Reaction device for measuring arsenic in water bath

Abstract

The utility model relates to the technical field of hydrometallurgy, in particular to a reaction device for measuring arsenic in water bath, which comprises a water bath cup and a reaction cup, the inner side of the water bath cup is hermetically provided with the reaction cup with the top edge higher than the water bath cup, the top of the reaction cup is hermetically connected with a teflon cover, and the top of the teflon cover is provided with two vertically through mounting holes. A sealing plug is hermetically sleeved in one mounting hole, an air outlet pipe is hermetically sleeved in the other mounting hole, one end of the air outlet pipe far away from the reaction cup is fixedly communicated with a hose, one end of the hose far away from the air outlet pipe is fixedly communicated with a single-hole air pipe, and one end of the single-hole air pipe far away from the hose is hermetically and fixedly communicated with an absorption bottle; a water bath module and a reaction module are separated through a split type water bath, so that cleaning after reaction is facilitated, and the problem that a large black object generated by a standard sample is difficult to clean in the arsenic measurement process of a silver salt method is solved; the requirements of manual measurement, automatic measurement and arsenic spot method measurement are met, the operation is simple and rapid, and the arsenic measurement efficiency is improved.

Description

TECHNICAL FIELD

[0001] The utility model relates to the technical field of hydrometallurgy, especially relates to a reaction device for water bath arsenic determination. BACKGROUND

[0002] In the hydrometallurgical production process, silver salt method is a common arsenic determination method. In the nickel salt refining and purification industry, the complex nickel sulfate solution is often used as raw material, and the common impurity metal elements in the nickel sulfate solution include copper, arsenic, antimony, bismuth, zinc, iron, cobalt, lead, calcium, magnesium and the like, so that the technology involved in the nickel salt refining and purification industry is mainly the deep removal technology of various impurity elements in the nickel salt solution and the testing technology of trace impurity elements.

[0003] The current commonly used arsenic content testing methods in the hydrometallurgical industry include silver salt method, arsenic spot method, atomic fluorescence method and the like. The silver salt method has low detection limit and high sensitivity, but the device used in the silver salt method is complex to operate, a water bath kettle is needed in the testing process, and when the arsenic standard solution is used as the to-be-tested solution for reaction, a large amount of black gray substance is generated, the reaction bottle is mostly a ground-in mouth conical bottle with a small bottle opening, the bottle opening is easy to be blocked, and the bottle opening is difficult to clean. Therefore, the current silver salt method arsenic determination device can only meet manual measurement, and cannot meet the demand of automatic measurement. UTILITY MODEL CONTENT

[0004] The utility model provides a kind of reaction device for water bath arsenic determination, overcome the above-mentioned prior art, it can effectively solve the problem of existing silver salt method arsenic determination device only manual measurement cannot be automated measurement.

[0005] To solve the above problems, the utility model discloses a kind of reaction device for water bath arsenic determination, including water bath cup and reaction cup, reaction cup is sealedly installed in water bath cup inside, and the top edge of reaction cup is higher than the height of water bath cup, reaction cup is inverted conical, four fluorine cover is sealedly connected in the top of reaction cup, two upper and lower through installation holes are located in the top of four fluorine cover, one installation hole is sealedly equipped with sealing plug in it, another installation hole is sealedly equipped with gas outlet pipe in it, gas outlet pipe is fixedly communicated with hose away from reaction cup, hose is fixedly communicated with single-hole gas pipe away from gas outlet pipe, single-hole gas pipe is fixedly communicated with absorption bottle away from hose, and single-hole gas pipe outlet is located in the bottom of absorption bottle, and upwardly inclined exhaust port is fixedly communicated on the outside of absorption bottle upper side;Reagent inlet and water suction port that inner tube penetrates are located in the top of four fluorine cover;Water bath inlet is fixedly communicated on the outside of water bath cup lower side, and water bath outlet is fixedly communicated on the outside of water bath cup upper side.

