CN113899735A - Automatic determination system and method for water-soluble hexavalent chromium in cement - Google Patents
Automatic determination system and method for water-soluble hexavalent chromium in cement Download PDFInfo
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- CN113899735A CN113899735A CN202111414437.6A CN202111414437A CN113899735A CN 113899735 A CN113899735 A CN 113899735A CN 202111414437 A CN202111414437 A CN 202111414437A CN 113899735 A CN113899735 A CN 113899735A
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- 239000004568 cement Substances 0.000 title claims abstract description 35
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000001514 detection method Methods 0.000 claims abstract description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 65
- 239000012153 distilled water Substances 0.000 claims abstract description 47
- 230000007246 mechanism Effects 0.000 claims abstract description 25
- 239000000243 solution Substances 0.000 claims description 61
- 239000007788 liquid Substances 0.000 claims description 32
- 239000002699 waste material Substances 0.000 claims description 25
- 238000002156 mixing Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 5
- 230000008676 import Effects 0.000 claims description 3
- 239000012528 membrane Substances 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 13
- 238000010521 absorption reaction Methods 0.000 description 7
- 238000011161 development Methods 0.000 description 7
- 238000005259 measurement Methods 0.000 description 6
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 5
- 229910052804 chromium Inorganic materials 0.000 description 5
- 239000011651 chromium Substances 0.000 description 5
- 238000009434 installation Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- WURBFLDFSFBTLW-UHFFFAOYSA-N benzil Chemical group C=1C=CC=CC=1C(=O)C(=O)C1=CC=CC=C1 WURBFLDFSFBTLW-UHFFFAOYSA-N 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000011083 cement mortar Substances 0.000 description 2
- 239000012916 chromogenic reagent Substances 0.000 description 2
- 238000000227 grinding Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- ZFWAHZCOKGWUIT-UHFFFAOYSA-N 1-anilino-3-phenyliminourea Chemical compound C=1C=CC=CC=1N=NC(=O)NNC1=CC=CC=C1 ZFWAHZCOKGWUIT-UHFFFAOYSA-N 0.000 description 1
- 235000019738 Limestone Nutrition 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical group C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical class [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000012864 cross contamination Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 238000001471 micro-filtration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/27—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands using photo-electric detection ; circuits for computing concentration
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
- G01N21/80—Indicating pH value
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Abstract
The invention relates to an automatic measuring system and method for water-soluble hexavalent chromium in cement, which comprises a distilled water tank, wherein a water outlet pipe of the distilled water tank is provided with a first control valve, the first control valve is respectively connected with inlets of a first mixer and a second mixer, an inlet of the second mixer is also respectively connected with a first reagent supply mechanism and a second reagent supply mechanism, an inlet of the second mixer is connected with the first mixer through a first pump body, a pH value detection element is arranged in the second mixer, an outlet of the second mixer is connected with an inlet of a detection container through a second control valve, and the periphery of the detection container is provided with a photoelectric detection device capable of performing photoelectric detection on solution in the detection container.
Description
Technical Field
The invention relates to the technical field of cement experimental equipment, in particular to an automatic measuring system and method for water-soluble hexavalent chromium in cement.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
The cement raw material such as marl or limestone, clay, iron ore, etc. often contains trace chromium, and the broken raw material, raw material and grinding body of cement can be introduced into cement due to chromium-containing broken and grinding medium abrasion.
Water-soluble chromium, typically as chromium in chromates or dichromates, of 3+And 6+Two valence states exist, wherein the toxicity of hexavalent chromium is strong, and once soil or underground water is polluted by chromium, serious consequences that the soil cannot be cultivated and the underground water cannot be drunk are caused, so that the water-soluble hexavalent chromium in the cement needs to be measured.
The existing method for measuring the water-soluble hexavalent chromium in the cement is carried out by referring to a method in a standard, and the currently published patent application CN110118869A describes a measuring method, so that the problem of complex operation of the existing measuring method is solved, but the inventor finds that the method still needs measuring steps of manual preparation of cement mortar, manual suction filtration, solution color development and the like, and has the disadvantages of complex operation, high labor intensity and low measuring precision.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides an automatic measuring system for water-soluble hexavalent chromium in cement, which can realize the automatic measurement of the water-soluble hexavalent chromium in the cement, reduce the labor intensity and improve the measuring precision.
