CN110927242A - Method for measuring environmental metal impurities - Google Patents
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- CN110927242A CN110927242A CN201911326748.XA CN201911326748A CN110927242A CN 110927242 A CN110927242 A CN 110927242A CN 201911326748 A CN201911326748 A CN 201911326748A CN 110927242 A CN110927242 A CN 110927242A
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Abstract
The application discloses a method for measuring environmental metal impurities, which comprises the steps of placing a sampling container with a preset weight and a preset opening area in an environment to be measured with an upward opening, receiving particles falling from the air, and continuing for a preset time; weighing the sampling container to obtain the weight of the deposited particles; dissolving metal impurities in the particles into metal ions by using a volume of acid solution matched with the weight of the deposited particles; and testing the concentration of the metal ions, and calculating the content of the settled metal impurities in unit time and unit opening area. The method for measuring the environmental metal impurities can detect the content and the variable quantity of the environmental metal impurities on the basis of low cost, and provides more accurate data support for production.
Description
Technical Field
The invention belongs to the technical field of photovoltaic equipment manufacturing, and particularly relates to a method for measuring environmental metal impurities.
Background
The polycrystalline silicon is used for manufacturing the photovoltaic equipment, and in the post-treatment cleaning management and control of the polycrystalline silicon, elements such as Fe, Cr, Ni, Cu and Zn in metal elements belong to deep-level impurities, so that the downstream use of the polycrystalline silicon is greatly influenced, and the control of surface metal impurities in the polycrystalline silicon packaging process is particularly important. The existing control method is to use an air conditioner filter element to filter efficiently to control the number of air particles in a certain specific area, so as to realize air cleaning management and control of the environment, which are usually thousands, tens of thousands, hundreds of thousands and the like.
In the prior art, an online particle collecting device is commonly used for collecting and detecting metal impurities, but the method needs expensive filter membranes, so that the detection cost is very high, and the method is not suitable for the production occasions of polycrystalline silicon.
Disclosure of Invention
In order to solve the problems, the invention provides a method for measuring environmental metal impurities, which can detect the content and the variable quantity of the environmental metal impurities on the basis of low cost and provide more accurate data support for production.
The invention provides a method for determining environmental metal impurities, which comprises the following steps:
placing a sampling container with a preset weight and a preset opening area in an environment to be detected with an upward opening, receiving particles falling in the air, and continuing for a preset time;
weighing the sampling container to obtain the weight of the deposited particles;
dissolving metal impurities in the particles into metal ions by using a volume of acid solution matched with the weight of the deposited particles;
and testing the concentration of the metal ions, and calculating the content of the settled metal impurities in unit time and unit opening area.
Preferably, in the method for measuring environmental metal impurities, before placing the sampling container with a preset weight and a preset opening area in the environment to be measured with the opening facing upwards, the method further comprises:
the silicon block was placed in the sampling vessel.
Preferably, in the method for measuring the environmental metal impurities, the size of the silicon block ranges from 20mm to 30mm in length, width and height.
Preferably, in the method for measuring environmental metal impurities, the acid solution is a mixed acid of hydrofluoric acid and nitric acid having a concentration of 5% and a volume ratio of 1: 1.
Preferably, in the method for measuring environmental metal impurities described above, the concentration of the metal ions is measured using an ICP-MS apparatus.
Preferably, in the method for measuring environmental metal impurities, the dissolving of the metal impurities in the particles into metal ions by the acid solution is:
and heating the acid solution to 70-100 ℃ for 30-45 minutes to dissolve the metal impurities in the particles into metal ions.
Preferably, in the method for measuring environmental metal impurities, the diameter of the sampling vessel is in the range of 80 mm to 100 mm.
Preferably, in the method for measuring environmental metal impurities, the predetermined time is in a range of 2 hours to 24 hours.
Preferably, in the method for measuring environmental metal impurities, after the particles falling in the receiving air last for a preset time, the method further includes:
the sampling vessel was capped with a cap.
Preferably, in the method for measuring environmental metal impurities, the sampling container is an FEP sampling tube.
