CN104964937A - Method for conducting spectrophotometric determination on formaldehyde content of water-based coating through acetylacetone - Google Patents
Method for conducting spectrophotometric determination on formaldehyde content of water-based coating through acetylacetone Download PDFInfo
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- CN104964937A CN104964937A CN201510358683.2A CN201510358683A CN104964937A CN 104964937 A CN104964937 A CN 104964937A CN 201510358683 A CN201510358683 A CN 201510358683A CN 104964937 A CN104964937 A CN 104964937A
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Abstract
The invention provides a method for conducting spectrophotometric determination on the formaldehyde content of a water-based coating through acetylacetone. The method comprises the steps that 1, a standard curve is drawn; 2, the formaldehyde content is measured. The method aims at solving the problems that a lot of bubbles will be produced in the distilling process and the distilling effect is hard to control. Defoaming agents are added to optimize the distilling effect and speed in the distilling process. The method has the advantages that the precision degree and the repeatability are high; the reproducibility is good; on the repeatability condition, the relative deviation of two testing results does not exceed 5%; on the reproducibility condition, the relative deviation of testing results of different laboratories does not exceed 10%.
Description
Technical field
The invention belongs to chemical field, particularly, relate to the method for content of formaldehyde in a kind of diacetone spectrophotometry water paint.
Background technology
Nowadays, national standard is more and more stricter to the limitation of water paint Free-formaldehyde, and is the compulsory standard that each enterprise must perform.Therefore, the accuracy of formaldehyde determination had both been related to the interests of each enterprise, was also related to the health of numerous people.The method always continued to use in national standard and environmental standard is diacetone spectrophotometric method, and the method is also widely used in food, textile industry etc., is a classical method of generally acknowledging, but due to detection material different, operationally different.Owing to numerous air-bubble can be produced in still-process, be difficult to the effect controlling distillation, so the bubble how reduced in still-process is the key of technical solution problem.
Summary of the invention
For defect of the prior art, the object of this invention is to provide the method for content of formaldehyde in a kind of diacetone spectrophotometry water paint.
The present invention is achieved by the following technical solutions:
The present invention relates to the method for content of formaldehyde in a kind of diacetone spectrophotometry water paint, described method comprises the steps:
Step 1, the drafting of typical curve: get 8 50mL tool plug graduated tubes, add 0.00 respectively, 0.02,0.50,1.00,3.00,5.00,8.00,10.00mL formaldehyde standard uses solution, add water to 50mL, add 2.5mL diacetone solution again in each brace plug graduated tube, shake up, in 60 DEG C of water-baths, heat 30min, be cooled to room temperature after taking-up, measure; Use 10mm cuvette, at wavelength 412nm place, measure absorbance, with absorbance and corresponding formaldehyde quality drawing standard working curve;
Step 2, the mensuration of content of formaldehyde: take 2g water paint sample, be placed in 50mL volumetric flask, and the scale of dilute with water, shake up; Use pipette, extract 10mL, move into and added in the 100mL cucurbit of 10mL distilled water, and in cucurbit, add a small amount of zeolite, instill a defoamer, first should add appropriate water logging in the bottle of collection cut and not have condenser pipe to export; Add thermal distillation and collect cut, evaporate to dryness, the cut of collection being transferred in 50mL tool plug graduated tube, being diluted with water to scale, to be measured; Sample to be tested adds 2.5mL diacetone solution, shake up, 30min is heated in 60 DEG C of water-baths, room temperature is cooled to after taking-up, measure the content of formaldehyde: use 10mm cuvette, at wavelength 412nm place, measure absorbance, deduct the absorbance measured by blank test, find the content of formaldehyde in sample from typical curve.
Preferably, described content of formaldehyde is calculated as follows:
Wherein: C-content of formaldehyde, mg/kg
M-from the formaldehyde amount that typical curve checks in, μ g;
W-test the sample size got, g;
F-dilution gfactor.
