CN107957400A - A kind of water-based emulsion adhesive free formaldehyde demulsification detection reagent and the free formaldehyde detection method using the reagent - Google Patents
A kind of water-based emulsion adhesive free formaldehyde demulsification detection reagent and the free formaldehyde detection method using the reagent Download PDFInfo
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Abstract
The invention discloses a kind of water-based emulsion adhesive free formaldehyde demulsification detection reagent and the free formaldehyde detection method using the reagent, its key points of the technical solution are that:The reagent is mixed by the one or more in 20%~40% methanol, ethanol, ether organic solution with 1 5g sodium chloride;A kind of detection method of water-based emulsion adhesive free formaldehyde includes the following steps:A, water-based emulsion adhesive sample is weighed, is placed in centrifuge tube, demulsification detection reagent is added, mixes;B, stand, centrifugation, transfer supernatant, with suitable 20%~40% ethanol solution rinse centrifuge tube, between adjusting pH to 6.0 ± 0.2 with dilute hydrochloric acid solution or diluted sodium hydroxide solution, adds ethanol solution to scale in colorimetric cylinder;C, acetylacetone,2,4-pentanedione solution is added to shake up;D, 20~50min in 50~60 DEG C of water-baths is placed on, taking-up is cooled to room temperature;E, and then at 410~415nm its absorbance is surveyed, is contrasted by standard curve and obtains concentration of formaldehyde.
Description
【Technical field】
The present invention relates to coating detection field, and in particular to a kind of water-based emulsion adhesive free formaldehyde demulsification detection reagent
And the free formaldehyde detection method using the reagent.
【Background technology】
Formaldehyde is a kind of colourless, has the gas of intense irritation, has volatile characteristic.Formaldehyde in indoor air is
It is maximum as the major pollutants for influencing human body health, particularly harm of the formaldehyde in air in winter to human body.China
Formaldehyde source in family's air mainly has the following aspects:(1) glued board, core-board, the Midst density being used for indoor ornamentation
The artificial board such as fiberboard and particieboard.The adhesive that production wood-based plate uses is remaining in plate using formaldehyde as main component
It can gradually be discharged with the formaldehyde for having neither part nor lot in reaction to surrounding environment, be the main body to form formaldehyde in indoor air.(2) formaldehyde is contained
Component is simultaneously possible to the other kinds ornament materials outwardly distributed, such as wall covering fabric, wallpaper, chemical fibre carpet, paint and coating
Deng.From the foregoing, it will be observed that the free formaldehyde in adhesive, is one of source of formaldehyde pollution in family.
The detection of free formaldehyde content, is the leading indicator of water-based emulsion adhesive environmental protection evaluation, according to existing detection
Standard GB 18582-2008 use conventional distillation, but conventional distillation has the following disadvantages:(1) the rate of recovery is made the problem of gas leakage
It is relatively low;(2) water-based emulsion adhesive is extremely easy to condense in flask walls in weighing apparatus was distilled, and divides in continuous heating
Solution, produces false positive results;(3) time-consuming, manually stares at and keeps, efficiency is low.Therefore attempt by using ethanol solution and change the hard of water
Degree makes water-based emulsion adhesive fast emulsion breaking, and the method for detecting free formaldehyde content therein rapidly.
【The content of the invention】
The present invention provides a kind of water-based emulsion adhesive free formaldehyde demulsification detection reagent, and formula is simple, and raw material is easy to take
, accuracy in detection is high.
The present invention also provides a kind of detection method of water-based emulsion adhesive free formaldehyde, and step is easy, as a result reappearance
It is good.
The present invention is achieved by the following technical solutions:
A kind of water-based emulsion adhesive free formaldehyde is demulsified detection reagent, methanol of the reagent by 20%~40%, second
One or more in alcohol, ether organic solution are mixed with 1-5g sodium chloride.Dissolve and compare in water for free formaldehyde
The characteristics of stablizing, using the mechanism of chemical demulsification, using with higher active organic solvent, is distributed on oil-water interface, can
Emulsifying agent is supplanted, controls oneself and forms a new easily rupturable interfacial film, add the strong electrolyte material such as sodium chloride, destroy
The interfacial film protected by electric charge, it is more easily rupturable under electric field action, easy to oil, water separation stratification.
