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This standard is developed in accordance with the rules given in GB/T 1.1-2009.
This standard was proposed by the China Petroleum and Chemical Industry Association.
This standard is under the jurisdiction of SAC/TC 134 Technical Committee on Dyestuff of Standardization Administration of China.
Determination of aniline derivatives in dye products
Warning: the personnel using this standard shall have practical experience in standard laboratory work. This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any national regulatory conditions.
1 Scope
This standard specifies the methods for determining 19 kinds of aniline derivatives (see Annex A) in dye products.
This standard is applicable to determination of 19 kinds of aniline derivatives in various dosage forms of dye products.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
GB/T 8170-2008 Rules of rounding off for numerical values & expression and judgement of limiting values
3 Theory
Taking dichloromethane as the extracting agent, extract the specimen with ultrasonic wave, then analyze the extract liquor qualitatively with gas chromatography-mass spectrometer, and quantify it with internal standard method.
4 Determination method
4.1 General requirements
Unless otherwise specified, only recognized analytically pure reagents shall be adopted. The inspection result shall be judged according to the rounding-off value comparison method specified in 4.3.3 of GB/T 8170-2008.
4.2 Reagents and materials
4.2.1 Aniline derivative mixed standard: 1,000 mg/L, dissolved in toluene.
4.2.2 Dichloromethane.
4.2.3 Aniline derivative standard stock solution: 1,000 mg/L, dissolved in dichloromethane.
4.2.4 Internal standard 1: 1,2-dichlorobenzene-d4, 2,000 mg/L, dissolved in methanol.
4.2.5 Internal standard 2: phenanthrene-d10, 1,000 mg/L, dissolved in dichloromethane.
4.2.6 Mixed internal standard working solution: take appropriate amounts of internal standard 1 and internal standard 2 and dilute them with dichloromethane to a concentration of 100 mg/L.
4.3 Instruments and apparatus
4.3.1 Gas chromatograph-mass spectrometer (GC-MSD).
4.3.2 Chromatographic column: with a length of 60 m, an inner diameter of 0.25 mm and a film thickness of 0.25 μm.
4.3.3 Stationary phase: (5% phenyl) methylpolysilicone, or stationary phases with equivalent separating capacity.
4.3.4 Ultrasonic generator.
4.3.5 Chromatographic working station
4.3.6 Extractor: 25 mL, made of hard glass, tubular, with grind and stopper.
4.3.7 Micro-column measuring syringe or autosampler.
4.3.8 PTFE filter head: 0.45 μm.
4.4 Chromatographic analysis conditions
As the test result depend on the instrument used, it is not possible to give general parameters for chromatographic analysis. The following parameters (see Table 1) have proven to be suitable for the test.
Foreword i
1 Scope
2 Normative references
3 Theory
4 Determination method
5 Detection limit, precision and recovery rate
6 Test report
Annex A (Normative) Information of 19 kinds of aniline derivatives and 2 kinds of internal standards