Preferably, the volumetric concentration of described diacetone solution is 0.25%, and its collocation method is: claim 25g ammonium acetate, add a small amount of water-soluble solution, add the diacetone that 3mL ice second and 0.25mL newly distill, move in 100mL volumetric flask, be settled to scale with water, adjustment pH=6.0, stores in 2 ~ 5 DEG C.
Preferably, the collocation method of described formaldehyde standard use solution is: pipette formaldehyde standard reserving solution 10mL, be placed in 1000mL volumetric flask, be diluted with water to scale, store for 2 ~ 5 DEG C.
Preferably, the collocation method of described formaldehyde standard reserving solution: pipette 20.00mL formaldehyde standard reserving solution and be placed in 250ml iodine flask, add 0.05mol/L iodine solution 25.0mL, immediately dropwise add 1mol/L sodium hydroxide solution to color take off faint yellow, after leaving standstill 15min, add the acid-soluble 11mL acidifying of 1mol/L salt, with the sodium thiosulfate demarcated molten be titrated to faint yellow, add the 1g/100mL starch instruction 1mL of new preparation, continuing to be titrated to blueness has just disappeared for terminal, record consume sodium thiosulfate standard solution volume V1, carry out blank determination simultaneously, record consume sodium thiosulfate standard solution volume V0, be calculated as follows Standardization Concentration of Formaldehyde Standard Solution:
In formula:
V0---the blank volume consuming hypo solution, mL;
V1---demarcate the volume that formaldehyde consumes hypo solution, mL;
---hypo solution concentration, mol/L;
15.0---formaldehyde (1/2HCHO) molal weight;
10.0---formaldehyde standard reserving solution sample volume, mL.
Preferably, described hydrochloric acid solution is 1mol/L, and described sodium hydroxide solution is 1mol/L, described iodine solution is 0.05mol/L, described starch solution is 1g/100mL, and described sodium thiosulfate standard solution is 0.1mol/L, and in described formalin, the massfraction of formaldehyde is 37%.
Compared with prior art, the present invention has following beneficial effect:
1, the inventive method can produce numerous air-bubble in the process because of distillation, is difficult to the problem of the effect controlling distillation, adds defoamer to optimize distilling effect and speed in still-process.
2, the precision of the inventive method is high, and repeatability is strong; Repeatability is good, and under repeated condition, the relative deviation of twice test result is no more than 5%; Under repeatability condition, between different experiments room, the relative deviation of test result is no more than 10%.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
The present embodiment relates to the method for content of formaldehyde in a kind of diacetone spectrophotometry water paint, and described method comprises the steps:
Step 1, the drafting of typical curve: get 8 50mL tool plug graduated tubes, add 0.00 respectively, 0.02,0.50,1.00,3.00,5.00,8.00,10.00mL formaldehyde standard uses solution, add water to 50mL, add 2.5mL diacetone solution again in each brace plug graduated tube, shake up, in 60 DEG C of water-baths, heat 30min, be cooled to room temperature after taking-up, measure; Use 10mm cuvette, at wavelength 412nm place, measure absorbance, with absorbance and corresponding formaldehyde quality drawing standard working curve;
Step 2, the mensuration of content of formaldehyde: take 2g water paint sample, be placed in 50mL volumetric flask, and the scale of dilute with water, shake up; Use pipette, extract 10mL, move into and added in the 100mL cucurbit of 10mL distilled water, and in cucurbit, add a small amount of zeolite, instill a defoamer, first should add appropriate water logging in the bottle of collection cut and not have condenser pipe to export; Add thermal distillation and collect cut, evaporate to dryness, the cut of collection being transferred in 50mL tool plug graduated tube, being diluted with water to scale, to be measured; Sample to be tested adds 2.5mL diacetone solution, shake up, 30min is heated in 60 DEG C of water-baths, room temperature is cooled to after taking-up, measure the content of formaldehyde: use 10mm cuvette, at wavelength 412nm place, measure absorbance, deduct the absorbance measured by blank test, find the content of formaldehyde in sample from typical curve.