As can be seen from the above description, the method for measuring environmental metal impurities provided by the present invention comprises placing a sampling container with a predetermined weight and a predetermined opening area in an environment to be measured with the opening facing upward, receiving particles falling from the air, continuing for a predetermined time, then weighing the sampling container to obtain the weight of the deposited particles, dissolving the metal impurities in the particles into metal ions by using an acid solution with a volume matched with the weight of the deposited particles, finally testing the concentration of the metal ions, calculating the content of the settled metal impurities in unit time and unit opening area, therefore, the method realizes the detection of the environmental metal impurities on the basis of not using a filter membrane, therefore, the content and the variable quantity of the metal impurities in the environment can be detected on the basis of low cost, and more accurate data support is provided for production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic diagram of a method for determining environmental metal impurities provided by the present application.
Detailed Description
The core of the invention is to provide a method for measuring the environmental metal impurities, which can detect the content and the variable quantity of the environmental metal impurities on the basis of low cost and provide more accurate data support for production.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Fig. 1 is a schematic view of an embodiment of a method for measuring environmental metal impurities, where the method includes:
s1: placing a sampling container with a preset weight and a preset opening area in an environment to be detected with an upward opening, receiving particles falling in the air, and continuing for a preset time;
it should be noted that, in this step, the value of the preset weight and the value of the preset opening area may be recorded as the basis of the subsequent step, and the environment to be measured may be a static environment or a dynamic environment, that is, an environment in which no person moves and equipment operates, or an environment in which a person moves and equipment operates in a normal working state, and the method may be used to measure the content of the environmental metal impurities, and the sampling container may be placed at a position far from the air inlet of the air conditioner or a ventilation position.
S2: weighing the sampling container to obtain the weight of the deposited particles;
that is, after the sampling is completed, the weight of the sampling vessel at that time is obtained, and the weight of the particles deposited in the process is obtained by subtracting the preset weight measured in the previous step.
S3: dissolving metal impurities in the particles into metal ions by using a volume of acid solution matched with the weight of the deposited particles;
specifically, when testing a static environment, the obtained sediment is less, and the corresponding acid solution can be selected to be 10g, when testing a dynamic environment, the obtained sediment is more, and the corresponding acid solution can be based on immersing the sediment, as long as the particles can be dissolved.
S4: and testing the concentration of the metal ions, and calculating the content of the settled metal impurities in unit time and unit opening area.
It should be noted that, the ICP-MS apparatus may be used to test the concentration of the metal ions to obtain the concentrations of a plurality of metal ions, so that the content of the corresponding metal impurities that are effectively deposited can be known, and the distribution of the metal impurity elements deposited on the surface of the object in a certain space can be known, so that the content of the metal impurities in the environment can be analyzed.
As can be seen from the above description, in the examples of the method for determining the environmental metal impurities provided by the present application, because the sampling container with the preset weight and the preset opening area is placed in the environment to be measured with the opening facing upwards to receive the particles falling from the air for the preset time, then weighing the weight of the sampling container to obtain the weight of the deposited particles, dissolving the metal impurities in the particles into metal ions by utilizing an acid solution with the volume matched with the weight of the deposited particles, finally testing the concentration of the metal ions, calculating the content of the settled metal impurities in unit time and unit opening area, and showing that the method also realizes the detection of the environmental metal impurities without using a filter membrane, therefore, the content and the variable quantity of the metal impurities in the environment can be detected on the basis of low cost, and more accurate data support is provided for production.
In an embodiment of the method for measuring environmental metal impurities, before placing the sampling container with a preset weight and a preset opening area in the environment to be measured with the opening facing upwards, the method may further include the following steps: the silicon block was placed in a sampling vessel. Specifically, the size of the silicon block can be in the range of 20mm to 30mm in length, width and height, and the number of the silicon blocks can be 6, that is, dust-free clean PE gloves can be worn, the 6 silicon blocks with the length, width and height of 20mm to 30mm are placed in the same clean sampling container, two parallel samples can be prepared in the same way and weighed to the accuracy of 0.1g, the total weight of all the silicon blocks is ensured to be not less than 150g, can be between 150g and 200g, and the total weight error is within 5g, and the good sealing performance is ensured, which is a preferred scheme, and actually, silicon blocks with other numbers and other sizes can be selected according to actual needs, and the scheme is not limited herein.
