CN110132863A - A kind of detection method of phthalate - Google Patents
A kind of detection method of phthalate Download PDFInfo
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- CN110132863A CN110132863A CN201810105650.0A CN201810105650A CN110132863A CN 110132863 A CN110132863 A CN 110132863A CN 201810105650 A CN201810105650 A CN 201810105650A CN 110132863 A CN110132863 A CN 110132863A
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- phthalate
- aqueous solution
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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Abstract
The invention discloses a kind of detection methods of phthalate of technical field of chemical detection, and the mixed organic solvents of acetone and n-hexane is first used to extract the phthalate in test sample;After being evaporated mixed organic solvents, redissolved with alcohols solvent;Solution is extracted with methylene chloride again, removes the oil soluble material in aqueous solution, retains aqueous solution;Finally it is measured with aqueous solution of the spectrophotometry to reservation;The content for obtaining the phthalate in test sample is calculated with the content of phthalic acid sodium standard solution and absorbance value relationship.This method can quickly and easily obtain the testing result of phthalate kind compound content, and detection speed is fast, and testing cost is low.This method can be used for the phthalate content detection of stationery, plastics, toy etc..
Description
Technical field
Invention is related to a kind of detection method of phthalate, belongs to technical field of chemical detection.The scope of application includes
But be not limited to stationery, plastics, toy etc..
Background technique
Phthalate (PAEs) is most common a kind of plasticizer.A kind of detection method of phthalate is general
All over applied to toy, packaging material for food, medical blood bag and sebific duct, vinyl flooring and wallpaper, detergent, lubricating oil, personal shield
It manages in hundreds of products such as articles.Phthalic acid salts substances may interfere with organism endocrine system, have estrogenic effect
It is acted on antiandrogen.Countries in the world are increasingly paid close attention to by phthalate.
There are many phthalate type, and in the toy and articles for children of various countries, mainly having for being limited extensively is as follows
Six kinds: phthalic acid (2- ethylhexyl) ester (DEHP), n-butyl phthalate (DBP), O-phthalic acid butyl benzyl
Ester (BBP), diisononyl phthalate (DINP), diisooctyl phthalate (DIDP) and di-n-octyl phthalate
(DNOP).Many countries such as American-European and China all provide that in toy and articles for children, DEHP, DBP, BBP concentration be must not exceed
0.1wt% is that 3 years old or less children use and can be placed into the toy and articles for children in mouth, DINP, DIDP, DNOP concentration
It must not exceed 0.1wt%.OEKO-TEX Standard 100 then limits 11 kinds of phthalates in textile.European Union
Requirement to product is gone on along in the forefront in the world, REACH regulation " registration, assessment, authorization and the limitation of chemicals ", high
In degree concern substance (SVHC) inventory, the type of the phthalate of limitation is increasing always.
The examination criteria and document for detecting a kind of detection method of phthalate mostly use greatly GC, GC-MS,
The methods of HPLC, LC-MS require to use although these chromatographies and mass spectrometry method have the advantages that rigorous, accurate, sensitive
The disadvantages of large-scale instrument, long, cumbersome, the professional degree of generally existing detection time is high.In the prior art, lack practical
Easy rapid detection method.
Summary of the invention
The object of the present invention is to provide a kind of detection methods of phthalate, can quickly and easily obtain adjacent benzene
The testing result of diformate compounds content, detection speed is fast, and testing cost is low.
The object of the present invention is achieved like this: a kind of detection method of phthalate, including as follows
Step:
1) extract: by sample treatment at the particle for being not more than 5mm*5mm, be put into 1050 times of test sample weight of acetone with just oneself
The mixed organic solvents of alkane extract, and are fully dissolved in phthalate in mixed organic solvents, in the mixed organic solvents
The volume ratio of acetone and n-hexane is 1:(1-5);
2) it extracts: being evaporated mixed organic solvents, be put into alcohol organic solvent and dissolve, add distilled water mixing；With dichloromethane
Alkane extracts above-mentioned solution, then removes the oil soluble material in aqueous solution, retains aqueous solution;The alcohols solvent is first
One of alcohol, ethyl alcohol, propyl alcohol or butanol;
3) it detects: being measured with aqueous solution of the spectrophotometry to reservation;Use sodium phthalate molten as standard when measurement
Liquid is compareed, to obtain the content of the phthalate in test sample.
The present invention extracts phthalate by the mixed liquor of acetone and n-hexane, can using above-mentioned mixed organic solvents
Guarantee that phthalate can faster, be more thoroughly dissolved in mixed organic solvents, and facilitates subsequent processing;It is evaporated organic
Solvent is simultaneously redissolved with alcohols solvent, is then extracted again with organic solvent, and organic matter is removed, to lower the interference to then detecting.