[0006] The fixed sleeve is provided with at least two groups of fixing components which are symmetrically arranged in the radial direction on the fixing gasket, each group of fixing components comprises a fixing screw, and the fixing gasket at the position of each group of fixing components is provided with an upper threaded hole which is vertically penetrated.

[0007] The absorption bottle is placed in the absorption bottle base.

[0008] The water bath cup is sealingly connected with the reaction cup through the sealing gasket one.

[0009] The reaction cup is sealingly connected with the tetrafluoro cover through the sealing gasket two.

[0010] The tetrafluoro cover is provided with a circular boss which can be embedded in the inner side of the reaction cup, and the circular boss and the reaction cup are provided with an O-shaped sealing ring two.

[0011] The utility model discloses a split type water bath which separates the water bath and the reaction two modules, and the reaction cup is designed as an inverted cone, so that the reaction cup is convenient to clean after reaction, and the problem that the standard sample generates large black objects which are difficult to clean in the process of measuring arsenic by the silver salt method is solved. BRIEF DESCRIPTION OF DRAWINGS

[0012] The specific embodiments of the utility model will be further and specifically explained in combination with the drawings.

[0013] Figure 1 It is the overall structure schematic diagram of the utility model.

[0014] Figure 2 It is the overhead structure schematic diagram of the tetrafluoro cover in the utility model.

[0015] Figure 3 It is the structure schematic diagram of the water bath cup in the utility model.

[0016] Figure 4 It is the structure schematic diagram of the absorption bottle base in the utility model.

[0017] In the diagram: 1-Water bath cup, 2-Reaction cup, 3-PTFE cap, 4-Sealing plug, 5-Gas outlet pipe, 6-Hose, 7-Single-hole gas pipe, 8-Absorption bottle, 9-Exhaust port, 10-Reagent inlet, 11-Water outlet, 12-Water bath inlet, 13-Water bath outlet, 14-Fixing gasket, 15-Fixing screw, 16-O-ring one, 17-Absorption bottle base, 18-Sealing gasket one, 19-Sealing gasket two, 20-Circular boss, 21-O-ring two. Detailed Implementation

[0018] This utility model is not limited to the following embodiments, and the specific implementation method can be determined according to the technical solution of this utility model and the actual situation.

[0019] like Figures 1-3 As shown, a reaction apparatus for arsenic determination in a water bath includes a water bath cup 1 and a reaction cup 2. The reaction cup 2, with its top edge higher than the height of the water bath cup 1, is sealed inside the water bath cup 1. The reaction cup 2 is inverted conical in shape. A PTFE cap 3 is sealed to the top of the reaction cup 2. The PTFE cap 3 has two through-holes on its top. A sealing plug 4 is sealed in one of the holes, and an outlet pipe 5 is sealed in the other hole. A flexible tube 6 is fixedly connected to the end of the outlet pipe 5 away from the reaction cup 2. A single-hole gas pipe 7 is fixedly connected to the end of the single-hole gas pipe 7 away from the flexible tube 6. An absorption bottle 8 is sealed and fixedly connected to the end of the single-hole gas pipe 7 away from the flexible tube 6, and the outlet of the single-hole gas pipe 7 is located at the bottom of the absorption bottle 8. An upwardly inclined exhaust port 9 is fixedly connected to the upper side of the absorption bottle 8. The top of the PTFE cap 3 has a reagent inlet 10 and a water outlet 11 with an inner tube. A water bath inlet 12 is fixedly connected to the lower side of the water bath cup 1, and a water bath outlet 13 is fixedly connected to the upper side of the water bath cup 1.

[0020] Among them, the water bath cup 1, reaction cup 2, gas outlet pipe 5, single-hole gas pipe 7, and absorption bottle 8 are all made of high borosilicate glass; the PTFE cap 3 is made of polytetrafluoroethylene; the flexible tube 6 is made of latex or rubber; and the sealing plug 4 is made of polytetrafluoroethylene.

[0021] The system includes a flexible hose 6 that connects the outlet pipe 5 to the single-hole pipe 7, facilitating cleaning after the reaction is complete.