A kind of detection method of water-based emulsion adhesive free formaldehyde, the detection method include the following steps:
A, water-based emulsion adhesive sample is weighed, is placed in centrifuge tube, demulsification detection reagent is added, mixes;
B, stand, centrifugation, transfer supernatant is centrifuged in colorimetric cylinder with suitable 20%~40% ethanol solution rinse
Pipe, between adjusting pH to 6.0 ± 0.2 with dilute hydrochloric acid solution or diluted sodium hydroxide solution, adds ethanol solution to scale;
C, acetylacetone,2,4-pentanedione solution is added to shake up;
D, 20~50min in 50~60 DEG C of water-baths is placed on, taking-up is cooled to room temperature;
E, and then at 410~415nm its absorbance is surveyed, is contrasted by standard curve and obtains concentration of formaldehyde.For water-based
The metastable feature of free formaldehyde in lotion adhesive, destroys original macro-radical, using acetylacetone,2,4-pentanedione using demulsifier
Reacted completely Deng with formaldehyde, then the sensitivity of PARA FORMALDEHYDE PRILLS(91,95) test is improved using ultraviolet-visible spectrophotometer analysis, and reacted
Rapidly, the interference of acetaldehyde in environment, propionic aldehyde to test result is on the other hand reduction of, method is examined better than the existing way of distillation
Survey, result precision higher
Preferably, 0.25% acetylacetone,2,4-pentanedione solution is used in the step C.
Preferably, bath temperature is 30min in 60 DEG C of water-baths in the step D
Preferably, the detection method of the step E by the external standard method of spectrophotometer in water-based emulsion adhesive
Free formaldehyde carries out quantitative analysis.
Preferably, the preparation method of the standard curve of detection method is in the step E:
It is respectively 0mL, 0.2Ml, 0.4mL quantitatively to weigh formaldehyde standard working solution volume respectively, 0.6mL, 1.0mL,
2.0mL, adds in colorimetric cylinder, adds demulsification detection reagent dissolving, mixes, adjusted with dilute hydrochloric acid solution or diluted sodium hydroxide solution
Between pH to 6.0 ± 0.2, ethanol solution is added to add acetylacetone,2,4-pentanedione solution to scale and shake up, then be placed in 20 in 50~60 DEG C of water-baths
~50min, taking-up are cooled to room temperature, its absorbance is then surveyed at 412nm, with the absorption cell of 1cm, are demulsified with blank and are detected examination
Agent is reference, using absorbance A as ordinate, using concentration of formaldehyde as abscissa, draws to obtain standard curve.
Compared with prior art, the invention has the advantages that:
A kind of water-based emulsion adhesive free formaldehyde demulsification detection reagent of the present invention, dissolves in water for free formaldehyde
The characteristics of more stable, using the mechanism of chemical demulsification, using with higher active organic solvent, be distributed to oil-water interface
On, emulsifying agent can be supplanted, control oneself and form a new easily rupturable interfacial film, add the strong electrolyte thing such as sodium chloride
Matter, destroys the interfacial film protected by electric charge, more easily rupturable under electric field action, each in emulsion easy to oil, water separation stratification
Phase separation, makes free formaldehyde therein get enter into water phase, and detection sensitivity is high, and other factors influence is small, and timeliness is fast, detection
Accuracy is high;
A kind of detection method of water-based emulsion adhesive free formaldehyde of the present invention, for first of dissociating in water-based emulsion adhesive
The metastable feature of aldehyde, is destroyed original macro-radical using demulsifier, is reacted completely with formaldehyde using acetylacetone,2,4-pentanedione, then adopt
The sensitivity of PARA FORMALDEHYDE PRILLS(91,95) test is improved with ultraviolet-visible spectrophotometer analysis, and is swift in response, is on the other hand reduction of
The interference of acetaldehyde, propionic aldehyde to test result in environment, method are detected better than the existing way of distillation, result precision higher.
