CN107941958A - A kind of method of free formaldehyde in measure water paint - Google Patents
A kind of method of free formaldehyde in measure water paint Download PDFInfo
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- CN107941958A CN107941958A CN201711340369.7A CN201711340369A CN107941958A CN 107941958 A CN107941958 A CN 107941958A CN 201711340369 A CN201711340369 A CN 201711340369A CN 107941958 A CN107941958 A CN 107941958A
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- water paint
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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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- 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
- G01N2030/067—Preparation by reaction, e.g. derivatising the sample
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Abstract
The invention discloses a kind of method for measuring free formaldehyde in water paint, 0.1 1.0g of sample is taken to 50ml volumetric flasks, add dual distilled water fully dispersed and constant volume, take the above-mentioned solution of 1 10ml to add 0.5 5ml 2 into the volumetric flask of certain volume, 4 dinitrophenylhydrazine derivative reagents, add the acetate salt buffer salting liquid of 0.5 5ml pH=5, add organic diluent constant volume, seal and shake up, avoid light place filters after a certain period of time under certain temperature, and filtrate is tested into HPLC.The present invention can accurately and rapidly measure content of formaldehyde in water paint, will be of great significance for the safety of coating quality control and environment.
Description
Technical field
The present invention relates to a kind of detection method of formaldehyde, and in particular to a kind of side for measuring free formaldehyde in water paint
Method.
Background technology
In recent years, with economic fast development and the continuous improvement of national life level, caused by main city zone is removed
Real estate industry's development prospect is fine, and due to the relieving of national two tire policies, young couple two child in small and medium-sized cities leads notable growth,
Resident's house-purchase ratio significantly increases, with the improvement of living standards, indoor decorating is increasingly becoming a kind of fashion.Interior decoration
Room air pollution caused by finishing material and the health problem thus triggered have increasingly caused the concern of people.At present,
Formaldehyde has become that indoor pollution is most universal, one of pollutant of most serious.Harm of the formaldehyde to health has been mainly manifested in
Stimulate, sensitization and mutagenesis are made.When Formaldehyde in Atmosphere concentration reaches a certain level, eyes, the respiratory tract of people just have discomfort, skin
Skin can cause allergic dermatitis, eye can be caused to itch, be envious, shedding tears, the symptom such as Nausea and vomiting, uncomfortable in chest, general weakness, and suction is high
Concentration formaldehyde can cause respiratory inflammation, bronchial asthma, lung's major injury.Long Term Contact low dosage formaldehyde can cause chronic
Breathing problem, decrease of memory, chromosome abnormality, immunologic dysfunction etc..Formaldehyde has nervous system strong toxic action,
It can be suppressed the activity of a variety of enzymes in organ and tissue, immune level can also be affected, moreover it is possible to cause mammal thin
The gene mutation of born of the same parents' strain, suppresses the reparation of DNA damage, influences DNA synthesis transcriptions, damages chromosome.The World Health Organization (WHO)
Formaldehyde is classified as potential dangerous carcinogenic substance and important environmental contaminants with Environmental Protection Agency (US EPA).Formaldehyde is dirty
Dye problem has caused the extensive concern of society.Water paint used in decorations be Formaldehyde Pollution of Indoor Air important sources it
One, thus the assay method for studying formaldehyde in coating is significant to reducing indoor pollution.
At present, had many methods be applied to formaldehyde measure, but due to the complicated variety of coating sample matrix,
The problems such as influence of interference component, detection method used today takes there are sample pre-treatments, is cumbersome, poor selectivity,
The problems such as sensitivity is not high, therefore, is badly in need of establishing a kind of analysis side that is simple, fast and accurately measuring formaldehyde in water paint
Method.
The content of the invention
To make up the deficiencies in the prior art, the present invention provides a kind of high sensitivity, the measure water that detection limit is low, reproducible
The method of free formaldehyde in property coating.
The present invention is achieved through the following technical solutions：
A kind of method of free formaldehyde in measure water paint, it is characterized in that：
Comprise the following steps：
（1）Take sample to be tested 0.1-1.0g to be placed in 50ml volumetric flasks, add dual distilled water ultrasonic disperse 10-20min and constant volume；
（2）Take step（1）Solution 1-10ml into volumetric flask, be separately added into derivative reagent and buffer salt solution, added
Machine diluent constant volume, seals and shakes up；
（3）By step（2）Solution avoid light place 2-24h, filtering, filtrate tested using high performance liquid chromatography.
