CN112763630A - Method for detecting hexabromododecane in electronic and electric products - Google Patents
Method for detecting hexabromododecane in electronic and electric products Download PDFInfo
- Publication number
- CN112763630A CN112763630A CN202110073150.5A CN202110073150A CN112763630A CN 112763630 A CN112763630 A CN 112763630A CN 202110073150 A CN202110073150 A CN 202110073150A CN 112763630 A CN112763630 A CN 112763630A
- Authority
- CN
- China
- Prior art keywords
- extraction
- hexabromododecane
- sample
- mixed solution
- electronic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
-
- 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
- G01N2030/062—Preparation extracting sample from raw material
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for detecting hexabromododecane in an electronic and electric product, which comprises the steps of weighing 0.5g of a sample, placing the sample in a microwave extraction tank, adding 10mL of dichloromethane, carrying out vortex oscillation for 2min, carrying out ultrasonic extraction at 70-75 ℃ for 1h, fully cooling an extraction solution after extraction is finished, taking a small column, activating by using a methanol mixed solution, washing the inner wall of the extraction tank and a cover by using the methanol mixed solution, eluting the small column by using a washing solution, combining and collecting an eluent into a rotary evaporation bottle, carrying out vacuum rotary evaporation until the eluent is nearly dry, adding the methanol mixed solution into the evaporation bottle to dissolve residues, transferring the dissolved residues into a volumetric flask to carry out constant volume, carrying out gas chromatography detection, controlling the column temperature to be 30 ℃, directly carrying out ultrasonic extraction for 1h by using dichloromethane, not adding acetone for extraction, saving reagent cost compared with the traditional mode, and being simple in operation, the time is shortened, and the bromine residue in the gas chromatographic column can be eliminated.
Description
Technical Field
The invention relates to the technical field of hexabromododecane detection methods, in particular to a detection method of hexabromododecane in an electronic and electric product.
Background
In the existing hexabromododecane detection method in electronic and electric products, dichloromethane and acetone are mixed in equal proportion, microwave extraction is adopted for 2 hours, and the mixture passes through a solid phase extraction column and is concentrated into a gas chromatography column, so that the cost is increased, the time is long, and the bromine residue in the gas chromatography column cannot be eliminated, so that an improved technology is urgently needed to solve the problem in the prior art.
Disclosure of Invention
The invention aims to provide a method for detecting hexabromododecane in an electronic and electric product, which directly uses dichloromethane for ultrasonic extraction for 1 hour, does not need to add acetone for extraction, saves reagent cost compared with the traditional mode, is simple to operate, shortens time, and can eliminate bromine residue in a gas chromatographic column so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for detecting hexabromododecane in electronic and electric products comprises the following steps:
the method comprises the following steps: splitting a sample according to requirements, then crushing the sample by using a crusher, uniformly mixing, and storing at room temperature in a dryer for later use;
step two: weighing 0.5g of sample, placing the sample in a microwave extraction tank, adding 10mL of dichloromethane, and then carrying out vortex oscillation for 1-2 min;
step three: carrying out ultrasonic extraction at 70-75 ℃ for 1h, and fully cooling the extract liquor after the extraction is finished;
step four: taking a small column, and activating by using a methanol mixed solution;
step five: washing the inner walls of the extraction tank and the cover with a methanol mixed solution, eluting the small column with the washing solution, merging and collecting the eluent to a rotary evaporation bottle, and performing vacuum rotary evaporation until the eluent is nearly dry;
step six: adding a methanol mixed solution into the evaporation bottle to dissolve the residue, and transferring the residue into a volumetric flask to fix the volume;
step seven: gas chromatography detection was performed and the column temperature was controlled at 30 ℃.
Preferably, the particle size of the crushed sample in the first step is less than or equal to 1 mm.
Preferably, the vortex oscillation in the second step is performed by using a vortex oscillator.
Preferably, the ultrasonic extraction in the third step is performed by using a microwave extractor.
Preferably, the ratio of methanol to water in the methanol mixture in the fourth step, the fifth step and the sixth step is 2 to 8.
Preferably, the gas chromatography detection in the seventh step adopts a gas chromatography-mass spectrometer.
