System and method for detecting cyanide in water

Abstract

The invention provides a system and method for detecting cyanide in water, and the system comprises a distillation device which comprises a distillation flask and a collection flask disposed at the outlet end of the distillation flask; the transfer device comprises a transfer assembly I arranged at the inlet end of the distillation bottle and a transfer assembly II arranged at the outlet end of the collection bottle; and the color developing device is connected with the transfer assembly II. According to the system and method for detecting cyanide in water, the whole process of sample injection, distillation, distillate transfer, color development, waste liquid discharge and cleaning is free of uncovering operation, the whole process is free of manual contact, full-automatic operation is achieved, the detection efficiency and operation safety are remarkably improved, and the risk that operators make contact with cyanide is effectively avoided.

Description

TECHNICAL FIELD

[0001] The present application relates to a detection method, in particular to a cyanide detection system and method in water. BACKGROUND

[0002] In the current cyanide detection field, existing technical means mainly rely on manual operation. Although this method can meet some needs, it has many limitations. First, manual detection method is easily affected by human factors, such as the skill level difference of the operator will lead to different detection results, which limits the accuracy and reliability of the detection. Secondly, manual detection is time-consuming, which requires a lot of manpower and time investment, which greatly reduces the work efficiency in emergency situations. Finally, manual operation also faces health and safety risks, and the operating personnel need to work in a dangerous environment, which poses a threat to the safety of personnel.

[0003] In recent years, automation technology has developed rapidly, and many fields are trying to apply automated detection systems to improve work efficiency and detection accuracy. However, cyanide detection technology is still relatively backward in this regard. Most existing automated detection systems are limited to applications in other fields, and specialized automated systems for cyanide detection are still relatively scarce. This is mainly because cyanide is highly toxic, and has high requirements for detection equipment and environment, and the chemical properties of cyanide require specific processing methods to ensure the accuracy of detection. Therefore, it is urgent to develop a cyanide detection technology that can be automated, reduce the risk of manual operation, and improve detection efficiency and accuracy. SUMMARY

[0004] The technical problem to be solved by the present application is to provide a cyanide detection system in water that can realize automatic operation, high detection efficiency and good accuracy.

[0005] The present application provides a cyanide detection system in water, comprising: a distillation device comprising a distillation flask and a collection flask arranged at the outlet end of the distillation flask; a transfer device comprising a transfer assembly I arranged at the inlet end of the distillation flask and a transfer assembly II arranged at the outlet end of the collection flask; a color developing device connected with the transfer assembly II for color development.

[0006] The present application sets up a distillation device, a transfer device and a color developing device, which can realize automation, closure and integration of the process, and significantly improve the safety, accuracy, efficiency and convenience of detection.

[0007] By setting the transfer assembly I and the transfer assembly II, the whole detection process (from sample distillation to distillate collection, and then to color reaction) can be carried out in a closed or semi-closed pipeline, forming a closed operation of detection; the opportunities of direct contact of experimental personnel with toxic cyanide and strong acid can be minimized, and the personal safety of the operating personnel can be effectively ensured.

[0008] Further, the distillation device further comprises a heating device for heating the distillation flask and a weighing device arranged at the lower end of the collection flask for weighing; the heating device can accurately control the distillation temperature, avoid the risk of local overheating or violent boiling caused by traditional open flame heating, and at the same time, can be adapted to the system to realize full automation detection; the weighing device can monitor the mass change of the distillate in the collection flask in real time, so as to accurately control the reaction process and the amount of reagent added, and ensure the accuracy and repeatability of the detection results.

[0009] Further, the distillation flask is connected with the collection flask through a liquid outlet pipe, and a pinch valve is arranged on the liquid outlet pipe; the pinch valve can pinch the liquid outlet pipe and block the communication between the distillation flask and the collection flask; the pinch valve is provided with a driving mechanism such as a motor, a pneumatic cylinder or an electromagnet, and the opening and closing of the pinch valve is controlled by the driving mechanism; when the weighing device detects that the collection flask reaches a threshold value, the pinch valve realizes instantaneous cutting off of the communication between the distillation flask and the collection flask by extruding the hose, so as to block the passage of hydrogen cyanide vapor at any time during the distillation process and realize immediate physical isolation.

[0010] Further, the collection flask is of a sealed structure, which ensures zero escape of distillate vapor, especially prevents release of residual gas after distillation, completely blocks the leakage path of toxic gas, and has high safety; the sealing property is controlled by the pinch valve; when it is necessary to extract the liquid in the collection flask, the pinch valve is in an open state to avoid negative pressure during extraction.

[0011] Further, the inlet pipe of the distillation flask extends to the bottom of the distillation flask and can realize liquid inlet and liquid outlet; the outlet pipe of the collection flask is located at the bottom of the collection flask and can realize liquid outlet and liquid inlet; the pipeline design is implemented by double bottom pipeline architecture, the pipeline extends to the bottom of the bottle, and when liquid is inlet, the sample is injected into the bottom of the bottle body along the bottle wall to avoid direct impact on the liquid surface, prevent liquid splashing and foam generation, and at the same time ensure that the liquid in the bottle is completely discharged when liquid is outlet to avoid residue; further, the automatic detection process and cleaning can be realized, and the automatic operation of the detection system can be realized, thereby reducing the need for manual intervention and improving the continuity and stability of the detection process.

[0012] Further, the transfer assembly I comprises an injection pump II, a peristaltic pump I, a three-way valve and a rotary valve I, one interface of the injection pump II, a common interface of the rotary valve I and the peristaltic pump I are connected with the three-way valve respectively, and the common interface of the rotary valve I is selectively connected with the injection pump II or the peristaltic pump I, one or more sub-interfaces of the rotary valve I are connected with the inlet end of the distillation flask; the injection pump II is a multi-channel injection pump, the rotary valve I is a multi-channel rotary valve, and the three-way valve is an electrically controlled three-way valve; the transfer assembly I realizes ultra-precision fluid processing and intelligent process switching through the injection pump-peristaltic pump-multi-valve joint control architecture, can realize accurate distribution of various reagents and automatic switching of complex paths, and greatly improves the flexibility and adaptability of the system.

[0013] Further, the sub-interfaces of the rotary valve I are also connected with a waste liquid end and an air end, the waste liquid end is used for discharging liquid in the pipeline, and the air end is used for accurate pushing of solution reagents, so that automatic detection is realized.

[0014] Further, the remaining interfaces of the injection pump II are connected with pure water, an air end, a waste liquid end and a reagent bottle group I respectively.

[0015] Further, the reagent bottle group I comprises EDTA-2Na reagent bottles, zinc nitrate reagent bottles, methyl orange reagent bottles, tartaric acid reagent bottles and phosphoric acid reagent bottles.

[0016] Further, the transfer assembly I further comprises a diaphragm pump I, and an outlet end of the diaphragm pump I is connected with the three-way valve in parallel after the peristaltic pump I.

