CN114002339A - Method and equipment for measuring semi-volatile organic compounds - Google Patents
Method and equipment for measuring semi-volatile organic compounds Download PDFInfo
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- CN114002339A CN114002339A CN202111041377.8A CN202111041377A CN114002339A CN 114002339 A CN114002339 A CN 114002339A CN 202111041377 A CN202111041377 A CN 202111041377A CN 114002339 A CN114002339 A CN 114002339A
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- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000012855 volatile organic compound Substances 0.000 title claims abstract description 32
- 238000001514 detection method Methods 0.000 claims abstract description 11
- 239000000523 sample Substances 0.000 claims description 67
- 238000005259 measurement Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 13
- 238000012360 testing method Methods 0.000 claims description 12
- 238000007664 blowing Methods 0.000 claims description 9
- 238000002360 preparation method Methods 0.000 claims description 8
- 239000012496 blank sample Substances 0.000 claims description 4
- 238000001819 mass spectrum Methods 0.000 claims description 4
- 238000007689 inspection Methods 0.000 claims description 3
- 239000012521 purified sample Substances 0.000 claims description 3
- 238000003556 assay Methods 0.000 claims 1
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 24
- 239000000243 solution Substances 0.000 description 21
- 239000002689 soil Substances 0.000 description 12
- 239000007789 gas Substances 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000012086 standard solution Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 239000013049 sediment Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- OYNXPGGNQMSMTR-UHFFFAOYSA-N bis(2,3,4,5,6-pentafluorophenyl)-phenylphosphane Chemical compound FC1=C(F)C(F)=C(F)C(F)=C1P(C=1C(=C(F)C(F)=C(F)C=1F)F)C1=CC=CC=C1 OYNXPGGNQMSMTR-UHFFFAOYSA-N 0.000 description 3
- 239000002274 desiccant Substances 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000012421 spiking Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 239000006004 Quartz sand Substances 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- -1 decafluorotriphenylphosphine ions Chemical class 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 239000011491 glass wool Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical class [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
- 239000012085 test solution Substances 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The invention relates to the technical field of detection, in particular to a method and equipment for measuring semi-volatile organic compounds.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a method and equipment for determining semi-volatile organic compounds.
Background
The semi-volatile organic compound generally refers to an organic compound with the boiling point of 24-400 ℃ and the vapor pressure of (0.1-10-7) multiplied by 133.322Pa, and along with the acceleration of the urbanization process in China and the increasing improvement of the living standard of residents, the demand of corresponding resources is increased year by year, so that the total amount and the types of the solid waste are in an increasing trend.
The existing method for detecting semi-volatile organic compounds is not highly accurate, so it is urgently needed to design a method for detecting semi-volatile organic compounds accurately.
Disclosure of Invention
The invention aims to provide a method and equipment for measuring semi-volatile organic compounds, which aim to solve the problem of low accuracy of detecting the semi-volatile organic compounds in the prior art.
In order to achieve the above object, the present invention provides a method for measuring semi-volatile organic compounds, which comprises the following steps:
collecting and storing samples;
preparing a sample;
preparing a blank sample;
drawing a standard curve and a linear range;
measuring the detection limit and the measurement lower limit;
samples were tested for precision and accuracy.
Before the step of preparing the sample, the method further comprises the steps of:
the samples were subjected to moisture determination.
The specific steps for preparing the sample are as follows:
drying the sample;
extracting the prepared sample;
carrying out nitrogen-blowing concentration on the extracted sample;
purifying the sample after nitrogen-blowing concentration;
and carrying out constant volume measurement on the purified sample.
The specific steps for drawing the standard curve and the linear range are as follows:
performing performance inspection on the mass spectrum;
a standard curve is established.
The method for testing the precision and the accuracy of the sample comprises the following specific steps:
carrying out low-concentration standard adding precision and accuracy tests on the sample;
performing medium concentration standard adding precision and accuracy tests on the sample;
the samples were tested for high concentration standard precision and accuracy.
The invention also provides a determination device for the determination method of the semi-volatile organic compounds, which comprises a determination box and a gas chromatography-mass spectrometer, wherein the determination box is provided with a drying chamber and a preparation chamber, the drying chamber and the preparation chamber are arranged at intervals, the gas chromatography-mass spectrometer is fixedly connected with the determination box, and the gas chromatography-mass spectrometer is positioned at the top of the determination box.
The method and the device for measuring the semi-volatile organic compounds solve the problem of low accuracy in detecting the semi-volatile organic compounds in the prior art, and realize efficient and accurate detection of the semi-volatile organic compounds.
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.
FIG. 1 is a flow chart of a method for measuring semi-volatile organic compounds according to the present invention.
