CN111982952A - Organic halide detection device and use method - Google Patents
Organic halide detection device and use method Download PDFInfo
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- CN111982952A CN111982952A CN202010916249.2A CN202010916249A CN111982952A CN 111982952 A CN111982952 A CN 111982952A CN 202010916249 A CN202010916249 A CN 202010916249A CN 111982952 A CN111982952 A CN 111982952A
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- 150000004820 halides Chemical class 0.000 title claims abstract description 60
- 238000001514 detection method Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 34
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 238000005303 weighing Methods 0.000 claims abstract description 8
- 238000004876 x-ray fluorescence Methods 0.000 claims description 19
- 238000007789 sealing Methods 0.000 claims description 9
- 238000005086 pumping Methods 0.000 claims description 6
- 238000011088 calibration curve Methods 0.000 abstract 1
- 238000009835 boiling Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 230000002085 persistent effect Effects 0.000 description 3
- DEIGXXQKDWULML-UHFFFAOYSA-N 1,2,5,6,9,10-hexabromocyclododecane Chemical compound BrC1CCC(Br)C(Br)CCC(Br)C(Br)CCC1Br DEIGXXQKDWULML-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 238000004895 liquid chromatography mass spectrometry Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 238000002076 thermal analysis method Methods 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- GHSVBKGWTWVLFP-UHFFFAOYSA-M [Br+].[Br-] Chemical compound [Br+].[Br-] GHSVBKGWTWVLFP-UHFFFAOYSA-M 0.000 description 1
- 239000012237 artificial material Substances 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- DDTBPAQBQHZRDW-UHFFFAOYSA-N cyclododecane Chemical class C1CCCCCCCCCCC1 DDTBPAQBQHZRDW-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical class C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical group 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2206—Combination of two or more measurements, at least one measurement being that of secondary emission, e.g. combination of secondary electron [SE] measurement and back-scattered electron [BSE] measurement
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/071—Investigating materials by wave or particle radiation secondary emission combination of measurements, at least 1 secondary emission
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/303—Accessories, mechanical or electrical features calibrating, standardising
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/637—Specific applications or type of materials liquid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/60—Specific applications or type of materials
- G01N2223/652—Specific applications or type of materials impurities, foreign matter, trace amounts
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Abstract
The invention discloses an organic halide detection device and a using method thereof. The using method comprises the following steps: s1, weighing the empty sample cup; s2, adding the sample into the sample cup; s3, reweighing, and calculating the mass (a) of the added sample; s4, conveying the sample cup to a heating pool; s5, vacuumizing the box body, and performing filter pressing on a membrane on a sample cup after the vacuum reaches the standard; s6, heating the sample cup; s7, moving the filter membrane to the detection window of the X-ray fluorescent rod for reading; s8, moving the sample cup to a balance for weighing to obtain the residual mass (b) after heating; s9, calculating the concentration (c) of the selected organic halide in the sample by using the calibration curve; s10, moving the sample cup into the heating pool, covering the filter membrane, repeating the steps S6-S9, detecting and calculating the concentration of the selected organic halide.
Description
Technical Field
The invention relates to organic halide detection, in particular to an organic halide detection device and a using method thereof.
Background
The european union 'directive on the Restriction of the use of certain Hazardous components in electrical and electronic devices' (RoHS) and the 'stockholm convention on persistent organic matter' have included organic halides such as polychlorinated biphenyl, polybrominated diphenyl ether, hexabrominated cyclododecane, which require a reduction in the use of these compounds in products and the detection of their residues in the environment, which has led to a corresponding need for detection techniques.
At present, the organic halide is detected by adopting gas chromatography-mass spectrometry (GC/MS) and liquid chromatography-mass spectrometry (LC/MS) technologies generally, and the concentration of the organic halide can be accurately and quantitatively detected in a laboratory.