Wherein, described content of formaldehyde is calculated as follows:
Wherein: C-content of formaldehyde, mg/kg
M-from the formaldehyde amount that typical curve checks in, μ g;
W-test the sample size got, g;
F-dilution gfactor.
The volumetric concentration of described diacetone solution is 0.25%, and its collocation method is: claim 25g ammonium acetate, add a small amount of water-soluble solution, add the diacetone that 3mL ice second and 0.25mL newly distill, move in 100mL volumetric flask, be settled to scale with water, adjustment pH=6.0, stores in 2 ~ 5 DEG C.
The collocation method of described formaldehyde standard use solution is: pipette formaldehyde standard reserving solution 10mL, be placed in 1000mL volumetric flask, be diluted with water to scale, store for 2 ~ 5 DEG C.
The collocation method of described formaldehyde standard reserving solution: pipette 20.00mL formaldehyde standard reserving solution and be placed in 250ml iodine flask, add 0.05mol/L iodine solution 25.0mL, immediately dropwise add 1mol/L sodium hydroxide solution to color take off faint yellow, after leaving standstill 15min, add the acid-soluble 11mL acidifying of 1mol/L salt, with the sodium thiosulfate demarcated molten be titrated to faint yellow, add the 1g/100mL starch instruction 1mL of new preparation, continuing to be titrated to blueness has just disappeared for terminal, record consume sodium thiosulfate standard solution volume V1, carry out blank determination simultaneously, record consume sodium thiosulfate standard solution volume V0, be calculated as follows Standardization Concentration of Formaldehyde Standard Solution:
In formula:
V0---the blank volume consuming hypo solution, mL;
V1---demarcate the volume that formaldehyde consumes hypo solution, mL;
---hypo solution concentration, mol/L;
15.0---formaldehyde (1/2HCHO) molal weight;
10.0---formaldehyde standard reserving solution sample volume, mL.
Described hydrochloric acid solution is 1mol/L, described sodium hydroxide solution is 1mol/L, and described iodine solution is 0.05mol/L, and described starch solution is 1g/100mL, described sodium thiosulfate standard solution is 0.1mol/L, and in described formalin, the massfraction of formaldehyde is 37%.The present embodiment 1 is with not add test result compared with defoamer method as shown in table 1 below:
Table 1
Note: above-mentioned data are the time in step 2 in embodiment 1 required for still-process.
To sum up data illustrate, adding of the inventive method defoamer not only obviously can shorten distillation time, greatly can also improve distilling effect.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (6)
1., by a method for content of formaldehyde in diacetone spectrophotometry water paint, it is characterized in that, described method comprises the steps:
Step 1, the drafting of typical curve: get 8 50mL tool plug graduated tubes, add 0.00 respectively, 0.02,0.50,1.00,3.00,5.00,8.00,10.00mL formaldehyde standard uses solution, add water to 50mL, add 2.5mL diacetone solution again in each brace plug graduated tube, shake up, in 60 DEG C of water-baths, heat 30min, be cooled to room temperature after taking-up, measure; Use 10mm cuvette, at wavelength 412nm place, measure absorbance, with absorbance and corresponding formaldehyde quality drawing standard working curve;
Step 2, the mensuration of content of formaldehyde: take 2g water paint sample, be placed in 50mL volumetric flask, and the scale of dilute with water, shake up; Use pipette, extract 10mL, move into and added in the 100mL cucurbit of 10mL distilled water, and in cucurbit, add a small amount of zeolite, instill a defoamer, first should add appropriate water logging in the bottle of collection cut and not have condenser pipe to export; Add thermal distillation and collect cut, evaporate to dryness, the cut of collection being transferred in 50mL tool plug graduated tube, being diluted with water to scale, to be measured; Sample to be tested adds 2.5mL diacetone solution, shake up, 30min is heated in 60 DEG C of water-baths, room temperature is cooled to after taking-up, measure the content of formaldehyde: use 10mm cuvette, at wavelength 412nm place, measure absorbance, deduct the absorbance measured by blank test, find the content of formaldehyde in sample from typical curve.