FIG. 2 is a flowchart illustrating a detailed step S300 of the method for measuring semi-volatile organic compounds according to the present invention.
FIG. 3 is a flowchart illustrating a detailed step S340 of the method for measuring semi-volatile organic compounds according to the present invention.
FIG. 4 is a flowchart illustrating a detailed step S500 of the method for measuring semi-volatile organic compounds according to the present invention.
FIG. 5 is a flowchart illustrating a specific step S700 of the method for measuring semi-volatile organic compounds according to the present invention.
FIG. 6 is a schematic view showing the structure of an apparatus for measuring a semi-volatile organic compound according to the method for measuring a semi-volatile organic compound of the present invention.
1-measuring box, 11-drying chamber, 12-preparing chamber and 2-gas chromatography-mass spectrometer.
Detailed Description
Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to the same or similar elements or elements having the same or similar function throughout.
Referring to fig. 1 to 5, a method for measuring semi-volatile organic compounds includes the following steps:
s100: collecting and storing samples;
the soil sample is collected and stored according to the related requirements of HJ/T166, the sediment sample is collected and stored according to the related requirements of GB17378.3, the sample is stored in a clean brown glass bottle with a plug and a ground opening, and the sample is stored in a sealed and light-proof manner at the temperature of below 4 ℃ and is stored in a sealed and light-proof manner during transportation, and the storage time is not more than 10 days.
S200: carrying out moisture measurement on the sample;
soil sample dry matter content regulation was performed according to HJ613 and sediment sample moisture content determination was performed according to GB 17378.5.
S300: preparing a sample;
s310: drying the sample;
putting the sample on an enamel plate or a stainless steel plate, uniformly mixing, removing foreign matters such as branches, leaves and stones, and roughly dividing by a quartering method according to HJ/T166. Samples for the purpose of screening for contaminants should be treated with fresh samples. When the natural drying does not affect the analysis purpose, the sample can be naturally dried. Fresh soil or sediment samples can be dried using freeze drying methods and desiccant methods. If the water content in the soil and sediment samples is high (more than 30%), the water phase is separated by centrifugation and then dried.
The freeze drying method comprises the following specific steps: taking a proper amount of the uniformly mixed sample, and putting the sample into a vacuum freeze dryer for drying and dehydrating. The dried sample is ground, sieved by a 0.25mm pore size sieve and homogenized into particles of about 250 mu m (60 meshes). Then, 20g (to the nearest 0.01g) of the sample was weighed out and transferred to an extractor for further use.
The drying agent method comprises the following specific steps: weighing 20g (accurate to 0.01g) of fresh sample, adding a certain amount of desiccant, mixing, dehydrating, grinding into fine granules, stirring thoroughly until the granules are dispersed, and transferring into an extraction container for use.
S320: extracting the prepared sample;
the extraction method is implemented according to HJ 783, and if the extract contains obvious water, further filtering and dehydrating; a layer of glass wool or glass fiber filter membrane is padded on a glass funnel, about 5g of anhydrous sodium sulfate is added, and the extracting solution is filtered into a concentration vessel; washing the extraction container with a small amount of mixed solvent of dichloromethane and acetone for 3 times, filtering the washing solution in a funnel, washing the funnel with a small amount of mixed solvent of dichloromethane and acetone, collecting the filtrate in a concentration vessel, and concentrating.
S330: carrying out nitrogen-blowing concentration on the extracted sample;
under the condition of room temperature, starting nitrogen until the surface of the solvent has airflow fluctuation (avoiding forming air vortex), and washing nitrogen through the leaked concentrator pipe wall in the process by using methylene chloride for multiple times; concentrating to about 2mL, and stopping concentrating; when a specific kind of semi-volatile organic compound needs to be purified, the solvent conversion needs to be carried out according to appendix B of HJ834-2017, and then the concentrated solution is concentrated to about 1mL for purification.
S340: purifying the sample after nitrogen-blowing concentration;
the specific steps for purifying the sample after nitrogen-blowing concentration are as follows:
s341: purifying the sample after nitrogen-blowing concentration by a chromatographic column;
about 10g of the activated magnesium silicate filler was placed in a glass chromatography column, about 10g of anhydrous sodium sulfate was added thereto, and the column was tapped to fill the filler. The column was pre-eluted with about 40mL of dichloromethane and this fraction of the eluate was discarded. The concentrate was transferred to a column for purification, and the column was washed with about 30mL of dichloromethane to collect the whole effluent.
S342: and (4) purifying the sample purified by the chromatographic column by using a silica gel column.
The silica gel column was rinsed with dichloromethane and n-hexane (1:1) and the rinse was discarded. Pouring the concentrated extract into a silica gel column, collecting the filtrate, rinsing with 5mL of dichloromethane and n-hexane (1:1), collecting, and combining the filtrates.