It is finally measured with spectra photometric method, when measurement, is carried out using the solution of various concentration sodium phthalate as standard solution
Control, because phthalate has absorption to the light in particular range of wavelengths, by compareing available hydrolysate
Concentration the content of the phthalate in test sample can be obtained using calculating.Above-mentioned evaluation can be made
Standard curve quickly obtains result by content and absorbance relationship.Compared with prior art, beneficial effects of the present invention exist
In: this method detection speed is fast, and without relying on large scale equipment, testing cost is low.Its detection for being exclusively used in phthalate.It should
Method can be used for the phthalate content detection of stationery, plastics, toy etc..
As a further improvement of the present invention, in step 2), the aqueous solution of reservation is acidified with hydrochloric acid, keeps its pH value small
It can effectively reduce background interference after 3, acidification.
As a further improvement of the present invention, in step 2) by be dried with nitrogen or rotary evaporation be evaporated mixing it is organic molten
Agent.
For the dissolution for being further reduced other organic matters, in step 2), the salting liquid of high concentration is added into solution, it is described
The salting liquid of high concentration is the NaCl of 20% or more mass concentration under room temperature, KCl, and one of LiCl solution reaches as high as room temperature
Under saturated concentration.
Detailed description of the invention
Fig. 1 is the abosrption spectrogram of test sample of the invention after processing and background correction.
Fig. 2 is the corresponding relationship of absorbance and phthalic acid salinity.
Specific embodiment
Embodiment 1
A kind of detection method of one of plastic toys sample phthalate is detected, detection method is by as follows
Step carries out:
1) it extracts: plastic toys sample being crushed, makes its partial size in 5mm hereinafter, weighing 0. 1 grams of plastic toys sample works
For test sample, it is put into the mixed organic solvents of 50 times of test sample weight, about 5ml acetone and n-hexane, 40 after mixing
It is stood overnight at DEG C, is fully dissolved in phthalate in mixed organic solvents, acetone and n-hexane in mixed organic solvents
Volume ratio be 3:7;It in extraction process, can slightly be heated or not heated, can constantly shake;
2) it extracts: being evaporated mixed organic solvents using mode is dried with nitrogen, the solid after drying is redissolved with normal propyl alcohol;Then to
0. 5ml of LiCl salting liquid of saturated concentration under room temperature is added in solution, then the solution after hydrolysis is carried out with methylene chloride 2ml
Extraction removes the oil soluble material in aqueous solution, retains aqueous solution;The aqueous solution of reservation is acidified with hydrochloric acid, keeps its pH value small
In 3;
3) it detects: being measured with aqueous solution of the spectrophotometry to reservation;Use sodium phthalate molten as standard when measurement
Liquid is compareed, to calculate the content for obtaining the phthalate in test sample;When measurement, solution to be measured is moved into 1cm
In cuvette, its absorbance value is scanned within the scope of 220 ~ 400nm, using the absorbance value at 275nm as quantitative basis.
In Fig. 1, A is absorbance, and the absorbance value at 275nm is an acromion, and absorbance value is 0. 223, with the suction
Shading value is as quantitative basis;Extinction of four phthalic acid sodium standard solutions (0,0.05,0.1,0.2mM) at 275nm
Angle value is respectively 0. 003,0. 067,0. 130,0. 270, makees standard curve, obtains absorbance and phthalate
The corresponding relationship (as shown in Figure 2) of concentration;It is looked for a little on approximate straight line in figure, obtains after sample treatment adjacent benzene in solution
Diformate content is 0. 17 mM, and the detection method content for being converted into one of test sample phthalate is about 0.
3%。
Embodiment 2
Phthalate in PVC plastic sample is detected, detection method carries out as follows:
1) extract: weigh it is broken or 0. 1 grams of test sample after shredding, be put into 20 times of test sample weight of acetone with just oneself
In the mixed organic solvents of alkane, at normal temperature through being mixed, and 48 hours is stood, phthalate is made to be fully dissolved in mixing
In organic solvent, the volume ratio of acetone and n-hexane is 1:3 in the mixed organic solvents;
2) extract: rotary evaporation mode is evaporated mixed organic solvents, then is redissolved with alcohol solvent;Again with methylene chloride to hydrolysis
Solution afterwards is extracted, and is then removed the oil soluble material in aqueous solution, is retained aqueous solution;Hydrochloric acid is added to the water-soluble of reservation
Liquid is acidified with hydrochloric acid;
3) it detects: being measured with aqueous solution of the spectrophotometry to reservation;Use sodium phthalate molten as standard when measurement
Liquid is compareed, to calculate the content for obtaining the phthalate in test sample.