[0022] The absorption bottle 8 is equipped with an exhaust port 9 for the gas inside the absorption bottle 8 to be discharged. The exhaust port 9 is set in an upward-facing inclined shape to prevent the reaction inside the absorption bottle 8 from being too violent and causing the internal solution to overflow.

[0023] like Figures 1-2As shown, the water bath cup 1 top is equipped with sealing gasket one 18, water bath cup 1 and reaction cup 2 are sealedly connected through sealing gasket one 18.Sealing gasket one 18 is rubber material or silica gel material. Thus, effectively reduce the loss of water in water bath cup 1 in the reaction process.

[0024] Wherein, O type sealing ring one 16 is rubber material or silica gel material; Fixed washer 14 is polytetrafluoroethylene material.

[0025] As shown, the water bath cup 1 top is equipped with sealing gasket one 18, water bath cup 1 and reaction cup 2 are sealedly connected through sealing gasket one 18.Sealing gasket one 18 is rubber material or silica gel material. Thus, effectively reduce the loss of water in water bath cup 1 in the reaction process. Figure 4 As shown, the reaction cup 2 top is equipped with sealing gasket two 19, and the reaction cup 2 top and the tetrafluoro cap 3 are sealedly connected through the sealing gasket two 19. The sealing gasket two 19 is rubber material or silica gel material.

[0026] As shown, the water bath cup 1 top is equipped with sealing gasket one 18, water bath cup 1 and reaction cup 2 are sealedly connected through sealing gasket one 18.Sealing gasket one 18 is rubber material or silica gel material. Thus, effectively reduce the loss of water in water bath cup 1 in the reaction process. Figure 1 As shown, the reaction cup 2 top is equipped with sealing gasket two 19, and the reaction cup 2 top and the tetrafluoro cap 3 are sealedly connected through the sealing gasket two 19. The sealing gasket two 19 is rubber material or silica gel material.

[0027] As shown, the reaction cup 2 top is equipped with sealing gasket two 19, and the reaction cup 2 top and the tetrafluoro cap 3 are sealedly connected through the sealing gasket two 19. The sealing gasket two 19 is rubber material or silica gel material. Figure 1 As shown, the tetrafluoro cap 3 bottom is equipped with a circular boss 20 capable of being embedded in the inner side of the reaction cup 2, and the circular boss 20 and the reaction cup 2 are equipped with O type sealing ring two 21. The O type sealing ring two 21 is rubber material or silica gel material.

[0028] Figure 1 As shown, the tetrafluoro cap 3 bottom is equipped with a circular boss 20 capable of being embedded in the inner side of the reaction cup 2, and the circular boss 20 and the reaction cup 2 are equipped with O type sealing ring two 21. The O type sealing ring two 21 is rubber material or silica gel material.

[0029] The specific working process of the utility model is as follows:

[0030] ​The testing process of the DDTC-Ag method is as follows: the cotton in the air outlet tube 5 is replaced before measurement, the air outlet tube 5 is inserted into one mounting hole of the tetrafluoro cap 3, the sampler is controlled to quantitatively sample (arsenic standard solution / sample to be measured), a quantitative (settable) reagent (sulfuric acid, potassium iodide, stannous chloride, water) is extracted by using a syringe pump and is injected into the corresponding reaction cup 2; after standing for 10 minutes (settable), zinc particles are manually added (the zinc particles can be added through the other hole of the tetrafluoro cap 3), then the sealing plug 4 is covered, the generated arsine gas is completely absorbed in the prepared absorption bottle 8 containing the DDTC-Ag solution, and the absorption time is greater than 30 minutes (settable); after the reaction is completed, the liquid in the absorption bottle 8 is poured into a cuvette to measure the absorbance.

