CN106596789A - Detection method for phthalic acid ester plasticizer in plastic water supply pipeline - Google Patents
Detection method for phthalic acid ester plasticizer in plastic water supply pipeline Download PDFInfo
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- CN106596789A CN106596789A CN201611217962.8A CN201611217962A CN106596789A CN 106596789 A CN106596789 A CN 106596789A CN 201611217962 A CN201611217962 A CN 201611217962A CN 106596789 A CN106596789 A CN 106596789A
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- water supply
- benzene class
- adjacent benzene
- plastic water
- extraction
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- 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
Abstract
The invention discloses a detection method for a phthalic acid ester plasticizer in a plastic water supply pipeline. Directed at the characteristics for detection of the content of a phthalic acid ester plasticizer in a plastic water supply pipeline, the method includes: firstly conducting shearing, breaking, smashing and grinding for pretreatment, then performing extraction with a n-hexane solvent, conducting filtering and volume setting, and then determining and calculating the content of the phthalic acid ester plasticizer in the plastic water supply pipeline. By means of stirring extraction, microwave extraction and other means, the method provided by the invention effectively reduces the difficulty of Soxhlet extraction mentioned in the national standard at present, and the extraction process has simple and quick operation steps. The used n-hexane has basically negligible toxicity, thus greatly reducing the poison to detection personnel. And the standard recovery rate is 89%-102%, therefore the detection result is reliable.
Description
Technical field
The invention belongs to adjacent benzene class plasticizer in plastic water supply pipe road detection field, more particularly to a kind of plastic water supply pipe road
Detection method.
Background technology
Phthalic acid ester (PAEs) is plasticizer important in feedwater plastic conduit production process, can effectively improve product
Plasticity, pliability, intensity of product etc..Although PAEs has excellent plasticity, its will to the reproductive system of human body, exempt from
Epidemic disease system, digestive system bring harm, such as infringement male reproductive function, promote female precocious puberty, are likely to result in children's gender wrong
Disorderly, long-term huge uptake also results in hepatocarcinoma.Especially in feedwater with plastic conduit product, once substantial amounts of PAEs is migrated out,
Tremendous influence will be produced to people's health, and to the rare report of PAEs content detection of feedwater plastic conduit,
Therefore the PAEs migration content detection researchs to plastic conduit are very necessary.
Affecting the factor of PAEs migration amounts mainly has soak composition, soak pH value, extraction mode, plastic grain diameter
Size and GC-MS conditions.Gas chromatography-mass spectrum (GC-MS) the detection mode of PAEs has had many documents and standard to have correlation
Report, therefore the main presence situation for investigating variety classes feedwater plastic conduit PAEs contents on market herein, by ultrasound
Ripple extraction, stirring three kinds of extraction modes of extraction and soxhlet extraction method are extracted, and finally by GC-MS qualitative, quantitative is carried out
Analysis.
The content of the invention
Present invention aims to the deficiencies in the prior art, there is provided adjacent benzene class plasticizer in a kind of plastic water supply pipe road
Detection method, can be used for detect plastics feedwater pipeline in dimethyl phthalate (DMP), diethyl phthalate
(DEP), dibutyl phthalate (DBP), phthalic acid two (2- ethyl hexyls) ester (DEHP), dinoctyl phthalate
(DNOP), diisononyl phthalate (DINP).
The purpose of the present invention is achieved through the following technical solutions：Adjacent benzene class plasticizer in a kind of plastic water supply pipe road
Detection method, for adjacent benzene class plasticizer loading detection feature in plastics feedwater pipeline, first according to shredding, crush, crush,
Grinding carries out pretreatment, and then by solvent extraction, constant volume after filtration determines and calculates adjacent benzene class in plastics feedwater pipeline and increases
Modeling agent content.Specifically include following steps：
(1) the plastics feedwater pipeline containing adjacent benzene class plasticizer is taken, is shredded to sample diameter less than 5mm, then passed through
Grinding or pulverized under liquid nitrogen powdering granule under room temperature.
