Some standard content:
ICS87.060
Chemical Industry Standard of the People's Republic of China
HG/T3608—1999
Polyester polyurethane coatings for woodenware
Polyester polyurethane coatings for woodenware1999-04-20 Issued
2000-04-01 Implementation
State Administration of Petroleum and Chemical Industry
W.bzsoso.cOIHG/T3608—1999
In recent years, polyester polyurethane coatings for woodenware (trade name PU polyester wood coatings) have developed rapidly in my country, but the national standard or industry standard for this product has not yet been formulated. In order to stabilize and improve the quality of this product and adapt to the needs of international trade, technology and economic exchanges as soon as possible, this standard is specially formulated.
This standard is formulated based on the product quality of major domestic manufacturers of polyester polyurethane wood coatings. The products included in this standard are divided into three categories: polyester polyurethane varnish (glossy, semi-glossy or matte), colored transparent paint (glossy, semi-glossy or matte), and magnetic paint (glossy, semi-glossy or matte). Each category of products is divided into standard products and qualified products. Appendix A of this standard is the appendix of the standard.
Appendix B of this standard is the appendix of the suggestion.
This standard was proposed by the Technical Supervision Department of the former Ministry of Chemical Industry of the People's Republic of China, and this standard is under the jurisdiction of the National Technical Committee for Standardization of Paints and Pigments. The main drafting units of this standard are: Shunde Jinguan Paint Industry Co., Ltd. and Changzhou Paint Chemical Research Institute of the Ministry of Chemical Industry. The main drafters of this standard are: Zhou Weibin, Shi Lei, Liu Jiyuan, and Zhou Xiaogang. 1
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Chemical Industry Standards of the People's Republic of China
Polyester polyurethane coatings for woodenware
Polyester polyurethane coatings for woodenwareHG/T3608—1999
This standard specifies the requirements, test methods, marking, packaging, safety, and sanitation of polyester polyurethane wood coatings. This standard applies to packaged wood coatings composed of the adduct of toluene diisocyanate (TDI) and dimethylolpropane or the trimer of TDI as component A, and the reaction product of polyol and polyacid or its modified product as component B as the base material. 2Cited Standards
The provisions contained in the following standards constitute the provisions of this standard through reference in this standard. When this standard is published, the versions shown are valid. All standards will be revised, and parties using this standard should explore the possibility of using the latest version of the following standards. GB1250—1989 Method for expressing and determining limit values GB/T1724—1979 (1989) Method for determining the fineness of paint GB/T1725—1979 (1989) Method for determining the solid content of paint) Method for determining the hiding power of paint
GB/T1726—1979 (1989)
GB/T1727—1992 Paint film—General preparation method GB/T1728—1979 (1989) Method for determining the drying time of paint film and putty film GB/T1768—1979 (19 89）Determination of abrasion resistance of paint film GB3186—1982 (1989)
Sampling of coating products (neqISO1512:1974) GB/T4893.3—1985 Determination of dry heat resistance of paint film on furniture surface GB/T6682—1992 Specification and test method for water used in analytical laboratories (eqvISO3696:1987) GB/T6739—1996 Determination of hardness of coating film by pencil Standard test panel for paint and varnish (eqvISo1514:1984) GB/T9271—19 88
GB/T9274—1988
Determination of resistance of paints and varnishes to liquid media (eqvISO2812:1974)GB9278—1988Coating sample condition adjustment and test temperature and humidity (eqvISO3270:1984)GB/T9286—1998
GB/T9750—1988
GB/T9754—1988
Scratch test of paint and varnish films (eqvISO2409:1972)Coatings Product packaging mark
Determination of 20°60° and 85° specular gloss of paint and varnish without metallic pigments (eqvISO2813:1978)
GB/T13452.2—1992Determination of film thickness of paint and varnish (eqvISO2808:1974)GB/T13491—1992
2 General rules for packaging of coating products
3 Product classification and grading
Products are divided into Class 1: varnish, Class 2: colored transparent paint, Class 3: enamel. Each class of products is divided into first-class products and qualified products. 4 Requirements
Products should meet the requirements listed in Table 1.