In order to achieve the purpose, the invention adopts the following technical scheme
In a first aspect, an embodiment of the present invention provides an automatic determination system for water-soluble hexavalent chromium in cement, including a distilled water tank, a first control valve is installed on a water outlet pipe of the distilled water tank, the first control valve is respectively connected with inlets of a first mixer and a second mixer, an inlet of the second mixer is further respectively connected with a first reagent supply mechanism and a second reagent supply mechanism, an inlet of the second mixer is connected with the first mixer through a first pump body, a pH detection element is installed in the second mixer, an outlet of the second mixer is connected with an inlet of a detection container through a second control valve, and a photoelectric detection device capable of performing photoelectric detection on a solution inside the detection container is installed on the periphery of the detection container.
Optionally, a second pump body is mounted on a pipeline between the first control valve and the first mixer.
Optionally, a filter element is mounted on a pipeline between the outlet of the first mixer and the inlet of the second mixer.
Optionally, the filter element is an aqueous microporous filter membrane.
Optionally, the first reagent supply mechanism comprises a first reagent tank installed at a height higher than the inlet of the second mixer, and the outlet of the first reagent tank is connected with the inlet of the second mixer through a third control valve.
Optionally, the second reagent supply mechanism comprises a second reagent tank installed at a height higher than the inlet of the second mixer, and the outlet of the second reagent tank is connected with the inlet of the second mixer through a fourth control valve.
Optionally, a constant volume detection element is installed at the end of the pipeline between the distilled water tank and the second mixer, which extends into the second mixer, and is used for detecting the liquid level information of the solution in the second mixer.
Optionally, the waste liquid outlet of the first mixer is connected to a first waste liquid tank through a fifth control valve.
Optionally, the waste liquid outlet of the detection container is connected to a second waste liquid tank through a sixth control valve.
In a second aspect, an embodiment of the present invention provides an operating method of the automatic measuring system for water-soluble hexavalent chromium in cement according to the first aspect, wherein a distilled water tank injects a first set amount of distilled water into a first mixer through a first control valve, the first mixer mixes a cement sample pre-placed in the first mixer with water, after a set time of mixing, a first pump pumps a second set amount of mixed solution into a second mixer, a first reagent supply mechanism adds a third set amount of chromogenic reagent into the second mixer, a second reagent supply mechanism adds a fourth set amount of pH adjusting reagent into the second mixer until a pH detecting element detects that a pH of the solution reaches a set value, the first control valve controls the distilled water tank to add distilled water into the second mixer until a water level of the solution in the second mixer reaches a set water level value, and the second control valve controls the distilled water tank to add distilled water into the second mixer, and (4) sending the solution which is well developed in the second mixer into a detection container, and carrying out photoelectric detection on the solution in the detection container by using a photoelectric detection device to obtain a hexavalent chromium concentration value.
The invention has the beneficial effects that:
1. the system provided by the invention is provided with the parts such as the distilled water tank, the first mixer, the first pump body, the second mixer, the detection container, the corresponding control valve, the two reagent supply mechanisms and the like, can realize the automatic mixing of the cement sample and the distilled water, automatically enters the second mixer through the first pump body to adjust the pH value and develop color, can utilize the control valve to enable the solution after the color development is finished to enter the detection container, and utilizes the photoelectric detection device to carry out photoelectric detection, the whole process is automatically carried out, the measurement steps such as manual preparation of cement mortar, manual suction filtration, solution color development and the like are not needed, the operation is simple and rapid, the automation degree is high, the experiment efficiency is improved, and the labor intensity is reduced.
2. In the system, the first reagent supply mechanism and the second reagent supply mechanism are both provided with control valves, the second mixer is internally provided with a pH value detection element, so that the solution in the second mixer can reach the set pH value accurately, and in addition, the end part of the pipeline between the first control valve and the second mixer, which extends into the second mixing device, is provided with a constant volume detection element, so that the distilled water volume of the solution can be continuously added after the pH value is adjusted accurately, and the subsequent measurement result is more accurate.
3. According to the system, the first mixer and the detection container are connected with the waste liquid tank, so that waste liquid after a test can be recovered in a centralized manner, centralized treatment is facilitated, and the pollution to the surrounding external environment is avoided.