Compared with the prior art, the invention has the beneficial effects that:
the method can directly perform ultrasonic extraction for 1 hour by using dichloromethane, does not need to add acetone for extraction, saves reagent cost compared with the traditional mode, is simple to operate, shortens time, and can eliminate bromine residues in a gas chromatographic column.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
The invention provides a technical scheme that: a method for detecting hexabromododecane in electronic and electric products comprises the following steps:
the method comprises the following steps: splitting a sample according to requirements, then crushing the sample by using a crusher until the particle size is less than or equal to 1mm, uniformly mixing, and storing at room temperature in a dryer for later use;
step two: weighing 0.5g of sample, placing the sample in a microwave extraction tank, adding 10mL of dichloromethane, and then carrying out vortex oscillation for 1-2min by adopting a vortex oscillator;
step three: performing ultrasonic extraction for 1h at 70-75 ℃ by using a microwave extractor, and fully cooling the extract liquor after the extraction is finished;
step four: taking a small column, and activating by using a methanol mixed solution (methanol: water =2: 8);
step five: washing the inner walls of the extraction tank and the cover with a methanol mixed solution, eluting the small column with the washing solution, merging and collecting the eluent to a rotary evaporation bottle, and performing vacuum rotary evaporation until the eluent is nearly dry;
step six: adding a methanol mixed solution into the evaporation bottle to dissolve the residue, and transferring the residue into a volumetric flask to fix the volume;
step seven: the GC MS was used for gas chromatography detection, and the column temperature was controlled at 30 ℃.
The first embodiment is as follows:
a method for detecting hexabromododecane in electronic and electric products comprises the following steps:
the method comprises the following steps: splitting a sample according to requirements, then crushing the sample by using a crusher until the particle size is less than or equal to 1mm, uniformly mixing, and storing at room temperature in a dryer for later use;
step two: weighing 0.5g of sample, placing the sample in a microwave extraction tank, adding 10mL of dichloromethane, and then carrying out vortex oscillation for 1min by adopting a vortex oscillator;
step three: performing ultrasonic extraction for 1h at 70 deg.C with a microwave extraction apparatus, and cooling the extractive solution;
step four: taking a small column, and activating by using a methanol mixed solution (methanol: water =2: 8);
step five: washing the inner walls of the extraction tank and the cover with a methanol mixed solution, eluting the small column with the washing solution, merging and collecting the eluent to a rotary evaporation bottle, and performing vacuum rotary evaporation until the eluent is nearly dry;
step six: adding a methanol mixed solution into the evaporation bottle to dissolve the residue, and transferring the residue into a volumetric flask to fix the volume;
step seven: the GC MS was used for gas chromatography detection, and the column temperature was controlled at 30 ℃.
Example two:
a method for detecting hexabromododecane in electronic and electric products comprises the following steps:
the method comprises the following steps: splitting a sample according to requirements, then crushing the sample by using a crusher until the particle size is less than or equal to 1mm, uniformly mixing, and storing at room temperature in a dryer for later use;
step two: weighing 0.5g of sample, placing the sample in a microwave extraction tank, adding 10mL of dichloromethane, and then carrying out vortex oscillation for 2min by adopting a vortex oscillator;
step three: performing ultrasonic extraction for 1h at 75 ℃ by using a microwave extraction instrument, and fully cooling the extract liquor after the extraction is finished;
step four: taking a small column, and activating by using a methanol mixed solution (methanol: water =2: 8);
step five: washing the inner walls of the extraction tank and the cover with a methanol mixed solution, eluting the small column with the washing solution, merging and collecting the eluent to a rotary evaporation bottle, and performing vacuum rotary evaporation until the eluent is nearly dry;
step six: adding a methanol mixed solution into the evaporation bottle to dissolve the residue, and transferring the residue into a volumetric flask to fix the volume;
step seven: the GC MS was used for gas chromatography detection, and the column temperature was controlled at 30 ℃.
Example three:
a method for detecting hexabromododecane in electronic and electric products comprises the following steps:
the method comprises the following steps: splitting a sample according to requirements, then crushing the sample by using a crusher until the particle size is less than or equal to 1mm, uniformly mixing, and storing at room temperature in a dryer for later use;
step two: weighing 0.5g of sample, placing the sample in a microwave extraction tank, adding 10mL of dichloromethane, and then carrying out vortex oscillation by adopting a vortex oscillator for 1.5 min;
step three: performing ultrasonic extraction for 1h at 72 ℃ by using a microwave extraction instrument, and fully cooling the extract liquor after the extraction is finished;
step four: taking a small column, and activating by using a methanol mixed solution (methanol: water =2: 8);
step five: washing the inner walls of the extraction tank and the cover with a methanol mixed solution, eluting the small column with the washing solution, merging and collecting the eluent to a rotary evaporation bottle, and performing vacuum rotary evaporation until the eluent is nearly dry;
step six: adding a methanol mixed solution into the evaporation bottle to dissolve the residue, and transferring the residue into a volumetric flask to fix the volume;
step seven: the GC MS was used for gas chromatography detection, and the column temperature was controlled at 30 ℃.
