Pretreatment device for detecting metal ions in organic sample and operation method thereof

Abstract

The invention discloses a pretreatment device for detecting metal ions in an organic sample. The pretreatment device comprises a liquid storage bottle I, a measuring cylinder, a liquid storage bottle II, a peristaltic pump I, a peristaltic pump II, a peristaltic pump III, a six-way plane valve, an ion exchange column, a three-way switching valve, a waste liquid bottle and a collection bottle. The metal ions in the organic sample are separated by adopting an ion exchange resin method, the operation is simple, and the separation speed is high; and high-temperature burning is not needed, smoke is not generated, and safety and environment friendliness are achieved.

Description

Technical Field

[0001] The present invention belongs to the field of organic sample detection, and is particularly applicable to the pretreatment stage when detecting the metal ion content in organic samples. Background Art

[0002] Generally, when detecting the metal ion content in organic samples, due to the high content of organic matter interfering with the detection results and causing inaccurate detection results, it is necessary to pretreat the sample to be detected to remove the organic matter in the sample and ensure the accuracy of the detection results. At present, when most enterprises detect metal ions in organic samples, they usually use the method of burning and ashing or catalytic digestion to remove the organic matter in the sample to be detected. However, both the burning and ashing method and the catalytic digestion method need to be carried out under high-temperature conditions, with high energy consumption, certain safety hazards, and long processing time. Especially, the burning and ashing method will generate a large amount of flue gas during the processing, and sometimes incomplete digestion will occur, resulting in organic matter residues. Summary of the Invention

[0003] Based on the problems existing in the prior art, the purpose of the present invention is to provide a pretreatment device for detecting metal ions in organic samples, which is simple to operate, has a fast separation speed, does not require high-temperature burning, does not generate flue gas, and is safe and environmentally friendly.

[0004] The purpose of the present invention is achieved through the following technical solutions: The pretreatment device for detecting metal ions in organic samples includes a storage bottle I, a measuring cylinder, a storage bottle II, a peristaltic pump I, a peristaltic pump II, a peristaltic pump III, a six-way flat valve, an ion exchange column, a three-way switching valve, a waste liquid bottle, and a collection bottle.

[0005] For the pretreatment device for detecting metal ions in organic samples, the six-way flat valve has six pipeline connection points and two rotary valve positions, which are respectively: the on position is that the ① position is communicated with the ② position, the ③ position is communicated with the ④ position, and the ⑤ position is communicated with the ⑥ position; the off position is that the ② position is communicated with the ③ position, the ④ position is communicated with the ⑤ position, and the ⑥ position is communicated with the ① position.

[0006] For the pretreatment device for detecting metal ions in organic samples, the three-way switching valve has three pipeline connection points and two rotary valve positions, which are respectively: the A position is that the inlet end is communicated with the A position, and the B position is that the inlet end is communicated with the B position.

[0007] For the pretreatment device for detecting metal ions in organic samples, the inlet end of the peristaltic pump I is connected to the storage bottle I through a pipeline; the outlet end is divided into two parts, one part is connected to the ① position of the six-way flat valve through a pipeline, and the other part is connected to the outlet end of the peristaltic pump II through a pipeline.

[0008] The pretreatment device for detecting metal ions in organic samples, the inlet end of the peristaltic pump II is connected to the measuring cylinder.

[0009] The pretreatment device for detecting metal ions in organic samples, the inlet end of the peristaltic pump III is connected to the storage bottle II through a pipeline, and the outlet end is connected to the 5th position of the six-way flat valve.

[0010] The pretreatment device for detecting metal ions in organic samples, the 6th position of the six-way flat valve is connected to the measuring cylinder through a pipeline, the 2nd position is connected to the inlet end of the ion exchange column through a pipeline, and the 4th position is connected to the outlet end of the ion exchange column through a pipeline.

[0011] The pretreatment device for detecting metal ions in organic samples, the inlet end of the three-way switching valve is connected to the 3rd position of the six-way flat valve through a pipeline, the A position of the outlet end of the three-way switching valve is connected to the waste liquid bottle, and the B position is connected to the collection bottle.