4. According to the system, the filtering element is arranged between the outlet of the first mixer and the inlet of the second mixer, so that the solution entering the second mixer can be filtered, and the influence of impurities on the subsequent measurement result is prevented.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
FIG. 1 is a schematic view of the overall structure of embodiment 1 of the present invention;
the system comprises a distilled water tank 1, a first mixer 2, a second mixer 3, a detection container 4, a first electromagnetic valve 5, a second metering pump 6, a constant volume detection element 7, a first magnetic stirrer 8, a second magnetic stirrer 9, a first metering pump 10, a filter element 11, a first reagent box 12, a third electromagnetic valve 13, a second reagent box 14, a fourth electromagnetic valve 15, a pH value sensor 16, a second electromagnetic valve 17, a first waste liquid box 18, a fifth electromagnetic valve 19, a second waste liquid box 20, a sixth electromagnetic valve 21 and a photoelectric detection device 22.
Detailed Description
Example 1
The present embodiment provides an automatic measuring system for water-soluble hexavalent chromium in cement, as shown in fig. 1, which includes a distilled water tank 1, a first mixer 2, a second mixer 3, a detection container 4, a first reagent supply mechanism, a second reagent supply mechanism, and a photoelectric detection device 22.
Distilled water in the distilled water tank 1 can enter the first mixer 2 and is mixed with a cement sample which is placed in the first mixer 2 in advance to form a solution, the mixed solution in the first mixer 2 enters the second mixer 3, a chromogenic reagent is added into the second mixer 3 by using the first reagent supply mechanism, a pH value adjusting reagent is added into the second mixer 3 by using the second reagent supply mechanism, when the pH value of the solution in the second mixer 3 reaches a set pH value, distilled water is added into the second mixer 3 through the distilled water tank 1 until the water level reaches the set water level value, then the developed solution is sent into the detection container 4 by the second mixer 3, and the photoelectric detection device 22 performs photoelectric detection on the solution in the detection container 4 to further obtain the concentration of hexavalent chromium.
The specific connection relationship of each device in this embodiment is as follows:
the distilled water tank 1 is used for containing distilled water, the distilled water tank 1 is provided with an outlet, a first control valve is installed at the outlet, in order to realize automatic control of the first control valve, the first control valve adopts a first electromagnetic valve 5, is connected with a control system and can receive an instruction of the control system to work.
The first solenoid valve 5 has two outlets, one of which is connected to the inlet of the first mixer 2 via a line.
In one embodiment, the height of the inlet of the first mixer 2 is less than the height of the outlet of the first electromagnetic valve 5, so that the distilled water can flow into the first mixer 2 by gravity, but it is inconvenient to control the entering amount of the distilled water, therefore, in this embodiment, a second pump body is installed on the pipeline between the first electromagnetic valve 5 and the first mixer 2, preferably, the second pump body adopts a second metering pump 6, the second metering pump 6 is connected with a control system, and can receive the instruction of the control system to work, the second metering pump 6 can pump the distilled water in the distilled water tank 1 into the first mixer 2, and accurately control the amount of the distilled water pumped into the first mixer 2.
The other outlet of the first electromagnetic valve 5 is connected with the second inlet of the second mixer 3 through a pipeline, and the installation height of the second mixer 3 is less than that of the outlet of the first electromagnetic valve 5, so that the distilled water can flow into the second mixer 3 under the action of gravity.
Pipeline between first solenoid valve 5 and the second blender 3 stretches into the tip of second blender and installs constant volume detecting element 7, preferred, constant volume detecting element adopts level sensor, and level sensor is used for detecting the liquid level information of solution in the second blender 3, consequently can control the distilled water yield of adding second blender 3, consequently need not to install the measuring pump on the pipeline between first solenoid valve 5 and second blender 3.
The export of first blender 2 passes through the first access connection of pipeline and second blender 3, and the solution in the first blender 2 can get into second blender 3, for the convenience control the solution volume that gets into second blender 2, install the first pump body, preferred on the pipeline between the export of first blender 2 and the 3 import of second blender, first pump body adopts first measuring pump 10, first measuring pump 10 is connected with control system, can receive control system's instruction work.
Further, in order to filter the solution entering the second mixer 3 and prevent impurities from entering the second mixer to affect the subsequent measurement effect, a filtering element 11 is installed on the pipeline between the first metering pump and the first mixer and used for filtering the impurities.
Preferably, the filter element 11 is an aqueous microfiltration membrane with a pore size of 0.4 μm to 0.5 μm, preferably 0.45 μm, which is a consumable and needs to be replaced after each use.
The third inlet of the second mixer 3 is connected to the first reagent supply means and the fourth inlet of the second mixer 3 is connected to the second reagent supply means.
