CN103869016A - Method for detecting PBDEs (Poly Brominated Diphenyl Ethers) in plastic components of electronic components and devices - Google Patents
Method for detecting PBDEs (Poly Brominated Diphenyl Ethers) in plastic components of electronic components and devices Download PDFInfo
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Abstract
The invention relates to a method for detecting PBDEs (Poly Brominated Diphenyl Ethers) in plastic components of electronic components and devices. The method comprises the following steps: (a) processing a sample into granules, of which the mass of each is not greater than 0.2g; (b) putting the sample processed in the step (a) into toluene, and carrying out ultrasonic extraction, wherein the ratio of sample to toluene is 1g: (5-20)g/ml; (c) after the extraction is completed, filtrating, and then fixing volume with toluene, wherein the volume-fixed volume is equal to that of toluene used during extraction; (d) carrying out GC-MS (Gas Chromatography-Mass Spectrometry) analysis on a volume-fixed solution obtained in the step (c), and setting specific chromatographic conditions. The method provided by the invention has good accuracy, repeatability and reproducibility.
Description
Technical field
The present invention relates to the detection method of a kind of PBDEs, relate in particular to the detection method of PBDEs in a kind of electronic devices and components plastic components.
Background technology
PBDE (Poly Brominated Diphenyl Ethers is called for short PBDEs), has 209 kinds of homologs such as tetrabromo Biphenyl Ether, pentabromo-, hexabromo, eight bromines, ten bromines.Its commodity PBDE is one group of Biphenyl Ether potpourri that bromine atoms number is different, is therefore generically and collectively referred to as PBDE.Due to its excellent fire resistance, the maximum purposes of PBDE is as fire retardant, adds in compound substance and goes, to improve the fire protecting performance of product in manufacture course of products.Because PBDE can discharge free radical under the condition of high temperature, blocking-up combustion reaction, very wide in usable range, as for products such as various electronic apparatuss and automatic control equipment, building materials, textile, furniture.
But along with constantly report detecting of PBDEs in environmental sample, the environmental problem that this compounds causes also more and more receives everybody the particularly concern of environmental science.PBDEs gets off and can cause hypothyroidism for a long time, affects fetus IQ and growth, and children have learning and Memory obstacle, in addition, also can destroy women's ovary, reduces male reproductive function, even carcinogenic.PBDEs is the global organic contaminant extensively existing in a class environment.Because it has environmental persistence, long-distance transmissions, biology can cumulative bad and biological and human body is had to the characteristics such as toxic effect, the research of its environmental problem has been become to a large focus of current environment science.In May, 2009, in " Convention of Stockholm " formally listed tetrabromo Biphenyl Ether and pentabromo-Biphenyl Ether, hexabromobiphenyl ether and seven bromo biphenyl ethers by United Nations Environment Programme (UNEP).
At present, the detection method of PBDEs is mainly gas chromatograph-mass spectrometer (GC/MS), CN101526508A discloses in a kind of sample the method for quick of polybrominated diphenyl ether residue in textile especially, it is characterized in that said method comprising the steps of: (1), by after sample pulverizing, end immersion stain and the ultrasonic assisted extraction of water-bath, adopts solid-phase microextraction enrichment target compound; (2) after thermal desorption, measure PBDE with gas chromatography combined with mass spectrometry qualitative, quantitative.Also has the detection method to PBDEs in aquatic products.And the detection method of the PBDEs in plastics is need to further exploitation.And at present in these detection methods the pre-treatment of sample more complicated.
Summary of the invention
The object of the present invention is to provide the detection method of PBDEs in a kind of electronic devices and components plastic components.Whether method of the present invention is by selecting suitable solvent by the extraction of sample ultrasonic ripple, makes PBDEs class extracting substances wherein to solution, then carry out in analytic sample containing PBDEs and content thereof with GC-MS.Method of the present invention is easy, and shows through large quantity research, and method accuracy of the present invention is high, repeatability and repeatability excellence.