[0012] The pretreatment device for detecting metal ions in organic samples, the medium in the storage bottle I is deionized water, the medium in the measuring cylinder is the organic sample to be measured, the medium in the storage bottle II is 5-10 (wt)% hydrochloric acid solution, and the pipelines connected to the storage bottle I, the measuring cylinder, and the storage bottle II should extend to the bottom of the bottle.

[0013] The pretreatment device for detecting metal ions in organic samples has the following operating method: First, the organic sample in the graduated cylinder enters the inlet end of the ion exchange column successively through peristaltic pump II and positions ① and ② of the six-way flat valve, so that the organic sample contacts the strongly acidic cation resin in the ion exchange column, and the metal ions in the organic sample will be adsorbed on the strongly acidic cation resin. Then, deionized water in storage bottle I is injected into the graduated cylinder through peristaltic pump I and positions ① and ⑥ of the six-way flat valve. After the deionized water fills the graduated cylinder, it successively passes through peristaltic pump II, position ① of the six-way flat valve, position ② of the six-way flat valve, the ion exchange column, position ④ of the six-way flat valve, position ③ of the six-way flat valve, and the A position of the three-way exchange valve and then enters the waste liquid bottle. The operation is repeated three times to fully wash the organic sample attached to the inner wall of the graduated cylinder, the pipeline, and the ion exchange column. Then, deionized water directly passes through peristaltic pump I, position ① of the six-way flat valve, position ② of the six-way flat valve, the ion exchange column, position ④ of the six-way flat valve, position ③ of the six-way flat valve, and the A position of the three-way exchange valve and then enters the waste liquid bottle to wash the residual organic matter in the pipeline and the ion exchange column. Finally, the hydrochloric acid solution in storage bottle II is successively injected into the outlet end of the ion exchange column through peristaltic pump III and positions ⑤ and ④ of the six-way flat valve to backwash the ion exchange column, so that the metal ions adsorbed on the strongly acidic cation resin are desorbed under the flushing of the hydrochloric acid solution and enter the solution. The solution successively passes through the inlet end of the ion exchange column, positions ② and ③ of the six-way flat valve, and the B position of the three-way switching valve and then enters the collection bottle. The solution in the collection bottle is fixed to a certain volume with a volumetric flask and then used for analyzing the metal ion content.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) The device of the present invention does not need to be operated under high-temperature conditions, does not generate flue gas during the operation process, and the generated waste liquid can be harmlessly treated by a sewage treatment plant, which is safe and environmentally friendly; (2) The ion exchange resin of the present invention can be reused and has a low price, the power consumption of the whole device is very small, and the analysis cost is low; (3) The device of the present invention can prepare samples quickly, and the average preparation time for each sample is about 5 minutes, which improves the work efficiency; (4) The device of the present invention has a simple operation and a wide application range, and can be applied to the detection of metal ions in foods, drugs, chemical products, and organic samples that produce insoluble substances during high-temperature ashing. Description of the Drawings

[0015] The drawings are used to provide a further understanding of the present invention, and constitute a part of the specification. Together with the embodiments of the present invention, they are used to explain the present invention, but do not constitute a limitation to the present invention.

[0016] Figure 1 It is a schematic structural diagram of the present invention.

[0017] Figure 1Among them, 1 is the liquid storage bottle I, 2 is the graduated cylinder, 3 is the liquid storage bottle II, 4 is the peristaltic pump I, 5 is the peristaltic pump II, 6 is the peristaltic pump III, 7 is the six-way flat valve, 8 is the three-way switching valve, 9 is the waste liquid bottle, 10 is the collection bottle, and 11 is the ion exchange column. Embodiment

[0018] Refer to the attached Figure 1 , an embodiment of the present invention provides a pretreatment device for detecting metal ions in organic samples, including a liquid storage bottle I, a graduated cylinder, a liquid storage bottle II, a peristaltic pump I, a peristaltic pump II, a peristaltic pump III, a six-way flat valve, an ion exchange column, a three-way switching valve, a waste liquid bottle, and a collection bottle.