2. the method with content of formaldehyde in diacetone spectrophotometry water paint as claimed in claim 1, it is characterized in that, described content of formaldehyde is calculated as follows:
Wherein: C-content of formaldehyde, mg/kg
M-from the formaldehyde amount that typical curve checks in, μ g;
W-test the sample size got, g;
F-dilution gfactor.
3. the method with content of formaldehyde in diacetone spectrophotometry water paint as claimed in claim 1, it is characterized in that, the volumetric concentration of described diacetone solution is 0.25%, its collocation method is: claim 25g ammonium acetate, add a small amount of water-soluble solution, adds the diacetone that 3mL ice second and 0.25mL newly distill, move in 100mL volumetric flask, be settled to scale with water, adjustment pH=6.0, stores in 2 ~ 5 DEG C.
4. the method with content of formaldehyde in diacetone spectrophotometry water paint as claimed in claim 1, it is characterized in that, the collocation method of described formaldehyde standard use solution is: pipette formaldehyde standard reserving solution 10mL, be placed in 1000mL volumetric flask, be diluted with water to scale, store for 2 ~ 5 DEG C.
5. the method with content of formaldehyde in diacetone spectrophotometry water paint as claimed in claim 4, it is characterized in that, the collocation method of described formaldehyde standard reserving solution: pipette 20.00mL formaldehyde standard reserving solution and be placed in 250ml iodine flask, add 0.05mol/L iodine solution 25.0mL, immediately dropwise add 1mol/L sodium hydroxide solution to color take off faint yellow, after leaving standstill 15min, add the acid-soluble 11mL acidifying of 1mol/L salt, with the sodium thiosulfate demarcated molten be titrated to faint yellow, add the 1g/100mL starch instruction 1mL of new preparation, continuing to be titrated to blueness has just disappeared for terminal, record consume sodium thiosulfate standard solution volume V1, carry out blank determination simultaneously, record consume sodium thiosulfate standard solution volume V0, be calculated as follows Standardization Concentration of Formaldehyde Standard Solution:
In formula:
V0---the blank volume consuming hypo solution, mL;
V1---demarcate the volume that formaldehyde consumes hypo solution, mL;
---hypo solution concentration, mol/L;
15.0---formaldehyde (1/2HCHO) molal weight;
10.0---formaldehyde standard reserving solution sample volume, mL.
6. the method with content of formaldehyde in diacetone spectrophotometry water paint as claimed in claim 5, it is characterized in that, described hydrochloric acid solution is 1mol/L, described sodium hydroxide solution is 1mol/L, described iodine solution is 0.05mol/L, described starch solution is 1g/100mL, and described sodium thiosulfate standard solution is 0.1mol/L, and in described formalin, the massfraction of formaldehyde is 37%.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105866114A (en) * | 2016-05-04 | 2016-08-17 | 合肥聚合辐化技术有限公司 | Determination method of formaldehyde content in waterborne coating adhesive |
| CN107300556A (en) * | 2017-06-12 | 2017-10-27 | 浙江检创检测技术服务有限公司 | A kind of assay method of formaldehyde in textile |
| 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 |
| CN107505314A (en) * | 2017-08-14 | 2017-12-22 | 山东南山铝业股份有限公司 | A kind of assay method of aluminium alloy cover coating material free formaldehyde |
| CN107957400A (en) * | 2017-12-13 | 2018-04-24 | 中山永恒检测科技有限公司 | A kind of water-based emulsion adhesive free formaldehyde demulsification detection reagent and the free formaldehyde detection method using the reagent |