S350: and carrying out constant volume measurement on the purified sample.
And concentrating the purified test solution again according to the nitrogen blowing concentration step, adding a proper amount of internal standard intermediate solution, metering the volume to 1.0mL, uniformly mixing, transferring to an injection bottle, and testing.
S400: preparing a blank sample;
a blank sample was prepared in the same procedure as the preparation of the sample, using quartz sand instead of the actual sample.
S500: drawing a standard curve and a linear range;
the specific steps for drawing the standard curve and the linear range are as follows:
s510: performing performance inspection on the mass spectrum;
before each analysis, mass spectrum automatic tuning is carried out, then the gas chromatography and the mass spectrometer are set to the instrument conditions required by the analysis method and are in a standby state, 1.0 mu L of decafluorotriphenylphosphine solution with the concentration of 50mg/L is directly injected through a gas chromatography sample inlet, a decafluorotriphenylphosphine mass spectrogram is obtained, and the ion abundance of mass fragments of the decafluorotriphenylphosphine mass spectrogram completely meets the requirements in the table 1. Otherwise, the mass spectrometer ion source must be cleaned.
| Mass to charge ratio (m/z) | Specification of relative abundance | Mass to charge ratio (m/z) | Specification of relative abundance |
| 51 | 198 Peak (base Peak) 30-60% | 199 | 198 Peak (base Peak) 5-9% |
| 68 | Less than 2% of the 69 peak | 275 | 10-30% of the base peak |
| 70 | Less than 2% of the 69 peak | 365 | More than 1 percent of the basic peak |
| 127 | 40-60% of base peak | 441 | There is a peak less than 443 |
| 197 | Less than 1% of the 198 peak | 442 | 40% of base peak or more than 198 peak |
| 198 | Base peak, |
443 | 17-23% of peak 442 |
TABLE 1 Specification for abundance of decafluorotriphenylphosphine ions
S520: a standard curve is established.
200 mu g/mL standard solutions of 5 mu L, 25 mu L, 50 mu L, 100 mu L and 250 mu L are respectively transferred by a micro syringe and added into corresponding 5 sample bottles of 1mL, 6 substitute standard solutions with the volume same as that of the standard solution and the concentration of 200 mu g/mL are synchronously added into the series of standard solutions, simultaneously, 100 mu L of 6 internal standard solution standard solutions with the concentration of 400 mu g/mL are respectively added into the sample bottles, and the volume is increased to 1.0mL by using dichloromethane. According to the reference condition of the instrument, samples are sequentially injected from low concentration to high concentration for analysis. Taking the concentration of the target compound as an abscissa; and drawing a standard curve by taking the product of the ratio of the quantitative ion response value of the target compound to the internal standard compound and the mass concentration of the internal standard compound as a vertical coordinate.
TABLE 2 Standard Curve
S600: measuring the detection limit and the measurement lower limit;
the sample was replaced with quartz sand, and 5.0. mu.g of the standard use solution and 10. mu.g of the 6 substitute standard use solutions were added to the microsyringe so that the concentrations of the target substance and the 6 substitute were 5.0. mu.g/mL and 10. mu.g/mL, respectively. The pretreatment process is carried out according to the sample experiment steps, the measurement conditions are the same as the working curve, and the mean value, the relative deviation, the detection limit and the measurement lower limit are calculated.
TABLE 3 detection limits and lower measurement limits
S700: samples were tested for precision and accuracy.
The method for testing the precision and the accuracy of the sample comprises the following specific steps:
s710: carrying out low-concentration standard adding precision and accuracy tests on the sample;
taking 200g of a soil sample with the sample number of T21043010001, adding 200 mug/mL of standard use solution for artificial pollution, wherein 6 parts of 20.0g of soil are weighed, 15 mug/mL of standard use solution with the concentration of 200 mug/mL is respectively added, and the addition amount is 3.0 mug; weighing 1 part of the standard use solution, adding 7 parts of the pretreatment process according to the sample experiment steps, respectively adding 50 mu L of 6 substitute standard use solutions with the concentration of 200 mu g/mL by using a micro-injector, wherein the measurement conditions are the same as the working curve, and calculating the mean value, the relative deviation and the standard addition recovery rate.
TABLE 4 precision of Low concentration spiking
S720: performing medium concentration standard adding precision and accuracy tests on the sample;
taking 200g of a soil sample with the sample number of T21043010002, adding 200 mug/mL of standard use solution for artificial pollution, wherein 6 parts of 20.0g of soil are weighed, 25 mug/mL of standard use solution with the concentration of 200 mug/mL is respectively added, and the addition amount is 5.0 mug; weighing 1 part of the standard use solution, adding 7 parts of the pretreatment process according to the sample experiment steps, respectively adding 50 mu L of 6 substitute standard use solutions with the concentration of 200 mu g/mL by using a micro-injector, wherein the measurement conditions are the same as the working curve, and calculating the mean value, the relative deviation and the standard addition recovery rate.