[0017] Further, the transfer assembly II comprises a rotary valve II, a peristaltic pump II, a constant-volume pump I and an injection pump I, one interface of the injection pump I, the peristaltic pump II and the constant-volume pump I are connected with a common interface of the rotary valve II in parallel, one or more sub-interfaces of the rotary valve II are connected with an outlet end of a collection bottle, and one interface of the injection pump I is connected with a color developing device.

[0018] Further, the sub-interfaces of the rotary valve II are connected with a waste liquid end, an air end and the outlet end of the collection bottle respectively, and the remaining interfaces of the injection pump I are connected with a waste liquid end, an air end, a mother liquor end, a pure water end, a cuvette and a reagent bottle group II respectively.

[0019] Further, the reagent bottle group II comprises phosphate buffer reagent bottles and chloramine T reagent bottles.

[0020] Further, the transfer assembly II further comprises a diaphragm pump II, and an outlet end of the diaphragm pump II is connected with the common interface of the rotary valve II.

[0021] Further, the color developing device comprises a quantitative pump II and a rotary valve III, a common end of the rotary valve III is connected with the quantitative pump II and the injection pump I of the transfer assembly II respectively, and sub-interfaces of the rotary valve III are connected with the waste liquid end and the colorimetric tube respectively.

[0022] Meanwhile, the application further provides a cyanide detection method in water, which comprises the following steps: S0, system starting: S01, the injection pump I performs an extraction action on the colorimetric dish to empty the colorimetric dish; S02, according to the need, a sample is selected to make a sample type, the type including total cyanide or easily released cyanide; S03, sample and reagent quantitative transfer and distillation are performed on the distillation flask; The total cyanide sample preparation comprises the following steps: S1, pre-distillation and total cyanide sample preparation: S11, sample transfer I, the peristaltic pump I is connected with the distillation flask and the sample is transferred to the distillation flask; S12, distillation sample reagent addition: S121, EDTA-2Na addition, after the EDTA-2Na fills the injection pump II pipeline, 10ml of EDTA-2Na is transferred to the distillation flask through air; S122, phosphoric acid addition, after the phosphoric acid fills the injection pump II pipeline, 10ml of phosphoric acid is transferred to the distillation flask through air; S13, weighing starting and zeroing; S14, absorption liquid addition, after the NaOH fills the rotary valve II, 10ml of NaOH is transferred to the collection bottle through the quantitative pump I; S15, heating distillation and weighing; S16, after the distillation sample weighing reaches a set value (100ml), heating is stopped, and the communication between the distillation flask and the collection bottle is blocked through the pinch valve.

[0023] The easily released cyanide sample preparation comprises the following steps: S1, pre-distillation and easily released cyanide sample preparation: S11, sample transfer II, the peristaltic pump I is connected with the distillation flask and the sample is transferred to the distillation flask; S12, distillation sample reagent addition: S121, zinc nitrate addition, after the zinc nitrate fills the injection pump II pipeline, 10ml of zinc nitrate is transferred to the distillation flask through air; S122, methyl orange addition, after the methyl orange fills the injection pump II pipeline, 0.4ml of methyl orange is transferred to the distillation flask through air; S123, tartaric acid is added. After the syringe pump II1 line is filled with tartaric acid, 5 ml of tartaric acid is transferred to the distillation flask through air; S13, weighing starts and returns to zero; S14, add absorption liquid, NaOH fills rotary valve II and then transfers 10ml NaOH to the collection bottle through quantitative pump I; S15, heating, distilling and weighing; S16. Stop heating after the distilled sample is weighed to the set value (100 ml), and cut off the connection between the distillation flask and the collection flask through the pinch valve.

[0024] S2, distillate transfer: S21, mixing, syringe pump I delivers 10ml of air through rotary valve II into the collection bottle, and mixes by blowing air; S22, cleaning and filling the pipeline, syringe pump I draws 10ml of sample from the collection bottle through rotary valve II and fills the rotary valve III pipeline; S23, sample transfer, syringe pump I draws 10ml of sample from the collection bottle through rotary valve II, and transfers the sample to the colorimetric tube after passing through rotary valve III with air; S24, pipeline cleaning, syringe pump I draws 5ml of pure water and cleans the pipeline of rotary valve III, and drains the liquid in the pipeline of rotary valve III through air; S3. Reaction and reagent addition: S31, adding buffer solution, after the potassium dihydrogen phosphate buffer solution fills the syringe pump I pipeline, 5 ml of potassium dihydrogen phosphate buffer solution is transferred to the colorimetric tube through the rotary valve III by air; S32, chloramine T is added. After the chloramine T is filled in the syringe pump I, 0.3 ml of chloramine T is transferred to the colorimetric tube through the rotary valve III 14 by air; S33, pipeline cleaning, syringe pump I draws 5ml of pure water and cleans the pipeline of rotary valve III, and drains the liquid in the pipeline of rotary valve III through air; S34, let it stand for 2 minutes; S35, isonicotinic acid-barbituric acid addition: after the isonicotinic acid-barbituric acid fills the syringe pump I line, 6 ml of isonicotinic acid-barbituric acid is transferred to the colorimetric tube through the rotary valve III by air; S36, pipeline cleaning, syringe pump I draws 5ml of pure water and cleans the pipeline of rotary valve III, and drains the liquid in the pipeline of rotary valve III through air; S4, constant volume: Syringe pump I transfers 2.7 ml of pure water to the colorimetric tube to constant volume; S5, color development, heat the colorimetric tube to a constant temperature of 30°C and color development for 10 minutes; S6, colorimetry; S61, zero adjustment: S611, colorimetric cell cleaning, injection pump I transfers pure water to the colorimetric cell, and stands for 30s to make the light path zero; S612, zero waste liquid discharge, the waste liquid in the colorimetric cell is discharged; S62, sample colorimetric: S621, rinse, the solution in the colorimetric tube is extracted by injection pump I and the solution is used to rinse the colorimetric cell; S622, 3ml solution in the colorimetric tube is extracted by injection pump I and transferred to the colorimetric cell by air; S623, stand for 30s, read the absorbance and substitute into the curve to calculate the concentration; S624, waste liquid discharge, the solution in the colorimetric cell is extracted and cleaned by pure water; S7, waste discharge and cleaning of the collection bottle: S71, after the sample is transferred to the colorimetric tube, the waste liquid in the collection bottle is discharged by peristaltic pump II; S72, 100ml pure water is transported to the colorimetric cell by diaphragm pump II, and air is transported by peristaltic pump II for mixing; S73, the collection bottle is emptied by peristaltic pump II; S8, waste discharge and cleaning of the distillation bottle; S81, the waste liquid in the distillation bottle is discharged by peristaltic pump I; S82, 100ml pure water is transported to the distillation bottle by diaphragm pump I, and air is transported by peristaltic pump I for mixing; S83, the distillation bottle is emptied by peristaltic pump I; S9, waste discharge and cleaning of the colorimetric tube; S91, the liquid in the colorimetric tube is discharged by injection pump I, and the colorimetric tube is cleaned by pure water multiple times and emptied.