Preferably, the method for measuring free formaldehyde in water paint of the invention, step（2）The derivative of middle addition
Reagent is the 2,4 dinitrophenyl hydrazine derivative reagent of 0.5-5ml.
Further, 2,4-dinitrophenylhydrazine derivative reagent is formulated as follows：Add DNPH 0.05- in 100ml volumetric flasks
0.3g, adds sulfuric acid 1-3ml, and with methanol dissolving and constant volume, 0-4 DEG C saves backup.
Preferably, the method for measuring free formaldehyde in water paint of the invention, step（2）The buffering of middle addition
Salting liquid is the acetate salt buffer salting liquid of pH=5 of 0.5-5ml.
Further, the acetate salt buffer salting liquid of pH=5 is formulated as follows：In 100ml volumetric flasks, the anhydrous second of 3-10g is added
Sour sodium, 1-5ml glacial acetic acid, with water dissolving and constant volume.
Preferably, the method for measuring free formaldehyde in water paint of the invention, step（2）Middle addition it is organic
Diluent is methanol, one or more of mixed solvents in ethanol, isopropanol, acetonitrile, acetone, ethyl acetate.
Preferably, the method for measuring free formaldehyde in water paint of the invention, step（3）Derived temperature is not
More than 65 DEG C.
Further, step（3）Middle liquid chromatogram mobile phase is acetonitrile：Water=40:60-75:25.
Further, step（3）Middle liquid phase detection range is 250-380nm.
The beneficial effects of the invention are as follows：The present invention uses content of formaldehyde in Water By High Performance Liquid coating, leads to
Cross ultrasonic dissolution and cause the Form aldehyde release and soluble in water of dissociating in coating, utilize 2,4-dinitrophenylhydrazine derivative reagent and free first
Aldehyde reaction generates phenylhydrazone, and with liquid phase external standard method content, this method detection limit is lower than ultraviolet spectrophotometry, reproducible,
The content of formaldehyde of the environment-friendlywater-based water-based paint of high quality standards can be coordinated to detect.
Brief description of the drawings
Attached drawing 1 is 1 Plays working curve drafting figure of embodiment.
Embodiment
The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments, to help the skill of this area
Art personnel have more complete, accurate and deep understanding, protection scope of the present invention bag to inventive concept of the invention, technical solution
Include but be not limited to following embodiments, it is any to technical scheme on the premise of without departing from spirit and scope
Details and the modification made of form each fall within protection scope of the present invention.
Embodiment 1
The preparation and calibration of formaldehyde standard solution, with reference to GB18582-2008《It is harmful in indoor decorating and refurnishing materials interior wall coating
Material is limited the quantity》Appendix C.Formaldehyde standard dilution is to be diluted to be formulated step by step by formaldehyde standard solution.
Following table is the formaldehyde standard dilution and peak area and relative retention time of various concentrations：
The 2ml formaldehyde standard dilution of various concentrations is taken to add 1ml 2,4- dinitro benzenes into the volumetric flask of certain volume respectively
Hydrazine derivative reagent, adds the acetate salt buffer salting liquid of 1ml pH=5, adds isopropanol constant volume, seal and shake up, under certain temperature
Avoid light place is directly tested into HPLC after a certain period of time.
Wherein, 2,4-dinitrophenylhydrazine derivative reagent is prepared：Add DNPH 0.05-0.3g in 100ml volumetric flasks, add sulphur
Sour 1-3ml, is saved backup with methanol dissolving and constant volume, 0-4 DEG C of refrigerator；The acetate salt buffer salting liquid of pH=5 is prepared：100ml holds
In measuring bottle, 3-10g anhydrous sodium acetates, 1-5ml glacial acetic acid, with water dissolving and constant volume are added.
Chromatographic condition：Agilent liquid chromatograph 1260, chromatographic column：Agilent C18 long columns.Mobile phase：40-75% acetonitriles；
Flow velocity：0.5-1.5ml/min；Column temperature：20-35℃；Detection wavelength：250-380nm；Sample size：20ul.
Using abscissa as sample introduction concentration, ordinate is peak area, draws standard working curve as shown in drawings.