Precision of concentration spiking in Table 5
S730: the samples were tested for high concentration standard precision and accuracy.
Taking 200g of a soil sample with the sample number of T21043010003, adding 200 mug/mL of standard use solution for artificial pollution, wherein 6 parts of 20.0g of soil are weighed, and 50 mug of standard use solution with the concentration of 200 mug/mL is respectively added into the soil sample, and the addition amount is 10.0 mug; weighing 1 part of the standard use solution, adding 7 parts of the pretreatment process according to the sample experiment steps, respectively adding 50 mu L of 6 substitute standard use solutions with the concentration of 200 mu g/mL by using a micro-injector, wherein the measurement conditions are the same as the working curve, and calculating the mean value, the relative deviation and the standard addition recovery rate.
TABLE 6 high concentration spiking precision
The test results of detection limit, precision and accuracy of various test levels of soil aniline are summarized as follows:
table 7 method confirmation summary table
Referring to fig. 6, the present invention further provides a measurement apparatus for a method for measuring semi-volatile organic compounds, the measurement apparatus includes a measurement box and a gas chromatography-mass spectrometer, the measurement box has a drying chamber and a preparation chamber, the drying chamber and the preparation chamber are spaced apart from each other, the gas chromatography-mass spectrometer is fixedly connected to the measurement box, and the gas chromatography-mass spectrometer is located at the top of the measurement box.
In this embodiment, the drying chamber is configured to dry a sample, the preparation chamber is configured to prepare the sample, the gas chromatograph/mass spectrometer is configured to detect the sample, and the parameters of the gas chromatograph/mass spectrometer are as follows: a chromatographic column: the stationary phase of Rtx-5MS capillary column (30m × 0.25mm × 0.25 μm) is 5% -phenyl-methyl polysiloxane; flow rate of the chromatographic column: 1.0 mL/min; and (3) sample introduction mode: split 2: 1; sample introduction volume: 1 mu L of the solution; temperature rising procedure: 40 ℃ (1min) → 10 ℃/min → 150 ℃ (2min) → 10 ℃/min → 300 ℃ (6 min); ion source temperature: 250 ℃; interface temperature: 300 ℃; ionization energy: 70 eV; the mass range is as follows: 40-550 amu; solvent delay time: 3 min; the scanning mode is as follows: full scanning; detector voltage: and the detection box is consistent with the tuning voltage, and the semi-volatile organic compounds are accurately detected through the mutual matching of the detection box and the gas chromatography-mass spectrometer so as to solve the problem of low accuracy in detecting the semi-volatile organic compounds in the prior art.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (6)
1. The method for measuring the semi-volatile organic compounds is characterized by comprising the following steps:
collecting and storing samples;
preparing a sample;
preparing a blank sample;
drawing a standard curve and a linear range;
measuring the detection limit and the measurement lower limit;
samples were tested for precision and accuracy.
2. The method for determining semi-volatile organic compounds according to claim 1,
before the step of preparing the sample, the method further comprises the steps of:
the samples were subjected to moisture determination.
3. The method for determining semi-volatile organic compounds according to claim 2,
the specific steps for preparing the sample are as follows:
drying the sample;
extracting the prepared sample;
carrying out nitrogen-blowing concentration on the extracted sample;
purifying the sample after nitrogen-blowing concentration;
and carrying out constant volume measurement on the purified sample.
4. The method for determining semi-volatile organic compounds according to claim 3,
the specific steps for drawing the standard curve and the linear range are as follows:
performing performance inspection on the mass spectrum;
a standard curve is established.
5. The method for determining semi-volatile organic compounds according to claim 4,
the method for testing the precision and the accuracy of the sample comprises the following specific steps:
carrying out low-concentration standard adding precision and accuracy tests on the sample;
performing medium concentration standard adding precision and accuracy tests on the sample;
the samples were tested for high concentration standard precision and accuracy.
6. An assay apparatus used for the method for assaying semi-volatile organic compounds according to claim 5,
the measuring equipment comprises a measuring box and a gas chromatography-mass spectrometer, wherein the measuring box is provided with a drying chamber and a preparation chamber, the drying chamber and the preparation chamber are arranged at intervals, the gas chromatography-mass spectrometer is fixedly connected with the measuring box, and the gas chromatography-mass spectrometer is positioned at the top of the measuring box.
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