For reaching above-mentioned purpose, the present invention by the following technical solutions:
In electronic devices and components plastic components, a detection method of PBDEs, comprises the steps:
(a) sample preparation being become to every tablet quality≤0.2g, for example, is the particle of 0.05g, 0.12g, 0.14g, 0.18g etc.;
(b) step (a) sample after treatment is put into toluene and carry out ultrasonic extraction; The ratio of sample and toluene is 1:5-20g/mL, for example, be 1:7g/mL, 1:11g/mL, 1:14g/mL, 1:18g/mL etc.;
(c) after having extracted, filter, then use toluene constant volume; Volume after described constant volume with when extraction volume of toluene used identical;
(d) solution after step (c) constant volume is carried out to GC-M S analysis;
Wherein the chromatographic column of GC-MS is low pole, for example, be OV-5, DB-5, SE-54, HP-5, RTX-5, BP-5, DB-5MS etc.; When GC-MS analyzes, the temperature programmed control of GC part is set to: initial temperature 90-110 DEG C, and be for example 93 DEG C, 96 DEG C, 105 DEG C etc. and keep 0.5-2min, be for example 0.7min, 1.6min etc.; With 15-25 DEG C/min, be for example that 17 DEG C/min, 21 DEG C/min, 24 DEG C/min etc. rise to 320-340 DEG C, be for example 323 DEG C, 328 DEG C, 335 DEG C etc., more than keeping 4min, for example, be 7min, 15min etc.
Carrying out before GC-MS quantitative test, first use GC-MS to carry out qualitative analysis to sample, determine whether the PBDEs that contains PBDEs and contain which type, the type of the PBDEs then containing in is per sample prepared corresponding standard solution and is carried out quantitative test.
The present invention by a large amount of determined use ultrasonic extraction then carry out that GC-MS analyzes can be accurate, obtain reliably the content of the PBDEs in electronic devices and components, wherein choosing of ultrasonic extraction solvent has important impact to the extraction completely of PBDEs, can better PBDEs be extracted from product, solvent selects and accuracy to analysis result of the setting of chromatographic condition and repeatability, repeatability have material impact.
As optimization technique method, detection method of the present invention, the ratio of described sample and toluene is 1:10g/mL.
As optimization technique method, detection method of the present invention, the condition of described ultrasonic extraction is: be 50-80 DEG C in temperature, be for example under 52 DEG C, 56 DEG C, 59 DEG C, 65 DEG C, 72 DEG C, 79 DEG C etc., more than vibration 60min, for example, be 66min, 72min, 80min, 85min, 95min etc.
Preferably, be at 70 DEG C in temperature, vibration 90min.
As optimization technique method, detection method of the present invention, the chromatographic column of GC-MS is DB-5MS, and length is 15m, and internal diameter is 0.25mm, and thickness is 0.1 μ m.
Preferably, carrier gas is helium, and flow is 1.8-2.2mL/min, for example, be 1.9mL/min, 2.1mL/min etc., is preferably 2mL/min, adopts split sampling, and injection temperature is 310-330 DEG C, for example, be 315 DEG C, 323 DEG C, 328 DEG C etc., is preferably 320 DEG C.
As optimization technique method, detection method of the present invention, when GC-MS analyzes, the temperature programmed control of GC part is set to: 100.0 DEG C of maintenance 1.00min of initial temperature; Rise to 330 DEG C with 20.0 DEG C/min, keep 5.00min.
As optimization technique method, detection method of the present invention, when GC-MS analyzes, the condition setting of MS part is: interface temperature 310-330 DEG C, it is for example 314 DEG C, 320 DEG C, 328 DEG C etc., source temperature 240-260 DEG C, for example, be 244 DEG C, 251 DEG C etc., sweep limit 50 to 1200amu; Be preferably 320 DEG C of interface temperature, 250 DEG C of source temperature, sweep limit 50 is to 1200amu.