Embodiment 2
Residual matrix adds formaldehyde standard dilution as blank after being distilled using coating sample solution, takes 2ml above-mentioned molten after fully mixing
Liquid adds 1ml 2,4-dinitrophenylhydrazine derivative reagents into the volumetric flask of certain volume, adds the acetate salt buffer salt of 1ml pH=5
Solution, adds isopropanol constant volume, seals and shakes up, and avoid light place filters after a certain period of time under certain temperature, and filtrate is surveyed into HPLC
Examination.
As shown above, each 3 parts of Duplicate Samples of concentration selection are tested, and measure mark-on reclaims average recovery rate in 95-
Between 105%, and relative standard deviation RSD is respectively less than 1.0%, illustrates that this method is reliable, stablize and repeatability is good.
Preparation of reagents, the preparation of buffer salt solution and chromatographic condition are the same as embodiment 1 derived from the present embodiment.
Embodiment 3
The method of free formaldehyde, comprises the following steps in a kind of measure water paint：Sample to be tested 0.2g is taken to 50ml volumetric flasks
In, add dual distilled water to fill ultrasonic 15min and disperse simultaneously constant volume；The above-mentioned solution of 2ml is taken to add 1ml into the volumetric flask of certain volume
2,4-dinitrophenylhydrazine derivative reagent, adds the acetate salt buffer salting liquid of 1ml pH=5, adds isopropanol constant volume, seal and shake up,
Avoid light place filters after a certain period of time under certain temperature, and filtrate is tested into HPLC.
Test result is as shown in the table, surveys the sample of below 5ppm, and relative standard deviation RSD is respectively less than 5.0%, demonstrates
This method feasibility is preferable.
Preparation of reagents, the preparation of buffer salt solution and chromatographic condition are the same as embodiment 1 derived from the present embodiment.
Embodiment 4
The method of free formaldehyde, comprises the following steps in a kind of measure water paint：Sample to be tested 0.1g is taken to 50ml volumetric flasks
In, add dual distilled water to fill ultrasonic 10min and disperse simultaneously constant volume；The above-mentioned solution of 1ml is taken to add into the volumetric flask of certain volume
0.5ml 2,4-dinitrophenylhydrazine derivative reagents, add the acetate salt buffer salting liquid of 0.5ml pH=5, add ethyl acetate constant volume, close
Seal and shake up, avoid light place filters after a certain period of time under certain temperature, and filtrate is tested into HPLC.
Preparation of reagents, the preparation of buffer salt solution and chromatographic condition are the same as embodiment 1 derived from the present embodiment.
Embodiment 5
The method of free formaldehyde, comprises the following steps in a kind of measure water paint：Sample to be tested 1.0g is taken to 50ml volumetric flasks
In, add dual distilled water to fill ultrasonic 20min and disperse simultaneously constant volume；The above-mentioned solution of 10ml is taken to add 5ml into the volumetric flask of certain volume
2,4-dinitrophenylhydrazine derivative reagent, adds the acetate salt buffer salting liquid of 5ml pH=5, adds acetone constant volume, seal and shake up, in
Avoid light place filters after a certain period of time under certain temperature, and filtrate is tested into HPLC.
Preparation of reagents, the preparation of buffer salt solution and chromatographic condition are the same as embodiment 1 derived from the present embodiment.
Embodiment 6
The method of free formaldehyde, comprises the following steps in a kind of measure water paint：Sample to be tested 0.5g is taken to 50ml volumetric flasks
In, add dual distilled water to fill ultrasonic 15min and disperse simultaneously constant volume；The above-mentioned solution of 2ml is taken to add 2ml into the volumetric flask of certain volume
2,4-dinitrophenylhydrazine derivative reagent, adds the acetate salt buffer salting liquid of 2ml pH=5, adds acetonitrile constant volume, seal and shake up, in
Avoid light place filters after a certain period of time under certain temperature, and filtrate is tested into HPLC.
Preparation of reagents, the preparation of buffer salt solution and chromatographic condition are the same as embodiment 1 derived from the present embodiment.
