1. The purpose of triethylamine detection Standardize the quality of raw material triethylamine inspection operations. 2. Application scope of triethylamine detection It is suitable for the quality inspection of triethylamine for synthesis. 3. Reference standards for triethylamine testing (1) The People's Republic of China Chemical Industry Standard HG / T2721-95 (2) Internal control quality standards of triethylamine enterprises 4. Triethylamine testing product name Triethylamine Molecular formula: (CH3CH2) 3N Molecular weight: 101.19 5. Responsibilities of triethylamine detection gas chromatograph The inspector of the Quality Inspection Department is responsible for the implementation of this document. When an abnormal situation occurs, the person in charge of the laboratory should be notified in time; Measures. 6. Quality standards for the detection of triethylamine products by gas chromatograph Project statutory standards (first-class product standards) internal control standards remarks Properties: colorless transparent liquid, no mechanical impurities, colorless transparent liquid, no mechanical impurities-- Identification In the gas chromatogram, the retention time of the main peak of the sample and the reference substance should be consistent. In the gas chromatogram, the retention time of the main peak of the sample and the reference substance should be consistent. Triethylamine content ≥98.8% ≥99.0%- Water content≤0.4% ≤0.3%- 7. Gas chromatograph test method for triethylamine 7.1 Character Measured by sensory method, the product should be colorless and transparent liquid, and should be free of mechanical impurities. 7.2 Identification (gas chromatography) 7.2.1 Chromatographic conditions Chromatographic conditions under the same content determination. 7.2.2 Operation method Precisely measure 0.5ul of the triethylamine reference substance and inject it into the chromatograph, and record the chromatogram as the reference spectrum. The spectrum under the content determination is used as the spectrum of the test product, and the retention time of the main peak of the test product and the reference product should be consistent. 7.3 Moisture 7.3.1 Main instruments and materials KF moisture analyzer, KF platinum electrode. 7.3.2 Reagent methanol (chemically pure), KF reagent 7.3.3 Calibration of KF reagent: Add an appropriate amount of methanol (the exposed end of the immersed electrode) to the reaction bottle of the titrator, titrate with KF reagent to the end under stirring, take about 10 to 30 mg of pure water, weigh accurately, place in the titration bottle, and immediately titrate with KF reagent , Titrate to the end and record the amount of KF reagent (V). Calculate the titer of KF reagent according to the following formula: T = M / V In the formula: T: KF reagent titer mg / ml; M: quality of added water (mg); V: Dosage (ml) of KF reagent when titrating water. Calibrate three times in parallel, and the relative deviation of the three titers is not more than 0.5%. 7.3.4 Determination of moisture in the sample Titrate the appropriate amount of methanol (the exposed end of the submerged electrode) in the reaction flask to the end. Take about 5ml of the test sample, accurately measure it, calculate its mass, quickly add it to the reaction bottle, titrate to the end point, and record the amount of KF reagent, measured in parallel twice with the same method, the relative deviation between the two results is not more than 3.0%, Take the average. 7.3.5 Calculation of moisture in the sample: X = (V1 × T) / (V2 × Ï Ã— 1000) × 100% In the formula: X- mass percentage of water in the sample,%; V1- The amount of Karl Fischer reagent used when titrating the sample (ml); T-Karl Fischer reagent titer (g / ml); V2- Volume of sample added (ml); Ï-Density (g / cm3) of the sample at 20 ° C. 7.4 Triethylamine content 7.4.1 Instrument and chromatographic conditions 7.4.1.1 Instruments: gas chromatograph (hydrogen flame detector) 7.4.1.2 Chromatographic conditions (a) Column: a capillary column with polyethylene glycol as the stationary phase; (b) Carrier gas and flow rate: nitrogen, 3ml / min; (c) Column temperature: 70 ° C; injector temperature: 150 ° C; detector temperature: 150 ° C; injection volume: 0.5 μl. 7.4.2 Operation steps 7.4.2.1 Preparation of standard solution Precisely weigh 30ml (about 21.9000g) of the triethylamine reference substance into a 50ml volumetric flask and mix as a standard solution 7.4.2.2 Determination Take 0.5ul of the prepared standard solution and record the chromatogram as a control spectrum. Take 0.5μl sample, inject two consecutive times, record the chromatogram, the relative deviation of the area of ​​the two main peaks should not be greater than 2.0%, and the measurement result is based on the average of two injections. 7.4.3 Calculate the purity of triethylamine according to the area normalization method, and calculate according to the anhydrous substance. The calculation formula is as follows: Triethylamine purity = (S triethylamine / S total) (1-water%) In the formula: S triethylamine: the peak area of ​​triethylamine in the sample chromatography; S Total: The total area of ​​each chromatographic peak in the sample chromatogram. The measurement results are based on the average of two injections.
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