[0025] The water cyanide detection system and detection method can realize automation, closure and integration of the process, and significantly improve the safety, accuracy, efficiency and convenience of detection. By setting the transfer assembly I and the transfer assembly II, the whole detection process can be carried out in a closed or semi-closed pipeline, forming a closed operation of detection. The opportunities of directly contacting the toxic cyanide and strong acid by the experimental personnel are minimized, and the personal safety of the operator is effectively guaranteed. The water cyanide detection system and detection method can realize full-automatic operation, significantly improve the detection efficiency and operation safety, and effectively avoid the risk of the operator contacting cyanide. BRIEF DESCRIPTION OF DRAWINGS

[0026] Figure 1 Fig. 1 is a schematic diagram of the system principle of the cyanide detection system in water according to the present application; In the figure: 1, injection pump II, 2, peristaltic pump I, 3, diaphragm pump I, 4, three-way valve, 5, rotary valve I, 6, distillation flask, 7, collection flask, 8, rotary valve II, 9, peristaltic pump II, 10, diaphragm pump II, 11, quantitative pump I, 12, injection pump I, 13, quantitative pump II, 14, rotary valve III. DETAILED DESCRIPTION

[0027] The embodiments of the present application will be described in detail below with reference to the accompanying drawings.

[0028] Referring to Figure 1 The present application provides a cyanide detection system in water, which comprises a distillation device, a transfer device and a color developing device.

[0029] The distillation device is mainly used for distilling water samples. The distillation device comprises a distillation flask 6 and a collection flask 7 arranged at the outlet end of the distillation flask 6. Meanwhile, the distillation device further comprises a heating device and a weighing device. The heating device is used for heating the distillation flask 6, and the heating temperature and heating time can be set and constant temperature heating is realized. The weighing device is arranged at the lower end of the collection flask 7 and is used for weighing the collection flask 7 and the solution inside. The heating device can accurately control the distillation temperature, avoid the risk of local overheating or violent boiling caused by traditional open flame heating, and can be adapted to the system to realize fully automated detection. The weighing device can monitor the mass change of the distillate in the collection flask 7 in real time, so as to accurately control the reaction progress and the amount of reagent added, and ensure the accuracy and repeatability of the detection results. One distillation flask 6 and one collection flask 7 form a set of distillation device. Multiple sets of distillation devices can be arranged in the present application to realize the simultaneous distillation of multiple samples, and then batch detection is realized to improve the detection efficiency.

[0030] The distillation flask 6 is connected to the collection flask 7 through a liquid outlet pipe. The liquid outlet pipe comprises a glass tube and a silica gel hose connected to each other. The glass tube can be inserted into the collection flask 7 to absorb the liquid and realize the connection with the collection flask 7. A pipe clamp valve is arranged at the silica gel hose part of the liquid outlet pipe. The pipe clamp valve can clamp the liquid outlet pipe (silica gel hose) and block the communication between the distillation flask 6 and the collection flask 7. The pipe clamp valve is provided with a driving mechanism such as a motor, a pneumatic cylinder or an electromagnet. The opening and closing of the pipe clamp valve is controlled by the driving mechanism. When the weighing device detects that the collection flask 7 reaches the threshold value, the pipe clamp valve realizes instantaneous cutting off of the communication between the distillation flask 6 and the collection flask 7 by extruding the hose. The passage of hydrogen cyanide vapor can be blocked at any time during the distillation process to realize instant physical isolation and automatic control.

[0031] In order to realize automatic drainage and cleaning, in the application, the inlet end pipeline of the distillation flask 6 extends to the bottom of the distillation flask 6, thereby realizing liquid inlet and drainage; at the same time, the outlet end pipeline of the collection bottle 7 is located at the bottom of the collection bottle 7, thereby realizing liquid inlet and drainage, the pipeline design is realized by a double bottom pipeline structure, the pipeline extends to the bottom of the bottle, when liquid is inlet, the sample is injected into the bottom of the bottle along the pipeline, avoiding direct impact on the liquid surface, preventing liquid splashing and foam generation, at the same time, when liquid is drained, the liquid in the bottle is completely drained, avoiding residue, thereby realizing automatic detection process and cleaning, ensuring cleaning efficiency and cleaning effect, thereby realizing automatic operation of the detection system, reducing the need for manual intervention, and improving the continuity and stability of the detection process.

[0032] The transfer device is used to realize the transfer of samples, reagents, water and other liquids, realize liquid supply and cleaning operation of the distillation device, and comprises a transfer assembly I arranged at the inlet end of the distillation flask 6 and a transfer assembly II arranged at the outlet end of the collection bottle 7. In the application, the transfer assembly I comprises a syringe pump II1, a peristaltic pump I2, a three-way valve 4 and a rotary valve I5, one interface of the syringe pump II1, a common interface of the rotary valve I5 and the peristaltic pump I2 are respectively connected with the three-way valve 4, so that the common interface of the rotary valve I5 is selectively connected with the syringe pump II1 or the peristaltic pump I2, one or more sub-interfaces of the rotary valve I5 are connected with the inlet end of the distillation flask 6; the above-mentioned syringe pump II1 is a multi-channel syringe pump, the rotary valve I5 is a multi-channel rotary valve, and the three-way valve 4 is an electrically controlled three-way valve; the transfer assembly I realizes ultra-precision fluid processing and intelligent process switching through the syringe pump-peristaltic pump-multi-valve joint control architecture, can realize accurate distribution of various reagents and automatic switching of complex paths, and greatly improves the flexibility and adaptability of the system; the sub-interfaces of the rotary valve I5 are also connected with a waste liquid end and an air end, the waste liquid end is used for discharging liquid in the pipeline, and the air end is used for accurate pushing of solution reagents, realizing automatic detection; the remaining interfaces of the syringe pump II1 are respectively connected with pure water, an air end, a waste liquid end and a reagent bottle group I, the reagent bottle group I comprises EDTA-2Na reagent bottles, zinc nitrate reagent bottles, methyl orange reagent bottles, tartaric acid reagent bottles and phosphoric acid reagent bottles, at the same time, the transfer assembly I further comprises a diaphragm pump I3, the outlet end of the diaphragm pump I3 is connected with the peristaltic pump I2 in parallel and then communicates with the three-way valve 4, and the inlet end of the diaphragm pump I3 is connected with a pure water end, which is mainly used for cleaning water supply.

