A cleaning device and cleaning method for ICP atomization chamber

Abstract

The present invention discloses a cleaning device and a cleaning method for an ICP atomization chamber. The cleaning device includes an ICP atomization chamber, a conversion tee, a filter, a solution tank, and a circulation pump, etc. The circulation pump is mainly used to drive the cleaning solution to repeatedly circulate and rinse the ICP atomization chamber, and the sample inlet, sample outlet, and waste liquid end of the ICP atomization chamber are simultaneously cleaned by the conversion tee, so as to avoid the risk of long-term contact with high-concentration strong acid in the traditional cleaning method, and the operation is simple, the cleaning efficiency is high, the safety is non-hazardous, and the damage to the ICP atomization chamber is avoided. At the same time, since the filter is a detachable structure, the filtration of cleaning dirt can be achieved, the secondary contamination of the cleaning solution tank or the ultrapure water tank can be avoided, and a group of cleaning solutions can be repeatedly used, which greatly reduces the cleaning cost. In addition, the ICP atomization chamber is clean and clean after cleaning and drying. After the instrument is installed, no effusion is generated at the sample inlet, and the atomization effect is good, so that the atomization gas flow rate and atomization pressure indicators of the instrument are normal, and the accuracy of the test results is guaranteed.

Description

Technical Field

[0001] The invention relates to a cleaning structure and a processing method of an ICP atomization chamber, namely, a cleaning device and a cleaning method of an ICP atomization chamber. Background Art

[0002] The ICP spray chamber is the sample atomization site for inductively coupled plasma emission spectrometers and inductively coupled plasma mass spectrometers. The ICP spray chamber is generally used in conjunction with a nebulizer, usually made of quartz glass, and a small number of polymer materials such as polytetrafluoroethylene. The structure of the ICP spray chamber is unique, with small inner diameters at the sample inlet, sample outlet, and waste liquid ends and a wide internal cavity, so it is quite difficult to clean. In the daily testing process, since the ICP spray chamber is used to atomize samples of different types and concentrations for a long time, it is easy to scale inside, resulting in a poor atomization effect, and even the introduction of impurities in the dirt, affecting the accuracy of the test results. Therefore, it is particularly important to ensure the cleanliness of the ICP spray chamber.

[0003] Generally speaking, when the sample inlet of the ICP atomization chamber generates liquid accumulation or abnormal yellowing, the ICP atomization chamber needs to be cleaned in time. The traditional cleaning method is to dismantle the ICP atomization chamber and soak it in a high-concentration strong acid. However, due to the strong adhesion of dirt, it needs to be soaked for 12 hours or even 24 hours, and then cleaned with pure water. This cleaning method is time-consuming and dangerous, and the cleaning solution cannot be reused, which increases the cleaning cost. At the same time, the existing patents do not involve a better cleaning method for the ICP atomization chamber. For example, the Chinese patent CN210520359U mentions a method of using a cleaning brush to extend into the interior of the ICP atomization chamber for brushing. The operation process is quite troublesome, especially due to the limitation of the brush's surface, which easily leads to incomplete cleaning, poor cleaning effect, and even scratches the inner wall of the ICP atomization chamber. If you are not careful, it will also cause the ICP atomization chamber to be broken and damaged.

[0004] In summary, the traditional ICP spray chamber cleaning method is not only time-consuming and dangerous, but also has the risk of damaging the ICP spray chamber. Obviously, it is very necessary to provide a cleaning method that is simple to operate, safe, harmless, fast and effective, and does not cause any damage to the ICP spray chamber. Summary of the invention

[0005] The technical problem to be solved by the present invention is to overcome the defects of the prior art and provide an ICP atomization chamber cleaning device and a cleaning method which are simple to operate, safe, non-hazardous, fast and effective, have low cleaning costs, good cleaning effects, and will not cause any damage to the ICP atomization chamber.

[0006] The technical problem of the present invention is achieved through the following technical solutions:

[0007] A cleaning device for an ICP atomization chamber comprises an ICP atomization chamber, a filter, a solution tank and a circulation pump. The ICP atomization chamber has an injection end, an output end and a waste liquid end. The filter has a filter inlet and a filter outlet. The solution tank has a solution inlet and a solution outlet. The output end and the waste liquid end of the ICP atomization chamber are combined and connected to the filter inlet of the filter, the filter outlet of the filter is connected to the solution inlet of the solution tank, the solution outlet of the solution tank is connected to the circulation pump, and then connected to the injection end of the ICP atomization chamber.

[0008] The solution tank is a cleaning solution tank or an ultrapure water tank.

[0009] A conversion tee is provided between the ICP atomization chamber and the filter, and the conversion tee has a first port, a second port and a third port; the sample outlet and waste liquid end of the ICP atomization chamber are respectively connected to the first port and the second port of the conversion tee; the third port of the conversion tee is connected to the filter inlet of the filter.