The testing conditions that the present invention sets can make detection material separate, and makes quantitative result more accurate.
As optimization technique method, detection method of the present invention, comprises the steps:
(a) sample preparation is become to the particle of every tablet quality≤0.2g;
(b) step (a) sample after treatment is put into toluene and carry out ultrasonic extraction; The ratio of sample and toluene is 1:5-20g/mL; The condition of described ultrasonic extraction is: be at 50-80 DEG C in temperature, more than vibration 60min;
(c) after having extracted, filter, then use toluene constant volume; Volume after described constant volume with when extraction volume of toluene used identical;
(d) solution after step (c) constant volume is carried out to GC-MS analysis; The chromatographic column of GC-MS is low pole; Carrier gas when GC-MS analyzes is helium, and flow is 1.8-2.2mL/min, adopts split sampling, and injection temperature is 310-330 DEG C; The temperature programmed control of GC part is set to: initial temperature 90-110 DEG C keeps 0.5-2min; Rise to 320-340 DEG C with 15-25 DEG C/min, more than keeping 4min; The condition setting of MS part is: interface temperature 310-330 DEG C, and source temperature 240-260 DEG C, sweep limit 50 is to 1200amu.
As optimization technique method, detection method of the present invention, comprises the steps:
(a) sample preparation is become to the particle of every tablet quality≤0.1g;
(b) step (a) sample after treatment is put into toluene and carry out ultrasonic extraction; The ratio of sample and toluene is 1:10g/mL; The condition of described ultrasonic extraction is: be at 70 DEG C in temperature, and vibration 90min;
(c) after having extracted, filter, then use toluene constant volume; Volume after described constant volume with when extraction volume of toluene used identical;
(d) solution after step (c) constant volume is carried out to GC-MS analysis; The chromatographic column of GC-MS is DB-5MS, and length is 15m, and internal diameter is 0.25mm, and thickness is 0.1 μ m; Carrier gas when GC-MS analyzes is helium, and flow is 2mL/min, adopts split sampling, and injection temperature is 320 DEG C; The temperature programmed control of GC part is set to: 100.0 DEG C of maintenance 1.00min of initial temperature; Rise to 330 DEG C with 20.0 DEG C/min, keep 5.00min; The condition setting of MS part is: 320 DEG C of interface temperature, and 250 DEG C of source temperature, sweep limit 50 is to 1200amu.
Detection method of the present invention is easy, and accuracy is high, repeatability and repeatability good.
The present invention is described in more detail below.But following example is only simple and easy example of the present invention, does not represent or limit the scope of the present invention, and protection scope of the present invention is as the criterion with claims.
Embodiment
For the present invention is described better, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows.
Instrument and equipment in embodiment:
10ml volumetric flask (A level), GC-MS analyzes with bottle (2ml), transfer pipet (1ml), safe rubber pipette bulb, electronic balance (degree of accuracy 0.01mg), ultrasonic oscillator;
Gas chromatography mass spectrometer GC/MS, chromatographic column: Column (DB-5MS) length 15m, internal diameter 0.25mm, thickness 0.1 μ m, resistance to extreme temperature: 400 DEG C.
Agents useful for same in embodiment:
Toluene, C
6h
5cH
3, M.W=92 (HPLC);
Standard items STD is as (be dissolved in isooctane)
Nine bromo biphenyl ethers: NonaBromoBiphenyl Ether, C
12hBr
9o, 50ppm
Octa-BDE: OctaBromoBiphenyl Ether, C
12h
2br
8o, 50ppm
Taking nine bromo biphenyl ethers as example, preparation series concentration.By the nine bromo biphenyl ether standard items called after A of 50ppm, make solvent with isooctane, prepare with 1ml volumetric flask.Dilute according to following table 1 again:
Table 1
With A, A1, A2, A3, five concentration point of A4 are done the working curve of nine bromo biphenyl ethers, and the linearity of working curve requires more than 0.95.If the working curve of preparation is less than 0.95, remove deflection curve larger a bit, again recall working curve, observe adjust after linear coefficient whether be greater than 0.95, if linear coefficient is greater than 0.95 use, otherwise, again prepare series concentration.