[0033] In the application, the injection pump II 1 is a multi-channel injection pump, i.e. has multiple injection channels, and has 10 interfaces (channels), specifically, the No. 1 interface is connected to an air port, the No. 2 interface is connected to a pure water port, the No. 3 interface is connected to an EDTA-2Na reagent bottle, the No. 4 interface is connected to zinc nitrate, the No. 5 interface is connected to methyl orange, the No. 6 interface is connected to tartaric acid, the No. 7 interface is connected to phosphoric acid, the No. 8 interface is connected to a waste liquid port, and the No. 9 interface is connected to the a interface of the three-way valve 4; the peristaltic pump I 2 can realize forward and reverse rotation, and is mainly used for waste discharge; the diaphragm pump I 3 and the peristaltic pump I 2 are connected to the b interface of the three-way valve 4; the peristaltic pump I 2 is connected to the waste liquid port, and is used for forward rotation to discharge waste and reverse rotation to fill air (mixing); the c interface of the three-way valve 4 is connected to the common interface of the rotary valve I 5, and the three-way valve 4 can connect the a and c interfaces or the b and c interfaces; the rotary valve I 5 is a multi-channel rotary valve, and has a common interface and multiple sub-interfaces; the common interface can selectively connect one of the sub-interfaces; in the application, the No. 1 interface of the rotary valve I 5 is connected to the waste liquid port, the No. 2 interface is connected to the air port, and the Nos. 3-8 interfaces are respectively connected to the inlet ends of the six distillation bottles 6.

[0034] The transfer assembly II includes a rotary valve II 8, a peristaltic pump II 9, a constant volume pump I 11, and an injection pump I 12; one interface of the injection pump I 12, the outlet of the peristaltic pump II 9, and the outlet of the constant volume pump I 11 are connected in parallel to the common interface of the rotary valve II 8; one or more sub-interfaces of the rotary valve II 8 are connected to the outlet end of the collection bottle 7; one interface of the injection pump I 12 is connected to a color developing device; wherein the sub-interfaces of the rotary valve II 8 are respectively connected to the waste liquid port, the air port, and the outlet end of the collection bottle 7; the remaining interfaces of the injection pump I 12 are respectively connected to the waste liquid port, the air port, the mother liquor port, the pure water port, the cuvette, and the reagent bottle group II; the reagent bottle group II includes a phosphate buffer reagent bottle and a chloramine T reagent bottle; the transfer assembly II further includes a diaphragm pump II 10; the outlet end of the diaphragm pump II 10 is connected to the common interface of the rotary valve II 8; and the inlet of the diaphragm pump II 10 is connected to the pure water port, and is used for cleaning the water supply.

[0035] In the present application, the injection pump 112 is a multi-channel injection pump, that is, it has multiple injection channels, and its specific configuration includes 10 interface channels. Among them, No. 1 port is connected to the common end of the rotary valve 114, No. 2 port is connected to the mother liquor end, No. 3 port is connected to the pure water end, No. 4 port is connected to the phosphate buffer reagent bottle, No. 5 port is connected to the chloramine T reagent, No. 6 port is connected to the isonicotinic acid-barbituric acid solution, No. 7 port is connected to the waste liquid end, No. 8 port is connected to the air end, and No. 9 port is connected to the cuvette; the peristaltic pump 109 can realize forward and reverse rotation, the diaphragm pump 110, the peristaltic pump 109, the quantitative pump 111 and the No. 10 port of the injection pump 112 are connected in parallel to the common interface of the rotary valve 108, wherein the inlet end of the quantitative pump 111 is connected to NaOH for delivering NaOH solution, which is alkaline, as an independent transfer module; the inlet end of the diaphragm pump 110 is connected to pure water, and the peristaltic pump 109 is connected to the waste liquid end, for forward rotation to discharge waste and reverse rotation to fill air (mixing); the rotary valve 108 is a multi-channel rotary valve, which has a common end and multiple sub-interfaces, inside the rotary valve, the common interface can selectively communicate with one of the sub-interfaces, and outside the rotary valve, the common end can selectively communicate with the peristaltic pump 109, the diaphragm pump 110, the quantitative pump 111 and the injection pump 112; No. 1 port of the rotary valve 108 is connected to the waste liquid end, No. 2 port is connected to the air end, and No. 3-8 ports are respectively connected to the outlet ends of the six collection bottles 7.

[0036] The color developing device is connected with the transfer assembly II for color development, which includes a quantitative pump 113 and a rotary valve 114, the common end of the rotary valve 114 is connected with the outlet end of the quantitative pump 113 and the injection pump 112 of the transfer assembly II respectively, and the sub-interfaces of the rotary valve 114 are connected with the waste liquid end and the cuvette respectively; specifically, the rotary valve 114 is a multi-channel rotary valve, inside the valve body, the common end can selectively communicate with one of the sub-interfaces, and outside, the common end selectively communicates with No. 1 port of the injection pump 112 or the outlet of the quantitative pump 113, No. 1 port of the rotary valve 114 is connected with the cuvette, No. 10 port is connected with the waste liquid end, and the inlet end of the quantitative pump 113 is connected with NaOH for NaOH liquid supply.

[0037] The cyanide detection system in water in the present application realizes the intrinsic safety, precise automation and high throughput of toxic substance detection through the design of fully closed flow path, intelligent valve and pump collaborative control and modular function integration; from sample injection, distillation, distillate transfer, color development, waste liquid discharge and cleaning, the whole process is operated without opening the cover, and the whole process is zero manual contact, realizing full automatic operation, significantly improving the detection efficiency and operation safety, and effectively avoiding the risk of operators contacting cyanide; The present application can realize the automation, closure and integration of the process by setting the distillation device, the transfer device and the color developing device, which significantly improves the safety, accuracy, efficiency and convenience of detection.

[0038] By setting the transfer assembly I and the transfer assembly II, the whole detection process (from sample distillation to distillate collection, to color reaction) can be carried out in a closed or semi-closed pipeline, forming a closed operation of detection; the opportunities of directly contacting toxic cyanide and strong acid by experimenters can be minimized, and the personal safety of the operators is effectively ensured; the cyanide detection is promoted from "high-risk manual operation" to "intelligent closed assembly line", and a safe, reliable, accurate and efficient complete solution of cyanide detection is provided for the fields of environmental monitoring, chemical industry, disease control and the like.

[0039] Meanwhile, the application also provides a detection method, comprising the following steps: I. starting the system; II. preparing samples: 1. first step: emptying the cuvette (switching injection pump I 12 to No. 9 port), extracting 5ml, and resetting the switch to No. 7 waste liquid port to push out.

[0040] 2. sample preparation: customers select sample types according to needs: total cyanide or easily released cyanide.

[0041] Pre-distillation + total cyanide sample preparation, taking No. 1 distillation position as an example; 1. sample quantification + transfer: (1) positioning the sample injector to the position required by the customer, and inserting the mechanical arm into the sample bottle; (2) quantification: if the customer selects the automatic quantification function, the mechanical arm is inserted into the automatic quantification position, rotary valve I 5 is rotated to No. 1 position, three-way valve 4 is rotated to the lower passage (i.e. connected to the bc port), and peristaltic pump I 2 (sample injection peristaltic pump) is started (discharge excess sample, peristaltic pump speed, time open), and after running for a fixed time, peristaltic pump I 2 is closed.

[0042] Each time three-way valve 4 is used up, it is switched to a power-off state, i.e. not connected, and the following steps are operated in this way.

[0043] (3) sample transfer: the mechanical arm runs to the bottom position of the bottle, rotary valve I 5 is rotated to No. 3 position (No. 3 corresponds to No. 1 position of the distillation instrument), and peristaltic pump I 2 is started. After a fixed transfer time, peristaltic pump I 2 is stopped.