[0010] Connecting pipes are provided between the sample inlet and the circulation pump, between the sample outlet and the first port, and between the waste liquid end and the second port. The connecting pipes are acid-resistant polytetrafluoroethylene hoses.

[0011] The filter is provided with a 0.22 μm high molecular microporous filter membrane.

[0012] The first port, the second port and the third port of the conversion tee are respectively provided with valves which can be independently controlled to open and close.

[0013] The cleaning solution tank is filled with dilute nitric acid with a mass concentration of 2% to 10%, and the ultrapure water tank is filled with ultrapure water.

[0014] The rotation speed of the circulating pump is 60rpm~100rpm.

[0015] A method for cleaning an ICP atomization chamber comprises the following steps:

[0016] ① Assemble the removed ICP spray chamber to be cleaned together with the conversion tee, filter, cleaning solution tank, and circulation pump into a complete cleaning device, that is, the sample outlet and waste liquid end of the ICP spray chamber are connected to the first port and the second port of the conversion tee respectively, the third port of the conversion tee is connected to the filter inlet of the filter, the filter outlet of the filter is connected to the solution inlet of the cleaning solution tank, and the solution outlet of the cleaning solution tank is connected to the sample inlet of the ICP spray chamber through the circulation pump;

[0017] ② Close the first port of the conversion tee and keep the second and third ports open;

[0018] ③ Start the circulation pump and clean the injection end and waste liquid end of the ICP nebulizer chamber;

[0019] ④ After the sample inlet and waste liquid ends of the ICP spray chamber are cleaned, turn off the circulation pump;

[0020] ⑤ Close the second port of the conversion tee and keep the first and third ports open;

[0021] ⑥ Start the circulation pump and clean the sample inlet and outlet of the ICP spray chamber;

[0022] ⑦ After the sample inlet and sample outlet of the ICP spray chamber are cleaned, turn off the circulation pump;

[0023] ⑧ Remove the filter from the cleaning device, clean it with ultrapure water, and then reinstall it into the cleaning device;

[0024] ⑨ Remove the cleaning solution tank in the cleaning device, replace it with an ultrapure water tank, and then reinstall it into the cleaning device;

[0025] ⑩Repeat steps ② to ⑧;

[0026] ⑪ Remove the ICP atomization chamber in the cleaning device and use pure compressed air to blow the ICP atomization chamber until it is dry;

[0027] ⑫ Observe whether there is any residual attachment in the ICP atomization chamber. If it is still not clean, repeat steps ① to ⑪ until the ICP atomization chamber is clean.

[0028] The time for cleaning the injection end and the waste liquid end of the ICP nebulizer chamber in step ③ is 10min~30min; the time for cleaning the injection end and the sample outlet end of the ICP nebulizer chamber in step ⑥ is 10min~20min; the time for blowing the ICP nebulizer chamber with compressed air until it is dry in step ⑪ is 10min~15min.

[0029] Compared with the prior art, the present invention provides a unique cleaning device and cleaning method that can be used for cleaning an ICP atomization chamber. The cleaning device is mainly composed of an ICP atomization chamber, a conversion tee, a filter, a solution tank and a circulation pump, etc. The ICP atomization chamber has an injection end, an output end and a waste liquid end, the filter has a filter inlet and a filter outlet, the solution tank has a solution inlet and a solution outlet, and the output end and the waste liquid end of the ICP atomization chamber are connected to the filter inlet of the filter through the conversion tee, the filter outlet of the filter is connected to the solution inlet of the solution tank, and the solution outlet of the solution tank is connected to the circulation pump, and then connected to the injection end of the ICP atomization chamber; in this way, the circulation pump can be used to drive the cleaning solution to circulate and rinse the ICP atomization chamber repeatedly, and by controlling the on-off opening and closing of the conversion tee, the three ends of the injection end, the output end and the waste liquid end of the ICP atomization chamber are simultaneously cleaned, avoiding the risk of long-term contact with high-concentration strong acid in the traditional cleaning method. Obviously, the cleaning method is simpler to operate, has high cleaning efficiency, is safe and has no danger, and will not cause any damage to the ICP atomization chamber. At the same time, since the filter installed in the cleaning device is a detachable structure, it can filter the cleaning dirt, avoid secondary pollution of the cleaning solution tank or ultrapure water tank, and make a set of cleaning solutions can be used repeatedly, thus greatly reducing the cleaning cost. In addition, the ICP atomization chamber is clean after cleaning and drying. After being installed back on the instrument, there is no liquid accumulation at the injection end, and the atomization effect is good, so that the instrument's atomization gas flow rate and atomization pressure indicators can remain normal. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 It is a structural schematic diagram of the present invention. DETAILED DESCRIPTION

[0031] The embodiments of the present invention will be described in detail below with reference to the above-mentioned drawings.

