CN102539219A - Method for purifying dioxin-like chemicals in environmental matrix extraction liquid - Google Patents

Method for purifying dioxin-like chemicals in environmental matrix extraction liquid Download PDF

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CN102539219A
CN102539219A CN201110396419XA CN201110396419A CN102539219A CN 102539219 A CN102539219 A CN 102539219A CN 201110396419X A CN201110396419X A CN 201110396419XA CN 201110396419 A CN201110396419 A CN 201110396419A CN 102539219 A CN102539219 A CN 102539219A
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silica gel
dioxin
magnesium silicate
luoli
purifying
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CN102539219B (en
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任明忠
张漫雯
张素坤
宁慧平
海景
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South China Institute of Environmental Science of Ministry of Ecology and Environment
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Abstract

The invention discloses a method for purifying dioxin-like chemicals in an environmental matrix extraction liquid; the method comprises the two steps of purifying a composite gel column and then purifying a florisil magnesium silicate-alkaline aluminum oxide composite column, wherein padding in the composite gel column is sequentially glass cotton, quartz sand, neutral silica gel, alkaline silica gel, neutral silica gel, acid silica gel and anhydrous sodium sulfate from bottom to top; and padding in the florisil magnesium silicate-alkaline aluminum oxide composite column is sequentially silanization glass cotton, quartz sand, florisil magnesium silicate, alkaline aluminum oxide and anhydrous sodium sulfate. The method has the advantages that the purification process is short, the purification step is simple, the time of purification processing can be shortened, the purification efficiency is improved, the usage amount of a solvent is reduced, the cost is reduced, and the dioxin detection can be facilitated to be rapidly carried out.

Description

The method of dioxin-like chemical in a kind of purifying environmental matrices extract
Technical field
The present invention relates to the environment measuring technical field, be specifically related to the method for dioxin-like chemical in a kind of purifying environmental matrices extract.
Background technology
Dioxin is claimed the dioxa glutinous rehmannia again, is a kind of colorless and odorless, liposoluble substance that toxicity is serious, and is serious to human harm.Dioxin is actually abbreviation of dioxin; What it referred to is not a kind of one matter; But the structure two big type organic compounds comprising numerous congeners or isomeride all very similar with character, promptly polychlorinated dibenzo-2 is disliked English (PCDDs) and polychlorinated dibenzo (PCDFs).
The analysis of dioxin belongs to ultratrace, multicomponent analysis in the environment, and matrix effect is complicated, and qualitative and quantitative detection is complicated, and it is key link that complete purification process detects for organic micro-pollutant.In the development of purification process, mainly be at present to filler selection and robotization and systematized improvement.At present; The purification method of carrying out has the five step methods of purification of promoting in International Standards Method, national standard method and the industry; Wherein, Five commonly used step purification methods are thorough to sample purification, flow process simple, can accurately measure the content of dioxin and polychlorinated biphenyl, and returning to contract etc. for environmental evaluation, risk assessment and research pollutant source provides reliable experimental technique guarantee.This method comprises that acidic silica gel column purification, multistage silicagel column purify, gel permeation chromatographic column purifies, five purifying step of alkali alumina column purification Fu Luoli magnesium silicate column purification; But have following shortcoming: whole purification process is long; Step is more loaded down with trivial details; The time that needs is longer, and purification method is complicated,, having relatively high expectations to laboratory condition high to analyst's requirement.Above issues limit carrying out fast of dioxin testing.
Summary of the invention
The object of the present invention is to provide the method for dioxin-like chemical in a kind of purifying environmental matrices extract, this method is quick, stable, simple and easy, cheap, can extensively apply to common organic analysis laboratory, promotes carrying out fast of dioxin testing.
For realizing above-mentioned purpose, the present invention adopts following technical scheme:
The method of dioxin-like chemical in a kind of purifying environmental matrices extract is characterized in that comprising following purifying step:
1) compound adhesive column purification: the filler in the said compound adhesive post is followed successively by glass wool, silica sand, neutral silica gel, alkaline silica gel, neutral silica gel, acidic silica gel, anhydrous sodium sulfate by reaching down; After environmental matrices extraction drop advances this compound adhesive post, use the normal hexane wash-out.This step purpose is with the disposable removal of most interference matrix in the sample, comprises grease, fatty acid, pigment, multiring aromatic hydrocarbon substance and various polar materials etc.