[0044] 2. distillation sample reagent addition: 2.1 adding 10ml EDTA-2Na: (1) filling the pipeline with EDTA-2Na: switching injection pump II 1 to No. 3 position, extracting 3ml (filling volume open) reagent, and pushing into No. 8 port waste liquid end of injection pump II 1.

[0045] (2) Inject EDTA-2Na: Inject pump II 1 turn to 3# port to extract 10ml, inject pump II 1 turn to 9# port, 3-way valve 4 switch to upper pass (connect ac), push out 10ml.

[0046] (3) Air push reagent: inject pump II 1 turn to 1# port, extract 5ml air, then turn to 9# port, push out, transfer all reagent in pipeline into distillation flask 6, 2.2 Add 10ml phosphoric acid reagent: (1) Fill the pipeline with phosphoric acid reagent: inject pump II 1 turn to 7# port, extract 3ml reagent, push into 8# port waste end of inject pump II.

[0047] (2) Inject phosphoric acid reagent: inject pump II 1 turn to 7# port to extract 10ml, inject pump II 1 turn to 9# port, 3-way valve 4 switch to upper pass (connect ac), push out 10ml.

[0048] (3) Air push reagent: inject pump II 1 turn to 1# port, extract 5ml air, then turn to 9# port, push out, transfer all reagent in pipeline into distillation flask 6.

[0049] 3, Distillation weighing start: weigh and return to zero; 4, Absorption liquid addition: (1) Fill the pipeline: rotate valve II 8 turn to 1# port waste end, open quantitative pump I, fill the pipeline, stop after completion, only fill the pipeline for the first sample, (2) Add absorption liquid: rotate valve II 8 turn to 3# port, open quantitative pump I, open quantitative pump I 10ml sodium hydroxide for a period of time, stop quantitative pump I to add reagent, 5, Distillation sample weighing: Start 1# distillation position heating and weighing, stop heating when weighing to 100ml, clamp 1# position pinch valve.

[0050] Pre-distillation + easily released cyanide sample preparation: take 1# distillation position as an example 1, Sample quantification + transfer: (1) Position the sample injector to the position required by the customer, insert the mechanical arm into the sample bottle, (2) Quantification: if the customer chooses automatic quantification function, insert the mechanical arm into the automatic quantification position, rotate valve I 5 turn to 1# position, 3-way valve 4 turn to lower pass (connect bc), start peristaltic pump I 2 (sample feeding peristaltic pump), wait for a fixed time to run, then close peristaltic pump I; (3) Sample transfer: run the mechanical arm to the bottom position of the bottle, rotate valve I 5 turn to 3# position (3# corresponds to 1# position of the distillation instrument), start peristaltic pump I 2. Stop peristaltic pump I after a fixed transfer time.

[0051] 2, Distillation sample reagent addition: 2.1 Add 10 ml of zinc nitrate: (1) Fill the pipeline with zinc nitrate solution: rotate the injection pump II 1 to the 4th position, extract 3 ml of reagent, and push it into the waste liquid end of the 8th port of the injection pump II.

[0052] (2) Inject zinc nitrate: rotate the injection pump II 1 to the 10th port to extract 10 ml, rotate the injection pump II 1 to the 9th port, and switch the three-way valve 4 to the upper passage (connect ac), and push out 10 ml.

[0053] (3) Push the reagent with air: rotate the injection pump II 1 to the 1st port, extract 5 ml of air, then rotate to the 9th port, and push it out, transferring all the reagent in the pipeline into the distillation flask 6, 2.2 Add 0.4 ml of methyl orange reagent: (1) Fill the pipeline with methyl orange: rotate the injection pump II 1 to the 5th position, extract 3 ml of reagent, and push it into the 8th port of the injection pump II.

[0054] (2) Inject 0.4 ml of methyl orange reagent: rotate the injection pump II 1 to the 5th port to extract 0.4 ml, rotate the injection pump II 1 to the 9th port, and switch the three-way valve 4 to the upper passage, and push out 0.4 ml.

[0055] (3) Push the reagent with air: rotate the injection pump II 1 to the 1st port, extract 5 ml of air, then rotate to the 9th port, and push it out, transferring all the reagent in the pipeline into the distillation flask 6.

[0056] 2.3 Add 5 ml of tartaric acid solution reagent: (1) Fill the pipeline with tartaric acid: rotate the injection pump II 1 to the 6th position, extract 3 ml of reagent, and push it into the 8th port of the injection pump II.

[0057] (2) Inject 5 ml of tartaric acid reagent: rotate the injection pump II 1 to the 6th port to extract 5 ml, rotate the injection pump II 1 to the 9th port, and switch the three-way valve 4 to the upper passage, and push out 5 ml.

[0058] (3) Push the reagent with air: rotate the injection pump II 1 to the 1st port, extract 5 ml of air, then rotate to the 9th port, and push it out, transferring all the reagent in the pipeline into the distillation flask 6.

[0059] 3. Start distillation and weighing: weigh and return to zero 4. Add absorption liquid: (1) Fill the pipeline: rotate the valve II 8 to the 1st port, start the quantitative pump I 11, fill it, and stop after the first sample is filled. (2) Add absorption liquid: rotate the valve II 8 to the 3rd port, start the quantitative pump I 11, and start the quantitative pump I 10 ml of sodium hydroxide for a certain time, then stop the quantitative pump I to add reagent.

[0060] 5. Weigh the distillation sample: Start heating and weighing of distillation position 1, stop heating when the weight reaches 100 ml, and clamp the pipe valve of position 1.

[0061] III. Transferring of distillate: taking position 1 as an example 1. After distillation ends when the weight reaches 100 g, transfer the distillate: (1) Mix: inject pump I 12 turns to 8, extract 10 ml of air, inject pump I 12 turns to 10, rotary valve II 8 turns to 3, connect collection bottle 7, inject pump I pushes out 10 ml, and mix.

[0062] (2) Clean the flow path + fill the pipeline: inject pump I 12 turns to 10, rotary valve II 8 turns to 3 (corresponding to extract 10 ml of reagent in collection bottle 1 7), inject pump I 12 turns to 1, rotary valve III 14 turns to 10, and push out waste (fill the pipeline).

[0063] (3) Transfer 10 ml of sample in the absorption bottle: inject pump I 12 turns to 10, rotary valve II 8 turns to 3 to extract 10 ml of sample, inject pump I 12 turns to 1, rotary valve III 14 turns to 1, and push out 10 ml.

[0064] (4) Push the absorption liquid into the colorimetric tube with air: inject pump I 12 turns to 8 to extract 5 ml of air, push to 1, and the air pushes the sample into the colorimetric tube.

[0065] (5) Clean the pipeline with pure water: inject pump I 12 turns to 3 to extract 5 ml of pure water, inject pump I 12 turns to 1, rotary valve III 14 turns to 10, and push out to achieve pipeline cleaning.