The first reagent supply mechanism is used for adding a color reagent into the second mixer 3, in the embodiment, the color reagent adopts diphenylcarbazone color development solution, the second reagent supply mechanism is used for adding a pH value adjusting reagent into the second mixer 3, and in the embodiment, the pH value adjusting reagent adopts 1.0mol/L hydrochloric acid solution.
The first reagent supply mechanism comprises a first reagent box 12, the first reagent box 12 is used for containing dibenzoyl dihydrazide color development solution, the installation height of the first reagent box 12 is higher than the height of the inlet of the second mixer 3, the outlet of the first reagent box 12 is connected with the third inlet of the second mixer 3 through a pipeline, a third control valve is installed on the pipeline between the outlet of the first reagent box 12 and the third inlet of the second mixer 3, preferably, the third control valve adopts a third electromagnetic valve 13, and the third electromagnetic valve 13 is connected with a control system and can receive the instruction of the control system for operation. First reagent case 12 is detachable mode, and is preferred, adopts the bolt to be connected rather than supporting the support body, because of the developer has 7 days validity periods, convenient manual empting after the experiment finishes.
The second reagent supply mechanism comprises a second reagent box 14, the second reagent box 14 is used for containing hydrochloric acid solution, the installation height of the second reagent box 14 is higher than the height of the inlet of the second mixer 3, the outlet of the second reagent box 14 is connected with the fourth inlet of the second mixer 3 through a pipeline, a fourth control valve is installed on the pipeline between the outlet of the second reagent box 14 and the fourth inlet of the second mixer 3, preferably, the fourth control valve adopts a fourth electromagnetic valve 15, and the fourth electromagnetic valve 15 is connected with a control system and can receive the instruction of the control system to work. The second reagent box 14 is detachable, preferably, the second reagent box is detachably fixed on a support frame of the second reagent box by bolts, so that the second reagent box can be conveniently cleaned when the hydrochloric acid solution is replaced. The fourth electromagnetic valve 15 is used for controlling micro-slow dripping so as to achieve accurate pH adjustment.
The mixing container internally mounted of second blender 3 has pH value detecting element, pH value detecting element adopts pH value sensor 16, pH value sensor 16 is connected with control system, can transmit the solution pH value that obtains to control system, and when solution reached the pH value of settlement, control system can send the instruction to fourth solenoid valve 15, controls fourth solenoid valve 15 and closes.
The outlet of the second mixer 3 is connected with the inlet of the detection container 4 through a pipeline, in this embodiment, the outlet height of the second mixer 3 is greater than the inlet height of the detection container 4, so that the solution in the second mixer 3 can flow into the detection container 4 through gravity, a second control valve is installed on the pipeline between the second mixer 3 and the detection container 4, the second control valve is used for controlling the connection and the closing of the pipeline between the second mixer and the detection container, preferably, the second control valve adopts a second electromagnetic valve 17, and the second electromagnetic valve 17 is connected with a control system and can receive the instruction of the control system to work.
The periphery of detection container 4 is provided with photoelectric detection device 22, photoelectric detection device 22 adopt current photoelectric detection equipment can, photoelectric detection device 5 can carry out photoelectric detection to the solution of detection container 4 inside to survey hexavalent chromium's concentration.
In this embodiment, the detection container is an absorption cell that can satisfy the quartz material of light transmissivity or the glass material, and in order to prevent the influence of external environment light, the absorption cell is installed inside an opaque box, and monochromator and halogen tungsten lamp are installed to absorption cell periphery one side, and the light that the halogen tungsten lamp sent can utilize the monochromator to separate, the monochromator adopts the light filter, and the installation of absorption cell opposite side is detector and signal indication system. The detector can receive the light that permeates the absorption cell that the halogen tungsten lamp sent, and after the solution that the colour development was accomplished flowed into the absorption cell through the pipeline in the second blender, the halogen tungsten lamp permeates the light filter and separates 540nm monochromatic light and jets into the absorption cell, and there is certain proportional relation according to lambert beer's law concentration of material in the solution and absorbance, and the detector obtains signal value output result.
Further, in order to realize the recovery of the waste liquid generated in the test process and prevent the pollution to the surrounding environment, the mixing container of the first mixer 2 has a waste liquid discharge port, the waste liquid discharge port is connected with the first waste liquid tank 18 through a pipeline, and a fifth control valve is installed on the pipeline between the waste liquid discharge port and the first waste liquid tank 18, preferably, the fifth control valve adopts a fifth electromagnetic valve 19, and the fifth electromagnetic valve 19 is connected with a control system and can receive the instruction of the control system to work.
