CN105203473B - A kind of detection method of phthalic ester plasticizer - Google Patents
A kind of detection method of phthalic ester plasticizer Download PDFInfo
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Abstract
The invention discloses a kind of detection methods of phthalic ester plasticizer of technical field of chemical detection, first use the phthalic acid ester in the mixed organic solvents of acetone and n-hexane extraction test sample;After being evaporated mixed organic solvents, redissolved with alcohols solvent;Strong base solution is added after redissolution, phthalic acid ester is hydrolyzed into phthalate;The solution after hydrolysis is extracted with dichloromethane again, removes the oil soluble material in aqueous solution, retains aqueous solution;Finally the aqueous solution of reservation is measured with spectrophotometry;The content for obtaining the phthalic acid ester 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 compound content, and detection speed is fast, and without relying on large scale equipment, testing cost is low.This method can be used for the phthalic acid ester content detection of plastics, toy, painting layer, packaging material for food etc..
Description
Technical field
The present invention relates to a kind of detection methods of phthalic ester plasticizer, belong to technical field of chemical detection.It is suitable
Include but not limited to plastics, toy, painting layer, packaging material for food etc. with range.
Background technology
Phthalic acid ester(PAEs)It is most common a kind of plasticizer.Phthalic ester plasticizer is commonly used
In toy, packaging material for food, medical blood bag and sebific duct, vinyl flooring and wallpaper, detergent, lubricating oil, personal-care supplies
Etc. in hundreds of products.Phthalate substance may interfere with organism endocrine system, have estrogenic effect and anti-hero
Sex hormone function.Countries in the world are increasingly paid close attention to by phthalic acid ester.Exceeded phthalic acid ester is also Abroad in Recent Years pair
The main reason for China's export product notification is recalled.
There are many phthalic acid ester 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- ethylhexyls)Ester(DEHP), n-butyl phthalate(DBP), O-phthalic acid butyl benzyl
Ester(BBP), diisononyl phthalate(DINP), diisooctyl phthalate(DIDP )And phthalic acid two is just pungent
Ester(DNOP).Many countries such as American-European and China all provide that with articles for children, DEHP, DBP, BBP concentration must not surpass toy
Cross 0.1wt%, it 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 must not exceed 0.1wt%.OEKO-TEX Standard 100 then limit 11 kinds of phthalic acid esters in textile.Europe
Requirement of the alliance to product is gone on along in the forefront in the world, REAC H regulations《Registration, assessment, mandate and the limitation of chemicals》
In, height concern substance(SVHC)In inventory, the type of the phthalic acid ester of limitation is increasing always.Phthalic acid ester also may be used
It can be present in food, such as " the plasticizing event agent " that 5 months 2011 bottom TaiWan, Chinas occur, the Ministry of Public Health was June 1 in 2011
Evening day promptly issues bulletin, by plasticiser phthalate substance, is included in the non-edible object of possible illegal addition in food
Matter and the food additives list easily abused.
The examination criteria and document for detecting phthalic ester plasticizer mostly use greatly GC, GC-MS, HPLC, LC-MS etc.
Method is required for using large-scale instrument, generally although these chromatographies and mass spectrometry method have the advantages that rigorous, accurate, sensitive
The shortcomings of there are detection times long, cumbersome, professional degree is high.In the prior art, lack highly practical easy quick inspection
Survey method.
Invention content
The object of the present invention is to provide a kind of detection methods of phthalic ester plasticizer, can be quickly and easily
The testing result of phthalate compound content is obtained, detection speed is fast, without relying on large scale equipment, testing cost
It is low.
The object of the present invention is achieved like this:A kind of detection method of phthalic ester plasticizer, including it is as follows
Step:
1)Extraction:Quantitatively weigh test sample broken or after shredding, be put into the acetone of 10 ~ 50 times of test sample weight with
The mixed organic solvents of n-hexane extract, and phthalic acid ester is made to be fully dissolved in mixed organic solvents, and the mixing is organic molten
The volume ratio of acetone and n-hexane is 1 in agent:(1~5);
2)Processing:Mixed organic solvents are evaporated, then are redissolved with alcohols solvent;Strong base solution is added after redissolution by O-phthalic
Acid esters is hydrolyzed into phthalate;The solution after hydrolysis is extracted with dichloromethane again, is then removed in aqueous solution
Oil soluble material retains aqueous solution;The alcohols solvent is one kind in methanol, ethyl alcohol, propyl alcohol or butanol;
3)Detection:The aqueous solution of reservation is measured with spectrophotometry;Use sodium phthalate as mark when measurement
Quasi- solution is compareed, to obtain the content of the phthalic acid ester in test sample.
