CN110470760A - The detection method of polylactic acid content in plastic products - Google Patents
The detection method of polylactic acid content in plastic products Download PDFInfo
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- CN110470760A CN110470760A CN201910756499.1A CN201910756499A CN110470760A CN 110470760 A CN110470760 A CN 110470760A CN 201910756499 A CN201910756499 A CN 201910756499A CN 110470760 A CN110470760 A CN 110470760A
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The invention discloses a kind of detection methods of polylactic acid content in plastic products; the following steps are included: step S1, sample to be tested is taken to be placed in a beaker; lytic agent is added according to sample to be tested and lytic agent mass volume ratio (g/ml) 1:2~1:4; add the chain extender that quality is sample to be tested quality 0.01~0.1%; 110~120 DEG C of 1~2h of oil bath heating, nitrogen protection；Step S2, it is filtered with filter paper, filtrate water is transferred in volumetric flask, with water constant volume；Step S3, after being diluted with water, 0.45 μm of filtering with microporous membrane obtains sample hydrolyzate, and injection ion chromatograph measures polylactic acid content.The method of the present invention using 1- butyl -3- methylimidazole acetate as lytic agent, it is more environmentally protective, while adding a small amount of chain extender as catalyst, it can react with the carboxyl end group of PLA, accelerate polylactic acid course of dissolution, shorten detection time, working efficiency is improved, method is simple and direct, efficient.
Description
Technical field
The present invention relates to a kind of detection methods of polylactic acid content in detection technique field more particularly to plastic products.
Background technique
Polylactic acid (PLA) is a kind of novel biodegradation material, is mentioned using reproducible plant resources (such as corn)
Starch raw material out is made.It, can be degradable by microorganism in nature after use with good biodegradability, most
Free from environmental pollution throughout one's life at carbon dioxide and water, this is highly beneficial to protection environment, is generally acknowledged environment-friendly material.Poly- cream
Sour plastics are to be buried in soil to degrade, and the carbon dioxide of generation is directly entered the soil organism or is absorbed by plants, no
It can be discharged into air, be ideal Green Polymer Material, not will cause greenhouse effects.
Polylactic acid has good mechanical properties and physical property, and compatibility is good with degradability, polylactic acid (PLA) and stone
The basic physical properties for being combined to plastics are similar.Polylactic acid (PLA) has most good tensile strength and extensibility, and polylactic acid can also be with
Various common process modes produce, and polylactic acid (PLA) film has two carbon of good gas permeability, oxygen permeability and saturating dioxy, it
Also there is the characteristic of isolation smell, it is to incinerate tradition that when incinerating polylactic acid (PLA), combustion heat value is identical as stationery is incinerated
The half of plastics (such as polyethylene), and incineration polylactic acid can never release the toxic gases such as nitride, sulfide, human body
Also containing with lactic acid existing for morphon, this has meant that the safety that this decomposability product has.
The polylactic acid characteristic absolutely harmless to human body makes polylactic acid disposable in disposable tableware, packaging material for food etc.
Articles field has unique advantage.It can complete biodegradable also comply with countries in the world, especially European Union, the U.S. and Japan
For the high request of environmental protection.But the disposable tableware processed using polylactic acid raw material is there is not heatproof, oil resistant etc. does not lack
It falls into.Its function discount is resulted in this way to subtract greatly, and tableware deformation, material become fragile in transit, cause a large amount of times
Product.But, develop by technology, city market has by the modified material of PLA at present, the shortcomings that can effectively overcoming raw material,
Some even heat resisting temperatures are up to 120 degree or more, may be used as micro-wave oven apparatus material.Polylactic acid product is widely used in
Disposable product automotive field, electronics, mobile phone component, light CD, biomedicine field etc..
However, to the detection method of polylactic acid, there are no national standards, only Jilin Province's provincial standard (DB22/T at present
2105-2014-2018, the polylactic acid assay chromatography of ions in polylactic acid article), used in dissolution polylactic acid it is molten
Agent is chloroform, is more toxic, and the sodium hydroxide hydrolysis time is also longer.Therefore research is found out more green, more economical, faster
Prompt, more effective detection method can more efficiently, quickly analyze product quality, can be more advantageous to polylactic acid production
Product reduce environmental pollution in the popularization and application in the whole nation, and benefit is in the present age, and function is in an eternal lasting.
Summary of the invention
The object of the present invention is to provide a kind of detection methods of polylactic acid content in plastic products, with green economy, fastly
Prompt effective advantage.
To achieve the goals above, technical solution provided by the invention is as follows:
The detection method of polylactic acid content in plastic products, comprising the following steps:
Step S1, take sample to be tested to be placed in a beaker, according to sample to be tested and lytic agent mass volume ratio (g/ml) 1:2~
Lytic agent is added in 1:4, adds the chain extender that quality is sample to be tested quality 0.01~0.1%, 110~120 DEG C of oil bath heatings 1
~2h, nitrogen protection；
Step S2, it is filtered with filter paper, filtrate water is transferred in volumetric flask, with water constant volume；
Step S3, after being diluted with water, 0.45 μm of filtering with microporous membrane obtains sample hydrolyzate, and injection ion chromatograph is surveyed
Determine polylactic acid content.