Approved by the State Administration of Petroleum and Chemical Industry on April 20, 1999, and implemented on April 1, 2000
Appearance of original paint
Semi-gloss or matte
Color and appearance of paint film
Solid content, %
Component A
Component B
Fineness um
Component A
Component B: glossy
Semi-gloss or matte
Hiding power (component B), g/m
Other colors
Drying time,||t t||Surface dry, min
Actually dry, h
Gloss, 600
Semi-gloss or matte
Cross-cut test, grade
Water resistance, 72h
Alcohol resistance (50% ethanol by volume)
Abrasion resistance (750g/500r), g
Dry heat resistance [(90±2)℃, 15min grade
Free TDI content (component A), %
5 Test method
5.1 Sampling
First-class product||tt ||HG/T3608—1999
Requirements in Table 1
Qualified products
Transparent, free of mechanical impurities
Free of mechanical impurities
Smooth and even
No bubbles, wrinkles, or peeling
The paint film is allowed to turn white, and will recover after 2h
No bubbles, wrinkles, or abnormal changes in the paint
Colored transparent paint
First-class products
Qualified products
Transparent, free of mechanical impurities
Free of mechanical impurities|| tt||Smooth and flat, in line with the color difference range
No blistering, no wrinkling, no peeling
, the paint film is allowed to turn white, 2h recovery
No blistering, no wrinkling, no abnormal changes in the paint
Qualified products
Smooth and flat, in line with the color difference range
No blistering, no wrinkling, no peeling
, the paint film is allowed to turn white, 2h recovery
No blistering, no wrinkling, no abnormal changes in the paint
Products are sampled according to GB3186. The sample should be divided into two parts, one for sealed storage for reference, and the other for inspection. If it is found that the product quality does not meet the technical indicators of this standard, the supply and demand parties shall jointly re-sample and re-test according to the provisions of GB3186. If it still does not meet the requirements of this standard, the product shall be unqualified. 5.2 General conditions of the test
5.2.1 The proportion of the components shall be prepared according to the proportion requirements of each manufacturer. 5.2.2 Unless otherwise specified or agreed, the test plates are all tinplate plates and shall comply with the provisions of GB/T9271. 5.2.3 The preparation of the paint film shall be carried out in accordance with the provisions of GB/T1727. 5.2.4 The thickness of the paint film shall be measured in accordance with the provisions of GB/T13452.2. The film thickness used for the test is 20μm±3μm for varnish, 20μm±3μm for colored transparent paint, 23μm±3μm for enamel, and 45μm±5μm for abrasion resistance test. 5.2.5 The state adjustment of the sample and the temperature and humidity of the test shall comply with the provisions of GB9278. When testing gloss and adhesion, the sample shall be dried for 48h; when testing hardness, water resistance, alcohol resistance, abrasion resistance, and dry heat resistance, the sample shall be dried for 7d. 5.3 Appearance of the original paint, color and appearance of the paint film
Visual observation.
5.4 Solid content
Perform according to the provisions of Method A in Chapter 2 of GB/T1725-1979 (1989), and the baking temperature is (120±2)℃. 5.5 Fineness
Perform according to the provisions of GB/T1724.
5.6 Hiding power
According to Method A of GB/T1726-1979 (1989). 5.7 Drying time
Surface drying shall be carried out according to Method B of Chapter 2 of GB/T1728-1979 (1989), and actual drying shall be carried out according to Method A of Chapter 3 of GB/T1728-1979 (1989).
5.8 Gloss
According to GB/T9754.
5.9 Cross-cut test
According to GB/T9286, the cutting interval is 1mm, and the adhesive tape tearing test is not carried out. 5.10 Hardness
According to GB/T6739, the result evaluation: paint film scratch. 5.11 Water resistance
Perform according to the provisions of Chapter 5 of GB/T9274-1988. The test water should meet the requirements of Grade 3 water of GB/T6682. The test temperature is (23±2)℃.
5.12 Alcohol resistance
Perform according to the provisions of Chapter 5 of GB/T9274-1988. Make the plate on a glass plate of 90mmX120mmX(2~3)mm and seal the edge with paraffin.
5.13 Dry heat resistance
Perform according to the provisions of GB/T4893.3. Make the plate on a tinplate of 250mmX200mm×(0.2～0.3)mm. 5.14 Abrasion resistance
Perform according to the provisions of GB/T1768.
5.15 Free TDI monomer
Perform according to the provisions of Appendix A.