(2) 1 ± 0.2g of precise sample powders are put in 100ml conical flasks；30ml normal hexane is added to enter in bottle, beyond the Great Wall
Bottle stopper is extracted.
(3) conical flask is repeatedly rinsed with normal hexane, collects constant volume after all of filtrate, sampling detection.
(4) adjacent benzene class plasticizer loading in solution is determined using GC-MS, calculates adjacent benzene class plasticising in plastics feedwater pipeline
Agent content.
Further, the extraction mode is stirring extraction, starts magnetic stirring apparatuss, and continuing will after at the uniform velocity stirring 30min
Constant volume after solution filtration.
Further, the extraction mode is microwave extracting, starts ultrasonic cleaner with 40kHz frequencies and extracts 20min
After filter constant volume.
Further, in the step (3), also including mark-on step：Weak solution is further prepared using normal hexane, it is extremely molten
The ultimate density of adjacent benzene class plasticizer is in linearity correction concentration range present in liquid.
Further, the adjacent benzene class plasticizer is DMP, DEP, DBP, DEHP, DNOP, DINP.
Further, the normal hexane is chromatographically pure rank.
Further, described sample powder needs 25 μm of pore size screen clothes of Jing to sieve.
6 kinds of adjacent benzene class plasticizer qualitative, quantitative ions are shown in Table 1.
The quota ion of the phthalonitrile compound of table 1
| Phthalonitrile compound | Quota ion 1 | Quota ion 2 | Quota ion 3 | Quota ion 4 |
| DMP | 163 | 194 | ||
| DEP | 149 | 177 | ||
| DBP | 149 | 150 | 223 | 205 |
| DEHP | 149 | 279 | 167 | 150 |
| DNOP | 149 | 279 | 150 | |
| DINP | 149 | 293 | 127 |
Using quantified by external standard method, computing formula is as follows：
Wherein：Target compound content in X-sample, mg/kg；The peak area of A-sample；A1The peak face of-standard solution
Product；B1The concentration of-standard solution；The final constant volume of V-sample；The quality of m-sample.
The beneficial effects of the present invention is：Adjacent presently relevant of benzene class plasticizer in present invention detection plastics feedwater pipeline
It is bright to have no report；By modes such as normal hexane stirring extraction, microwave extracting, the Soxhlet extraction mentioned in current GB is effectively reduced
Difficulty is taken, extraction process operating procedure is simple, quick；The normal hexane toxicity for using is ignored substantially, and it is right to greatly reduce
The murder by poisoning of testing staff；Mark-on reclaims are between 89%-102%, therefore testing result reliability.
Specific embodiment
The present invention is described in further detail with reference to specific embodiment.
Embodiment 1
3 parts of commercially available feedwater plastic conduits are taken respectively, and material is PVC, and per part is detected as follows：
(1) shredded to less than 5mm particle diameters using shears, further grind to form powdered granule；
(2) 1 ± 0.2g of precise sample powders are put in 100ml conical flasks, add 30ml normal hexane to enter in bottle, beyond the Great Wall
Bottle stopper.Ultrasonic cleaner is started to pour solution in 100ml volumetric flasks into after 40kHz frequencies extraction 20min, use normal hexane weight
It is multiple repeatedly to rinse conical flask, collect constant volume after all of filtrate, sampling detection.
(3) adjacent benzene class plasticizer loading in solution is determined using GC-MS, calculates adjacent benzene class plasticizer in plastic conduit and contain
Amount, the results are shown in Table 2.
23 parts of the table commercially available PVC feedwater different neighbour's benzene class plasticizer detection values of plastic conduit
| Phthalonitrile compound | Commercially available 1#, mg/kg | Commercially available 2#, mg/kg | Commercially available 3#, mg/kg |
| DMP | N.D. | N.D. | N.D. |
| DEP | 3.44 | 2.31 | 7.3 |
| DBP | 8.26 | 25.18 | 24.51 |
| DEHP | 39.81 | 7.39 | 12.63 |
| DNOP | N.D. | N.D. | N.D. |
| DINP | 18.34 | 22.15 | 30.81 |
Wherein N.D. is not detect.