In another specific example of the method for measuring environmental metal impurities, the acid solution may be a mixed acid of 5% hydrofluoric acid and nitric acid at a volume ratio of 1:1, and each sample in the sampling container may be immersed by the mixed acid.
In another specific example of the method for measuring environmental metal impurities, the dissolving of metal impurities in particles into metal ions using an acid solution is: the acid solution is heated to 70-100 ℃, the acid is volatilized and impurities are concentrated due to the fact that the heat-resistant range of the sampling container and the heating temperature are too high, the test result is high, therefore, the acid solution is set to be not higher than 100 ℃, the time lasts for 30-45 minutes preferably, the metal impurities in the particles are dissolved into the metal ions, the time range can guarantee that the metal impurities are completely dissolved into the metal ions, and the accuracy of the test result is guaranteed.
In a preferred embodiment of the method for measuring environmental metal impurities, the diameter of the sampling container is in the range of 80 mm to 100 mm, so as to ensure that there is enough area for receiving the particles in the environment, and the predetermined time period may preferably be in the range of 2 hours to 24 hours, and the specific value may be selected according to actual needs.
In another preferred embodiment of the method for measuring environmental metal impurities, after receiving the particles falling in the air for a preset time, the method may further include: utilize the lid to cover the sample container, under this condition, just can avoid in the follow-up step particle in the external environment to fall into the sample container and cause the interference to the test to guarantee that the test result is more accurate. In addition, the sampling container can be preferably an FEP sampling tube, and the total metal impurities in the tube after the FEP sampling tube is cleaned are less than or equal to 0.1ppbw, so that the FEP sampling tube is cleaner, impurity particles cannot be introduced, and the test result is more accurate.
The above method is described in detail below using two examples:
a first example is the collection of settled particles in an empty bottle in a static environment, comprising the following steps:
1) 1 clean FEP sampling cylinder is prepared (the total metal impurities in the cleaned cylinder is less than or equal to 0.1ppbw), the volume can be 500 milliliters, the weight of the sampling cylinder is recorded, the weight is accurate to 0.001g, and the sampling cylinder is sealed and stored.
2) In a room to be measured, selecting a position far away from an air inlet of an air conditioner or a ventilation position, wearing a dust-free glove, laying clean plastic cloth, placing a sampling tube, opening a cup cover, keeping the cup cover downwards buckled on the plastic cloth, and keeping the cup opening of the sampling tube upwards to ensure that air particles can fall into a bottle.
3) After the device is placed, the sampling start time and the name of a test room are recorded, a door and a window are closed, and people are forbidden to enter the device.
4) According to the evaluation requirement, after the determination time, the bottle cap is covered by wearing dust-free gloves, and the sample preparation is prepared.
5) The mass of the sampling cylinder is weighed, the sampling mass is calculated to be accurate to 0.001g, and 5 percent of mixed acid solution (the volume ratio is HF: HNO31: 1) to the nearest 0.001 g.
6) The sample cylinder was placed on a hot plate and heated at 70 ℃ for 30 minutes.
7) The samples were tested on ICP-MS and the results recorded.
8) And calculating the content of the settled metal elements in unit time/unit area according to the detection result.
The following table 1 shows the data of 8-hour sedimentation experiments performed in 5 rooms with the same specification and size in a certain area when no operation and no personnel flow, and the sedimentation data is blanked.
Table 15 results of static testing of settled metal particles in rooms
A second example is the collection of settled particles in an empty bottle under dynamic conditions, comprising the steps of:
1) wearing dust-free clean gloves, taking 6 blocks of silicon material with linear dimension of 30mm x 30mm, loading the silicon material into a clean sampling cylinder, covering a bottle cap, preparing two parallel samples according to the sampling mode, weighing the samples to be accurate to 0.01g, ensuring that the weight error is about 5g, and ensuring good sealing property.
2) In a room to be measured, selecting a position far away from an air inlet of an air conditioner or a ventilation position, wearing dust-free gloves, laying clean plastic cloth, opening one of the sampling cylinders, placing the sampling cylinder on the ground, opening the cup cover, keeping the cup cover downwards buckled on the plastic cloth, and keeping the cup opening of the sampling cylinder upwards to ensure that air particles can fall into a bottle, wherein the other unopened sampling cylinder is used as a blank.
3) After placement, the start time of the test sample and the name of the test room are recorded.