[0066] (6) Air back-pushing: inject pump I 12 turns to 8 to extract 5 ml of air, inject pump I 12 turns to 1, rotary valve III 14 turns to 10, and push out.

[0067] IV. Reaction + reagent addition: 1. Add 5.0 ml of potassium dihydrogen phosphate buffer solution: (1) Fill the potassium dihydrogen phosphate buffer solution pipeline: inject pump I 12 turns to 4, extract 3 ml to 7.

[0068] (2) Add the buffer solution: inject pump I 12 turns to 4, extract 5 ml, inject pump I 12 turns to 1, rotary valve III 14 turns to 1, and push out 5 ml.

[0069] (3) Push the reagent into the pipeline with air: inject pump I 12 turns to 8, extract 5 ml, inject pump I 12 turns to 1, rotary valve III 14 turns to 1, and push out the excess reagent.

[0070] (4) Pure water cleaning line: inject pump 112 turn to 3# port, extract 5ml pure water, inject pump 112 turn to 1# port, rotary valve 114 turn to 10# port, push out.

[0071] (5) Air back push: inject pump 112 turn to 8# port, extract 5ml air, inject pump 112 turn to 1# port, rotary valve 114 turn to 10# port, push out.

[0072] 2, 0.3ml chloramine T add: (1) Fill the chloramine-T solution line: inject pump 112 turn to 5# port, extract 3ml turn to 7# port.

[0073] (2) Add chloramine-T solution: inject pump 112 turn to 5# port, extract 0.3ml, inject pump 112 turn to 1# port, rotary valve 114 turn to 1# port, push out 0.3ml.

[0074] (3) Air push into line reagent: inject pump 112 turn to 8# port, extract 5ml, inject pump 112 turn to 1# port, rotary valve 114 turn to 1# port, push out excess reagent.

[0075] (4) Pure water cleaning line: inject pump 112 turn to 3# port, extract 5ml pure water, inject pump 112 turn to 1# port, rotary valve 114 turn to 10# port, push out.

[0076] (5) Air back push: inject pump 112 turn to 8# port, extract 5ml air, inject pump 112 turn to 1# port, rotary valve 114 turn to 10# port, push out.

[0077] 3, Stand for 2min; 4, Add 6.0ml isonicotinic acid-barbituric acid: (1) Fill the isonicotinic acid-barbituric acid solution line: inject pump 112 turn to 6# port, extract 3ml turn to 7# port.

[0078] (2) Add isonicotinic acid-barbituric acid solution: inject pump 112 turn to 6# port, extract 6ml, inject pump 112 turn to 1# port, rotary valve 114 turn to 1# port, push out 6ml.

[0079] (3) Air push into line reagent: inject pump 112 turn to 8# port, extract 5ml, inject pump 112 turn to 1# port, rotary valve 114 turn to 1# port, push out excess reagent.

[0080] (4) Pure water cleaning line: inject pump 112 turn to 3# port, extract 5ml pure water, inject pump 112 turn to 1# port, rotary valve 114 turn to 10# port, push out.

[0081] (5) Air push: injection pump 112 turns to No. 8 port, 5ml air is extracted, injection pump 112 turns to No. 1 port, rotary valve 114 turns to No. 10 port, and then it is pushed out.

[0082] 5. Constant volume: (1) Injection pump 112 turns to No. 3 port, 2.7ml pure water is extracted, injection pump 112 turns to No. 1 port, rotary valve 114 turns to No. 1 port, and then it is pushed out for constant volume. (10ml sample + 5ml potassium dihydrogen phosphate buffer solution + 0.3ml chloramine T + 1ml water + 6ml isonicotinic acid barbituric acid); (2) Air push: injection pump 112 turns to No. 8 port, 5ml is extracted, injection pump 112 turns to No. 1 port, rotary valve 114 turns to No. 1 port, and then it is pushed out.

[0083] 6. The heating temperature is constant at 30℃. The color of No. 1 sample is developed for 10min.

[0084] Five, colorimetry: 1. Zero adjustment: (only need to adjust zero once each time) (1) Clean the cuvette: injection pump 112 turns to No. 3 port, 3ml pure water is extracted, injection pump 112 turns to No. 9 port, and then it is pushed out. After pushing out, 5ml is extracted immediately, and then it is pushed out through No. 7 port.

[0085] (2) Zero adjustment: injection pump 112 turns to No. 3 port, 3ml pure water is extracted, and then it is pushed out through No. 9 port.

[0086] (3) Air push: injection pump 112 turns to No. 8 port, 5ml is extracted, and then it is pushed out through No. 9 port.

[0087] (4) Stand for 30s, and then the light path is set to zero.

[0088] (5) Zero adjustment waste discharge: after zero adjustment, injection pump 112 turns to No. 9 port, 5ml is extracted, and then it is pushed out through No. 7 port.

[0089] 2. Sample colorimetry: (1) Fill the pipeline: injection pump 112 turns to No. 1 port, rotary valve 114 turns to No. 1 port, 5ml is extracted, and then it is pushed out through No. 7 port.

[0090] (2) Rinse the cuvette: injection pump 112 turns to No. 1 port, rotary valve 114 turns to No. 1 port, 3ml is extracted, and then it is pushed out through No. 9 port. 5ml is extracted immediately, and then it is discharged through No. 7 port.

[0091] (3) Inject the reaction sample into the cuvette: injection pump 112 turns to No. 1 port, rotary valve 114 turns to No. 1 port, 3ml is extracted, and then it is pushed out through No. 9 port.

[0092] (6) The air pushes the sample in the pipeline into the cuvette: Syringe pump I12 turns to port 8 to extract 5 ml, and syringe pump I turns to port 9 to push it out.

[0093] (7) Let it stand for 30 seconds, read the absorbance, and substitute it into the curve to calculate the concentration.

[0094] (8) Waste liquid discharge: After the measurement is completed, syringe pump I12 turns to port 10 to extract 5 ml, and syringe pump I12 turns to port 7 to push out.

[0095] (9) Cleaning the cuvette: Turn the syringe pump I12 to port 3, draw out 3 ml of pure water, turn the syringe pump I12 to port 9, push it out, and immediately draw out 5 ml, turn the syringe pump I12 to port 7 and push it out.

[0096] 6. Automatic standard curve: (1) The mother liquid fills the common pipeline: the syringe pump I12 is turned to port 2 to extract 3 ml, the syringe pump I12 is turned to port 1, and the rotary valve III14 is turned to port 10 to push out.

[0097] (2) Injection of mother liquor: Turn the injection pump I12 to port 2, extract 10 ml, turn the injection pump I to port 1, turn the rotary valve III14 to ports 1-8 (colorimetric tubes), and inject: 0.00, 0.20, 0.50, 1.00, 2.00, 3.00 ml of mother liquor respectively. Since the mother liquor is insufficient, extract 10 ml again and inject 4.00 and 5.00 ml of mother liquor into the colorimetric tubes.

[0098] (3) Clean the injection pump + rotary valve: Turn the injection pump I12 to port 3, draw 5 ml of pure water, turn the injection pump I12 to port 1, turn the rotary valve III14 to port 10, and discharge the waste.