In actual work, the content of organic halides in products often needs to be rapidly determined on site, in order to realize rapid detection of the organic halides on site, an X-ray fluorescence analyzer is usually adopted, and the technology can determine the total content of certain elements (such as chlorine and bromine) in the organic halides in a sample, but cannot determine the organic halides from which the elements come, and cannot judge whether the organic halides exceed standards or not.
Disclosure of Invention
The invention aims to solve the problems and provides an organic halide detection device and a using method thereof, wherein the device is light in weight, small in size, portable to the site, and capable of rapidly detecting the concentration of a specific organic halide in a sample and helping a user to rapidly judge whether the organic halide exceeds the standard.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the utility model provides an organic halide detection device, includes a box that can the evacuation, the bracket that the direction of height along the box in the cavity of box was provided with the arm perpendicularly and was removed along the arm, the below of arm is provided with the balance, one side of balance is provided with the heating bath, one side of heating bath is provided with X ray fluorescence detection subassembly, heating bath, X ray fluorescence stick are located under the arm.
As a further improvement to the technical scheme, the mechanical arm comprises a base fixed at the bottom of the box body, a vertical arm vertically arranged on the base, and a horizontal arm horizontally arranged and perpendicular to the vertical arm, wherein a bracket is arranged on the horizontal arm, and the bracket is provided with a walking motor for driving the bracket to walk on the horizontal arm.
As a further improvement to the technical scheme, the X-ray fluorescence detection assembly comprises a sealing shell and an X-ray fluorescence rod arranged in the sealing shell, and the top of the sealing shell is provided with a detection window.
As a further improvement to the technical scheme, a filter membrane frame is further arranged in the cavity of the box body, and a filter membrane is placed on the filter membrane frame.
As a further improvement to the above technical solution, an air extraction opening for vacuum extraction is arranged at the top of the box body, and the air extraction opening is connected with a vacuum pump; the box is provided with a sample cell opening at the other side.
As a further improvement to the above technical solution, the heating tank is provided with a temperature sensor to detect the heating temperature of the heating tank.
As a further improvement to the above technical solution, the present invention further provides a method for using the above organic halide detection apparatus, the method comprising the steps of:
s1, vacuumizing the organic halide detection device, putting an empty sample cup on a bracket of the mechanical arm, and conveying the sample cup to a balance to weigh by the bracket moving along the mechanical arm;
s2, conveying the weighed sample cup to the opening of the sample pool by the mechanical arm, and manually adding the sample into the sample cup;
s3, conveying the sample cup to a balance by a mechanical arm, vacuumizing the organic halide detection device, weighing after the vacuum reaches a set value, and calculating the mass (a) of the added sample;
s4, the sample cup is sent to the heating pool by the mechanical arm;
s5, then performing filter pressing on the membrane on the sample cup;
s6, heating the sample cup to a set temperature value and keeping the temperature for a period of time;
s7, moving the filter membrane to an X-ray fluorescent bar detection window by the mechanical arm, and reading;
s8, moving the sample cup to a balance by a mechanical arm, and weighing to obtain the heated residual mass (b);
s9, calculating the concentration (c) of the selected organic halide in the sample by using a built-in software calibration curve;
s10, the mechanical arm moves the sample cup into the heating pool, a new filter pressing film is covered again, the steps S6-S9 are repeated, and the concentration of the selected organic halide is detected and calculated.
Compared with the prior art, the invention has the advantages and positive effects that:
the invention provides an organic halide detection device and a use method thereof. By utilizing the characteristic that different organic halides have different boiling points, different organic halides in a sample are separated by a vacuum thermal analysis method, and then are rapidly detected by X-ray fluorescence. The device is simple to operate, has sensitivity equivalent to that of the existing X-ray fluorescence technology, can identify different organic halides and detect the concentration of the organic halides, and provides a solution for fulfilling RoHS instructions and the 'Stockholm convention' about persistent organic matters.
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, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of the present invention.
Detailed Description
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 from the embodiments of the present invention by a person skilled in the art without any creative effort, should be included in the protection scope of the present invention.