5.16 The items listed in this standard are all type inspection items, among which the original paint appearance, paint film color and appearance, solid content, fineness, hiding power, drying time, gloss and adhesion are factory inspection items. Under normal production conditions, type inspection shall be carried out at least once every six months. From the date of production, the storage period of component A is six months, and the storage period of component B is one year. If it exceeds the storage period, it can still be used if it passes the inspection of the manufacturer. 5.17 The judgment of the inspection results in this standard shall be carried out according to the rounded value comparison method in GB1250. 3
Wbzsoso.cOn6 Marking and packaging
6.1 Marking
HG/T3608—1999
In addition to the provisions of GB/T9750, the standard number, net content, quality certification mark, production date, storage period and component ratio shall also be added. 6.2 Packaging
Please follow the provisions of GB/T13491.
7 Safety, hygiene and environmental protection regulations
This product contains organic solvents such as cyclohexanone, xylene and butyl acetate, which are flammable liquids. Component A contains a small amount of free TDI monomer, which is toxic. Therefore, the construction site should comply with the coating operation and safety operation regulations, and take fire prevention, dust prevention, anti-static and anti-toxic measures. 4
W.A1 Scope of application
HG/T3608—1999
Appendix A
(Appendix to the standard)
Determination of free toluene diisocyanate in polyurethane coatings by gas chromatography This appendix applies to the determination of free toluene diisocyanate (TDI) in polyurethane coatings. A2
Principle of the method
The sample is vaporized and passed through a chromatographic column to separate the free toluene diisocyanate to be measured from other components. It is detected by a hydrogen flame ionization detector and quantified by the internal standard method.
A3 Materials
A3.1 Carrier gas: nitrogen purity 99.8%;
A3.2 Fuel gas: hydrogen purity> 99.8%;
A3.3 Fuel-supporting gas: air.
A4 Reagents
A4.1 Ethyl acetate: analytical grade, dehydrated with 5A molecular sieve; A4.2
Tetradecane: chromatographic grade;
Toluene diisocyanate: analytical grade (mixture of 80% 2,4-toluene diisocyanate and 20% 2,6-toluene diisocyanate) A5 Instruments
A5.1 Gas chromatograph: any type of chromatograph that can meet the analytical conditions, equipped with a hydrogen flame ionization detector, the detection limit of benzene D<1X10-°g/s. The inner lining of the vaporizer can be replaced with a glass tube or a section of empty column in front of the column, and it should be cleaned regularly. A5.2 Chromatographic column: stainless steel column with an inner diameter of 2mm and a length of 1m. Column packing:
a Stationary liquid: 7% dimethyl silicone oil SE-30. b Carrier: 102 silanized white carrier, 80 mesh 100 mesh. A5.3 Injector: micro syringe 1μL. A6 chromatographic operating conditions
Internal standard: tetradecane;
Column temperature: 150℃;
Detector temperature: 200℃;
Vaporization chamber temperature: 150℃;
Carrier gas flow rate: nitrogen, 30mL/min;
Injection volume: 0.2μL.
A7 Preparation
A7.1 Preparation of stationary phase
According to the liquid-to-carrier ratio, accurately weigh a certain amount of stationary liquid dimethyl silicone oil, measure a solution of chloroform equivalent to 1.2 times the volume of the carrier, add 5
W.bzsoso.cOmHG/T3608—1999bZxz.net
into a ground-mouth round-bottom flask, connect a ground-mouth condenser, heat and reflux for half an hour, after the stationary liquid is completely dissolved, pour the carrier in, continue to reflux for 1.5h~2h, then cut off the power and remove the condenser, heat to about 50℃ with an infrared lamp in a fume hood, slowly evaporate the solvent until dry, raise the temperature to 60℃, dry for half an hour, sieve and set aside. A7.2 Filling and aging of the chromatographic column
Plug one end of the washed and dried column with a copper wire mesh and connect it to a vacuum pump to evacuate the air. Connect the other end to a funnel, slowly add the prepared stationary phase, and gently tap the chromatographic column until the stationary phase no longer enters. Plug both ends with glass wool. Then connect the column to the chromatograph (without connecting the detector) and pass nitrogen for segmented aging. Aging at 80℃, 120℃, and 160℃ for 2h respectively, and then aging at 185℃ until the baseline is straight. A7.3 Determination of correction factor
A7.3.1 Prepare the internal standard solution: Weigh 1.0g (accurate to 0.0002g) of tetradecane, put it into a dry volumetric flask, and dilute it to 100mL with anhydrous ethyl acetate.