Example four:
a method for detecting hexabromododecane in electronic and electric products comprises the following steps:
the method comprises the following steps: splitting a sample according to requirements, then crushing the sample by using a crusher until the particle size is less than or equal to 1mm, uniformly mixing, and storing at room temperature in a dryer for later use;
step two: weighing 0.5g of sample, placing the sample in a microwave extraction tank, adding 10mL of dichloromethane, and then carrying out vortex oscillation for 1min by adopting a vortex oscillator;
step three: performing ultrasonic extraction for 1h at 75 ℃ by using a microwave extraction instrument, and fully cooling the extract liquor after the extraction is finished;
step four: taking a small column, and activating by using a methanol mixed solution (methanol: water =2: 8);
step five: washing the inner walls of the extraction tank and the cover with a methanol mixed solution, eluting the small column with the washing solution, merging and collecting the eluent to a rotary evaporation bottle, and performing vacuum rotary evaporation until the eluent is nearly dry;
step six: adding a methanol mixed solution into the evaporation bottle to dissolve the residue, and transferring the residue into a volumetric flask to fix the volume;
step seven: the GC MS was used for gas chromatography detection, and the column temperature was controlled at 30 ℃.
Example five:
a method for detecting hexabromododecane in electronic and electric products comprises the following steps:
the method comprises the following steps: splitting a sample according to requirements, then crushing the sample by using a crusher until the particle size is less than or equal to 1mm, uniformly mixing, and storing at room temperature in a dryer for later use;
step two: weighing 0.5g of sample, placing the sample in a microwave extraction tank, adding 10mL of dichloromethane, and then carrying out vortex oscillation for 2min by adopting a vortex oscillator;
step three: performing ultrasonic extraction for 1h at 70 deg.C with a microwave extraction apparatus, and cooling the extractive solution;
step four: taking a small column, and activating by using a methanol mixed solution (methanol: water =2: 8);
step five: washing the inner walls of the extraction tank and the cover with a methanol mixed solution, eluting the small column with the washing solution, merging and collecting the eluent to a rotary evaporation bottle, and performing vacuum rotary evaporation until the eluent is nearly dry;
step six: adding a methanol mixed solution into the evaporation bottle to dissolve the residue, and transferring the residue into a volumetric flask to fix the volume;
step seven: the GC MS was used for gas chromatography detection, and the column temperature was controlled at 30 ℃.
As shown in the first to fifth embodiments, the method disclosed by the invention can realize recovery, the recovery rate is 80-115%, and the method is different from the traditional method, but can be used for directly performing ultrasonic extraction for 1 hour by using dichloromethane, and acetone is not required to be added for extraction, so that the reagent cost is saved compared with the traditional method, the operation is simple, the time is shortened, and the bromine residue in a gas chromatographic column can be eliminated.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A detection method of hexabromododecane in electronic and electric products is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: splitting a sample according to requirements, then crushing the sample by using a crusher, uniformly mixing, and storing at room temperature in a dryer for later use;
step two: weighing 0.5g of sample, placing the sample in a microwave extraction tank, adding 10mL of dichloromethane, and then carrying out vortex oscillation for 1-2 min;
step three: carrying out ultrasonic extraction at 70-75 ℃ for 1h, and fully cooling the extract liquor after the extraction is finished;
step four: taking a small column, and activating by using a methanol mixed solution;
step five: washing the inner walls of the extraction tank and the cover with a methanol mixed solution, eluting the small column with the washing solution, merging and collecting the eluent to a rotary evaporation bottle, and performing vacuum rotary evaporation until the eluent is nearly dry;
step six: adding a methanol mixed solution into the evaporation bottle to dissolve the residue, and transferring the residue into a volumetric flask to fix the volume;
step seven: gas chromatography detection was performed and the column temperature was controlled at 30 ℃.
2. The method for detecting hexabromododecane in an electronic and electric product as claimed in claim 1, wherein: the particle size of the crushed sample in the first step is less than or equal to 1 mm.
3. The method for detecting hexabromododecane in an electronic and electric product as claimed in claim 1, wherein: and in the second step, vortex oscillation is performed by adopting a vortex oscillator.
4. The method for detecting hexabromododecane in an electronic and electric product as claimed in claim 1, wherein: and the ultrasonic extraction in the third step is carried out by adopting a microwave extractor.
5. The method for detecting hexabromododecane in an electronic and electric product as claimed in claim 1, wherein: the ratio of methanol to water in the methanol mixed solution in the fourth step, the fifth step and the sixth step is 2 to 8.