Embodiment 2
Commercially available 4# feedwater plastic conduit is taken, material is PE, is detected as follows：
(1) shredded to less than 5mm particle diameters using shears, further grind to form powdered granule；
(2) 1 ± 0.2g of precise sample powders are put in 100ml conical flasks, add 30ml normal hexane to enter in bottle, beyond the Great Wall
Bottle stopper.Magnetic stirring apparatuss are started, is continued at the uniform velocity to stir and is poured solution in 100mL volumetric flasks into after 30min, repeat many with normal hexane
Secondary flushing conical flask, is separately added into variable concentrations neighbour's benzene class list mark, plus scalar is shown in Table 4, table 5, and subsequent constant volume is sampled to be measured；
(3) adjacent benzene class plasticizer loading in solution is determined using GC-MS, calculates adjacent benzene class plasticizer in plastic conduit and contain
Amount, the results are shown in Table 3, table 4.
The recovery of standard addition of 36 kinds of PAEs of table
Wherein N.D. is not detect.
The recovery of standard addition of 46 kinds of PAEs of table
| Sequence number | PAEs | Sample size, mg/kg | Sample mark-on measures content, mg/kg | Standard specimen content, mg/kg | Recovery of standard addition, % |
| 1 | DMP | 8.26 | 13.25 | 5.36 | 93.10 |
| 2 | DEP | 5.44 | 9.89 | 4.97 | 89.54 |
| 3 | DBP | N.D. | 4.85 | 5.20 | 93.27 |
| 4 | DEHP | 24.81 | 29.90 | 5.67 | 89.77 |
| 5 | DNOP | N.D. | 5.02 | 5.04 | 99.60 |
| 6 | DINP | N.D. | 5.29 | 5.18 | 102.12 |
There are several adjacent benzene class plasticizers in feedwater plastic tube commercially available as can be seen from Table 3.By table 3,4 it can be seen that stirring
Mix extraction mode and lose less, recovery of standard addition is more than 89%, illustrate the inventive method to adjacent in plastics feedwater plastic conduit
Benzene class plasticizer treatment effect is preferable, it is ensured that the reliability of measurement result.
Embodiment 3
By Focus DSQII gas chromatograph-mass spectrometer (GC-MS)s, chromatographic column is TG-5MS capillary column (30m × 0.25mm
× 0.25 μm), mixing mark to 6 kinds of adjacent benzene class plasticizers carries out detection limit detection and analysis, the results are shown in Table 5.
The detection limit of the phthalonitrile compound of table 5
| Phthalonitrile compound | DMP | DEP | DBP | DEHP | DNOP | DINP |
| Detection limit, mg/kg | 0.217 | 0.313 | 0.572 | 0.427 | 0.853 | 0.686 |
As can be seen from Table 5, different neighbour's benzene class plasticizer detection limits are all very low, it is adaptable to which plastic conduit plasticizer is used in feedwater
The detection of content.
Claims (6)
1. in a kind of plastic water supply pipe road adjacent benzene class plasticizer detection method, it is characterised in that comprise the following steps：
(1) the plastics feedwater pipeline containing adjacent benzene class plasticizer is taken, is shredded to sample diameter less than 5mm, then by room temperature
Lower grinding or pulverized under liquid nitrogen powdering granule.
(2) 1 ± 0.2g of precise sample powders are put in 100ml conical flasks；30ml normal hexane is added to enter in bottle, beyond the Great Wall bottle stopper
Extraction.
(3) conical flask is repeatedly rinsed with normal hexane, collects constant volume after all of filtrate, sampling detection.
(4) adjacent benzene class plasticizer loading in solution is determined using GC-MS, calculates adjacent benzene class plasticizer in plastics feedwater pipeline and contain
Amount.
2. in a kind of plastic water supply pipe road according to claim 1 adjacent benzene class plasticizer detection method, it is characterised in that
Further, the extraction mode is stirring extraction, starts magnetic stirring apparatuss, continues at the uniform velocity to stir and filters solution after 30min
Constant volume afterwards.