[0099] (4) Empty the syringe pump + rotary valve: Turn the syringe pump I12 to port 8, extract 5 ml of air, turn it to port 1, and turn the rotary valve III14 to port 10 to push it out.

[0100] (5) Fill the pipeline with NaOH solution: Rotate valve III14 to port 10, start metering pump II13, and stop when filling is completed.

[0101] (6) Add sodium hydroxide solution to make up the volume to 10 ml: Rotate valve III 14 to port 1, start metering pump II 13, and add sodium hydroxide solution to colorimetric tubes 1-8 to make up the volume to 10 ml (the specific volume of solution added is calculated using the formula).

[0102] (7) Start the four-step reaction process.

[0103] (8) Start the five-step colorimetry and draw the standard curve.

[0104] 7. Collection bottle waste discharge + cleaning: Take collection bottle No. 1 as an example 1. Collecting bottle waste: After the sample is transferred to the cuvette, the waste is opened, the rotary valve II 8 is transferred to No. 3 port, and the peristaltic pump II 9 is started. When the collecting liquid in the collecting bottle 7 is completely emptied, stop running the peristaltic pump II 9.

[0105] 2. Clean the collecting bottle: Start the diaphragm pump II 10, and stop running after adding 100 ml.

[0106] 3. Mix: Start the peristaltic pump II 9 in reverse, open the time, and stop running after reversing.

[0107] 4. Clean the collecting bottle water discharge: Rotate the valve II 8 to No. 3 port, and start the peristaltic pump II 9. When the collecting liquid in the collecting bottle 7 is completely emptied, stop running the peristaltic pump II.

[0108] Eight, distillation flask 6 waste + cleaning: Take No. 1 distillation flask 6 as an example 1. Distillation flask waste: After the distillation is completed and the collecting bottle 7 is cleaned, the distillation flask 6 waste is opened, the rotary valve I 5 is transferred to No. 3 port, the three-way valve 4 is connected, and the peristaltic pump I 2 is started in reverse. When the waste liquid in the distillation flask 6 is completely emptied, stop running the peristaltic pump I.

[0109] 2. Clean the distillation: Start the diaphragm pump I 3, and stop running after adding 50 ml.

[0110] 3. Mix: Start the peristaltic pump I 2 in forward direction, and stop running after the time.

[0111] 4. Discharge and clean the distillation flask liquid: Rotate the valve I 5 to No. 3 port, and start the peristaltic pump I 2 in reverse. When the waste liquid is completely emptied, stop running the peristaltic pump I.

[0112] Nine, cuvette waste + cuvette cleaning: Take No. 1 reaction site as an example 1. Cuvette waste: After the colorimetric completion, rotate the valve III 14 to No. 1 port, and the injection pump I 12 to No. 1 port. Extract 10 ml multiple times and discharge to No. 7 port.

[0113] 2. Clean the cuvette: Rotate the injection pump I 12 to No. 3 port and extract 25 ml (10 ml each time), and then rotate to No. 1 port and inject into the No. 1 port of the rotary valve III 14.

[0114] 3. Cuvette waste discharge: Rotate the valve III 14 to No. 1 port, and the injection pump I 12 to No. 1 port. Extract 10 ml multiple times and discharge to No. 7 port.

[0115] From sample quantification, distillation, reagent addition, distillate transfer to colorimetric detection, the whole process is completed by pump valve cooperation, without manual intervention, realizing unattended operation; Each step (such as distillation, addition of absorbent, transfer of distillate) is automatically connected through valve position switching, avoiding cross contamination caused by manual transfer, realizing intelligent process connection, realizing full process automation, liberating manpower; The syringe pump has high precision conveying, and the error rate is much lower than manual pipetting. Key steps such as "air pushing reagent" ensure that the reagent is completely transferred, avoiding concentration deviation caused by residue; A multi-stage cleaning mechanism is adopted to realize high-efficiency anti-pollution design and ensure pure results; It has the functions of total cyanide and easily released cyanide dual-mode detection, which meets the needs of different scenes; The distillation site, absorption bottle site and colorimetric tube site can be expanded, supporting batch sample continuous detection and improving detection efficiency; The present application The application water cyanide detection system has high reliability and high throughput in the fields of environmental monitoring and chemical quality inspection by converting complex distillation-colorimetric process into standardized automatic operation through mechatronic liquid integration.

[0116] The above is only the preferred embodiment of the present application. It should be noted that for ordinary skilled persons in the art, without departing from the technical principles of the present application, several improvements and refinements can be made, which should also be considered within the protection scope of the present application.

Claims

1. A system for detecting cyanide in water, characterized by The application relates to a distillation device and a transfer device. The distillation device comprises a distillation bottle and a collection bottle arranged at the outlet end of the distillation bottle, wherein the distillation bottle is connected with the collection bottle through a liquid outlet pipe, a pinch valve is arranged on the liquid outlet pipe, and the pinch valve can pinch the liquid outlet pipe and block the communication between the distillation bottle and the collection bottle. The transfer device comprises a transfer assembly I arranged at the inlet end of the distillation bottle and a transfer assembly II arranged at the outlet end of the collection bottle. The transfer assembly I comprises an injection pump II, a peristaltic pump I, a three-way valve and a rotary valve I, one interface of the injection pump II, a common interface of the rotary valve I and the peristaltic pump I are connected with the three-way valve, the common interface of the rotary valve I is selectively communicated with the injection pump II or the peristaltic pump I, and one or more sub-interfaces of the rotary valve I are connected with the inlet end of the distillation bottle. The transfer assembly II comprises a rotary valve II, a peristaltic pump II, a constant pump I and an injection pump I, one interface of the injection pump I, the peristaltic pump II and the constant pump I are connected with the common interface of the rotary valve II in parallel, one or more sub-interfaces of the rotary valve II are connected with the outlet end of the collection bottle, one interface of the injection pump I is connected with a color developing device, and the color developing device comprises a constant pump II and a rotary valve III. The color developing device is connected with the transfer assembly II, the common end of the rotary valve III is connected with the outlet end of the constant pump II and the injection pump I respectively, and the sub-interfaces of the rotary valve III are connected with a waste liquid end and a cuvette respectively.

2. The system for cyanide detection in water of claim 1, wherein: The distillation device further comprises a heating device for heating the distillation bottle and a weighing device arranged at the lower end of the collection bottle and used for weighing.

3. The in-water cyanide detection system of claim 1, wherein: The inlet end pipeline of the distillation bottle extends to the bottom of the distillation bottle and can realize liquid inlet and liquid discharge; the outlet end pipeline of the collection bottle is located at the bottom of the collection bottle and can realize liquid discharge and liquid inlet.

4. The system for cyanide detection in water of claim 1, wherein: The transfer assembly I further comprises a diaphragm pump I, the outlet end of the diaphragm pump I is connected with the three-way valve in parallel after being connected with the peristaltic pump I; the transfer assembly II further comprises a diaphragm pump II, and the outlet end of the diaphragm pump II is connected with the common interface of the rotary valve II.