2) Fu Luoli magnesium silicate-alkali alumina combined column purifies: the filler in said Fu Luoli magnesium silicate-alkali alumina combined column is followed successively by silanized glass cotton, silica sand, Fu Luoli magnesium silicate, alkali alumina, anhydrous sodium sulfate by reaching down; After environmental matrices extraction drop after step 1) purified advances this Fu Luoli magnesium silicate-alkali alumina combined column; Earlier with normal hexane/methylene chloride mixed liquor wash-out; Wash-out must contain the sample solution of PCBs and other components; This part solution is discarded, obtain to contain the sample solution of PCDD/Fs again with eluent methylene chloride.This step purpose is to remove organo-chlorine pesticide, low pole material, and separating most polychlorinated biphenyl (PCBs) and PBDE (PBDEs) etc., finally reaches the purpose of purification of target thing PCDD/Fs.The Fu Luoli magnesium silicate is a kind of silicon alkaline soil material that uses at U.S. Register, and it has similar purification function with alkali alumina, can optionally remove organo-chlorine pesticide and low pole material.In addition, experiment showed, that it has good effect to separating PCDD/Fs and PCBs.The chemical property of PCBs and PCDD/Fs is similar, and its chromatographic behavior is also similar.Just do not carry out instrumental analysis if in the pre-treatment flow process, do not separate, the phenomenon that some compound will occur overflowing altogether causes the phase mutual interference, has influenced the accurate mensuration of PCDD/Fs.Therefore, must be with two groups of compound separation in pre-treatment.
Preferably, normal hexane the step 2)/normal hexane of methylene chloride mixed liquor and the volume ratio of methylene chloride are 95: 5.
Preferably, compound adhesive post selection blade diameter length ratio is 1: 5~10 normal pressure pressure glass chromatography column, bottom band tetrafluoro joint door.What this compound adhesive post played a major role is the sulfurization of sulfuric acid, so acidic silica gel is placed the upper strata, removes most matrix effect earlier, helps the clean-up effect of lower post chromatography.And between the alkaline silica gel, it is separated to add one deck neutral silica gel work pad, influences clean-up effect with the neutralization reaction of avoiding alkaline silica gel.
Preferably, in the step 1), the internal diameter 2.5cm of compound adhesive post, column length 25cm, the high 1cm of glass wool filler, the high 1cm of quartz sand filler, neutral silica gel 3g, alkaline silica gel 4g, neutral silica gel 3g, acidic silica gel 40g, the high 1cm of anhydrous sodium sulfate.
Preferably, step 1) and step 2) filler pass through following processing before use:
Neutral silica gel: with 550 ℃ of activation>12h of muffle furnace be placed on preserve in the exsiccator subsequent use;
Alkali alumina: with 500 ℃ of muffle furnace activation 8 hours, place exsiccator to reduce to room temperature, sealing is preserved, and uses in 72 hours;
The Fu Luoli magnesium silicate: more than 140 ℃ of activation 24h, taking-up places exsiccator to reduce to room temperature and uses in half an hour;
Anhydrous sodium sulfate: more than 450 ℃ of roasting 4h, be cooled to room temperature, be contained in place in the port grinding bottle preserve in the exsiccator subsequent use;
Silanized glass cotton and silica sand: 450 ℃ of roastings are subsequent use more than 4 hours;
Cotton and filter paper: with after methylene chloride ultrasonic half an hour three times, after vacuum is drained solvent, place preserve in the exsiccator subsequent use.
Preferably, the blade diameter length ratio of Fu Luoli magnesium silicate-alkali alumina combined column is 1: 5~10.
Preferably, the high 1cm of silanized glass cotton packing, the high 1cm of quartz sand filler, Fu Luoli magnesium silicate 1g, alkali alumina 1g, the high 1cm of anhydrous sodium sulfate step 2).