3. in a kind of plastic water supply pipe road according to claim 1 adjacent benzene class plasticizer detection method, it is characterised in that
The extraction mode is microwave extracting, starts ultrasonic cleaner to filter constant volume after 40kHz frequencies extraction 20min.
4. in a kind of plastic water supply pipe road according to claim 1 adjacent benzene class plasticizer detection method, it is characterised in that
In the step (3), also including mark-on step：Weak solution is further prepared using normal hexane, to adjacent benzene class present in solution
The ultimate density of plasticizer is in linearity correction concentration range.
5. in a kind of plastic water supply pipe road according to claim 1 adjacent benzene class plasticizer detection method, it is characterised in that
The normal hexane is chromatographically pure rank.
6. in a kind of plastic water supply pipe road according to claim 1 adjacent benzene class plasticizer detection method, it is characterised in that
Described sample powder needs 25 μm of pore size screen clothes of Jing to sieve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611217962.8A CN106596789A (en) | 2016-12-26 | 2016-12-26 | Detection method for phthalic acid ester plasticizer in plastic water supply pipeline |
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|---|---|---|---|
| CN201611217962.8A CN106596789A (en) | 2016-12-26 | 2016-12-26 | Detection method for phthalic acid ester plasticizer in plastic water supply pipeline |
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| CN201611217962.8A Pending CN106596789A (en) | 2016-12-26 | 2016-12-26 | Detection method for phthalic acid ester plasticizer in plastic water supply pipeline |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113607510A (en) * | 2021-06-22 | 2021-11-05 | 广东华声电器实业有限公司 | Microwave pretreatment method of plastic material special for electronics |
| CN114878762A (en) * | 2022-05-05 | 2022-08-09 | 宁夏回族自治区食品检测研究院 | Detection method, detection system and detection device for accumulation amount of plasticizer in linseed oil |
Citations (3)
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| JPH10249189A (en) * | 1997-03-17 | 1998-09-22 | Toshiba Corp | Absorbent of phthalic ester, housing container of absorbent and analysis of component in the air |
| CN103852535A (en) * | 2014-03-26 | 2014-06-11 | 昆山洛丹伦生物科技有限公司 | Detecting method for phthalate acid in plastic component of electronic element |
| CN105738511A (en) * | 2016-02-19 | 2016-07-06 | 国家再生有色金属橡塑材料质量监督检验中心（安徽） | Method for detecting 1,2-benzenedicarboxylic acid-dialkyl ester plasticizer in plastic through gas chromatography-mass spectrometry |
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2016
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH10249189A (en) * | 1997-03-17 | 1998-09-22 | Toshiba Corp | Absorbent of phthalic ester, housing container of absorbent and analysis of component in the air |
| CN103852535A (en) * | 2014-03-26 | 2014-06-11 | 昆山洛丹伦生物科技有限公司 | Detecting method for phthalate acid in plastic component of electronic element |
| CN105738511A (en) * | 2016-02-19 | 2016-07-06 | 国家再生有色金属橡塑材料质量监督检验中心（安徽） | Method for detecting 1,2-benzenedicarboxylic acid-dialkyl ester plasticizer in plastic through gas chromatography-mass spectrometry |
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| Title |
|---|
| MAIS AL-NATSHEH 等: "Simultaneous GC–MS determination of eight phthalates in total and migrated portions of plasticized polymeric toys and childcare articles", 《JOURNAL OF CHROMATOGRAPHY B》 * |
| 宋继霞 等: "果汁饮料包装材料中邻苯二甲酸酯类塑化剂的同时测定", 《塑料科技》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113607510A (en) * | 2021-06-22 | 2021-11-05 | 广东华声电器实业有限公司 | Microwave pretreatment method of plastic material special for electronics |
| CN114878762A (en) * | 2022-05-05 | 2022-08-09 | 宁夏回族自治区食品检测研究院 | Detection method, detection system and detection device for accumulation amount of plasticizer in linseed oil |
| CN114878762B (en) * | 2022-05-05 | 2024-04-19 | 宁夏回族自治区食品检测研究院 | Method, system and device for detecting plasticizer accumulation amount in sesame oil |
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Application publication date: 20170426 |