As shown in fig. 1, the organic halide detection device of the present invention includes a box 1 capable of being vacuumized, wherein a mechanical arm and a bracket 10 moving along the mechanical arm are vertically disposed in a cavity of the box 1 along a height direction of the box, a balance 2 is disposed below the mechanical arm, a heating cell 6 is disposed on one side of the balance 2, an X-ray fluorescence detection assembly 7 is disposed on one side of the heating cell 6, and the heating cell 6 and the X-ray fluorescence detection assembly 7 are located under the mechanical arm.
The mechanical arm comprises a base fixed to the bottom of the box body 1, a vertical arm 3 vertically arranged on the base, and a horizontal arm 9 horizontally arranged and perpendicular to the vertical arm 3, wherein a bracket 10 is arranged on the horizontal arm 9, and the bracket 10 is provided with a walking motor to drive the bracket 10 to walk on the horizontal arm 9. The X-ray fluorescence detection assembly 7 comprises a sealing shell and an X-ray fluorescence rod arranged in the sealing shell, and a detection window 8 is arranged at the top of the sealing shell. A filter membrane frame 4 is further arranged in the cavity of the box body 1, and a filter membrane is placed on the filter membrane frame 4.
The top of the box body 1 is provided with an air pumping port 11 for pumping vacuum, and the air pumping port 11 is connected with a vacuum pump; the box 1 is provided with a sample cell opening 5 at the other side. The heating tank 5 is provided with a temperature sensor to detect the heating temperature of the heating tank.
The invention also provides a using method of the organic halide detection device, which comprises the following steps:
s1, vacuumizing the organic halide detection device, putting an empty sample cup on a bracket of the mechanical arm, and conveying the sample cup to a balance to weigh by the bracket moving along the mechanical arm;
s2, conveying the weighed sample cup to the opening of the sample pool by the mechanical arm, and manually adding the sample into the sample cup;
s3, conveying the sample cup to a balance by a mechanical arm, vacuumizing the organic halide detection device, weighing after the vacuum reaches a set value, and calculating the mass (a) of the added sample;
s4, the sample cup is sent to the heating pool by the mechanical arm;
s5, then performing filter pressing on the membrane on the sample cup;
s6, heating the sample cup to a set temperature value and keeping the temperature for a period of time;
s7, moving the filter membrane to an X-ray fluorescent bar detection window by the mechanical arm, and reading;
s8, moving the sample cup to a balance by a mechanical arm, and weighing to obtain the heated residual mass (b);
s9, calculating the concentration (c) of the selected organic halide in the sample by using a built-in software calibration curve;
s10, the mechanical arm moves the sample cup into the heating pool, a new filter pressing film is covered again, the steps S6-S9 are repeated, and the concentration of the selected organic halide is detected and calculated.
The principle of the invention is as follows: the invention is mainly used for detecting organic halide in materials, the matrix in artificial materials is relatively single, and the organic halide is usually an artificially added compound, such as hexabromocyclododecane, added into a building thermal insulation material for flame retardance.
The mass concentration of specific halogen on the collection surface can be read by utilizing different boiling points of different organic halides, heating to the boiling points of different organic halides (common part of the boiling points of the organic halides are shown in the boiling points of several organic halides in the table 1), volatilizing, adsorbing the volatile onto the filter membrane through negative pressure, and then irradiating the collection surface adsorbing the sample with X-ray fluorescence.
The concentration of the organic halide in the sample can be calculated by using the following formula:
sample quality: a weight value of a
Residual mass of sample after heating: a weight value of b
The concentration value of Br on the collecting surface of the X-ray fluorescence detection sample is c
The organic halide concentration values in the samples were: weight loss on heating (weight loss) collection surface Br concentration/sample mass/target bromide bromine content (a-b) c/a/74.7% (taking hexabromocyclododecane as an example)
The boiling points of several organic halides are shown in the table;
the invention provides an organic halide detection device and a use method thereof. By utilizing the characteristic that different organic halides have different boiling points, different organic halides in a sample are separated by a vacuum thermal analysis method, and then are rapidly detected by X-ray fluorescence. The device is simple to operate, has sensitivity equivalent to that of the existing X-ray fluorescence technology, can identify different organic halides and detect the concentration of the organic halides, and provides a solution for fulfilling RoHS instructions and the 'Stockholm convention' about persistent organic matters.