The present invention extracts phthalic acid ester by the mixed liquor of acetone and n-hexane, can using above-mentioned mixed organic solvents
Ensure that phthalic acid ester can faster, be more thoroughly dissolved in mixed organic solvents, and contributes to subsequent processing;It is evaporated organic
Solvent and the process redissolved with alcohols solvent are to promote hydrolysis yield, after redissolution because alcohols solvent can dissolve each other with strong base solution
Be added strong base solution by phthalic acid ester hydrolysis salifying, then extracted again with organic solvent, organics removal, with lower to
The interference detected afterwards.It is finally measured with spectra photometric method, when measurement, using the solution conduct of various concentration sodium phthalate
Standard solution is compareed, because phthalic acid or phthalate have absorption to the light in particular range of wavelengths,
The concentration that hydrolysate can be obtained by control, using calculating, you can obtain the phthalic acid ester in test sample
Content.Standard curve can be made in above-mentioned evaluation, and result is quickly obtained by content and absorbance relationship.With the prior art
It compares, the beneficial effects of the present invention are:This method detection speed is fast, and without relying on large scale equipment, testing cost is low.Its is special
In the detection of phthalic acid ester.This method can be used for the O-phthalic of plastics, toy, painting layer, packaging material for food etc.
Acid and esters content detects.
As a further improvement on the present invention, in step 2)In, the aqueous solution of reservation is acidified with hydrochloric acid, keeps its pH value small
Background interference can be effectively reduced after 3, acidification.
As a further improvement on the present invention, step 2)In by nitrogen drying or rotary evaporation be evaporated mixing it is organic molten
Agent.
To be further reduced the dissolving of other organic matters, step 2)In, it is hydrolyzed into phthalic acid in phthalic acid ester
After salt, then the salting liquid of high concentration is added into solution, the salting liquid of the high concentration is 20% or more mass concentration under room temperature
One kind in NaCl, KCl, LiCl solution reaching as high as the saturated concentration under room temperature.
To ensure that hydrolysis is thorough, step 2)The highly basic of addition is one kind in NaOH, KOH, LiOH solution.
Description of the drawings
Fig. 1 is abosrption spectrogram of the test sample of the present invention after processing and background correction.
Fig. 2 is the correspondence figure of absorbance and phthalic acid salinity.
Specific implementation mode
Embodiment 1
A kind of phthalic ester plasticizer in plastic toys sample is detected, detection method is by following step
It is rapid to carry out:
1)Extraction:Plastic toys sample is crushed, makes its grain size in 2mm hereinafter, weighing 0.1 gram of plastic toys sample
As test sample, be put into the mixed organic solvents of 50 times of test sample weight, about 5ml acetone and n-hexane, after mixing
Stood overnight at 40 DEG C, phthalic acid ester made to be fully dissolved in mixed organic solvents, in mixed organic solvents acetone with just oneself
The volume ratio of alkane is 3:7;It in extraction process, can slightly be heated or not heated, can constantly shake;
2)Processing:Mixed organic solvents are evaporated using nitrogen drying mode, the solid after drying is redissolved with normal propyl alcohol;It is multiple
2 mL LiOH solution are added after molten, phthalic acid ester is hydrolyzed into phthalate;Then it is added under room temperature into solution
The LiCl salting liquid 0.5ml of saturated concentration, then the solution after hydrolysis is extracted with dichloromethane 2ml, it removes in aqueous solution
Oil soluble material, retain aqueous solution;The aqueous solution of reservation is acidified with hydrochloric acid, its pH value is made to be less than 3;
3)Detection:The aqueous solution of reservation is measured with spectrophotometry;Use sodium phthalate as mark when measurement
Quasi- solution is compareed, to calculate the content for obtaining the phthalic acid ester in test sample;When measurement, solution to be measured is moved into
In 1cm cuvettes, 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, absorbance value 0.223, with the suction
Shading value is as quantitative basis;Four phthalic acid sodium standard solutions(0、0.05、0.1、0.2 mM)Extinction at 275nm
Angle value is respectively 0.003,0.067,0.130,0.270, makees standard curve, obtains pair of absorbance and phthalic acid salinity
Answer relational graph(As shown in Figure 2);It is looked for a little on approximate straight line in figure, obtains after sample treatment phthalate in solution
Content is 0.17 mM, and the phthalic ester plasticizer content being converted into test sample is about 0.3 %.
Embodiment 2
Phthalic acid ester in PVC plastic sample is detected, detection method carries out as follows:
1)Extraction:Weigh 0.1 gram of test sample broken or after shredding, be put into the acetone of 20 times of test sample weight with just
In the mixed organic solvents of hexane, at normal temperatures through being mixed, and 48 hours is stood, so that phthalic acid ester is fully dissolved in mixed
It closes in organic solvent, the volume ratio of acetone and n-hexane is 1 in the mixed organic solvents: 3;
2)Processing:Rotary evaporation mode is evaporated mixed organic solvents, then is redissolved with alcohol solvent;It is strong that NaOH is added after redissolution
Phthalic acid ester is hydrolyzed into phthalate by aqueous slkali;The solution after hydrolysis is extracted with dichloromethane again, so
The oil soluble material in aqueous solution is removed afterwards, retains aqueous solution;Hydrochloric acid is added to be acidified the aqueous solution of reservation with hydrochloric acid;
3)Detection:The aqueous solution of reservation is measured with spectrophotometry;Use sodium phthalate as mark when measurement
Quasi- solution is compareed, to calculate the content for obtaining the phthalic acid ester in test sample.