Embodiment 1
(a) be cut into the particle of every tablet quality≤0.2g size with electronics capacity of balance sample wire strip electronic component plastic components 1.0034g, pour sample into port grinding bottle;
(b) pour in port grinding bottle and carry out ultrasonic extraction with the toluene that graduated cylinder measures 10ml, the condition of ultrasonic extraction is: be at 80 DEG C in temperature, and vibration 60min; After condition sets, after temperature rises, by starting button;
(c), after solution extraction completes, powered-down after naturally cooling, in 10ml volumetric flask, uses toluene constant volume to 10ml scale mark the liquid filtering in port grinding bottle pipe.
(d) pipette this solution of 1ml in vial with 1ml transfer pipet, sealing, upper machine analysis.
GC part condition:
Injection system: shunting (Split), (1) SPL1 is set as 0 at 0.80min; (2) SPL1 is set as 50 at 1.00min; (3) SPL1 is set as 30 at 3.00min; Injection temperature: 320 DEG C; Portable gas: adjusting its flow with He is 2ml/min;
Temperature programmed control: 100.0 DEG C of maintenance 1.00min of initial temperature, be warming up to 330 DEG C with 20.0 DEG C/min, keep 5.00min;
MS part condition: 320 DEG C of interface temperature, 250 DEG C of source temperature, sweep limit: 50 to 1200amu.
The calibration curve being used as, recording PBDEs in solution is that concentration is 2.5mg/L, in sample, PBDEs content is 24.9153mg/kg.Get 10 parts of same samples respectively through shredding, extract post analysis, the content obtaining in final sample is 24.9153mg/kg, 24.9874mg/kg, 24.9961mg/kg, 24.5127mg/kg, 24.8874mg/kg, 24.7899mg/kg, 24.8251mg/kg, 25.0033mg/kg, 25.1047mg/kg, 24.9456mg/kg, the relative standard deviation of ten test results is 0.66%, and the repeatability of visible this method is fine.Carry out repeatability test result by 5 laboratories respectively for same sample as follows: 24.8968mg/g, 24.6579mg/g, 25.2143mg/g, 24.5328mg/g, 25.3147mg/g, the relative standard deviation of the test result of 5 different experiments chambers is 1.36%, visible, method of testing of the present invention has also obtained extraordinary repeatability between different laboratories.The test of carrying out recovery of standard addition records the recovery between 98-102%, and visible detection method of the present invention has higher accuracy.
Embodiment 2
(a) be cut into the particle of every tablet quality≤0.1g size with the plastic components 1.1136g of the block electronic component of electronics capacity of balance sample wire, pour sample into port grinding bottle;
(b) pour in port grinding bottle and carry out ultrasonic extraction with the toluene that graduated cylinder measures 10ml, the condition of ultrasonic extraction is: be at 70 DEG C in temperature, and vibration 90min; After condition sets, after temperature rises, by starting button;
(c), after solution extraction completes, powered-down after naturally cooling, in 10ml volumetric flask, uses toluene constant volume to 10ml scale mark the liquid filtering in port grinding bottle pipe.
(d) pipette this solution of 1ml in vial with 1ml transfer pipet, sealing, upper machine analysis.
GC part condition:
Injection system: shunting (Split), (1) SPL1 is set as 0 at 0.80min; (2) SPL1 is set as 50 at 1.00min; (3) SPL1 is set as 30 at 3.00min; Injection temperature: 330 DEG C; Portable gas: adjusting its flow with He is 1.8ml/min;
Temperature programmed control: 110.0 DEG C of maintenance 1.00min of initial temperature, be warming up to 310 DEG C with 25.0 DEG C/min, keep 5.00min;
MS part condition: 330 DEG C of interface temperature, 260 DEG C of source temperature, sweep limit: 50 to 1200amu.