[0031] The testing process of the arsenic spot method is as follows: a special air guide tube for measuring arsenic by the arsenic spot method is used, the air guide tube is inserted into the mounting hole of the tetrafluoro cap 3, and then the measurement can be performed; the sampler is controlled to quantitatively sample (arsenic standard solution / sample to be measured), a quantitative (settable) reagent (sulfuric acid, potassium iodide, stannous chloride, water) is extracted by using a syringe pump and is injected into the corresponding reaction cup 2; after standing for 10 minutes (settable), zinc particles are manually added (the zinc particles can be added through the other hole of the tetrafluoro cap 3), then the sealing plug 4 is covered, the generated arsine gas is completely absorbed by the mercuric bromide test paper, the mercuric bromide test paper is removed after the reaction is completed, and the color of the arsenic spot of the sample to be measured is compared with the color of the arsenic spot of the standard solution. The concentration value of the arsenic content of the sample to be measured is determined, and the arsenic content in the sample is calculated according to the sampling amount of the sample.

[0032] Therefore, the two mounting holes of the tetrafluoro cap 3 are 19-gauge mounting holes, which can be compatible with the DDTC-Ag method and the arsenic spot method, thereby improving the use value of the device.

[0033] In summary, the water bath and the reaction module are separated by the split type water bath, so that the reaction can be cleaned after the reaction, and the problem that a large black object is difficult to clean in the process of measuring arsenic by the silver salt method is solved; meanwhile, the two mounting holes of the tetrafluoro cap 3 are convenient for subsequent use of other detection devices, so that the device is compatible with manual measurement, automatic measurement and arsenic spot measurement, the operation is simple and fast, and the efficiency of measuring arsenic is improved.

Claims

1. A reaction device for water bath arsenic determination, characterized in that, The utility model provides a water bath cup and reaction cup, the water bath cup inside sealed installation has the reaction cup of top edge higher than water bath cup height, the reaction cup is inverted conical, the reaction cup top sealed connection has tetrafluoro lid, tetrafluoro lid top is equipped with two up and down through -going mounting hole, one mounting hole is sealed in the sleeve and is equipped with sealed plug, another mounting hole is sealed in the sleeve and is equipped with the gas pipe, the gas pipe far away from the one end fixed communication of reaction cup has the hose, the hose far away from the one end fixed communication of gas pipe has single -hole gas pipe, single -hole gas pipe far away from the one end sealed fixed communication of hose has the absorption bottle, and single -hole gas pipe export is located absorption bottle's bottom, absorption bottle outside upper side fixed communication has the exhaust port of upwards inclination;Tetrafluoro lid top is equipped with the reagent import and pumping outlet of inner tube through -going;Water bath cup outside lower side fixed communication has water bath import, and water bath cup outside upper side fixed communication has water bath export.

2. The reaction device for water bath arsenic determination according to claim 1, characterized in that, Still include fixed sleeve, each mounting hole is sealed in the sleeve and is equipped with fixed sleeve, and the fixed sleeve is located one -end integral molding of fixed washer on mounting hole upper side, and fixed washer is equipped with at least two groups of fixed components on radial symmetry on fixed washer, and each group of fixed components includes a fixed screw, and the fixed washer on each group of fixed component position is equipped with the upper threaded hole of up and down through -going, and the threaded hole position of corresponding screw is equipped with the screw thread blind hole of opening upwards on tetrafluoro lid, and the lower end of each fixed screw is all screwed in threaded blind hole in corresponding position after passing through the upper threaded hole.

3. The reaction device for water bath arsenic determination according to claim 1, characterized in that, Still include absorption bottle base, absorption bottle bottom is equipped with absorption bottle base, and absorption bottle is placed in absorption bottle base.

4. The reaction device for water bath arsenic determination according to claim 1, characterized in that, The water bath cup top is equipped with sealing washer one, and the water bath cup and the reaction cup are sealedly connected through sealing washer one.

5. The reaction device for water bath arsenic determination according to claim 1, characterized in that, The reaction cup top is equipped with sealing washer two, and the reaction cup top and the tetrafluoro lid are sealedly connected through sealing washer two.

6. The reaction device for water bath arsenic determination according to claim 1, characterized in that, The tetrafluoro lid bottom is equipped with the circular boss of being able to embed the water bath cup inside, and the circular boss and the water bath cup are equipped with O type sealing washer two between.

Images