CN212392210U - ICP-MS online sampling system - Google Patents
ICP-MS online sampling system Download PDFInfo
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- CN212392210U CN212392210U CN202021650703.6U CN202021650703U CN212392210U CN 212392210 U CN212392210 U CN 212392210U CN 202021650703 U CN202021650703 U CN 202021650703U CN 212392210 U CN212392210 U CN 212392210U
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Abstract
The utility model discloses an ICP-MS online sampling system, including clean cabinet, sampling pipeline and play appearance pipeline, install sampling valve A and sampling valve B on the sampling pipeline, install out appearance valve A and play appearance valve B on the play appearance pipeline, connect the sample branch road on the pipeline between the export of sampling pipeline and the entry of play appearance pipeline, install sampling valve on the sample branch road, it is connected to the low-pressure jar to be equipped with the branch road on the pipeline of play appearance pipeline, install on the branch road that is connected to the low-pressure jar valve, the material that is located valve and pipeline in the clean cabinet is PFA or PTFE, sampling pipeline entry is connected with the sample container of waiting to analyze, it is connected with waste recovery device to go out appearance pipeline export. The utility model discloses sampling system can effectively avoid metal ion to pollute to simple structure, the easy operation of sampling method is fit for popularizing and applying.
Description
Technical Field
The utility model relates to a chemical analysis technical field, especially an ICP-MS online sampling system.
Background
With the development of industrial production in China, the varieties of chemical products are more and more, the requirements of production enterprises and users on the quality of the chemical products are higher and higher, and in the high-quality requirements, the content of metal impurities in some high-quality products is very high, for example, the requirements on metal ion impurities of various special gases, etching solutions and the like used in the chip and semiconductor industries reach the PPT level and are even higher.
Along with the requirements of the industries on raw and auxiliary materials, higher requirements are put forward on the analysis technology. At present, in the industry, ICP-MS equipment is adopted for analyzing metal ion impurities (trace), the stability of the ICP-MS equipment is undoubted, but the influence of a sampling process on the quality of a product (raw material) is not a little, misjudgment on the product (raw material) is caused by pollution in a sampling process, the misjudgment is not qualified in a single batch of the product (raw material), economic loss is caused, and the situation that an enterprise disappears from the industry is feared in the serious case. Therefore, it is very important to reduce, avoid and put an end to the pollution of the product (raw material) in the sampling process.
The traditional sampling process is as follows:
1. container external placing type
A certain amount of product (raw material) is discharged from a container of the product (raw material) to be detected, and then sample preparation, on-machine test and the like are carried out. In order to ensure safety, the tested product (raw material) is usually contained in a steel container, the inlet valve and the outlet valve are made of metal products, and when the tested product flows out of the metal valve of the steel cylinder, metal ion pollution is inevitably caused. Such contamination is generally large enough to judge a good product (raw material) as a bad product (raw material).
2. Pipeline sampling type
A certain amount of products (raw materials) are taken out from a container of the products (raw materials) to be detected through a pipeline, and then sample preparation, on-machine test and the like are carried out. But the pipeline material all is the metal material basically, and is same, in the sample process, because product (raw and other materials) flow the pipeline department of metal material and expose in the air, and the vast majority of material to be measured all can directly or indirectly corrode the metal, will appear metal ion pollution this moment, finally leads to the great deviation of analysis.
Taking an austenitic stainless steel as an example of a pipeline made of a metal material at the tail end, Fe, Cr, Ni and the like can react with oxygen in the air in a humid environment to generate oxides containing Fe, Cr and Ni, nitric acid and the like are added into a sampled sample to process the sample, and the oxides containing Fe, Cr and Ni can react with the nitric acid to generate Fe in the processing process3+、Cr2+、Ni2+Thus contaminating the sample to be analyzed.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide an ICP-MS online sampling system to when solving present ICP-MS equipment and carrying out chemical product sampling analysis, the problem that the sampling process caused metal ion to pollute easily.
