ICS87.080
Classification number: A17
Registration number: 23386-2008
Light Industry Standard of the People's Republic of China
QB/T2929-2008
Limits and determination method of residual solvent in solvent-based printing ink
Quality and Specification
Published on 2008-02-01
Special chapter for information
National Development and Reform Commission of the People's Republic of China Implemented on 2008-07-01
wwW.bzxz.NetThis standard is proposed by China Light Industry Federation. Foreword
QB/T2929-2008
This standard is under the jurisdiction of the National Technical Committee for Standardization of Printing Inks. The drafting units of this standard are: National Quality Supervision and Inspection Center for Printing and Decoration Products, Tianjin Toyo Ink Co., Ltd., Zhejiang Yongzai Chemical Co., Ltd., Hanghua Ink Chemical Co., Ltd., Shanghai DIC Ink Co., Ltd., Xuzhou Zhongqiao Ink Chemical Co., Ltd., Shanxi Xiongying Ink Industrial Co., Ltd., Yip's Ink (Shanghai) Co., Ltd., Huangshan Xinli Ink Chemical Factory, Ink/Coating Center of Polymer Research Institute, School of Chemistry, Zhongshan University of Science and Technology.
The main drafters of this standard are: Zhang Liming, Zhou Mei, Wu Min, Huang Ronghai, Shen Jian, Yu Peiyu, Zhao Yinghua, Wu Shaotang, Luo Pingping, and Wang Xiaomei.
This standard is published for the first time.
1 Scope
Limits of residual solvent content of solvent-based inks and their determination methods This standard specifies the limits of residual solvent content of solvent-based inks and their determination methods. This standard applies to solvent-based ink products. 2 Principle
QB/T2929—2008
The oil-climbing sample is made into an ink print of a certain area and thickness, and placed in a sealed balance bottle. Under certain time and temperature conditions, the solvent on the surface of the ink print evaporates. When equilibrium is reached, the gas at the top of the bottle is measured by gas chromatograph to calculate the solvent residue per unit area, expressed in milligrams per square meter (mg/m2). 3 Technical requirements
The solvent residue of solvent-based inks shall comply with the provisions of Table 1. Table 1
Total solvent residue
Total benzene, toluene and xylene residue
Determination method
4.1 Materials and tools
Residue/(mg/m2)
4.11 Biaxially oriented polypropylene film: After electrospark treatment, the surface tension is not less than 38x105N/cm: paper or other printing substrates suitable for solvent-based inks.
4.1.2 20mL headspace injection bottle.
4.1.3 10u micro-injector.
4.2 Tools for sample preparation
Chromatography, etc.
4.3 Measuring instruments
Gas chromatograph: with hydrogen flame detector (with headspace auto-injector)4.4 Reagents
4.4.1 Benzene (analytical grade).
4.4.2 Toluene (analytical grade)
Xylene (analytical grade)5
4.44 Ethanol (analytical grade).
Isopropanol (analytical grade).
4.4.6 Ethyl acetate (analytical grade)
Propyl acetate (analytical grade).
Butyl acetate (analytical grade).
Acetone (analytical grade)
QB/T2929—2008
4.4.10 Butanone (analytical grade)
4.4.11 Propylene glycol ethyl ether (analytical grade)
4.4.12 Propylene glycol methyl ether (analytical grade)
4.4.13 Other volatile solvents (analytical grade). 4.5 Preparation of standard solvent curve
4.5.1 For each standard solvent, use a 10uL micro-injector to inject 1uL of standard drop into 5 headspace injection bottles, then keep the temperature at 80C for 30min in the headspace automatic injector and take it out, then extract 0.2mL, 0.4mL, 0.6mL, 0.8mL, 1mL of gas from the top of 5 headspace injection bottles and inject them separately for testing, so as to obtain the standard peak area of different injection amounts of the standard solvent. 4.5.2 The injection volume of standard solvent is calculated according to formula (1): DxV
Wherein:
injection volume of standard solvent, in milligrams (mg); density of solvent, in grams per milliliter (g/mL); the amount of standard solvent injected into the headspace injection bottle
in microliters (μl):
headspace injection bottle capacity, in milliliters (mL): the amount of standard sample injected into the instrument, in milliliters (mL. (1)
4.5.3 The area of each chromatographic peak obtained is used as the ordinate, and the corresponding solvent injection volume is The sample volume w is marked as the horizontal axis to make the standard solvent curve of the solvent. 4.6 Chromatographic conditions
4.6.1 Quartz capillary column (30mx0.32mmx0.3um) Filler: PEG-20M (any chromatographic column that can effectively separate the solvents in 4.4 can be used). 4.6.2 Environmental temperature, humidity and instrument conditions
Sample preparation environmental conditions: temperature (25+1) C, sea degree (65±5)% column temperature 35℃ maintained for 12min,
Vaporization chamber: 145℃.
Then raise the temperature to 95℃ at 4℃/min and keep it for 10min. FID (oxygen flame ionization detector) 160℃ 4.7 Operation method and calculation
4.7.1 Take a proper amount of ink and use a colorimeter or other tools to coat and prepare the sample. The sample thickness is controlled at (35+5)um. After the sample is prepared, hang it in the air and let it stand for 2h. Cut the sample into 4 parts with a total area of 200cm, and immediately place it in a 20mL headspace injection bottle and cover it with a bottle cap. 4.7.2 Test temperature
Place the sample bottle in the headspace injector at a constant temperature of 80℃ 30min. 4.7.3 The automatic sampler captures 1mL of the gas from the sample in the bottle and injects it into the chromatograph for testing to obtain the peak area of each corresponding solvent in the sample. 4.7.4 According to the peak area of each solvent contained in the sample, find the content of the corresponding solvent (P) on the standard curve and calculate the residual amount of each solvent according to formula (2).
Where:
P×10*
The residual amount of each solvent in the sample, in milligrams per square meter (mg/mThe actual number of milligrams of each solvent in the sample, in milligrams (m ) Sample area, in square centimeters (cm): Sample volume, in milliliters (mL):
Sample bottle capacity, in milliliters (mL) 4.8 Results
The total residual solvent content of the sample is expressed as the sum of the average values of more than two determinations of each solvent. QB/T2929-2008
Note: The instrument model used is Aglient6890N gas chromatograph. The laboratory can choose appropriate working conditions according to other instrument types. 5 Test report
Test report The report shall include at least the following contents: a) Name of the product under test:
b) Test basis or inspection method
c) If the number of tests exceeds two, indicate the number of tests: d) Test results:
e) Any experimental conditions that deviate from the test basis; f) Any operation that is not specified in this standard and may affect the results g) Test date:
h) Test instrument
1. GB/T10004 Retort-resistant composite film and bag
2. QBT2024 Gravure composite plastic Film ink QB/T2929-2008
References
People's Republic of China
Light industry standard
Limits of residual solvents for solvent-based inks
and their determination methods
QB2929-2008
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