Preferably, lytic agent is 1- butyl -3- methylimidazole acetate in step S1.
Preferably, chain extender is ESO or ADR in step S1.
Preferably, sample to be tested is put in 50 DEG C of vacuum ovens dry 6h in advance in step S1.
Preferably, leacheate is 2.5mM sodium hydroxide solution in step S3.
Preferably, the flow of leacheate is 0.7mL/min in step S3.
Preferably, the production method of step S3 standard curve are as follows: using ion chromatograph to concentration 5.0,10.0,
20.0,50.0, the lactate standard working solution of 100.0mg/L is measured, and is cross with the mass concentration (X) of standard working solution
Coordinate, peak area (Y) are ordinate, draw standard working curve.
Preferably, in step S3 sample method for measuring are as follows: materials hydrolyzate 5ml, through C18 pretreatment column processing after
It is packed into sample bottle, is placed in autosampler, is tested by parameter preset, is calculated by following equation (1):
In formula: X --- the content of polylactic acid in sample, unit are gram every hectogram (g/100g)；
C --- the concentration of lactic acid in sample solution, unit are milligrams per liter (mg/L)；
V --- the final constant volume of test solution, unit are milliliter (mL)；
M --- the sample mass that final sample liquid represents, unit are gram (g)；
F --- polylactic acid content and lactic acid content ratio in its hydrolyzate in polylactic acid standard substance.
Compared with prior art, technical effect of the invention:
The detection method of polylactic acid content in plastic products provided by the invention, using 1- butyl -3- methylimidazole acetic acid
Salt is more environmentally protective as lytic agent, while adding a small amount of chain extender as catalyst, can occur with the carboxyl end group of PLA anti-
It answers, accelerates polylactic acid course of dissolution, shorten detection time, improve working efficiency, method is simple and direct, efficient, while guaranteeing test knot
The accuracy and precision of fruit.
Detailed description of the invention
In order to illustrate the technical solutions in the embodiments of the present application or in the prior art more clearly, below will be to institute in embodiment
Attached drawing to be used is needed to be briefly described, it should be apparent that, the accompanying drawings in the following description is only one recorded in the present invention
A little embodiments are also possible to obtain other drawings based on these drawings for those of ordinary skill in the art.
Fig. 1 is standard working solution ion chromatography testing result provided by the invention；
Fig. 2 is standard curve provided by the invention；
Fig. 3 is sample to be tested ion chromatography testing result provided by the invention.
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, below in conjunction with attached drawing to this hair
It is bright to be further detailed.Obviously, described embodiments are only a part of the embodiments of the present invention, rather than whole
Embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are obtained without making creative work
The every other embodiment obtained, shall fall within the protection scope of the present invention.Experimental method in following embodiments, such as without special theory
It is bright, it is conventional method.Test material as used in the following examples is unless otherwise specified from conventional biochemical reagent quotient
What shop was commercially available.
1 sample pretreating of embodiment
Sample (the polylactic acid shopping bag, poly- cream of different manufacturers, different polylactic acid contents, different size model are purchased in market
Sour cutlery box), these samples are handled, processing method is as follows:
It takes sample to be tested to crush, every kind of sample 0.5g is taken to be placed in a beaker respectively, lytic agent 1- butyl -3- methyl miaow is added
Azoles acetate 10ml~20ml adds the chain extender ESO or ADR of 0.05~0.5mg, 110~120 DEG C of 1~2h of oil bath heating,
Nitrogen protection；It is filtered with filter paper, filtrate water is transferred in 100ml volumetric flask, with water constant volume；Step S3,100 times are diluted with water
Afterwards, 0.45 μm of filtering with microporous membrane obtains sample hydrolyzate.See Table 1 for details for specific processing parameter.
Each sample to be tested processing parameter of table 1
| Sample to be tested | Polylactic acid content | Lytic agent | Chain extender | Oil bath temperature | The oil bath time |
| Polylactic acid shopping bag 1 | 35g/100g | 10ml | 0.05mgESO | 110℃ | 2h |
| Polylactic acid shopping bag 2 | 35g/100g | 10ml | 0.05mgADR | 110℃ | 2h |
| Polylactic acid shopping bag 3 | 35g/100g | 20ml | 0.5mgESO | 120℃ | 1h |
| Polylactic acid shopping bag 4 | 35g/100g | 20ml | 0.5mgADR | 120℃ | 1h |
| Polylactic acid cutlery box 1 | 70g/100g | 10ml | 0.05mgESO | 120℃ | 1h |
| Polylactic acid cutlery box 2 | 70g/100g | 10ml | 0.05mgADR | 120℃ | 1h |
| Polylactic acid cutlery box 3 | 70g/100g | 20ml | 0.5mgESO | 110℃ | 2h |
| Polylactic acid cutlery box 4 | 70g/100g | 20ml | 0.5mgADR | 110℃ | 2h |
2 standard curve making of embodiment
The production method of standard curve are as follows: peace ICS-3000 ion chromatograph: U.S. Dai Angong (is worn using ion chromatograph
Department) concentration 5.0,10.0,20.0,50.0, the lactate standard working solution of 100.0mg/L are measured, it is worked with standard molten
The mass concentration (X) of liquid is abscissa, and peak area (Y) is ordinate, draws standard working curve.Leacheate is 2.5mM hydrogen-oxygen
Change sodium solution, flow 0.7mL/min, C18 pretreatment column, 25 DEG C of column temperature.Map is tested as shown in Figure 1, Specification Curve of Increasing
As shown in Fig. 2, equation of linear regression are as follows: Y=1.602e+005+1.609e+005X, related coefficient: r=0.99988.