[0019] Another difference in another embodiment is that the valve core material of the six-way flat valve is polytetrafluoroethylene; the driving force is electric or manual; it has six pipeline connection points and two rotary valve positions, which are: the on position is that the first position is communicated with the second position, the third position is communicated with the fourth position, and the fifth position is communicated with the sixth position; the off position is that the second position is communicated with the third position, the fourth position is communicated with the fifth position, and the sixth position is communicated with the first position.

[0020] Another difference in another embodiment is that the valve core material of the three-way switching valve is polytetrafluoroethylene; the driving force is electric or manual; it has three pipeline connection points and two rotary valve positions, which are: the A position is that the inlet end is communicated with the A position, and the B position is that the inlet end is communicated with the B position.

[0021] Another difference in another embodiment is that the inlet end of the peristaltic pump I is connected to the liquid storage bottle I through a pipeline; the outlet end is divided into two parts, one part is connected to the first position of the six-way flat valve through a pipeline, and the other part is connected to the outlet end of the peristaltic pump II through a pipeline.

[0022] Another difference in another embodiment is that the inlet end of the peristaltic pump II is connected to the graduated cylinder.

[0023] Another difference in another embodiment is that the inlet end of the peristaltic pump III is connected to the liquid storage bottle II through a pipeline, and the outlet end is connected to the fifth position of the six-way flat valve.

[0024] Another difference in another embodiment is that the sixth position of the six-way flat valve is connected to the graduated cylinder through a pipeline, the second position is connected to the inlet end of the ion exchange column through a pipeline, and the fourth position is connected to the outlet end of the ion exchange column through a pipeline.

[0025] Another difference in another embodiment is that the inlet end of the three-way switching valve is connected to the third position of the six-way flat valve through a pipeline, the A position of the outlet end of the three-way switching valve is connected to the waste liquid bottle, and the B position is connected to the collection bottle.

[0026] Another embodiment is different in that the medium in the liquid storage bottle I is deionized water, the medium in the measuring cylinder is the organic sample to be measured, the medium in the liquid storage bottle II is a 5-10 (wt)% hydrochloric acid solution, and the pipelines connected to the liquid storage bottle I, the measuring cylinder and the liquid storage bottle II should all extend to the bottom of the bottle.

[0027] Another embodiment is different in that the pipeline is made of polytetrafluoroethylene with an inner diameter of 2-5 mm.

[0028] Another embodiment is different in that the outer tube of the ion exchange column is made of polytetrafluoroethylene or glass, with an inner diameter of 5-10 mm and a length of 10-20 cm, and is filled with strongly acidic cation resin inside; the inlet end and the outlet end are filled with absorbent cotton to filter out mechanical impurities in the organic sample and prevent resin particles from entering the pipeline to cause blockage.

[0029] The following will further elaborate on the detection method of the present invention in combination with specific embodiments. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention and are not used to limit the present invention.

[0030] The sample to be measured is the outlet material of the acetylenation reactor in the production of 1,4-butanediol by the acetylene aldehyde method. The material is an aqueous solution containing 40-55 (wt)% of 1,4-butynediol and 0.3-1.5 mg / L of copper ions. When detecting the copper ion content in the material, it is necessary to first prepare 50 mL of an aqueous solution with the same copper ion content as the sample to be measured and without 1,4-butynediol.

[0031] The operation steps are as follows: Step 1, use a measuring cylinder (2) to measure 50 mL of the sample to be measured, and insert the inlet pipeline of the peristaltic pump II (5) and the pipeline connecting to the ⑥ position of the six-way flat valve (7) into the bottom of the measuring cylinder at the same time.

[0032] Step 2, turn the six-way flat valve (7) to the on position and the three-way switching valve (8) to the A position, turn on the peristaltic pump II (5), and inject all the samples in the measuring cylinder (2) into the inlet end of the ion exchange column (11) successively through the peristaltic pump II (5), the ① position and the ② position of the six-way flat valve (7), so that the copper ions in the sample are adsorbed on the strongly acidic cation resin in the ion exchange column (11); the waste liquid flows out from the outlet end of the ion exchange column (11), passes through the ④ position and the ③ position of the six-way flat valve (7) and enters the three-way switching valve (8), and is discharged into the waste liquid bottle (9) from the outlet end A pipeline of the three-way switching valve (8).