4) According to the evaluation requirement, after the determination time, wearing dust-free gloves, covering the bottle cap, and preparing a sample.
5) The electronic balance peels off the sampling cylinder, and 10% mixed acid solution is added, volume ratio (HF: HNO31: 1) mainly immersing the silicon block.
6) The sample was weighed and placed on a hot plate and heated at 70 degrees for 30 minutes.
7) The samples were tested on ICP-MS and the results recorded.
8) And calculating the content of the metal elements in the unit space according to the detection result and the volume of the sampling cylinder.
Experimental cases: settlement experiments performed in room No. 2 of a certain area during operation. Experimental data has been blanked.
Table 22 table of results of room dynamic test for settling metal particles
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A method for measuring environmental metal impurities, comprising:
placing a sampling container with a preset weight and a preset opening area in an environment to be detected with an upward opening, receiving particles falling in the air, and continuing for a preset time;
weighing the sampling container to obtain the weight of the deposited particles;
dissolving metal impurities in the particles into metal ions by using a volume of acid solution matched with the weight of the deposited particles;
and testing the concentration of the metal ions, and calculating the content of the settled metal impurities in unit time and unit opening area.
2. The method for determining environmental metal impurities according to claim 1, wherein before placing the sampling container with the preset weight and the preset opening area in the environment to be measured with the opening facing upwards, the method further comprises:
the silicon block was placed in the sampling vessel.
3. The method of claim 2, wherein the silicon block has a length, a width and a height in a range of 20mm to 30 mm.
4. The method for measuring environmental metal impurities according to claim 1, wherein the acid solution is a mixed acid having a volume ratio of hydrofluoric acid to nitric acid of 1:1 at a concentration of 5%.
5. The method for measuring environmental metal impurities according to claim 1, wherein the concentration of the metal ions is measured by an ICP-MS apparatus.
6. The method for determining environmental metal impurities as claimed in claim 1, wherein the dissolving of the metal impurities in the particles into metal ions by the acid solution is:
and heating the acid solution to 70-100 ℃ for 30-45 minutes to dissolve the metal impurities in the particles into metal ions.
7. The method of claim 1, wherein the sampling vessel has a diameter in the range of 80 mm to 100 mm.
8. The method according to claim 1, wherein the predetermined time is in a range of 2 hours to 24 hours.
9. The method of claim 1, wherein the step of receiving the particles falling in the air for a predetermined time further comprises:
the sampling vessel was capped with a cap.
10. The method of determining environmental metal impurities as set forth in any one of claims 1 to 9, wherein said sampling vessel is an FEP sampling tube.
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| CN201911326748.XA CN110927242A (en) | 2019-12-20 | 2019-12-20 | Method for measuring environmental metal impurities |
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| CN201911326748.XA CN110927242A (en) | 2019-12-20 | 2019-12-20 | Method for measuring environmental metal impurities |
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Citations (3)
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| CN101598672A (en) * | 2009-07-06 | 2009-12-09 | 天津师范大学 | The monitoring method of heavy metals in particles captured in atmospheric falling dust of urban buildings |
| CN103175713A (en) * | 2013-03-01 | 2013-06-26 | 中国环境科学研究院 | Sample collecting and extracting method applicable to heavy metal analysis in atmospheric dry-wet deposition |
| CN104677790A (en) * | 2015-01-29 | 2015-06-03 | 北京林业大学 | Detection system and detection method for dry deposition flux of atmospheric particulates in forest |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101598672A (en) * | 2009-07-06 | 2009-12-09 | 天津师范大学 | The monitoring method of heavy metals in particles captured in atmospheric falling dust of urban buildings |
| CN103175713A (en) * | 2013-03-01 | 2013-06-26 | 中国环境科学研究院 | Sample collecting and extracting method applicable to heavy metal analysis in atmospheric dry-wet deposition |
| CN104677790A (en) * | 2015-01-29 | 2015-06-03 | 北京林业大学 | Detection system and detection method for dry deposition flux of atmospheric particulates in forest |
Non-Patent Citations (1)
| Title |
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| 李山泉 等: "南京市大气沉降中重金属特征及对土壤环境的影响", 《中国环境科学》 * |
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Application publication date: 20200327 |