The calibration curve being used as, recording PBDEs concentration in solution is 5.6mg/L, in sample, PBDEs content is 50.2874mg/g.Get 10 parts of same samples respectively through shredding, extract post analysis, the content obtaining in final sample is 50.2874mg/g, 50.0124mg/g, 50.5053mg/g, 50.4563mg/g, 49.8965mg/g, 50.5533mg/g, 50.4123mg/g, 50.0011mg/g, 50.0568mg/g, 50.5561mg/g, the relative standard deviation of ten test results is 0.51%, and the repeatability of visible this method is fine.Carry out repeatability test result by 5 laboratories respectively for same sample as follows: 50.2738mg/g, 50.6874mg/g, 49.7859mg/g, 50.5263mg/g, 49.5895mg/g, the relative standard deviation of the test result of 5 different experiments chambers is 0.94%, visible, method of testing of the present invention has also obtained extraordinary repeatability between different laboratories.
Applicant's statement, person of ordinary skill in the field is on the basis of above-described embodiment, by the concrete content point value of above-described embodiment component, combined with the technical scheme of summary of the invention part, thereby the new numerical range producing, also be one of record scope of the present invention, the application, for making instructions simple and clear, is no longer enumerated these numerical ranges.
Applicant's statement, the present invention illustrates manufacture craft of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned making step, does not mean that the present invention must rely on above-mentioned making step and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, and the selections of the equivalence replacement to the selected raw material of the present invention and the interpolation of auxiliary element, concrete mode etc., within all dropping on protection scope of the present invention and open scope.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characterictic described in above-mentioned embodiment, in reconcilable situation, can combine by any suitable mode, for fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible array modes.
In addition, also can carry out combination in any between various embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (9)
1. a detection method of PBDEs in electronic devices and components plastic components, comprises the steps:
(a) sample preparation is become to the particle of every tablet quality≤0.2g;
(b) step (a) sample after treatment is put into toluene and carry out ultrasonic extraction; The ratio of sample and toluene is 1:5-20g/mL;
(c) after having extracted, filter, then use toluene constant volume; Volume after described constant volume with when extraction volume of toluene used identical;
(d) solution after step (c) constant volume is carried out to GC-M S analysis;
Wherein the chromatographic column of GC-MS is low pole; When GC-MS analyzes, the temperature programmed control of GC part is set to: initial temperature 90-110 DEG C keeps 0.5-2min; Rise to 320-340 DEG C with 15-25 DEG C/min, more than keeping 4min.
2. detection method as claimed in claim 1, is characterized in that, the ratio of described sample and toluene is 1:10g/mL.
3. detection method as claimed in claim 1, is characterized in that, the condition of described ultrasonic extraction is: be at 50-80 DEG C in temperature, more than vibration 60min;
Preferably, be at 70 DEG C in temperature, vibration 90min.
4. the detection method as described in claim 1-3 any one, is characterized in that, the chromatographic column of GC-MS is DB-5MS, and length is 15m, and internal diameter is 0.25mm, and thickness is 0.1 μ m.
5. the detection method as described in claim 1-4 any one, is characterized in that, when GC-MS analyzes, carrier gas is helium, and flow is 1.8-2.2mL/min, is preferably 2mL/min, adopts split sampling, and injection temperature is 310-330 DEG C, is preferably 320 DEG C.
6. the detection method as described in claim 1-5 any one, is characterized in that, when GC-MS analyzes, the temperature programmed control of GC part is set to: 100.0 DEG C of maintenance 1.00min of initial temperature; Rise to 330 DEG C with 20.0 DEG C/min, keep 5.00min.