[0032] like Figure 1 As shown, 1. ICP nebulizer chamber, 11. injection end, 12. sample outlet, 13. waste liquid end, 2. filter, 21. filter inlet, 22. filter outlet, 3. solution tank, 31. solution inlet, 32. solution outlet, 4. circulation pump, 5. conversion tee, 51. first port, 52. second port, 53. third port, 6. connecting pipe.

[0033] A cleaning device and a cleaning method for an ICP atomization chamber, such as Figure 1 As shown, it can be used for fast and effective cleaning of the ICP spray chamber.

[0034] The cleaning device is mainly composed of an ICP atomization chamber 1, a conversion tee 5, a filter 2, a solution tank 3 and a circulation pump 4.

[0035] The ICP spray chamber 1 has an injection end 11, a sample outlet end 12 and a waste liquid end 13; the conversion tee 5 is arranged between the ICP spray chamber 1 and the filter 2, and the conversion tee 5 has a first port 51, a second port 52 and a third port 53, and the first port 51, the second port 52 and the third port 53 are respectively provided with valves that independently control opening and closing.

[0036] The filter 2 has a filter inlet 21 and a filter outlet 22. A 0.22 μm polymer microporous filter membrane is provided inside the filter 2, which can be used to filter cleaning residues to ensure that the cleaning solution and ultrapure water are not contaminated. The filter 2 is also designed as a detachable and cleanable structure, so that a set of cleaning solutions can be reused, greatly reducing the cleaning cost.

[0037] The solution tank 3 has a solution inlet 31 and a solution outlet 32, and can be selected as a cleaning solution tank or an ultrapure water tank according to actual use needs. The cleaning solution tank is filled with dilute nitric acid with a mass concentration of 2% to 10%, and the ultrapure water tank is filled with ultrapure water.

[0038] The circulating pump 4 is used to drive the cleaning solution to circulate and flush the ICP atomization chamber 1 repeatedly, and its rotation speed is 60rpm~100rpm.

[0039] The assembly structure of the cleaning device is as follows: the sample outlet 12 and the waste liquid end 13 of the ICP atomization chamber 1 are combined and connected to the filter inlet 21 of the filter 2. Specifically, the sample outlet 12 and the waste liquid end 13 of the ICP atomization chamber 1 are connected to the first port 51 and the second port 52 of the conversion tee 5 respectively, and the third port 53 of the conversion tee 5 is connected to the filter inlet 21 of the filter 2; the filter outlet 22 of the filter 2 is connected to the solution inlet 31 of the solution tank 3, and the solution outlet 32 ​​of the solution tank 3 is connected to the circulation pump 4, and then connected to the sample injection end 11 of the ICP atomization chamber 1.

[0040] The above-mentioned assembly connections are all realized through the connecting pipe 6, and the connecting pipe 6 connecting between the sample inlet 11 and the circulation pump 4, between the sample outlet 12 and the first port 51, and between the waste liquid end 13 and the second port 52 is mainly made of acid-resistant polytetrafluoroethylene hose.

[0041] Therefore, according to the structural composition of the above-mentioned cleaning device, the cleaning method of the ICP atomization chamber includes the following steps:

[0042] ① Assemble the removed ICP spray chamber 1 to be cleaned together with the conversion tee 5, the filter 2, the cleaning solution tank, and the circulation pump 4 into a complete cleaning device, that is, the sample outlet 12 and the waste liquid end 13 of the ICP spray chamber 1 are respectively connected to the first port 51 and the second port 52 of the conversion tee 5, the third port 53 of the conversion tee 5 is connected to the filter inlet 21 of the filter 2, the filter outlet 22 of the filter 2 is connected to the solution inlet 31 of the cleaning solution tank, and the solution outlet 22 of the cleaning solution tank is connected to the sample inlet 11 of the ICP spray chamber 1 through the circulation pump 4;

[0043] ② Close the first port 51 of the conversion tee 5, and keep the second port 52 and the third port 53 open;

[0044] ③ Start the circulation pump 4 and clean the injection end 11 and waste liquid end 13 of the ICP nebulizer 1. The cleaning time is 10 min to 30 min.

[0045] ④ After the sample inlet 11 and waste liquid end 13 of the ICP spray chamber 1 are cleaned, the circulation pump 4 is turned off;

[0046] ⑤ Close the second port 52 of the conversion tee 5, and keep the first port 51 and the third port 53 open;

[0047] ⑥ Start the circulation pump 4 and clean the sample inlet 11 and sample outlet 12 of the ICP spray chamber 1. The cleaning time is 10 min to 20 min.