【Embodiment】
1-7 in conjunction with specific embodiments, weighs 0.5~1g of test sample respectively, illustrates a kind of water-based breast of the present invention
The detection method of liquid adhesive free formaldehyde:
Embodiment 1:
A, water-based emulsion adhesive sample 1g is weighed, is placed in centrifuge tube, adds the methanol solution by 20% and 1g chlorinations
The demulsification detection reagent that sodium is mixed, mixes;
B, stand, centrifugation, transfer supernatant, with suitable 20% methanol solution rinse centrifuge tube, is used in colorimetric cylinder
Between dilute hydrochloric acid solution or diluted sodium hydroxide solution adjust pH to 6.0 ± 0.2, add methanol solution to scale;
C, the acetylacetone,2,4-pentanedione solution of addition 0.25% shakes up;
D, 30min in 60 DEG C of water-baths is placed on, taking-up is cooled to room temperature;
E, and then at 412nm its absorbance is surveyed, is contrasted by standard curve and obtains concentration of formaldehyde.
Embodiment 2:
A, water-based emulsion adhesive sample 1g is weighed, is placed in centrifuge tube, adds the ethanol solution by 20% and 1g chlorinations
The demulsification detection reagent that sodium is mixed, mixes;
B, stand, centrifugation, transfer supernatant, with suitable 20% ethanol solution rinse centrifuge tube, is used in colorimetric cylinder
Between dilute hydrochloric acid solution or diluted sodium hydroxide solution adjust pH to 6.0 ± 0.2, add ethanol solution to scale;
C, the acetylacetone,2,4-pentanedione solution of addition 0.25% shakes up;
D, 20min in 50 DEG C of water-baths is placed on, taking-up is cooled to room temperature;
E, and then at 410nm its absorbance is surveyed, is contrasted by standard curve and obtains concentration of formaldehyde.
Embodiment 3:
A, water-based emulsion adhesive sample 0.5g is weighed, is placed in centrifuge tube, is added by 20% diethyl ether solution and 3g chlorine
Change the demulsification detection reagent that sodium is mixed, mix;
B, stand, centrifugation, transfer supernatant, with suitable 20% diethyl ether solution rinse centrifuge tube, is used in colorimetric cylinder
Between dilute hydrochloric acid solution or diluted sodium hydroxide solution adjust pH to 6.0 ± 0.2, the solution that adds diethyl ether is to scale;
C, acetylacetone,2,4-pentanedione solution is added to shake up;
D, 50min in 55 DEG C of water-baths is placed on, taking-up is cooled to room temperature;
E, and then at 415nm its absorbance is surveyed, is contrasted by standard curve and obtains concentration of formaldehyde.
Embodiment 4:
A, water-based emulsion adhesive sample 1g is weighed, is placed in centrifuge tube, adds the methanol solution by 30% and 5g chlorinations
The demulsification detection reagent that sodium is mixed, mixes;
B, stand, centrifugation, transfer supernatant, with suitable 20% methanol solution rinse centrifuge tube, is used in colorimetric cylinder
Between dilute hydrochloric acid solution or diluted sodium hydroxide solution adjust pH to 6.0 ± 0.2, add methanol solution to scale;
C, the acetylacetone,2,4-pentanedione solution of addition 0.25% shakes up;
D, 30min in 60 DEG C of water-baths is placed on, taking-up is cooled to room temperature;
E, and then at 412nm its absorbance is surveyed, is contrasted by standard curve and obtains concentration of formaldehyde.
Embodiment 5:
A, water-based emulsion adhesive sample 1g is weighed, is placed in centrifuge tube, adds the ethanol solution by 40% and 4g chlorinations
The demulsification detection reagent that sodium is mixed, mixes;
B, stand, centrifugation, transfer supernatant, with suitable 20% ethanol solution rinse centrifuge tube, is used in colorimetric cylinder
Between dilute hydrochloric acid solution or diluted sodium hydroxide solution adjust pH to 6.0 ± 0.2, add ethanol solution to scale;
C, the acetylacetone,2,4-pentanedione solution of addition 0.25% shakes up;
D, 40min in 50 DEG C of water-baths is placed on, taking-up is cooled to room temperature;
E, and then at 412nm its absorbance is surveyed, is contrasted by standard curve and obtains concentration of formaldehyde.