Embodiment 3
Phthalic acid ester in toy cloth sample is detected, detection method carries out as follows:
1)Extraction:Shred toy cloth, take 0.2 gram of test sample, be put into the acetone of 40 times of test sample weight with just
In the mixed organic solvents of hexane, is vibrated 1 hour at 40 DEG C, phthalic acid ester is made to be fully dissolved in mixed organic solvents,
The volume ratio of acetone and n-hexane is 1 in the mixed organic solvents:1;
2)Processing:Mixed organic solvents are evaporated, then are redissolved with propanol solvent;KOH strong base solutions are added after redissolution by adjacent benzene
Dicarboxylic acid esters are hydrolyzed into phthalate;The salting liquid of high concentration is added into solution, the salting liquid of the high concentration is room temperature
One kind in NaCl, KCl, LiCl solution of 20% or more lower mass concentration, reaches as high as the saturated concentration under room temperature.Again with two
Chloromethanes extracts the solution after hydrolysis, then removes the oil soluble material in aqueous solution, retains aqueous solution;
3)Detection:The aqueous solution of reservation is measured with spectrophotometry;Use sodium phthalate as mark when measurement
Quasi- solution is compareed, to calculate the content for obtaining the phthalic acid ester in test sample.
Embodiment 4
Phthalic acid ester in food package box painting layer sample is detected, detection method is as follows
It carries out:
1)Extraction:Lacquer coat sample is scraped, test sample 0.15g is quantitatively weighed after smashing to pieces, is put into test sample weight 50
In the mixed organic solvents of acetone again and n-hexane, at normal temperatures through being mixed, and 10 hours is stood, make phthalic acid
Ester is fully dissolved in mixed organic solvents, and the volume ratio of acetone and n-hexane is 1 in the mixed organic solvents:5;
2)Processing:Mixed organic solvents are evaporated, then are redissolved with butanol solvent;LiOH strong base solutions are added after redissolution by adjacent benzene
Dicarboxylic acid esters are hydrolyzed into phthalate;The solution after hydrolysis is extracted with dichloromethane again, then removes aqueous solution
In oil soluble material, retain aqueous solution;
3)Detection:The aqueous solution of reservation is measured with spectrophotometry;Use sodium phthalate as mark when measurement
Quasi- solution is compareed, and the content for obtaining the phthalic acid ester in test sample is computed.
The invention is not limited in above-described 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 performing creative labour
A little to replace and deform, these are replaced and deformation is within the scope of the invention.
Claims (5)
1. a kind of detection method of phthalic ester plasticizer, it is characterised in that include the following steps:
1)Extraction:Broken test sample is quantitatively weighed, the acetone of 10 ~ 50 times of test sample weight and mixing for n-hexane are put into
Close organic solvent extraction, so that phthalic acid ester is fully dissolved in mixed organic solvents, in the mixed organic solvents acetone with
The volume ratio of n-hexane is 1:(1~5);
2)Processing:Mixed organic solvents are evaporated, then are redissolved with alcohols solvent;Strong base solution is added after redissolution by phthalic acid ester
It is hydrolyzed into phthalate;The solution after hydrolysis is extracted with dichloromethane again, the oil then removed in aqueous solution is molten
Property substance, retain aqueous solution;The alcohols solvent is one kind in methanol, ethyl alcohol, propyl alcohol or butanol;
3)Detection:The aqueous solution of reservation is measured with spectrophotometry;Use sodium phthalate molten as standard when measurement
Liquid is compareed, to obtain the content of the phthalic acid ester in test sample.
2. a kind of detection method of phthalic ester plasticizer according to claim 1, it is characterised in that step 2)
In, the aqueous solution of reservation is acidified with hydrochloric acid, so that its pH value is less than 3, to reduce background interference.
3. a kind of detection method of phthalic ester plasticizer according to claim 1, it is characterised in that step 2)
In, mixed organic solvents are evaporated by nitrogen drying or rotary evaporation.
4. a kind of detection method of phthalic ester plasticizer according to claim 1, it is characterised in that step 2)
In, after phthalic acid ester is hydrolyzed into phthalate, then into solution be added high concentration salting liquid, the high concentration
Salting liquid be room temperature under 20% or more mass concentration NaCl, KCl, LiCl solution in one kind.
5. according to a kind of detection method of phthalic ester plasticizer of claim 1-4 any one of them, feature exists
In step 2)The highly basic of addition is one kind in NaOH, KOH, LiOH solution.
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WO2024104886A1 (en) * | 2022-11-18 | 2024-05-23 | IFP Energies Nouvelles | Method for extraction and transformation by hydrolysis of phthalates contained in pvc plastics |
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