Embodiment 3
Phthalate in toy cloth sample is detected, detection method carries out as follows:
1) extract: shredding toy cloth, take 0. 2 grams of test sample, be put into 40 times of test sample weight of acetone with just oneself
In the mixed organic solvents of alkane, is vibrated 1 hour at 40 DEG C, be fully dissolved in phthalate in mixed organic solvents, institute
Stating the volume ratio of acetone and n-hexane in mixed organic solvents is 1:1;
2) it extracts: being evaporated mixed organic solvents, then redissolved with propanol solvent;The salting liquid of high concentration, the height are added into solution
The salting liquid of concentration is the NaCl of 20% or more mass concentration under room temperature, KCl, and one of LiCl solution reaches as high as room temperature
Under saturated concentration.The solution after hydrolysis is extracted with methylene chloride again, then removes the oil soluble material in aqueous solution,
Retain aqueous solution;
3) it detects: being measured with aqueous solution of the spectrophotometry to reservation;Use sodium phthalate molten as standard when measurement
Liquid is compareed, to calculate the content for obtaining the phthalate in test sample.
Embodiment 4
Phthalate in food package box painting layer sample is detected, detection method as follows into
Row:
1) it extracts: scraping lacquer coat sample, 0. 15g of test sample is quantitatively weighed after smashing to pieces, be put into 50 times of test sample weight
In the mixed organic solvents of acetone and n-hexane, at normal temperature through being mixed, and 10 hours is stood, fill phthalate
Divide and dissolve in mixed organic solvents, the volume ratio of acetone and n-hexane is 1:5 in the mixed organic solvents;
2) it extracts: being evaporated mixed organic solvents, then redissolved with butanol solvent;The solution after hydrolysis is carried out with methylene chloride again
Then extraction removes the oil soluble material in aqueous solution, retains aqueous solution;
3) it detects: being measured with aqueous solution of the spectrophotometry to reservation;Use sodium phthalate molten as standard when measurement
Liquid is compareed, and the content for obtaining the phthalate in test sample is computed.
The present invention is not limited to the above embodiments, on the basis of technical solution disclosed by the invention, the skill of this field
For art personnel according to disclosed technology contents, one can be made to some of which technical characteristic by not needing creative labor
A little replacements and deformation, these replacements and deformation are within the scope of the invention.
Claims (4)
1. a kind of detection method of phthalate, it is characterised in that include the following steps:
1) extract: by sample treatment at the particle for being not more than 5mm*5mm, be put into 1050 times of test sample weight of acetone with just oneself
The mixed organic solvents of alkane extract, and are fully dissolved in phthalate in mixed organic solvents, in the mixed organic solvents
The volume ratio of acetone and n-hexane is 1:(1-5);
2) it extracts: being evaporated mixed organic solvents, be put into alcohol organic solvent and dissolve, add the salting liquid mixing of high concentration；
Above-mentioned solution is extracted with methylene chloride, the oil soluble material in aqueous solution is then removed, retains aqueous solution;
3) it detects: being measured with aqueous solution of the spectrophotometry to reservation;Use sodium phthalate molten as standard when measurement
Liquid is compareed, to obtain the content of the phthalate in test sample.
2. a kind of detection method of phthalate according to claim 1, it is characterised in that in step 2), to reservation
Aqueous solution be acidified with hydrochloric acid, make its pH value less than 3, to reduce background interference.
3. a kind of detection method of phthalate according to claim 1-4, it is characterised in that step 2)
In alcohols solvent be one of methanol, ethyl alcohol, propyl alcohol or butanol.
4. a kind of detection method of phthalate according to claim 1, it is characterised in that in step 2), the height
The salting liquid of concentration is the NaCl of 20% or more mass concentration under room temperature, KCl, one of LiCl solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810105650.0A CN110132863A (en) | 2018-02-02 | 2018-02-02 | A kind of detection method of phthalate |
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| CN201810105650.0A CN110132863A (en) | 2018-02-02 | 2018-02-02 | A kind of detection method of phthalate |
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| CN110132863A true CN110132863A (en) | 2019-08-16 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516586A (en) * | 2011-12-16 | 2012-06-27 | 华南理工大学 | Method for reclaiming phthalate plasticizer from waste plastic products |
| CN105203473A (en) * | 2015-08-28 | 2015-12-30 | 江苏出入境检验检疫局轻工产品与儿童用品检测中心 | Detection method for phthalate ester plasticizer |
-
2018
- 2018-02-02 CN CN201810105650.0A patent/CN110132863A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102516586A (en) * | 2011-12-16 | 2012-06-27 | 华南理工大学 | Method for reclaiming phthalate plasticizer from waste plastic products |
| CN105203473A (en) * | 2015-08-28 | 2015-12-30 | 江苏出入境检验检疫局轻工产品与儿童用品检测中心 | Detection method for phthalate ester plasticizer |
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