Claims (9)
- A kind of 1. method for measuring free formaldehyde in water paint, it is characterised in that：Comprise the following steps：（1）Take sample to be tested 0.1-1.0g to be placed in 50ml volumetric flasks, add dual distilled water ultrasonic disperse and constant volume；（2）Take step（1）Solution 1-10ml into volumetric flask, be separately added into derivative reagent and buffer salt solution, added Machine diluent constant volume, seals and shakes up；（3）By step（2）Solution avoid light place 2-24h, filtering, filtrate tested using high performance liquid chromatography.
- A kind of 2. method for measuring free formaldehyde in water paint according to claim 1, it is characterised in that：Step（2） The derivative reagent of middle addition is the 2,4 dinitrophenyl hydrazine derivative reagent of 0.5-5ml.
- A kind of 3. method for measuring free formaldehyde in water paint according to claim 2, it is characterised in that：2,4- dinitros Base phenylhydrazine derivative reagent is formulated as follows：In 100ml volumetric flasks plus DNPH 0.05-0.3g, add sulfuric acid 1-3ml, it is molten with methanol Simultaneously constant volume is solved, 0-4 DEG C saves backup.
- 4. the method for free formaldehyde in a kind of measure water paint according to Claims 2 or 3, it is characterised in that：Step （2）The buffer salt solution of middle addition is the acetate salt buffer salting liquid of pH=5 of 0.5-5ml.
- A kind of 5. method for measuring free formaldehyde in water paint according to claim 4, it is characterised in that：The vinegar of pH=5 Hydrochlorate buffer salt solution is formulated as follows：In 100ml volumetric flasks, 3-10g anhydrous sodium acetates are added, 1-5ml glacial acetic acid, is dissolved with water And constant volume.
- A kind of 6. method for measuring free formaldehyde in water paint according to claim 1, it is characterised in that：Step（2） The organic diluent of middle addition is methanol, one or more of mixing in ethanol, isopropanol, acetonitrile, acetone, ethyl acetate are molten Agent.
- A kind of 7. method for measuring free formaldehyde in water paint according to claim 1, it is characterised in that：Derivative temperature No more than 65 DEG C.
- A kind of 8. method for measuring free formaldehyde in water paint according to claim 1, it is characterised in that：Step（3） Middle liquid chromatogram mobile phase is acetonitrile：Water=40:60-75:25.
- A kind of 9. method for measuring free formaldehyde in water paint according to claim 8, it is characterised in that：The liquid phase Detection range is 250-380nm.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711340369.7A CN107941958A (en) | 2017-12-14 | 2017-12-14 | A kind of method of free formaldehyde in measure water paint |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711340369.7A CN107941958A (en) | 2017-12-14 | 2017-12-14 | A kind of method of free formaldehyde in measure water paint |
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| CN107941958A true CN107941958A (en) | 2018-04-20 |
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| CN201711340369.7A Pending CN107941958A (en) | 2017-12-14 | 2017-12-14 | A kind of method of free formaldehyde in measure water paint |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114053755A (en) * | 2020-08-07 | 2022-02-18 | 中国石油化工股份有限公司 | Extracting agent and extracting method for detecting harmful substances in interior wall coating |
| CN114487219A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Extracting agent and extracting method for detecting harmful substances in coating |
Citations (2)
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| CN103792296A (en) * | 2012-11-01 | 2014-05-14 | 江苏汉邦科技有限公司 | Determination method of formaldehyde content in emulsion paint |
| CN107402261A (en) * | 2016-05-20 | 2017-11-28 | 立邦涂料（中国）有限公司 | A kind of method of content of formaldehyde in combination high performance liquid chromatography detection water paint |
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2017
- 2017-12-14 CN CN201711340369.7A patent/CN107941958A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103792296A (en) * | 2012-11-01 | 2014-05-14 | 江苏汉邦科技有限公司 | Determination method of formaldehyde content in emulsion paint |
| CN107402261A (en) * | 2016-05-20 | 2017-11-28 | 立邦涂料（中国）有限公司 | A kind of method of content of formaldehyde in combination high performance liquid chromatography detection water paint |
Non-Patent Citations (2)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114053755A (en) * | 2020-08-07 | 2022-02-18 | 中国石油化工股份有限公司 | Extracting agent and extracting method for detecting harmful substances in interior wall coating |
| CN114487219A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Extracting agent and extracting method for detecting harmful substances in coating |
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Application publication date: 20180420 |