[0048] ⑦ After the sample inlet 11 and sample outlet 12 of the ICP spray chamber 1 are cleaned, the circulation pump 4 is turned off;

[0049] ⑧ Remove the filter 2 in the cleaning device, clean it with ultrapure water, and then reinstall it into the cleaning device;

[0050] ⑨ Remove the cleaning solution tank in the cleaning device, replace it with an ultrapure water tank, and then reinstall it into the cleaning device;

[0051] ⑩Repeat steps ② to ⑧;

[0052] ⑪ Remove the ICP spray chamber 1 in the cleaning device and use pure compressed air to purge the ICP spray chamber until it is dry. The purge time is 10min~15min;

[0053] ⑫ Observe whether there is any residual attachment in the ICP spray chamber 1. If it is still not clean, repeat steps ① to ⑪ until the ICP spray chamber is clean.

[0054] The present invention utilizes a circulation pump 4 to drive a cleaning solution to circulate and flush the ICP atomization chamber 1 repeatedly, and realizes simultaneous cleaning of the three ends of the ICP atomization chamber, namely, the sample inlet end 11, the sample outlet end 12 and the waste liquid end 13, by controlling the on-off opening and closing of the three ports in the conversion tee 5, thereby avoiding the risk of long-term contact with high-concentration strong acid in the traditional cleaning method. Obviously, the cleaning method is simpler to operate, has high cleaning efficiency, is safe and has no danger, and will not cause any damage to the ICP atomization chamber.

[0055] In addition, since the filter 2 installed in the cleaning device is a detachable structure, it can filter the cleaning dirt, avoid secondary pollution of the cleaning solution tank or ultrapure water tank, and make a set of cleaning solutions can be used repeatedly, thus greatly reducing the cleaning cost. After cleaning and drying, the ICP atomization chamber 1 is clean and tidy. After being installed back on the instrument, no liquid is accumulated at the injection end, and the atomization effect is good, so that the atomization gas flow rate and atomization pressure indicators of the instrument can be kept normal.

[0056] The above description is only a specific embodiment of the present invention. Those skilled in the art should understand that any structural design similar to this embodiment should be included in the protection scope of the present invention.

Claims

1. A method for cleaning an ICP atomization chamber, characterized in that The cleaning method comprises the following steps: ① Assemble the removed ICP spray chamber (1) to be cleaned together with the conversion tee (5), the filter (2), the cleaning solution tank, and the circulation pump (4) into a complete cleaning device, that is, the sample outlet (12) and the waste liquid end (13) of the ICP spray chamber (1) are respectively connected to the first port (51) and the second port (52) of the conversion tee (5), the third port (53) of the conversion tee (5) is connected to the filter inlet (21) of the filter (2), the filter outlet (22) of the filter (2) is connected to the solution inlet (31) of the cleaning solution tank, and the solution outlet (32) of the cleaning solution tank is connected to the sample inlet (11) of the ICP spray chamber (1) via the circulation pump (4); ② Close the first port (51) of the conversion tee (5), and keep the second port (52) and the third port (53) open; ③ Start the circulation pump (4) and clean the injection end (11) and waste liquid end (13) of the ICP nebulizer chamber (1); ④ After the sample inlet (11) and waste liquid end (13) of the ICP nebulizer chamber (1) are cleaned, the circulation pump (4) is turned off; ⑤ Close the second port (52) of the conversion tee (5), and keep the first port (51) and the third port (53) open; ⑥ Start the circulation pump (4) and clean the sample inlet (11) and sample outlet (12) of the ICP nebulizer chamber (1); ⑦ After the sample inlet (11) and sample outlet (12) of the ICP nebulizer chamber (1) are cleaned, the circulation pump (4) is turned off; ⑧ Remove the filter (2) from the cleaning device, clean it with ultrapure water, and then reinstall it into the cleaning device; ⑨ Remove the cleaning solution tank in the cleaning device, replace it with an ultrapure water tank, and then reinstall it into the cleaning device; ⑩Repeat steps ② to ⑧; Remove the ICP spray chamber (1) from the cleaning device, and use pure compressed air to blow the ICP spray chamber (1) until it is dry; Observe the ICP atomization chamber (1) to see if there is any residual attachment. If it is still not clean, repeat steps ① to ②. , until the ICP spray chamber (1) is clean.

2. A method for cleaning an ICP atomization chamber according to claim 1, characterized in that The time for cleaning the injection end (11) and the waste liquid end (13) of the ICP nebulizer (1) in step ③ is 10 min to 30 min; the time for cleaning the injection end (11) and the sample outlet end (12) of the ICP nebulizer (1) in step ⑥ is 10 min to 20 min; The time for blowing the ICP spray chamber (1) with medium compressed air until it is dry is 10 minutes to 15 minutes.

Images