A7.3.2 Prepare toluene diisocyanate solution: weigh 1.0g (accurate to 0.0002g) toluene diisocyanate monomer, put it into a dry volumetric flask, and dilute it to 100mL with anhydrous ethyl acetate. The storage period of this solution is two days. A7.3.3 Prepare standard sample: use a pipette to accurately draw 5mL of internal standard solution and 5mL of toluene diisocyanate solution, inject them into the sample bottle, mix, and shake well.
A7.3.4 According to the chromatographic operating conditions, after the instrument is stabilized, inject the standard sample into the chromatograph and record the chromatogram. A7.3.5 Calculate the relative correction factor of toluene diisocyanate according to formula (A1): mTrAcy
mc,ArDI
Wherein: f——relative correction factor of toluene diisocyanate, mTDr——mass of toluene diisocyanate in standard sample, gmc.——mass of tetradecane in standard sample, g;——peak area of toluene diisocyanate;
Ac——peak area of tetradecane.
·(A1)
The relative correction factor measured by the above test steps can only be used when the difference between the two measurement results is less than 10%. A7.4 Determination of relative retention time
A7.4.1 According to the chromatographic operating conditions, after the instrument is stable, inject the standard sample into the chromatograph and record the retention time of each component. Take tetradecane as the benchmark, calculate the relative retention time of each component, and use this relative retention time for qualitative analysis. A7.4.2 The retention time of each component is as follows: ethyl acetate, toluene diisocyanate, tetradecane. The typical chromatogram of free toluene diisocyanate monomer in polyurethane coating is shown in Figure A1. 1-ethyl acetate, 2-solvent in coating Figure A1 Typical chromatogram of free toluene diisocyanate monomer in polyurethane coating 6
Wbzsoso, cOA8 Determination steps
HG/T3608-1999
A8.1 Determination of sample mass: The sample mass is determined according to the content of free toluene diisocyanate. See Table A1. Table A1
Percentage of free toluene diisocyanate
Weighing amount, g
A8.2 Pour the sample into the sample bottle according to the above table, weigh the mass of the sample by incremental method (accurate to 0.0002g), then add 5mL of internal standard solution with a pipette, add 5mL of anhydrous ethyl acetate with a 10mL measuring tube, and mix and shake well. A8.3 According to the chromatographic operating conditions, after the instrument is stable, inject 0.2mL of the sample prepared according to the above requirements into the chromatograph and record the chromatogram. A8.4 Qualitatively analyze the components according to the relative retention time. A8.5 Measure the peak areas of free toluene diisocyanate and dry tetradecane (internal standard). When measuring manually, measure the peak height and half-peak width. The peak area is obtained by multiplying the peak height by the half-peak width. If a data processor is used, the analysis and calculation program can be pre-programmed for automatic calculation. A9 Calculation
Calculate the percentage of free toluene diisocyanate according to formula (A2) to 0.01%. XTDr%
mcuATDLf
Where: XTDI——mass percentage of free toluene diisocyanate in the sample; -mass of the sample, g;
A10 Precision
-mass of added internal standard tetradecane, g;
-peak area of free toluene diisocyanate, cm2;-peak area of internal standard tetradecane, cm2
Relative correction factor for toluene diisocyanate. Use the following values to judge the reliability of the results. A10.1 Repeatability| |tt||The absolute value of the difference between two repeated measurements by the same operator should not be greater than 0.10%. A10.2 Reproducibility
The absolute value of the difference between the results of the same sample measured by two laboratories should not be greater than 0.20%. A11 Report
(A2)
Take the arithmetic mean of the results of two parallel measurements as the determination result of free toluene diisocyanate in the sample. The reported result is accurate to 0.01%.
Appendix B
(Suggested Appendix)
Construction Reference
B1Construct on the substrate with the prepared primer, mainly by spraying, but also by brushing, and adjust the construction viscosity with polyester polyurethane diluent. B2Before use, prepare the paint liquid according to the ratio specified on the manufacturer's packaging or instruction manual, and filter it with a gauze of specified mesh. The prepared paint liquid is best used up within 4 hours (23±2)℃. 7
W.
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