In order to achieve the above purpose, the utility model discloses a sampling system realizes through following technical scheme:
an ICP-MS online sampling system comprises a clean cabinet, a sample inlet pipeline and a sample outlet pipeline, wherein an outlet of the sample inlet pipeline is connected with an inlet of the sample outlet pipeline through a pipeline, a sample inlet valve A and a sample inlet valve B are installed on the sample inlet pipeline, a sample outlet valve A and a sample outlet valve B are installed on the sample outlet pipeline, a sampling branch is connected on the pipeline between the outlet of the sample inlet pipeline and the inlet of the sample outlet pipeline, a sampling valve is installed on the sampling branch, a branch is arranged on the pipeline of the sample outlet pipeline and connected to a low-pressure tank, a low-pressure tank removing valve is installed on the branch connected to the low-pressure tank, the sample inlet valve A, the sample outlet valve B and the low-pressure tank are arranged outside the clean cabinet, the sample inlet valve B, the sample outlet valve A, the sampling branch and the low-pressure tank removing valve are arranged in the clean cabinet, the valve and the pipeline in the clean cabinet are made of PFA or PFA, the outlet of the sample outlet pipeline is connected with a waste recovery device.
Compared with the prior art, the ICP-MS online sampling system adopting the technical scheme has the beneficial effects that: 1) the inlet of the sample inlet pipeline is connected with a sample container to be analyzed, and the outlet of the sample outlet pipeline is connected with the waste recovery device, so that the situation that a sample to be analyzed in the container flows out of a metal pipeline and is corroded by contacting with air, and finally the sample to be analyzed is polluted by metal ions is avoided; 2) the valves and pipelines in the cleaning cabinet are made of PFA or PTFE, so that the pollution of metal ions is essentially solved; 3) sampling pipeline and low-pressure tank design, safe and reliable avoids the too big rupture that arouses of pipeline pressure in the clean cabinet of sample process, arouses the contaminated problem of sample of waiting to analyze.
Furthermore, the pressure value in the low-pressure tank is 10-50 KPa.
Furthermore, a sample injection valve C is further installed on the sample injection pipeline, the sample injection valve C is arranged in the cleaning cabinet, and the material of the sample injection valve C is PFA or PTFE.
Furthermore, a sample outlet valve C is further arranged on the sample outlet pipeline, the sample outlet valve C is arranged in the cleaning cabinet, and the material of the sample outlet valve C is PFA or PTFE.
Furthermore, the valve and the pipeline outside the clean cabinet are made of EP-grade stainless steel.
Drawings
Fig. 1 is a schematic structural diagram provided in the embodiment of the present invention.
Fig. 2 is a schematic structural diagram according to another embodiment of the present invention.
Detailed Description
In order to make the present invention better understood by those skilled in the art, the technical solution of the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a schematic structural diagram of an ICP-MS online sampling system according to an embodiment of the present invention, as shown in FIG. 1, the ICP-MS online sampling system includes a clean cabinet 1, a sample inlet pipe 2 and a sample outlet pipe 3, an outlet of the sample inlet pipe 2 is connected to an inlet of the sample outlet pipe 3 through a pipe, the sample inlet pipe 2 is provided with a sample inlet valve A4 and a sample inlet valve B5, the sample outlet pipe 3 is provided with a sample outlet valve A6 and a sample outlet valve B7, a sampling branch 8 is connected to a pipe between the outlet of the sample inlet pipe 2 and the inlet of the sample outlet pipe 3, the sampling branch 8 is provided with a sampling valve 9, the pipe of the sample outlet pipe 3 is provided with a branch connected to a low pressure tank 10, a branch connected to the low pressure tank 10 is provided with a low pressure tank valve 11, the sample inlet valve A4, the sample outlet valve B7 and the low pressure tank 10 are disposed outside the clean cabinet 1, sampling valve B5, go out appearance valve A6, sample branch road 8 and go low-pressure tank valve 11 and set up in clean cabinet 1, and the material that is located the valve of clean cabinet 1 and pipeline is PFA or PTFE, in order to guarantee the security of the pipeline of clean cabinet 1 outside, the material that is located clean cabinet 1 outer valve and pipeline is the metal material, and 2 entrances of inlet pipeline are connected with waiting to analyze the sample container, and 3 exports of outlet pipeline are connected with waste recovery device.