| CN108426847A (en) * | 2018-03-30 | 2018-08-21 | 吉林冠界生物技术有限公司 | A kind of assay method of biological products vaccine residual formaldehyde |
| CN109632775A (en) * | 2018-12-14 | 2019-04-16 | 湖北省兴发磷化工研究院有限公司 | A kind of method of content of formaldehyde in measurement tetrakis hydroxymetyl phosphonium sulfuric |
| CN110849681A (en) * | 2019-11-25 | 2020-02-28 | 中国林业科学研究院木材工业研究所 | 1m3Detection method for comparison test of formaldehyde release amount by climate box method |
| CN113899708A (en) * | 2020-07-07 | 2022-01-07 | 温州交大科技发展有限公司 | Full-automatic intelligent formaldehyde detector based on use peristaltic pump to realize liquid measure circulation |
| CN114324112A (en) * | 2021-12-29 | 2022-04-12 | 昆山矽崴环保设备有限公司 | Method for testing purifying effect of drinking water filter element |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102621139A (en) * | 2012-04-18 | 2012-08-01 | 上海市毛麻纺织科学技术研究所 | Method for determining free formaldehyde in textile by using full-temperature shake flask cabinet |
| CN102706819A (en) * | 2012-06-11 | 2012-10-03 | 江南大学 | Acetylacetone extraction spectrophotometry method for measuring formaldehyde in food |
| CN102827516A (en) * | 2012-08-22 | 2012-12-19 | 福州丽彩装饰材料有限公司 | Environmentally friendly water-based paint capable of removing formaldehyde through reacting and preparation method thereof |
-
2015
- 2015-06-25 CN CN201510358683.2A patent/CN104964937A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102621139A (en) * | 2012-04-18 | 2012-08-01 | 上海市毛麻纺织科学技术研究所 | Method for determining free formaldehyde in textile by using full-temperature shake flask cabinet |
| CN102706819A (en) * | 2012-06-11 | 2012-10-03 | 江南大学 | Acetylacetone extraction spectrophotometry method for measuring formaldehyde in food |
| CN102827516A (en) * | 2012-08-22 | 2012-12-19 | 福州丽彩装饰材料有限公司 | Environmentally friendly water-based paint capable of removing formaldehyde through reacting and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 中国建筑装饰协会信息部，中国建筑装饰协会信息咨询委员会编: "《家庭装饰装修行业技术标准规范汇编》", 30 April 2004, 中国建筑工业出版社 * |
| 夏云生等: "《室内空气质量检测技术》", 31 March 2013, 中国石化出版社 * |
| 沈文洁等: "胶粘剂和涂料蒸馏过程沸溢现象的研究", 《广东化工》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105866114A (en) * | 2016-05-04 | 2016-08-17 | 合肥聚合辐化技术有限公司 | Determination method of formaldehyde content in waterborne coating adhesive |
| 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 |
| CN107300556A (en) * | 2017-06-12 | 2017-10-27 | 浙江检创检测技术服务有限公司 | A kind of assay method of formaldehyde in textile |
| CN107505314A (en) * | 2017-08-14 | 2017-12-22 | 山东南山铝业股份有限公司 | A kind of assay method of aluminium alloy cover coating material free formaldehyde |
| CN107957400A (en) * | 2017-12-13 | 2018-04-24 | 中山永恒检测科技有限公司 | A kind of water-based emulsion adhesive free formaldehyde demulsification detection reagent and the free formaldehyde detection method using the reagent |
| CN108426847A (en) * | 2018-03-30 | 2018-08-21 | 吉林冠界生物技术有限公司 | A kind of assay method of biological products vaccine residual formaldehyde |
| CN109632775A (en) * | 2018-12-14 | 2019-04-16 | 湖北省兴发磷化工研究院有限公司 | A kind of method of content of formaldehyde in measurement tetrakis hydroxymetyl phosphonium sulfuric |
| CN110849681A (en) * | 2019-11-25 | 2020-02-28 | 中国林业科学研究院木材工业研究所 | 1m3Detection method for comparison test of formaldehyde release amount by climate box method |
| CN113899708A (en) * | 2020-07-07 | 2022-01-07 | 温州交大科技发展有限公司 | Full-automatic intelligent formaldehyde detector based on use peristaltic pump to realize liquid measure circulation |
| CN114324112A (en) * | 2021-12-29 | 2022-04-12 | 昆山矽崴环保设备有限公司 | Method for testing purifying effect of drinking water filter element |
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