6. The method for detecting hexabromododecane in an electronic and electric product as claimed in claim 1, wherein: and seventhly, gas chromatography and mass spectrometry are adopted for gas chromatography detection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110073150.5A CN112763630A (en) | 2021-01-20 | 2021-01-20 | Method for detecting hexabromododecane in electronic and electric products |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110073150.5A CN112763630A (en) | 2021-01-20 | 2021-01-20 | Method for detecting hexabromododecane in electronic and electric products |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112763630A true CN112763630A (en) | 2021-05-07 |
Family
ID=75703358
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110073150.5A Pending CN112763630A (en) | 2021-01-20 | 2021-01-20 | Method for detecting hexabromododecane in electronic and electric products |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112763630A (en) |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101216467A (en) * | 2008-01-14 | 2008-07-09 | 谱尼测试科技（北京）有限公司 | Electronic material hexabromocyclododecane content determination method |
-
2021
- 2021-01-20 CN CN202110073150.5A patent/CN112763630A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101216467A (en) * | 2008-01-14 | 2008-07-09 | 谱尼测试科技（北京）有限公司 | Electronic material hexabromocyclododecane content determination method |
Non-Patent Citations (2)
| Title |
|---|
| 卢晓宇等: "快速溶剂萃取-固相萃取-液相色谱-串联质谱法同时检测小型家用电器中溴代阻燃剂", 《质谱学报》 * |
| 陈利娟等: "气相色谱-质谱法测定发泡聚苯乙烯材料中六溴环十二烷的含量", 《理化检验(化学分册)》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101735233B (en) | Method for producing high-purity glabridin | |
| CN103936837B (en) | Not Kangding B of a kind of purification knob0Method | |
| CN104262200B (en) | One recycles waste water and prepares N, N ' production method of-dicyclohexylcarbodiimide | |
| Carter | NP/MS since 1970: from the basement to the bench top | |
| Zhang et al. | Solvent extraction of rubidium from a sulfate solution with high concentrations of rubidium and potassium using 4-tert-butyl-2-(α-methylbenzyl)-phenol | |
| CN104713964B (en) | The pre-treating method of PBDE in a kind of environment solid matrix | |
| Huang et al. | Extraction of rubidium and cesium from brine solutions using a room temperature ionic liquid system containing 18-crown-6 | |
| Du et al. | Ionic liquid-based microwave-assisted extraction and HPLC analysis of dehydrocavidine in corydalis saxicola Bunting | |
| CN112763630A (en) | Method for detecting hexabromododecane in electronic and electric products | |
| CN101402577A (en) | Method for extracting and separating levorotation-synephrine from green tangerine orange peel | |
| Tong et al. | A consecutive preparation method based upon accelerated solvent extraction and high‐speed counter‐current chromatography for isolation of aesculin from C ortex fraxinus | |
| Tong et al. | Rapid extraction, discrimination and quantification of thermally unstable isomeric acteoside and isoacteoside in natural products by online extraction-quadrupole time-of-flight tandem mass spectrometry | |
| CN106588705A (en) | Technology for synthesizing glycol dibenzenesulfonate from nano-solid alkali catalyst | |
| CN113173835B (en) | Method for preparing high-purity bakuchiol by high-speed countercurrent chromatography separation | |
| CN104892642A (en) | Method for purifying vindesine | |
| Xinying et al. | Important progress in ion chromatography and its recent developments in China | |
| Hui et al. | Fingerprint profiling of Astragalus polysaccharides based on partial acid hydrolysis-hydrophilic interaction chromatography analysis and comprehensive quality evaluation of Astragalus membranaceus combined with reversed-phase liquid chromatography fingerprint analysis | |
| Liu | Microwave-assisted three-liquid-phase extraction of diosgenin and steroidal saponins from fermentation broth of Dioscorea zingiberensis CH Wright | |
| CN111635448A (en) | Method for treating cyproterone acetate mother liquor | |
| CN107621508B (en) | Method for detecting metabolic products of piperine in animal body | |
| Huimin et al. | Research advances of enrichment approaches based on chemical reactions in glycoproteomics | |
| CN112321489A (en) | Electrophilic molecular probe based on active sulfydryl and report ions and preparation method and application thereof | |
| CN110790811A (en) | Method for preparing diosgenin by aluminum chloride hydrolysis in two-phase system | |
| CN106198829B (en) | A kind of method of fire retardant and content of plasticizing agent in Rapid Simultaneous Determination electronic product | |
| Deliang et al. | Reactive extraction of nicotinic acid with trialkylamine in n-octanol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210507 |