Wash in advance and infiltration with normal hexane earlier behind the compound adhesive column packing, elder generation is with normal hexane flushing and infiltration in advance behind Fu Luoli magnesium silicate-alkali alumina combined column filler.
Compared with prior art, the beneficial effect that the present invention produces is: when guaranteeing clean-up effect, can shorten to the time of purification process, improve purification efficiency and promoted, reduce the purifying solvent use amount, save cost.
Description of drawings
Fig. 1 is the structural representation of compound adhesive post of the present invention;
Fig. 2 is the structural representation of Fu Luoli magnesium silicate of the present invention-alkali alumina combined column.
Embodiment
Below in conjunction with the practical implementation example the present invention is described in further detail.
Embodiment 1
1) preparation of purification reagent
1. neutral silica gel: 70~230 orders, available from Merk company (Darmstadt, Germany), it is subsequent use to be placed in the exsiccator preservation with 550 ℃ of activation>12h of muffle furnace before using;
2. acidic silica gel (40%H 2SO 4): in flask, take by weighing the 60g activated silica gel, add the 40g concentrated sulphuric acid, jumping a queue vibrates to silica gel becomes even flow state; The concentrated sulphuric acid (top grade is pure) is purchased in Guangzhou Chemical Reagent Factory;
3. alkaline silica gel (1.2%): in the 100g activated silica gel, adding 30g concentration is the sodium hydroxide solution of 1mol/L, shakes up, subsequent use; Solid sodium hydroxide is purchased in Guangzhou Chemical Reagent Factory;
4. alkali alumina: high-purity alkali alumina, all use 500 ℃ of muffle furnace activation 8 hours before the use, place exsiccator to reduce to room temperature, sealing is preserved, and uses in 72 hours;
5. Fu Luoli magnesium silicate: 60~100 orders, use more than preceding 140 ℃ of activation 24h, take out and place exsiccator to reduce to room temperature to use in half an hour;
6. anhydrous sodium sulfate: top grade is pure, is used for before the use being cooled to room temperature more than 450 ℃ of roasting 4h, be contained in place in the port grinding bottle preserve in the exsiccator subsequent use.
7. silanized glass cotton and silica sand, 450 ℃ of roastings are subsequent use more than 4 hours;
8. cotton and filter paper, with after methylene chloride ultrasonic half an hour three times, after vacuum is drained solvent, place preserve in the exsiccator subsequent use.
2) preparation of compound adhesive post
Select internal diameter 2.5cm for use; The normal pressure of column length 25cm bottom band tetrafluoro joint door is pressed glass chromatography column; Insert the high quartz sand filler of 1cm high glass wool filler, 1cm, 3g neutral silica gel, 4g alkaline silica gel, 3g neutral silica gel, 40g acidic silica gel, the high 1cm of anhydrous sodium sulfate successively by reaching down, as shown in Figure 1.Filling in the back washes with the 80ml normal hexane and infiltration glue post in advance.
3) Fu Luoli magnesium silicate-alkali alumina combined column preparation
Select internal diameter 2.5cm for use; The normal pressure of column length 25cm bottom band tetrafluoro joint door is pressed glass chromatography column; Insert the high silanized glass cotton of 1cm, the high silica sand of 1cm, 3g neutral silica gel, 4g alkaline silica gel, 3g neutral silica gel, 40g acidic silica gel, the high 1cm of anhydrous sodium sulfate successively by reaching down, as shown in the figure.Filling in the back washes with the 25ml normal hexane and infiltration glue post in advance.
4) environmental matrices is extracted drop and advance the compound adhesive post, with the normal hexane 120ml drip washing compound adhesive post of low polarity, and recovery sample solution.
5) get the sample solution that step 4) obtains and drip into Fu Luoli magnesium silicate-alkali alumina combined column; Elder generation's use 25ml volume ratio is the sample solution that normal hexane/eluent methylene chloride of 95: 5 obtains containing PCBs and other components; A little sample segment solution are discarded, obtain containing the sample solution of pure PCDD/Fs again with the 50ml eluent methylene chloride.