In the embodiment, the inlet of the sample inlet pipeline 2 is directly connected with the sample container to be analyzed, and the outlet of the sample outlet pipeline 3 is directly connected with the waste recovery device, so that the interior of the metal pipeline in the whole sampling system is not contacted with air, and the pollution of the metal pipeline can be avoided; and the utility model discloses a material of valve in the clean cabinet and pipeline is PFA or PTFE, and PFA or PTFE are non-metallic material, acid and alkali-resistance, oxytolerant, for the pureness thing, and have certain intensity and compliance, and more importantly has solved metallic ion's pollution from the essence. However, the strength of the PFA or PTFE pipe or valve is not as high as that of a metal material, and the PFA or PTFE pipe or valve is easily damaged under a large fluid pressure, so that the pressure in the pipe is reduced through the design of the low-pressure tank, the sample to be analyzed is automatically drained into the low-pressure tank with a lower pressure in the sampling process, and then the sample to be analyzed is obtained by opening the sampling pipe, so that the problem of breakage caused by too high pressure of the sample inlet pipe 2 and the sample outlet pipe 3 in the sampling process is avoided, and the sampling process is ensured to be carried out smoothly.
In order to ensure that the sample to be analyzed smoothly flows into the low-pressure tank 10, the pressure value in the low-pressure tank 10 is 10-50 KPa (gauge pressure).
The embodiment of the utility model provides an in each valve is selected from among the prior art valve, for example gate valve, stop valve, plug valve, ball valve, butterfly valve and diaphragm valve, preferred diaphragm valve, diaphragm valve simple structure, easy washing.
In order to avoid the pollution of the sample caused by the metal pipeline, the valve and the pipeline outside the cleaning cabinet 1 are made of EP-grade stainless steel.
Fig. 2 is a schematic structural diagram of an ICP-MS online sampling system in another embodiment of the present invention, in which a sample valve C12 and a sample outlet valve C13 are added on the basis of the previous embodiment, as shown in fig. 2, a sample valve C12 is further installed on the sample pipeline 2, the sample valve C12 is disposed in the clean cabinet 1, and the sample valve C12 is made of PFA or PTFE. The sampling pipeline 3 is also provided with a sampling valve C13, the sampling valve C13 is arranged in the cleaning cabinet 1, and the sampling valve C13 is made of PFA or PTFE. This embodiment is through setting up a plurality of sampling valves and a play appearance valve to when avoiding leaking the trouble in appearing in certain valve, liquid flow is uncontrolled in the pipeline, influences the sampling process and goes on smoothly.
The sampling method of the ICP-MS online sampling system according to the embodiment shown in FIG. 2 comprises the following steps:
step one, system preprocessing: and (3) carrying out air tightness detection on the system, blowing by using inert gas after the air tightness detection is qualified, and rinsing, soaking and passivating the system after the blowing is qualified.
Specifically, chlorine is introduced into the system, and when the chlorine leaked from the valve and the joint is less than or equal to 1.0 multiplied by 10-9atm/s/cm3And the air tightness is qualified. And purging a system pipeline by adopting inert gas, wherein the water content of the gas in the system is less than or equal to 1PPb, the oxygen content is less than or equal to 1PPb, and the granularity is less than or equal to 1um/L after purging is finished. The inert gas is nitrogen, argon or helium, the water content of the inert gas is less than or equal to 1PPb, the oxygen content is less than or equal to 1PPb, and the granularity is less than or equal to 1 um/L. The method comprises the steps of firstly rinsing a system by adopting a sample to be analyzed, then soaking and passivating for 24 hours, secondly rinsing, soaking and passivating for 24 hours, repeatedly rinsing, soaking and passivating for not less than 5 times, and manually switching on and off for many times in the rinsing processThe valve is arranged to achieve the effect of fully cleaning the internal structure of the valve.