[0033] Step 3: Turn off the peristaltic pump II (5), turn the six-way flat valve (7) to the off position, turn on the peristaltic pump I (4), and let the deionized water in the liquid storage bottle I (1) enter the measuring cylinder (2) successively through the peristaltic pump I (4), the first position and the sixth position of the six-way flat valve (7) to wash the inner wall of the measuring cylinder (2). When the deionized water fills the measuring cylinder (2) to form a displacement liquid, turn off the peristaltic pump I (4), turn the six-way flat valve (7) to the on position, turn on the peristaltic pump II (5), and inject the displacement liquid in the measuring cylinder (2) into the inlet end of the ion exchange column (11) successively through the peristaltic pump II (5), the first position and the second position of the six-way flat valve (7). The waste liquid flows out from the outlet end of the ion exchange column (11), enters the three-way switching valve (8) through the fourth position and the third position of the six-way flat valve (7), and is discharged into the waste liquid bottle (9) through the pipeline at the A position of the outlet end of the three-way switching valve (8).

[0034] Step 4: After repeating the operation in Step 3 three times, turn off the peristaltic pump II (5), turn on the peristaltic pump I (4), and let the deionized water in the liquid storage bottle I (1) be injected into the inlet end of the ion exchange column (11) through the peristaltic pump I (4), the first position and the second position of the six-way flat valve (7). Rinse the pipeline and the ion exchange column (11) for another 15 - 30 seconds to fully remove the residual 1,4-butynediol in the pipeline and the ion exchange column. The rinsed waste liquid flows out from the outlet end of the ion exchange column (11), enters the three-way switching valve (8) through the fourth position and the third position of the six-way flat valve (7), and is discharged into the waste liquid bottle (9) through the pipeline at the A position of the outlet end of the three-way switching valve (8).

[0035] Step 5: Turn off the peristaltic pump I (4), turn the six-way flat valve (7) to the off position and the three-way switching valve (8) to the B position, turn on the peristaltic pump III (6), and inject the hydrochloric acid solution in the liquid storage bottle II (3) into the outlet end of the ion exchange column (11) through the peristaltic pump III (6), the fifth position and the fourth position of the six-way flat valve (7) to backwash the ion exchange column (11). After the copper ions adsorbed on the ion exchange column (11) are desorbed, they enter the three-way switching valve (8) through the second position and the third position of the six-way flat valve (7), and are discharged into the collection bottle (10) through the pipeline at the B position of the outlet end of the three-way switching valve (8).

[0036] Step 6: Turn off the peristaltic pump III (6), turn the six-way flat valve to the on position and the three-way switching valve (8) to the A position, turn on the peristaltic pump I (4), and let the deionized water in the liquid storage bottle I (1) be injected into the inlet end of the ion exchange column (11) through the peristaltic pump I (4), the first position and the second position of the six-way flat valve (7). Rinse the ion exchange column (11) for 15 - 30 seconds to remove the residual hydrochloric acid solution. The waste liquid flows out from the outlet end of the ion exchange column (11), enters the three-way switching valve (8) through the fourth position and the third position of the six-way flat valve (7), and is discharged into the waste liquid bottle (9) through the pipeline at the A position of the outlet end of the three-way switching valve (8).

[0037] Step 7: Turn off the peristaltic pump I (4), reset the device, transfer all the solution in the collection bottle (10) to a 50 mL volumetric flask, make up the volume to the 50 mL graduation line with deionized water, and shake well to complete the sample preparation.

Claims

1. A pretreatment device for detecting metal ions in organic samples, characterized in that: It includes a liquid storage bottle Ⅰ, a graduated cylinder, a liquid storage bottle Ⅱ, a peristaltic pump Ⅰ, a peristaltic pump Ⅱ, a peristaltic pump Ⅲ, a six-way flat valve, an ion exchange column, a three-way switching valve, a waste liquid bottle, and a collection bottle; the six-way flat valve has six pipeline connection points and two rotary valve positions, which are respectively: the on position is that the ① position is communicated with the ② position, the ③ position is communicated with the ④ position, and the ⑤ position is communicated with the ⑥ position; the off position is that the ② position is communicated with the ③ position, the ④ position is communicated with the ⑤ position, and the ⑥ position is communicated with the ① position; the three-way switching valve has three pipeline connection points and two rotary valve positions, which are respectively: the A position is that the inlet end is communicated with the A position, and the B position is that the inlet end is communicated with the B position.