Embodiment 2 methods of the present invention and existing five contrasts of step purification method on solvent and time consumption
Prepare 12 identical environmental matrices extract samples; 6 existing methods of samples using purify; Promptly carry out acidic silica gel column purification, the purification of multistage silicagel column, gel permeation chromatographic column purification, five step of alkali alumina column purification Fu Luoli magnesium silicate column purification purification process successively; Record purifies employed quantity of solvent and clarification time, and results averaged is as shown in table 1; 6 samples using methods of the present invention purify, and record purifies employed quantity of solvent and clarification time, and results averaged is as shown in table 1; The model of using U.S. Waters company to produce is at last steamed concentrate as standardization in height explanation gas chromatography/high-resolution double focusing GC-MS utilization isotope of HP6890N GC/Autospec Premierr to revolving of 12 samples after purifying and is detected, the value basically identical of the FCDD/Fs in 12 samples.
The existing five step method of purification and the contrasts of the inventive method on solvent and time consumption of table 1
Figure BDA0000115661190000061
Can know that by table 1 contrast method of the present invention can reduce to 9 hours by 24 hours with the clarification time, purification efficiency has promoted more than 60%, and two kinds of purifying solvent use amounts have reduced 458ml and 122ml respectively, have saved 66% and 71% respectively.
Embodiment 3 methods of the present invention are applied in the result of actual sample extract
Use this optimization method; PCDD/Fs in environmental matrices (comprising soil, the sediment) extract carries out purifying; After final concentrate adds the interior mark of sample introduction; Use high-resolution gas chromatography/high-resolution double focusing magnetic substance spectrum combined instrument (HRGC/HRMS) to carry out instrumental analysis, instrument manufacturer is a U.S. Waters company, and model is " HP6890N GC/Autospec Premier ".The instrument analytical method that adopts is a scalar quantity method in the isotope.The analysis result of all samples all satisfies the quality control and the quality assurance of domestic and international standard-required.(1) quality control standard substance.
QCS or SRM are meant the sample that comprises concentration known all or part target compound, are used for the checking experiment chamber and carry out usefulness (US EPA, 1994).QCS (EDF-5184, the sediment) extract that adopts method of the present invention to add during two are detected batch purifies, and the purification concentrate that obtains carries out instrumental analysis, the analytical instrument of use.The experimental result of different batches is seen table 2: twice experimental result of this method test stone reference substance compared identical basically with standard value; Except that 234678-HxCDF; All within the deviation range of reference value; And the target recovery has proved the good reproduction property of this method at 46-93% in the extraction of 15 kinds of 13C marks.
Table 2: quality control standard substance (EDF-5184) analysis result (unit: ng/kg)
Figure BDA0000115661190000071
Figure BDA0000115661190000081
(2) actual sample.
Choose six soil and sediment samples that influenced by same pollution source, be numbered S1-S6, S1, S2, S3 are pedotheque, and S4, S5, S6 are sediment sample.Adopt this experimental technique, measured 17 kinds of PCDD/Fs of S1-S6.The recovery of each compound isotopic dilution agent of the precision and the recovery (OPR) is 43~100%, and each compound recovery of 12C-PCDD/Fs is at 90-140%.The mark recovery was 49-106% in the isotope of 15 kinds of PCDD/Fs of S1-S6 sample extracted.Specifically by shown in the table 3.
The analysis result of table 3 S1-S6 soil and sediment sample
(3) the 15 dioxin international comparison activities
Participate in the 15 dioxin international comparison activity (" the 15th round of the 2010international laboratory comparison of dioxin "); Comprise four sediment sample (sediment A; Sediment B, sediment C, sediment D).
This participation preside over " 2010 the 15 take turns the comparison of dioxin International Laboratory " activity by Sweden Orebro university, " International Laboratory comparison working group " chairman Albert van professor Bavel, the laboratory of effectively participating in has 64.According to the statistical method of international comparison in the past, deviation is greater than 2 times of standard deviations (SD), i.e. Z=(x-X)/SD, | Z| is considered to exceptional value greater than 2 data, and exceptional value is not used in assembly average.The relative standard deviation of single measurement data is defined as R=(x-X) * 100/X, can think the degree of closeness of single measurement data and mean value.