Embodiment 6:
A, water-based emulsion adhesive sample 0.5g is weighed, is placed in centrifuge tube, is added by 40% diethyl ether solution and 2g chlorine
Change the demulsification detection reagent that sodium is mixed, mix;
B, stand, centrifugation, transfer supernatant, with suitable 20% diethyl ether solution rinse centrifuge tube, is used in colorimetric cylinder
Between dilute hydrochloric acid solution or diluted sodium hydroxide solution adjust pH to 6.0 ± 0.2, the solution that adds diethyl ether is to scale;
C, acetylacetone,2,4-pentanedione solution is added to shake up;
D, 50min in 55 DEG C of water-baths is placed on, taking-up is cooled to room temperature;
E, and then at 415nm its absorbance is surveyed, is contrasted by standard curve and obtains concentration of formaldehyde.
Embodiment 7:
A, water-based emulsion adhesive sample 0.5g is weighed, is placed in centrifuge tube, is added and mixed by 30% methanol with ether
The demulsification detection reagent that solution is mixed with 2g sodium chloride, mixes;
B, stand, centrifugation, transfer supernatant, with suitable 30% methanol solution rinse centrifuge tube, is used in colorimetric cylinder
Between dilute hydrochloric acid solution or diluted sodium hydroxide solution adjust pH to 6.0 ± 0.2, add methanol solution to scale;
C, acetylacetone,2,4-pentanedione solution is added to shake up;
D, 40min in 50 DEG C of water-baths is placed on, taking-up is cooled to room temperature;
E, and then at 413nm its absorbance is surveyed, is contrasted by standard curve and obtains concentration of formaldehyde.
It is respectively 0mL, 0.2Ml, 0.4mL quantitatively to weigh formaldehyde standard working solution volume respectively, 0.6mL, 1.0mL,
2.0mL, adds in colorimetric cylinder, adds demulsification detection reagent dissolving, mixes, adjusted with dilute hydrochloric acid solution or diluted sodium hydroxide solution
Between pH to 6.0 ± 0.2, ethanol solution is added to add acetylacetone,2,4-pentanedione solution to scale and shake up, then be placed in 20 in 50~60 DEG C of water-baths
~50min, taking-up are cooled to room temperature, its absorbance is then surveyed at 412nm, with the absorption cell of 1cm, are demulsified with blank and are detected examination
Agent is reference, using absorbance A as ordinate, using concentration of formaldehyde as abscissa, draws to obtain standard curve.
The concentration of sample solution formaldehyde is read directly from standard curve according to absorbance.
Free formaldehyde content X in sample, calculation formula are:
In formula:X --- free formaldehyde content, unit are grams per kilogram (g/kg);
Ct --- concentration of formaldehyde in the sample solution read from standard curve, unit are micrograms per millilitre (ug/mL);
Cb --- concentration of formaldehyde in the blank solution read from standard curve, unit are micrograms per millilitre (ug/mL);
V --- the volume after distillate constant volume, unit are milliliter (mL),
The quality of m --- sample, unit are gram (g);
The dilution gfactor of f --- sample solution.
Detect the measure of precision:Same sample is detected using breaking method, sample is weighed, is operated according to above-mentioned steps
As a result, experimental data is directly read on spectrophotometer is shown in Table 1.
Table 1:The measure of embodiment 1-7 Data Detection precision
Recovery of standard addition measures:Same sample is detected using breaking method, sample is weighed respectively, adds a certain amount of formaldehyde
Standard liquid carries out mark-on reclaims experiment, is operated according to above-mentioned steps, experimental data is directly read on spectrophotometer and is shown in Table 2.