Claims (7)
1. An organic halide detection device, characterized in that: including a box that can the evacuation, the direction of height along the box is provided with the arm perpendicularly in the cavity of box and follows the bracket that the arm removed, the below of arm is provided with the balance, one side of balance is provided with the heating bath, one side of heating bath is provided with X ray fluorescence detection subassembly, heating bath, X ray fluorescence stick are located under the arm.
2. The organic halide detection device according to claim 1, wherein: the mechanical arm comprises a base fixed to the bottom of the box body, a vertical arm vertically arranged on the base, and a horizontal arm horizontally arranged and perpendicular to the vertical arm, wherein a bracket is arranged on the horizontal arm, and a walking motor is arranged on the bracket to drive the bracket to walk on the horizontal arm.
3. The organic halide detection device according to claim 1, wherein: the X-ray fluorescence detection assembly comprises a sealing shell and an X-ray fluorescence rod arranged in the sealing shell, and a detection window is arranged at the top of the sealing shell.
4. The organic halide detection device according to claim 1, wherein: and a filter membrane frame is also arranged in the cavity of the box body, and a filter membrane is placed on the filter membrane frame.
5. The organic halide detection device according to claim 1, wherein: the top of the box body is provided with an air pumping hole for pumping vacuum, and the air pumping hole is connected with a vacuum pump; the box is provided with a sample cell opening at the other side.
6. The organic halide detection device according to claim 1, wherein: the heating pool is provided with a temperature sensor to detect the heating temperature of the heating pool.
7. A method of using the organic halide detection device of claims 1 to 6, wherein: the using method comprises the following steps:
s1, vacuumizing the organic halide detection device, putting an empty sample cup on a bracket of the mechanical arm, and conveying the sample cup to a balance to weigh by the bracket moving along the mechanical arm;
s2, conveying the weighed sample cup to the opening of the sample pool by the mechanical arm, and manually adding the sample into the sample cup;
s3, conveying the sample cup to a balance by a mechanical arm, vacuumizing the organic halide detection device, weighing after the vacuum reaches a set value, and calculating the mass (a) of the added sample;
s4, the sample cup is sent to the heating pool by the mechanical arm;
s5, then performing filter pressing on the membrane on the sample cup;
s6, heating the sample cup to a set temperature value and keeping the temperature for a period of time;
s7, moving the filter membrane to an X-ray fluorescent bar detection window by the mechanical arm, and reading;
s8, moving the sample cup to a balance by a mechanical arm, and weighing to obtain the heated residual mass (b);
s9, calculating the concentration (c) of the selected organic halide in the sample by using a built-in software calibration curve;
s10, the mechanical arm moves the sample cup into the heating pool, a new filter pressing film is covered again, the steps S6-S9 are repeated, and the concentration of the selected organic halide is detected and calculated.
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| CN202010916249.2A CN111982952A (en) | 2020-09-03 | 2020-09-03 | Organic halide detection device and use method |
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Cited By (1)
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| CN114323856A (en) * | 2021-12-29 | 2022-04-12 | 安徽三义堂生物科技有限公司 | Intelligent detection equipment for residual heavy metals in traditional Chinese medicine decoction pieces |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114323856A (en) * | 2021-12-29 | 2022-04-12 | 安徽三义堂生物科技有限公司 | Intelligent detection equipment for residual heavy metals in traditional Chinese medicine decoction pieces |
| CN114323856B (en) * | 2021-12-29 | 2022-09-16 | 安徽三义堂生物科技有限公司 | Intelligent detection equipment for residual heavy metals in traditional Chinese medicine decoction pieces |
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Application publication date: 20201124 |