The detection container 4 is provided with a waste liquid discharge port, the waste liquid discharge port is connected with the second waste liquid tank 20 through a pipeline, and a sixth control valve is installed on the pipeline between the waste liquid discharge port and the second waste liquid tank 20, preferably, the sixth control valve adopts a sixth electromagnetic valve 21, and the sixth electromagnetic valve 21 is connected with a control system and can receive the instruction of the control system to work.
Example 2:
the embodiment provides a working method of the automatic measuring system for water-soluble hexavalent chromium in cement, which is described in embodiment 1:
opening a first electromagnetic valve 5 and a second metering pump 6, injecting a first set amount of distilled water into a first mixer 2 by a distilled water tank 1 through the first electromagnetic valve 5 and the second metering pump 6, mixing a cement sample pre-placed in the first mixer 2 with water, pumping a second set amount of mixed solution into a second mixer 3 by a first metering pump 10 after mixing for a set time, opening a third electromagnetic valve 13, adding a fourth set amount of diphenylcarbonyl dihydrazide color developing solution into the second mixer 3 by a first reagent supply mechanism, opening a fourth electromagnetic valve 15, slowly dropwise adding 1.0mol/L hydrochloric acid solution into the second mixer 3 by a second reagent supply mechanism until a pH value sensor 16 detects that the pH value of the solution reaches a set value and stops dropwise adding, opening the first electromagnetic valve 5 to control the distilled water tank 1 to add distilled water into the second mixer 3 until a water level sensor detects that the water level of the solution in the second mixer 3 reaches a set water level value, and opening a second electromagnetic valve 17, sending the developed solution in the second mixer 3 into the detection container 4, and carrying out photoelectric detection on the solution in the detection container 4 by using a photoelectric detection device 5 to obtain a hexavalent chromium concentration numerical value.
In a practical application of this embodiment, 50g of a cement sample is weighed and manually added into a first mixer 2, a first electromagnetic valve 5 and a second metering pump 6 are opened, 100ml of distilled water is sucked from a distilled water tank 1 and enters the first mixer 2, the first electromagnetic valve 5 is closed, a first magnetic stirrer 8 dispersedly stirs the cement sample, the operation is stopped after 5min, after 5min of standing, a control system controls a first metering pump 10 to start, an upper solution in the first mixer is pumped into a filter element 11 by the first metering pump for filtration, the filtered solution enters a second mixer 3, in this embodiment, the first metering pump 10 pumps 20ml (or other volume, which needs to be determined according to the cement sample to meet a detection concentration) in the first mixer 2 and enters the second mixer 3, a second magnetic stirrer 9 of the second mixer 3 starts to stir, and after a set time of stirring, and opening a third electromagnetic valve 13, adding 5ml of dibenzoyl dihydrazide color developing solution into the second mixer 3, then closing the third electromagnetic valve 13, opening a fourth electromagnetic valve 15, dropwise adding a dilute hydrochloric acid solution into the second mixer 3 until the pH value of the solution detected by the pH value sensor 16 reaches 2.1-2.5, sending a signal to a control system, and controlling the fourth electromagnetic valve 15 to be closed by the control system.
The first electromagnetic valve 5 is opened, distilled water in the distilled water tank 1 is injected into the second mixer 3 until the water level sensor detects that the liquid level of the solution in the second mixer 3 reaches a set liquid level value, the water level sensor sends a signal to the control system, and the control system controls the first electromagnetic valve 5 to be closed. At this time, the solution in the second mixer 3 reaches 50ml, during the operation, the second mixer 3 continuously stirs the solution, when the liquid level of the solution in the second mixer 3 reaches the set liquid level value, the stirring is stopped, and the solution is allowed to stand in the second mixer for 15 min.
And opening the second electromagnetic valve 17, allowing the solution in the second mixer 3 to enter the detection container 4, performing photoelectric detection on the solution in the detection container 4 by using the photoelectric detection device 5, converting an optical signal into an electric signal, and reporting the result through a display screen.
After the completion of the detection, the fifth solenoid valve 19 and the sixth solenoid valve 21 are opened to discharge the remaining solutions in the first mixer 2 and the detection container 3, respectively, and the solutions are collected by the first waste liquid tank 18 and the second waste liquid tank 20, respectively.
