HG/T 2621-1994 Determination of residual phenol content in phenolic resin by gas chromatography HG/T2621-1994 standard download decompression password: www.bzxz.net

Chemical Industry Standard of the People's Republic of China
HG / T 2621 -94
ISO 8974---1988
Gas chromatography method for determination
Residual phenol content in phenolic resin
Published on April 13, 1994
Ministry of Chemical Industry of the People's Republic of China
Implementation from January to January 1, 1995
Chemical Industry Standard of the People's Republic of China
Gas chromatography method for determination
Residual phenol content in phenolic resin
HG / T 2621 —94
ISO 8974-1988
This standard is equivalent to the international standard IS08974-1988 "Determination of residual phenol content in plastic phenolic resin by gas chromatography" Subject content and scope of application
This standard specifies the method for determining the residual phenol content in phenolic resin by gas chromatography. When determining trace phenol [<0.5% (m/m)], this standard must be improved.
This standard is not applicable to phenolic resins because phenol exists in the form of phenolate and cannot be completely eluted. Important note: The following instruments and conditions are recommended. However, if other instruments and conditions (such as other detectors and capillary columns) can obtain the same results with the same accuracy, they can also be used.
2 Principle
The sample is dissolved in an appropriate solvent and the phenol content is determined by gas chromatography. 3 Materials
3.1 Carrier gas: nitrogen.
3.2 Detector gas: hydrogen and air,
3.3 Internal standard: phenol-free m-cresol or phenol-free anisole, sample: In cases where interference may occur, such as the presence of cresol in the resin, anisole should be used as the internal standard. 4 Instruments
4.1 Chromatograph
Any laboratory gas chromatograph equipped with a flame ionization detector is suitable. 4.2 Syringe
Micro syringe: "μI..
4.3 Chromatographic column
4.3.1 Column tube
Material: Stainless steel:
Length: 2m;
Inner diameter: 2.2 mm.
4.3.2 Filler
4.3.2.1 Carrier: ChromosotbW/AW/DMCS, particle size 150~180um (80~100 ).4.3.2.2 Fixing liquid: For anhydrous products, 10gCarbowax20M is contained in every 100g dry carrier. For products containing water or aqueous solution, it is recommended to use a non-polar fixing liquid, such as silicone rubber OV1701.4.3.3 Aging of chromatographic column
China Approved by the Ministry of Chemical Industry of the People's Republic of China on April 13, 1994, and implemented on January 1, 1995
150t nitrogen flow for 15h.
4.4 Detector
Flame ionization detector.
4.5 Recorder
Potentiometer type.
5 Operating steps
5.1 Operating conditions
5.1.1 Injector
Temperature: 200
5.1.2 Chromatographic column
5. 1.2.1 Temperature: 150c.
5.1.2.2 Carrier gas flow rate: 30mL/min.
5.1.3 Detector
Hydrogen: 30mL/min:
Air: 250mL/min
5.1.4 Recorder
Full scale 1 mV
5.2 Calibration
HG/T 2621—94
Relative correction factor The correction factor is determined by the mass band of phenol relative to aldehyde in m-cresol or benzene. The correction factor should be determined using a standard mixture with a proportion close to that of the solution being analyzed. When operating within the dynamic linear range of the detector, the correction factor is valid for all concentrations. F (2 / 1) =
Where: F (2/ 1) -
-Relative correction factor, expressed as the mass of phenol relative to m-cresol or anisole; mass concentration of m-cresol or anisole;
c2-mass concentration of phenol;
A,-peak area of ​​m-cresol or anisole;
5.3 Determination
5.3.1 Preparation of test solution
Peak area of ​​phenol,
It is best to use acetone as solvent to dissolve the sample: in some cases, methanol or toluene that does not affect chromatographic separation can be used. Or 50% (V/V) toluene/acetone mixture as solvent - Use phenol-free m-cresol as internal standard. If the resin contains other substances, especially m-cresol, it will interfere with the use of m-cresol as internal standard. In this case, benzaldehyde without phenol should be used as internal standard. Note: Whether dilution is required depends on the required concentration. For example, when the concentration is 0.5%~5% (m/m), weigh 3g resin (mg), 0.25g m-cresol or benzaldehyde (m), and dissolve them in 10.00mL acetone.
5.3.2 Injection
Use a micro syringe to inject about 4L of the solution prepared in 5.3.1. 5.3.3 Record
Record the chromatogram and measure the peak area with a planimeter or integrator. 2
Expression of results
6.1 Calculation method
HG/T 2621--94
Calculate the residual phenol content according to the following formula and express it as mass fraction. m
In the formula:
× F(2/1) ×bzxz.net
mo mass of sample, g;
× 100
amount of internal standard (m-cresol or benzyl alcohol), g; m,
F(2/1), A, A,—5.2.
stone.2 Precision (test error)
6.2.1 Residual phenol ≤2% (m/m)
Repeatability 0.1% (m/m);
Reproducibility 0.2% (m/m).
6.2.2 Residual phenol>2% (m/m)
Repeatability: 5% (relative);
Reproducibility: 10% (relative).
7 Test report
The test report should include the following:
Indicate that this standard is adopted;
All identifications of the test resin;
Test conditions different from the specified conditions:
Test results specified in 6.
Additional remarks:
This standard was proposed by the Technical Supervision Department of the Ministry of Chemical Industry of the People's Republic of China. This standard is under the jurisdiction of the Chemical Method Branch of the National Plastic Standardization Technical Committee. This standard was drafted by the Shanghai Import and Export Commodity Inspection Bureau of the People's Republic of China, and the main drafters of this standard were Zhu Zongrui, Chen Qing, and Lu Shunshu. (2)
People's Republic of China
Chemical Industry Standard
Determination of Residual Phenol in Phenolic Resin by Gas Chromatography
HG/T 2621-94
ISO 8974-1988
Editor: Chemical Industry Standard Editorial Department
(Institute of Standardization, Ministry of Chemical Industry)
Postal Code: 100011
Printing: Institute of Standardization, Ministry of Chemical Industry
Copyright reserved. No reproduction allowed
Format: 8B0×12301/16 Printing Sheets: 4 Number of Lots: 600G First Edition: October 1994
First Printing: October 1994
Number of A: 1-500
Cost: RMB 2.70
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