AB DPT Method 1020 DuPont Polyester Technologies DPT Method 1020 Date of Issue: December 2000 ‘The gas chromatographic determination of methyl acetate, methanol, propyl acetate propanol, toluene and pXylene 1 Scope The method is for determination of the concentration of methyl acetate, methanol, propy! acetate propanol, toluene and pXylene at a detection limit of 0.01 % in acetic acid solutions 2 Summary ‘The sample is analysed by gas chromatography using 2 flame ionisation detector (FID), Quantitative results are achieved by measuring the areas of all the peaks of interest detected and using an internal standardisation procedure, 3 Safety instructions Hydrogen is explosive over a wide range of concentrations. All pipework associated with the hydrogen supply to the gas chromatograph must be checked for leaks, and rectified if found. The chemicals used in this method have varying degrees of hazards and reference to hazard data sheets should be undertaken. Handling of reagents in a fume cupboard is recommended. 4 Reagents and materials Chemicals and column materials 4.1 Methyl acetate > 99% purity 4.2 Acetic acid > 99% purity 4.3 Propylacetate > 99% purity . 4.4 Propanol > 99% purity 4.5 Toluene > 99% purity 46 pXylene > 99% purity 4.7 Volumetric flasks, 50 ml. snoenieeP/5 2 Pace 1 REV: A DEC2000 (CONFIDENTIAL ‘Copyrighe22000 E.. du Ponte Nemours an Company, Alighis reserved"rN DPT Method 1020 4.8 Pipettes, various. 4.9 Balance, capacity 200 g weighing to 0.1 mg. 5 Apparatus 5.1 Gas chromatograph fitted with an FID, heated injector and detector. 5.2 Data handling system 5.3 Column ~ Chrompak CP-WAXS8 (FFAP)-CB or equivalent 25 m * 0.25 mm ‘The column should be packed using the suction with vibration technique to ensure that the ‘maximum amount of packing is in the column, Install the column in the gas chromatograph and condition the packing by purging with carrier gas (nitrogen) for 24 hours at 250° C 5.4 FID fuel gases - Air GC grade ex purifier at 24 psig - Hydrogen GC grade ex generator at 55 Carter gas - Nitrogen, HP grade. 5.5 Syringe, 10 iL Hamilton with 5 em needle. 6 Sample preparation Mix the sample well, filter if required 6.1 Sample size: 0.2u 7 Gas chromatograph conditions Install the column into the GC, following the manufacturers instructions. Do not connect the end of the column to the detector. Apply the carrier gas inlet pressure to the column, check for leaks and that the gas is flowing through the column. 71 Colnmn temperature initial 70°C Iso-time initial 3.0 min Ramp rate 2 20°C/min ‘Column temperature final : 140°C Iso-time 2 5 min Injection temperature 250°C Detection temperature 250°C am Nitrogen flow 450 ml / min Equilibration time 0.0 min a FIDSENS ye High FIDZERO On + att BY swexecmea maces Rev ADECZIn0 | CONROENTIAL “Copyrgnt©2000 = cu Pont ds Nemours nd Company. Al rights ressDPT Method 1020 ‘These parameters represent one set of conditions that have provided repeatable results. Due to differences in instruments one or more of these stated parameters may require adjustment. “The parameters should therefore be regarded as guides by the analyst in establishing optimum conditions which result in well shaped peaks with adequate resolution of the components. A chromatogram should be produced which closely approximates typical results 8 Calibration 8.1 Preparation of standards 8.1.1 Standards should be prepared to cover the expected range of concentrations of each ‘component to be measured. Five standard solutions are prepared at 0.2 %, 0.4% 0.6%, 0.8% and 1.0% of each component in acetic acid and a calibration curve is produced. Each time the analysis is performed the 0.5% standard is checked to ensure that the calibration is correct. 8.2 Analysis of standards Inject 0.21 of each standard into the chromatograph. ‘The area of cach component will be recorded by the data handling system, which will automatically construct % wiw calibration curves. For each calibration curve the correlation coefficient, r, should lie between 0.99 and 1.00. 9 Analysis of samples Analyse samples in accordance with the instrument manufacturers operating instructions. 0.2uL of each sample is injected into the chromatograph 10 Performance check Inject 0.5 4 of one of the calibration standards into the GC everyday. If the updated correlation coefficients do not lie between 0.99 and 1.0 then carry out a new calibration 11 Calculation ‘Components will be automatically determined by the data handling system and reported as % wlw component to nearest 0.01% wlw. For further information on the calculation refer to the Instrument manufacturers operating instructions ees oa a paces REV: ADECZ000 CconrIvENTIAL “Copyight®2000 Edu Pont de Nemours and Company. Al rights reservedqb DPT Method 1020 HOBHDL TH WILLA Usiv NLSLVLZDY TALNO-W #31¥i30¥ TALMDSI‘O}D¥ 9139¥-21¥L30" THB % CCONFIDENTIAY “Copyaght©2000 Edy Pont de Nemours and Company. Alrights reserves"