03-22 | 2019-10-01 | 丰海（盘锦）水稻生物科技有限公司 | Biomass white carbon black and its preparation method and application |
| CN110294481B (en) * | 2018-03-22 | 2021-04-20 | 丰海（盘锦）水稻生物科技有限公司 | Biomass white carbon black and preparation method and application thereof |
| CN108802026A (en) * | 2018-06-19 | 2018-11-13 | 四川大学 | Peroxidase activity and ascorbic acid automatic measuring method and device simultaneously |
| CN110514610A (en) * | 2019-09-30 | 2019-11-29 | 南京润驰工程技术有限公司 | A kind of silicate measurement device and measurement method |
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