The sediment of the 15 international comparison of table 4 and the mensuration result of standard solution
Figure BDA0000115661190000092
The continuous table of going up
Figure BDA0000115661190000102
Figure BDA0000115661190000111
All breadboard ensemble average analysis levels from statistics (table 4) is participated in analysis come the judgment experiment ability from this laboratory report value and other breadboard compare of analysis results.Can judge that from the result Z value of each sample is basically in [2,2], this breadboard mensuration result is for satisfied.That is to say that the PCDD/Fs in this lab analysis sediment and the similar matrix thereof reaches or approaches advanced international standards.
Above-mentioned embodiment is merely preferred implementation of the present invention, can not limit protection scope of the present invention with this, and the variation of any unsubstantiality that those skilled in the art is done on the basis of invention and replacement all belong to the present invention's scope required for protection

Claims (8)

1. the method for dioxin-like chemical in the purifying environmental matrices extract is characterized in that comprising following purifying step:
1) compound adhesive column purification: the filler in the said compound adhesive post is followed successively by glass wool, silica sand, neutral silica gel, alkaline silica gel, neutral silica gel, acidic silica gel, anhydrous sodium sulfate by reaching down; The environmental matrices extract is used the normal hexane wash-out after being transferred to this compound adhesive post;
2) Fu Luoli magnesium silicate-alkali alumina combined column purifies: the filler in said Fu Luoli magnesium silicate-alkali alumina combined column is followed successively by silanized glass cotton, silica sand, Fu Luoli magnesium silicate, alkali alumina, anhydrous sodium sulfate by reaching down; After environmental matrices extract after step 1) purified is transferred to this Fu Luoli magnesium silicate-alkali alumina combined column; With normal hexane/methylene chloride mixed liquor wash-out, obtain to contain the sample solution of PCDD/Fs again with the methylene chloride wash-out earlier.
2. the method for dioxin-like chemical is characterized in that: step 2 in the purifying environmental matrices extract as claimed in claim 1) in the normal hexane/normal hexane of methylene chloride mixed liquor and the volume ratio of methylene chloride be 95:5.
3. the method for dioxin-like chemical in the purifying environmental matrices extract as claimed in claim 1, it is characterized in that: the blade diameter length ratio of compound adhesive post is 1:5~10.
4. like the method for dioxin-like chemical in claim 1 or the 3 described purifying environmental matrices extracts; It is characterized in that: in the step 1), the high 1cm of glass wool filler, the high 1cm of quartz sand filler, neutral silica gel 3g, alkaline silica gel 4g, neutral silica gel 3g, acidic silica gel 40g, the high 1cm of anhydrous sodium sulfate.
5. the method for dioxin-like chemical is characterized in that: step 1) and step 2 in the purifying environmental matrices extract as claimed in claim 1) filler pass through following processing before use:
Neutral silica gel: the interior preservation of exsiccator is subsequent use with being placed on more than 550 ℃ of activation 12h of muffle furnace;
Alkali alumina: with 500 ℃ of muffle furnace activation 8 hours, place exsiccator to reduce to room temperature, sealing is preserved, and uses in 72 hours;
The Fu Luoli magnesium silicate: more than 140 ℃ of activation 24h, taking-up places exsiccator to reduce to room temperature and uses in half an hour;
Anhydrous sodium sulfate: more than 450 ℃ of roasting 4h, be cooled to room temperature, be contained in place in the port grinding bottle preserve in the exsiccator subsequent use;
Silanized glass cotton and silica sand: 450 ℃ of roastings are subsequent use more than 4 hours;
Cotton and filter paper: with after methylene chloride ultrasonic half an hour three times, after vacuum is drained solvent, place preserve in the exsiccator subsequent use.
6. the method for dioxin-like chemical in the purifying environmental matrices extract as claimed in claim 1, it is characterized in that: the blade diameter length ratio of Fu Luoli magnesium silicate-alkali alumina combined column is 1:5~10.
7. like the method for dioxin-like chemical in claim 1 or the 6 described purifying environmental matrices extracts, it is characterized in that: step 2) in the high 1cm of silanized glass cotton packing, the high 1cm of quartz sand filler, Fu Luoli magnesium silicate 1g, alkali alumina 1g, the high 1cm of anhydrous sodium sulfate.