Before the experiment begins, a standard curve is established for the system, the distilled water tank 1, the first reagent supply mechanism and the second reagent supply mechanism are all in place and are completely consistent with those in normal sample measurement, and the difference is that a hexavalent chromium standard solution with the concentration of 5mg/L is added into the first mixer 2, and the hydrochloric acid solution in the second reagent tank 14 is 0.04 mol/L. The standard curve is established as follows: the control system controls the first metering pump 10 to sequentially transfer 0mL, 1.0mL, 2.0mL, 5.0mL, 10.0mL and 15.0mL of hexavalent chromium standard solution into the second mixer 3, the dibenzoyl dihydrazide color development solution is controlled to be added by the third electromagnetic valve 13 by 5.0mL, the 0.04mol/L hydrochloric acid solution is controlled to be added by the fourth electromagnetic valve 15 by 5mL, the first electromagnetic valve 13 controls the distilled water to be added into the second mixer 3 and the volume is 50mL, the mixture is uniformly stirred and developed for 15min, and the mixed solution enters the detection container 4 for determination. And (3) carrying out six times of color reaction and photoelectric detection to respectively obtain signal values, and automatically calculating by a control system to obtain a standard curve and automatically storing the standard curve corresponding to the hexavalent chromium concentration value.
The control system is connected with the upper computer, the upper computer controls the work of the control system, and the collected test state information can be displayed on the upper computer.
Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the present invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive efforts by those skilled in the art based on the technical solution of the present invention.
Claims (10)
1. The utility model provides a water-soluble hexavalent chromium automatic determination system in cement, a serial communication port, including distilled water tank, first control valve is installed to distilled water tank's outlet pipe, and first control valve is connected with the access connection of first blender and second blender respectively, and the import of second blender still is connected with first reagent feeding mechanism and second reagent feeding mechanism respectively, and the import of second blender is connected with first blender through the first pump body, install pH value detecting element in the second blender, the export of second blender passes through the access connection of second control valve with the detection container, and the detection container periphery is equipped with the photoelectric detection device that can carry out photoelectric detection to its inside solution.
2. The system for automatically measuring the water-soluble hexavalent chromium in the cement according to claim 1, wherein a second pump body is installed on a pipeline between the first control valve and the first mixer.
3. The system for automatically measuring the water-soluble hexavalent chromium in the cement according to claim 1, wherein a filtering element is installed on a pipeline between the outlet of the first mixer and the inlet of the second mixer.
4. The automatic measuring system of hexavalent chromium in cement according to claim 3, wherein said filtering element is a water-based microporous filter membrane.
5. The system for the automatic determination of the water-soluble hexavalent chromium in cement according to claim 1, wherein the first reagent supplying means comprises a first reagent tank installed at a height higher than an inlet of the second mixer, and an outlet of the first reagent tank is connected to an inlet of the second mixer through a third control valve.
6. The automatic measuring system for the water-soluble hexavalent chromium in cement according to claim 1, wherein the second reagent supplying means includes a second reagent tank installed at a height higher than that of the inlet of the second mixer, and the outlet of the second reagent tank is connected to the inlet of the second mixer through a fourth control valve.
7. The automatic measuring system of water-soluble hexavalent chromium in cement according to claim 1, wherein a constant volume detecting element is installed at an end of the pipeline between the distilled water tank and the second mixer, which extends into the second mixer, for detecting the liquid level information of the solution in the second mixer.
8. The system for automatically measuring water-soluble hexavalent chromium in cement according to claim 1, wherein the waste liquid discharge port of the first mixer is connected to a first waste liquid tank through a fifth control valve.
9. The system for automatically measuring water-soluble hexavalent chromium in cement according to claim 1, wherein the waste liquid discharge port of the inspection container is connected to a second waste liquid tank through a sixth control valve.
10. A method for operating an automatic measuring system for hexavalent chromium soluble in cement according to any one of claims 1 to 9, wherein the distilled water tank is filled with a first set amount of distilled water through a first control valve into a first mixer, the first mixer mixes a cement sample previously placed therein with water, after a set time of mixing, a first pump pumps a second set amount of mixed solution into a second mixer, a first reagent supplying means adds a third set amount of color developing reagent into the second mixer, a second reagent supplying means adds a fourth set amount of pH adjusting reagent into the second mixer until the pH detecting element detects that the pH of the solution reaches a set value, a first control valve controls the distilled water tank to add distilled water into the second mixer until the water level of the solution in the second mixer reaches a set water level value, and the second control valve, and (4) sending the solution which is well developed in the second mixer into a detection container, and carrying out photoelectric detection on the solution in the detection container by using a photoelectric detection device to obtain a hexavalent chromium concentration value.
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