7. the detection method as described in claim 1-6 any one, is characterized in that, when GC-MS analyzes, the condition setting of MS part is: interface temperature 310-330 DEG C, and source temperature 240-260 DEG C, sweep limit 50 is to 1200amu; Be preferably 320 DEG C of interface temperature, 250 DEG C of source temperature, sweep limit 50 is to 1200amu.
8. detection method as claimed in claim 1, is characterized in that, comprises the steps:
(a) sample preparation is become to the particle of every tablet quality≤0.2g;
(b) step (a) sample after treatment is put into toluene and carry out ultrasonic extraction; The ratio of sample and toluene is 1:5-20g/mL; The condition of described ultrasonic extraction is: be at 50-80 DEG C in temperature, more than vibration 60min;
(c) after having extracted, filter, then use toluene constant volume; Volume after described constant volume with when extraction volume of toluene used identical;
(d) solution after step (c) constant volume is carried out to GC-MS analysis; The chromatographic column of GC-MS is low pole; Carrier gas when GC-MS analyzes is helium, and flow is 1.8-2.2mL/min, adopts split sampling, and injection temperature is 310-330 DEG C; The temperature programmed control of GC part is set to: initial temperature 90-110 DEG C keeps 0.5-2min; Rise to 320-340 DEG C with 15-25 DEG C/min, more than keeping 4min; The condition setting of MS part is: interface temperature 310-330 DEG C, and source temperature 240-260 DEG C, sweep limit 50 is to 1200amu.
9. detection method as claimed in claim 1, is characterized in that, comprises the steps:
(a) sample preparation is become to the particle of every tablet quality≤0.1g;
(b) step (a) sample after treatment is put into toluene and carry out ultrasonic extraction; The ratio of sample and toluene is 1:10g/mL; The condition of described ultrasonic extraction is: be at 70 DEG C in temperature, and vibration 90min;
(c) after having extracted, filter, then use toluene constant volume; Volume after described constant volume with when extraction volume of toluene used identical;
(d) solution after step (c) constant volume is carried out to GC-MS analysis; The chromatographic column of GC-MS is DB-5MS, and length is 15m, and internal diameter is 0.25mm, and thickness is 0.1 μ m; Carrier gas when GC-MS analyzes is helium, and flow is 2mL/min, adopts split sampling, and injection temperature is 320 DEG C; The temperature programmed control of GC part is set to: 100.0 DEG C of maintenance 1.00min of initial temperature; Rise to 330 DEG C with 20.0 DEG C/min, keep 5.00min; The condition setting of MS part is: 320 DEG C of interface temperature, and 250 DEG C of source temperature, sweep limit 50 is to 1200amu.
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|---|---|---|---|
| CN201410114262.0A CN103869016A (en) | 2014-03-26 | 2014-03-26 | Method for detecting PBDEs (Poly Brominated Diphenyl Ethers) in plastic components of electronic components and devices |
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| CN201410114262.0A CN103869016A (en) | 2014-03-26 | 2014-03-26 | Method for detecting PBDEs (Poly Brominated Diphenyl Ethers) in plastic components of electronic components and devices |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105021745A (en) * | 2014-04-17 | 2015-11-04 | 苏州市产品质量监督检验所 | Purification and enrichment pretreatment technology of food organic pollutants hydroxylated polybrominated diphenyl ethers |
| CN105699526A (en) * | 2016-02-02 | 2016-06-22 | 环境保护部华南环境科学研究所 | Method for detecting contents of brominated flame retardant and phosphorus-based flame retardant in hairs |
-
2014
- 2014-03-26 CN CN201410114262.0A patent/CN103869016A/en active Pending
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105021745A (en) * | 2014-04-17 | 2015-11-04 | 苏州市产品质量监督检验所 | Purification and enrichment pretreatment technology of food organic pollutants hydroxylated polybrominated diphenyl ethers |
| CN105699526A (en) * | 2016-02-02 | 2016-06-22 | 环境保护部华南环境科学研究所 | Method for detecting contents of brominated flame retardant and phosphorus-based flame retardant in hairs |
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