8. the method for dioxin-like chemical in the purifying environmental matrices extract as claimed in claim 1; It is characterized in that: wash in advance and infiltration with normal hexane earlier behind the compound adhesive column packing, elder generation is with normal hexane flushing and infiltration in advance behind Fu Luoli magnesium silicate-alkali alumina combined column filler.
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CN103645086A (en) * 2013-12-30 2014-03-19 宁波市环境监测中心 Pretreatment method for simultaneously purifying persistent organic pollutants of multiple classes in environmental medium
CN104258596A (en) * 2014-09-25 2015-01-07 上海市农业科学院 Solid-phase extraction column for enriching and purifying deoxidized nivalenol
CN105259013A (en) * 2015-10-26 2016-01-20 哈尔滨工业大学 Method for purifying bisphenol compound in surface water sample extraction liquid
CN105974001A (en) * 2016-04-21 2016-09-28 广州普诺环境检测技术服务有限公司 Method for pretreating soil or sediment sample and method for determining dioxin
CN107064382A (en) * 2017-03-15 2017-08-18 广州普诺环境检测技术服务有限公司 A kind of preprocess method of plant leaf blade is Ji the assay method of bioxin
CN112666295A (en) * 2020-12-30 2021-04-16 生态环境部华南环境科学研究所 Method for extracting, cooperatively separating and detecting polychlorinated biphenyl and dioxin in soil
CN114518403A (en) * 2021-12-30 2022-05-20 通标标准技术服务有限公司 Method for detecting dioxin in iron ore sintering process
CN115963213A (en) * 2023-02-08 2023-04-14 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) Method for purifying and separating dioxin, polychlorinated biphenyl and polybrominated diphenyl ether in environmental medium
CN116908356A (en) * 2023-07-19 2023-10-20 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) Purifying device and method for brominated dioxin compounds in environmental sample

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CN103645086A (en) * 2013-12-30 2014-03-19 宁波市环境监测中心 Pretreatment method for simultaneously purifying persistent organic pollutants of multiple classes in environmental medium
CN103645086B (en) * 2013-12-30 2015-11-18 宁波市环境监测中心 The pre-treating method of multiclass persistence organic pollutant in environment purification medium while of a kind of
CN104258596A (en) * 2014-09-25 2015-01-07 上海市农业科学院 Solid-phase extraction column for enriching and purifying deoxidized nivalenol
CN105259013A (en) * 2015-10-26 2016-01-20 哈尔滨工业大学 Method for purifying bisphenol compound in surface water sample extraction liquid
CN105974001A (en) * 2016-04-21 2016-09-28 广州普诺环境检测技术服务有限公司 Method for pretreating soil or sediment sample and method for determining dioxin
CN107064382A (en) * 2017-03-15 2017-08-18 广州普诺环境检测技术服务有限公司 A kind of preprocess method of plant leaf blade is Ji the assay method of bioxin
CN107064382B (en) * 2017-03-15 2019-11-05 广州普诺环境检测技术服务有限公司 A kind of preprocess method of plant leaf blade and the measuring method of dioxin
CN112666295A (en) * 2020-12-30 2021-04-16 生态环境部华南环境科学研究所 Method for extracting, cooperatively separating and detecting polychlorinated biphenyl and dioxin in soil
CN114518403A (en) * 2021-12-30 2022-05-20 通标标准技术服务有限公司 Method for detecting dioxin in iron ore sintering process
CN115963213A (en) * 2023-02-08 2023-04-14 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) Method for purifying and separating dioxin, polychlorinated biphenyl and polybrominated diphenyl ether in environmental medium
CN115963213B (en) * 2023-02-08 2024-06-21 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) Purifying and separating method for dioxin, polychlorinated biphenyl and polybrominated biphenyl ether in environmental medium
CN116908356A (en) * 2023-07-19 2023-10-20 生态环境部华南环境科学研究所(生态环境部生态环境应急研究所) Purifying device and method for brominated dioxin compounds in environmental sample

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