The measurement of 3 sample of embodiment
Materials hydrolyzate 5ml, is packed into sample bottle after the processing of C18 pretreatment column, is placed in autosampler, by default
Parameter is tested, and test results are shown in figure 3.
Polylactic acid measurement result is calculated by following equation (1):
In formula: X --- the content of polylactic acid in sample, unit are gram every hectogram (g/100g)；
C --- the concentration of lactic acid in sample solution, unit are milligrams per liter (mg/L)；
V --- the final constant volume of test solution, unit are milliliter (mL)；
M --- the sample mass that final sample liquid represents, unit are gram (g)；
F --- polylactic acid content and lactic acid content ratio in its hydrolyzate in polylactic acid standard substance.
Calculated result is shown in Table 2.
2 polylactic acid content of table is compared with surveying polylactic acid content
Conclusion: dissolving sample to be tested using test method of the present invention, is worked using chromatography of ions test lactate standard bent
Line, then the content of determinand is obtained by external standard method, eventually by the content that polylactic acid in plastic products is calculated, result
In relative deviation within ± 3%, accuracy is good, meanwhile, each sample feeding 3 times is averaged, and calculates the coefficient of variation, knot
Fruit is respectively less than 5%, and precision is good.
It is above that certain exemplary embodiments of the invention are only described by way of explanation, undoubtedly, for ability
The those of ordinary skill in domain without departing from the spirit and scope of the present invention can be with a variety of different modes to institute
The embodiment of description is modified.Therefore, above-mentioned attached drawing and description are regarded as illustrative in nature, and should not be construed as to the present invention
The limitation of claims.
Claims (8)
1. the detection method of polylactic acid content in plastic products, which comprises the following steps:
Step S1, sample to be tested is taken to be placed in a beaker, according to sample to be tested and lytic agent mass volume ratio (g/ml) 1:2~1:4
Be added lytic agent, add quality be sample to be tested quality 0.01~0.1% chain extender, 110~120 DEG C of oil bath heatings 1~
2h, nitrogen protection；
Step S2, it is filtered with filter paper, filtrate water is transferred in volumetric flask, with water constant volume；
Step S3, after being diluted with water, 0.45 μm of filtering with microporous membrane obtains sample hydrolyzate, and injection ion chromatograph measurement is poly-
Lactic acid content.
2. the detection method of polylactic acid content in plastic products according to claim 1, which is characterized in that molten in step S1
Solution agent is 1- butyl -3- methylimidazole acetate.
3. the detection method of polylactic acid content in plastic products according to claim 2, which is characterized in that expand in step S1
Chain agent is ESO or ADR.
4. the detection method of polylactic acid content in plastic products according to claim 3, which is characterized in that in step S1 to
Sample is put in 50 DEG C of vacuum ovens dry 6h in advance.
5. the detection method of polylactic acid content in plastic products according to claim 1-4, which is characterized in that step
Leacheate is 2.5mM sodium hydroxide solution in rapid S3.
6. the detection method of polylactic acid content in plastic products according to claim 5, which is characterized in that drenched in step S3
The flow of washing lotion is 0.7mL/min.
7. the detection method of polylactic acid content in plastic products according to claim 6, which is characterized in that step S3 acceptance of the bid
The production method of directrix curve are as follows: using ion chromatograph to the lactate standard of concentration 5.0,10.0,20.0,50.0,100.0mg/L
Working solution is measured, and with the mass concentration (X) of standard working solution for abscissa, peak area (Y) is ordinate, draws mark
Quasi- working curve.
8. the detection method of polylactic acid content in plastic products according to claim 7, which is characterized in that sample in step S3
The method for measuring of product are as follows: materials hydrolyzate 5ml, is packed into sample bottle after the processing of C18 pretreatment column, is placed in autosampler
In, it is tested by parameter preset, is calculated by following equation (1):
In formula: X --- the content of polylactic acid in sample, unit are gram every hectogram (g/100g)；
C --- the concentration of lactic acid in sample solution, unit are milligrams per liter (mg/L)；
V --- the final constant volume of test solution, unit are milliliter (mL)；
M --- the sample mass that final sample liquid represents, unit are gram (g)；
F --- polylactic acid content and lactic acid content ratio in its hydrolyzate in polylactic acid standard substance.
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