5. The in-water cyanide detection system of claim 1, wherein: The remaining interfaces of the injection pump II are respectively connected with a pure water end, an air end, a waste liquid end and a reagent bottle group I, the reagent bottle group I comprises EDTA-2Na reagent bottles, zinc nitrate reagent bottles, methyl orange reagent bottles, tartaric acid reagent bottles and phosphoric acid reagent bottles.

6. The in-water cyanide detection system of claim 1, wherein: The sub-interfaces of the rotary valve II are respectively connected with a waste liquid end, an air end and the outlet end of the collection bottle, the remaining interfaces of the injection pump I are respectively connected with a waste liquid end, an air end, a mother liquor end, a pure water end, a cuvette and a reagent bottle group II, and the reagent bottle group II comprises phosphate buffer reagent bottles and chloramine T reagent bottles.

7. The in-water cyanide detection system of claim 1, wherein: The sub-interfaces of the rotary valve I are further connected with a waste liquid end and an air end, the waste liquid end is used for discharging liquid in the pipeline, and the air end is used for accurately pushing solution reagents.

8. A method of detection using the cyanide detection system in water according to any one of claims 1 to 7, characterized in that, The application further discloses a method for detecting total cyanide and easily released cyanide in water. S0, system starting; S01, the injection pump I performs an extraction action on the cuvette to empty the cuvette; S02, according to the need, a sample is selected to make a sample type, the type comprising total cyanide or easily released cyanide; S03, sample, reagent quantitative transfer and distillation are performed on the distillation bottle; S2, distillate transfer: S21, mixing, air is delivered to the collection bottle through the rotary valve II by the injection pump I, and mixed by air blowing; S22, pipeline cleaning and filling, 10 ml sample in the collection bottle is extracted by the injection pump I through the rotary valve II, and the pipeline of the rotary valve III is filled; S23, sample transfer, 10 ml sample in the collection bottle is extracted by the injection pump I through the rotary valve II, and the sample is transferred to the colorimetric tube through the rotary valve III by air; S24, pipeline cleaning, 5 ml pure water is extracted by the injection pump I, and the pipeline of the rotary valve III is cleaned, and the liquid in the pipeline of the rotary valve III is exhausted by air; S3, reaction and reagent addition: S31, buffer solution addition, after the potassium dihydrogen phosphate buffer solution fills the pipeline of the injection pump I, 5 ml potassium dihydrogen phosphate buffer solution is transferred to the colorimetric tube through the rotary valve III by air; S32, chloramine T addition, after chloramine T fills the injection pump I, 0.3 ml chloramine T is transferred to the colorimetric tube through the rotary valve III by air; S33, pipeline cleaning, pure water is extracted by the injection pump I, and the pipeline of the rotary valve III is cleaned, and the liquid in the pipeline of the rotary valve III is exhausted by air; S34, stand for 2 min; S35, isonicotinic acid-barbituric acid addition, after isonicotinic acid-barbituric acid fills the pipeline of the injection pump I, 6 ml isonicotinic acid-barbituric acid is transferred to the colorimetric tube through the rotary valve III by air; S36, pipeline cleaning, pure water is extracted by the injection pump I, and the pipeline of the rotary valve III is cleaned, and the liquid in the pipeline of the rotary valve III is exhausted by air; S4, constant volume, 2.7 ml pure water is transferred to the colorimetric tube by the injection pump I for constant volume; S5, color development, the colorimetric tube is heated to 30 DEG C constant temperature, and color development is carried out for 10 min; S6, colorimetry: S61, zero adjustment: S611, colorimetric cell cleaning, pure water is transferred to the colorimetric cell by the injection pump I, and stands for 30 s, so that the light path is zeroed; S612, zero adjustment waste liquid discharge, the waste liquid in the colorimetric cell is discharged; S62, sample colorimetry: S621, wetting, the solution in the colorimetric tube is extracted by the injection pump I, and the colorimetric cell is wetted with the solution; S622, 3 ml solution in the colorimetric tube is extracted by the injection pump I and transferred to the colorimetric cell by air; S623, stand for 30 s, read the absorbance and substitute into the curve to calculate the concentration; S624, waste liquid discharge, the solution in the colorimetric cell is extracted and cleaned by pure water; S7, collection bottle waste discharge and cleaning: S71, after the sample is transferred to the colorimetric tube, the waste liquid in the collection bottle is discharged by the peristaltic pump II; S72, pure water is delivered to the colorimetric cell by the diaphragm pump II, and air is delivered by the peristaltic pump II for mixing; S73, the collection bottle is emptied by the peristaltic pump II; S8, distillation bottle waste discharge and cleaning: S81, the waste liquid in the distillation bottle is discharged by the peristaltic pump I; S82, pure water is delivered to the distillation bottle by the diaphragm pump I, and air is delivered by the peristaltic pump I for mixing; S83, the distillation bottle is emptied by the peristaltic pump I; S9, colorimetric tube waste discharge and cleaning: S91, the liquid in the colorimetric tube is discharged by the injection pump I, and the colorimetric tube is cleaned by pure water several times and emptied.

9. The method of claim 8, wherein: The sample preparation of total cyanide includes the following steps: S1, pre-distillation and total cyanide sample preparation: S11, sample transfer I, connect the distillation flask with peristaltic pump I and transfer the sample to the distillation flask; S12, distillation sample reagent addition: S121, EDTA-2Na addition, after EDTA-2Na fills the injection pump II pipeline, transfer 10 ml of EDTA-2Na to the distillation flask by air; S122, phosphoric acid addition, after phosphoric acid fills the injection pump II pipeline, transfer 10 ml of phosphoric acid to the distillation flask by air; S13, start weighing and zero; S14, absorbent addition, after NaOH fills the rotary valve II, transfer 10 ml of NaOH to the collection flask by the quantitative pump I; S15, heating distillation and weighing; S16, stop heating after the distillation sample weighs to the set value, and block the connection between the distillation flask and the collection flask by the pinch valve.

10. The method of claim 8, wherein: The sample preparation of the easily released cyanide includes the following steps: S1, pre-distillation and total cyanide sample preparation: S11, sample transfer I, connect the distillation flask with peristaltic pump I and transfer the sample to the distillation flask; S12, distillation sample reagent addition: S121, zinc nitrate addition, after zinc nitrate fills the injection pump II pipeline, transfer 10 ml of zinc nitrate to the distillation flask by air; S122, methyl orange addition, after methyl orange fills the injection pump II pipeline, transfer 0.4 ml of methyl orange to the distillation flask by air; S123, tartaric acid addition, after tartaric acid fills the injection pump II pipeline, transfer 5 ml of tartaric acid to the distillation flask by air; S13, start weighing and zero; S14, absorbent addition, after NaOH fills the rotary valve II, transfer 10 ml of NaOH to the collection flask by the quantitative pump I; S15, heating distillation and weighing; S16, stop heating after the distillation sample weighs to the set value, and block the connection between the distillation flask and the collection flask by the pinch valve.

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