And step two, sampling and analyzing the analyzed sample.
The sample to be detected is injected from the inlet of the sample injection pipeline 1.
And opening a sample injection valve A4, a sample injection valve B5, a sample injection valve C12, a sample outlet valve A6, a sample outlet valve C13 and a sample outlet valve B7, and flushing and replacing the pipeline by using a sample to be analyzed.
And opening a valve 11 of the low-pressure tank after the washing and replacement are qualified, closing a sample outlet valve B7 and a sample outlet valve C13, and allowing a sample to be analyzed to enter the low-pressure tank 10.
When 1-10L of sample to be analyzed enters the low-pressure tank 10, the sampling valve 9 is opened slightly, and the sample to be analyzed is contained in the sampling vessel 14.
After sampling, the sampling valve 9, the sample injection valve A4, the sample injection valve B5, the sample injection valve C12 and the low-pressure tank valve 11 are closed in sequence.
And if the analysis results obtained by continuously sampling for more than three times are qualified, determining that the sample is qualified to be analyzed.
Although embodiments of the present invention have been shown and described, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art without departing from the scope of the present invention.
Claims (5)
1. An ICP-MS online sampling system comprises a clean cabinet, a sample inlet pipeline and a sample outlet pipeline, and is characterized in that an outlet of the sample inlet pipeline is connected with an inlet of the sample outlet pipeline through a pipeline, a sample inlet valve A and a sample inlet valve B are installed on the sample inlet pipeline, a sample outlet valve A and a sample outlet valve B are installed on the sample outlet pipeline, a sampling branch is connected on the pipeline between the outlet of the sample inlet pipeline and the inlet of the sample outlet pipeline, a sampling valve is installed on the sampling branch, a branch is arranged on the pipeline of the sample outlet pipeline and connected to a low-pressure tank, a low-pressure tank removing valve is installed on the branch connected to the low-pressure tank, the sample inlet valve A, the sample outlet valve B and the low-pressure tank are arranged outside the clean cabinet, the sample inlet valve B, the sample outlet valve A, the sampling branch and the low-pressure removing valve are arranged in the clean cabinet, the valve and the pipeline in the clean cabinet are made of PFA or PTFE, the, the outlet of the sample outlet pipeline is connected with a waste recovery device.
2. An ICP-MS online sampling system according to claim 1, wherein the pressure value in the low pressure tank is 10-50 KPa.
3. An ICP-MS online sampling system according to claim 1, wherein a sample valve C is further installed on the sample inlet pipeline, the sample valve C is arranged in the clean cabinet, and the sample valve C is made of PFA or PTFE.
4. An ICP-MS online sampling system according to claim 1, wherein the sampling pipeline is further provided with a sampling valve C, the sampling valve C is arranged in the clean cabinet, and the sampling valve C is made of PFA or PTFE.
5. An ICP-MS online sampling system according to claim 1, wherein the valves and pipes located outside the clean room are made of EP grade stainless steel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021650703.6U CN212392210U (en) | 2020-08-11 | 2020-08-11 | ICP-MS online sampling system |
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| CN202021650703.6U CN212392210U (en) | 2020-08-11 | 2020-08-11 | ICP-MS online sampling system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111816542A (en) * | 2020-08-11 | 2020-10-23 | 唐山三孚硅业股份有限公司 | ICP-MS (inductively coupled plasma-Mass Spectrometry) online sampling system and sampling method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111816542A (en) * | 2020-08-11 | 2020-10-23 | 唐山三孚硅业股份有限公司 | ICP-MS (inductively coupled plasma-Mass Spectrometry) online sampling system and sampling method |
| CN111816542B (en) * | 2020-08-11 | 2024-10-18 | 唐山三孚硅业股份有限公司 | ICP-MS online sampling system and sampling method |
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