Table 2:The recovery of standard addition measure of embodiment 1-7 data
Method compares:Weigh same actual sample, then traditional distillating method detection be respectively adopted, as a result respectively with implementation
Example 1-7 contrasts, specific comparison data are shown in Table 3.
Table 3:Traditional way of distillation and the experimental result using demulsification method is respectively adopted in same sample
Sequence number | Traditional way of distillation (mg/L) | Demulsification method (mg/L) |
1 | 0.834 | 0.83 |
2 | 0.847 | 0.83 |
3 | 0.822 | 0.83 |
4 | 0.832 | 0.83 |
5 | 0.826 | 0.83 |
6 | 0.831 | 0.83 |
7 | 0.834 | 0.83 |
Average value | 0.834 | 0.83 |
Experimental result shows, demulsification method is in the free formaldehyde measure of water-based adhesive, the result is that accurately and reliably,
Especially in the on-line checking work of production line, such data precision has been sufficient for data demand.Relative to traditional
The way of distillation more has the advantages of following:(1) experimentation list sample about 15 minutes, only with the time of traditional way of distillation a quarter;⑵
Manpower is saved, can be interspersed between multiple quality inspection projects and carry out;(3) the security of experimentation is improved;(4) can to online product
Quickly to provide data, for the content of formaldehyde in adjustment product.
Claims (6)
- The detection reagent 1. a kind of water-based emulsion adhesive free formaldehyde is demulsified, it is characterised in that:The reagent is by 20%~40% Methanol, ethanol, the one or more in ether organic solution are mixed with 1~5g sodium chloride.
- 2. a kind of detection method of water-based emulsion adhesive free formaldehyde, it is characterised in that the detection method includes the following steps:A, water-based emulsion adhesive sample is weighed, is placed in centrifuge tube, demulsification detection reagent is added, mixes;B, stand, centrifugation, transfer supernatant is in colorimetric cylinder, with appropriate solution rinse centrifuge tube, with dilute hydrochloric acid solution or dilute hydrogen Between sodium hydroxide solution adjusts pH to 6.0 ± 0.2, add ethanol solution to scale;C, acetylacetone,2,4-pentanedione solution is added to shake up;D, 20~50min in 50~60 DEG C of water-baths is placed on, taking-up is cooled to room temperature;E, and then at 410~415nm its absorbance is surveyed, is contrasted by standard curve and obtains concentration of formaldehyde.
- A kind of 3. detection method of water-based emulsion adhesive free formaldehyde according to claim 2, it is characterised in that:It is described 0.25% acetylacetone,2,4-pentanedione solution is used in step C.
- A kind of 4. detection method of water-based emulsion adhesive free formaldehyde according to claim 2, it is characterised in that:It is described Bath temperature is 30min in 60 DEG C of water-baths in step D.
- A kind of 5. detection method of water-based emulsion adhesive free formaldehyde according to claim 2, it is characterised in that:It is described The detection method of step E quantitatively divides the free formaldehyde in water-based emulsion adhesive by the external standard method of spectrophotometer Analysis.
- 6. the detection method of a kind of water-based emulsion adhesive free formaldehyde according to claim 2, it is characterised in that described The preparation method of the standard curve of detection method is in step E:It is respectively 0mL, 0.2Ml, 0.4mL quantitatively to weigh formaldehyde standard working solution volume respectively, 0.6mL, 1.0mL, 2.0mL, Add in colorimetric cylinder, add demulsification detection reagent dissolving, mix, with dilute hydrochloric acid solution or diluted sodium hydroxide solution adjust pH to Between 6.0 ± 0.2, add ethanol solution to scale, add acetylacetone,2,4-pentanedione solution and shake up, then be placed in 20 in 50~60 DEG C of water-baths~ 50min, taking-up are cooled to room temperature, its absorbance is then surveyed at 412nm, with the absorption cell of 1cm, are demulsified detection reagent with blank For reference, using absorbance A as ordinate, using concentration of formaldehyde as abscissa, standard curve is drawn to obtain.
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