2. The pretreatment device for detecting metal ions in organic samples according to claim 1, characterized in that: The inlet end of the peristaltic pump Ⅰ is connected to the liquid storage bottle Ⅰ through a pipeline; the outlet end of the peristaltic pump Ⅰ is divided into two parts, one part is connected to the ① position of the six-way flat valve through a pipeline, and the other part is connected to the outlet end of the peristaltic pump Ⅱ through a pipeline; the inlet end of the peristaltic pump Ⅱ is connected to the graduated cylinder; the inlet end of the peristaltic pump Ⅲ is connected to the liquid storage bottle Ⅱ through a pipeline, and the outlet end is connected to the ⑤ position of the six-way flat valve; the ⑥ position of the six-way flat valve is connected to the graduated cylinder through a pipeline, the ② position is connected to the inlet end of the ion exchange column through a pipeline, and the ④ position is connected to the outlet end of the ion exchange column through a pipeline; the inlet end of the three-way switching valve is connected to the ③ position of the six-way flat valve through a pipeline, the A position of the outlet end of the three-way switching valve is connected to the waste liquid bottle, and the B position is connected to the collection bottle.

3. The pretreatment device for detecting metal ions in organic samples according to claim 2, characterized in that: The medium in the liquid storage bottle Ⅰ is deionized water, the medium in the graduated cylinder is the organic sample to be measured, and the medium in the liquid storage bottle Ⅱ is a 5-10 (wt)% hydrochloric acid solution. The pipelines connected to the liquid storage bottle Ⅰ, the graduated cylinder, and the liquid storage bottle Ⅱ should all extend to the bottom of the bottle.

4. The pretreatment device for detecting metal ions in organic samples according to claim 2, characterized in that: The resin filled in the ion exchange column is a strongly acidic cation resin.

5. An operation method of the pretreatment device for detecting metal ions in organic samples, characterized in that: First, the organic sample in the graduated cylinder enters the inlet end of the ion exchange column successively through peristaltic pump II and the 1st position and 2nd position of the six-way flat valve, so that the organic sample contacts the strongly acidic cation resin in the ion exchange column, and the metal ions in the organic sample will be adsorbed on the strongly acidic cation resin. Then, deionized water in storage bottle I is injected into the graduated cylinder through peristaltic pump I and the 1st position and 6th position of the six-way flat valve. After the graduated cylinder is filled with deionized water, it successively passes through peristaltic pump II, the 1st position of the six-way flat valve, the 2nd position of the six-way flat valve, the ion exchange column, the 4th position of the six-way flat valve, the 3rd position of the six-way flat valve, and the A position of the three-way switching valve and then enters the waste liquid bottle. The operation is repeated three times to fully rinse the organic sample attached to the inner wall of the graduated cylinder, the pipeline, and the ion exchange column. Then, deionized water directly passes through peristaltic pump I, the 1st position of the six-way flat valve, the 2nd position of the six-way flat valve, the ion exchange column, the 4th position of the six-way flat valve, the 3rd position of the six-way flat valve, and the A position of the three-way switching valve and then enters the waste liquid bottle to rinse the residual organic matter in the pipeline and the ion exchange column. Finally, the hydrochloric acid solution in storage bottle II is injected into the outlet end of the ion exchange column successively through peristaltic pump III and the 5th position and 4th position of the six-way flat valve to backwash the ion exchange column, so that the metal ions adsorbed on the strongly acidic cation resin are desorbed and enter the solution under the flushing of the hydrochloric acid solution. The solution successively passes through the inlet end of the ion exchange column, the 2nd position and 3rd position of the six-way flat valve, and the B position of the three-way switching valve and then enters the collection bottle. The solution in the collection bottle is fixed to a certain volume with a volumetric flask and then used for analyzing the metal ion content.

Images