UOP 555-2010 Trace Impurities in Benzene by GC.pdf
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1、 IT IS THE USERS RESPONSIBILITY TO ESTABLISH APPROPRIATE PRECAUTIONARY PRACTICES AND TO DETERMINE THE APPLICABILITY OF REGULATORY LIMITATIONS PRIOR TO USE. EFFECTIVE HEALTH AND SAFETY PRACTICES ARE TO BE FOLLOWED WHEN UTILIZING THIS PROCEDURE. FAILURE TO UTILIZE THIS PROCEDURE IN THE MANNER PRESCRIB
2、ED HEREIN CAN BE HAZARDOUS. MATERIAL SAFETY DATA SHEETS (MSDS) OR EXPERIMENTAL MATERIAL SAFETY DATA SHEETS (EMSDS) FOR ALL OF THE MATERIALS USED IN THIS PROCEDURE SHOULD BE REVIEWED FOR SELECTION OF THE APPROPRIATE PERSONAL PROTECTION EQUIPMENT (PPE). COPYRIGHT 1970, 1977, 1992, 1996, 2010 UOP LLC.
3、All rights reserved. Nonconfidential UOP Methods are available from ASTM International, 100 Barr Harbor Drive, P.O. Box C700, West Conshohocken, PA 19428-2959, USA. The UOP Methods may be obtained through the ASTM website, www.astm.org, or by contacting Customer Service at serviceastm.org, 610.832.9
4、555 FAX, or 610.832.9585 PHONE. Trace Impurities in Benzene by GC UOP Method 555-10 Scope This gas chromatographic method is for determining individual and total trace hydrocarbon impurities in olefin-free, high-purity benzene. C8 and lower boiling paraffins, naphthenes, toluene, and C8 aromatics ar
5、e determined. The lower limit of quantitation for any single component is 1 mg/kg (mass-ppm). Benzene purity can also be determined by ASTM Method D4492, where the lower detection limit is 50 mg/kg per component. Although benzene is not listed in their scopes, ASTM Methods D2360, D5917, and D7504 ma
6、y also be used to measure impurities in benzene. All of these ASTM Methods determine the non-aromatics as a total whereas this method also provides a distribution. References ASTM Method D2360, “Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography,” www.astm.org ASTM D4307, “Pr
7、eparation of Liquid Blends for use as Analytical Standards,” www.astm.org ASTM Method D4492, “Standard Test Method for Analysis of Benzene by Gas Chromatography,” www.astm.org ASTM Method D5917, “Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography and External Calibration,” ww
8、w.astm.org ASTM Method D7504, “Trace Impurities in Monocyclic Aromatic Hydrocarbons by Gas Chromatography and Effective Carbon Number,” www.astm.org Scanlon, J. T. and Willis, D. E., Journal of Chromatographic Science, 23, 333-340 (1985) UOP Method 999, “Precision Statements in UOP Methods,” www.ast
9、m.org Outline of Method The sample is injected into a gas chromatograph that is equipped with an autoinjector, a fused silica capillary column internally coated with cross-linked methyl silicone, and a flame ionization detector. The concentrations of individual or group impurities are determined by
10、the external standard method of quantitation, wherein peak areas of the sample components are compared to the peak areas of a 2 of 11 555-10 calibration blend analyzed under identical conditions and injection volumes. See Note for an alternative means of calibration and calculation. Apparatus Refere
11、nces to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. Balance, analytical, readable to 0.0001 g Chromatographic column, 50 m of 0.21-mm ID fused silica capillary, internally coated to a film thickness of 0.5-m with cross-linked methyl si
12、licone, Agilent Technologies, Cat. No. 19091S-001 Gas chromatograph, temperature programmable, built for capillary column chromatography, utilizing a split injection system having a glass injection port insert, and equipped with a flame ionization detector that will give a minimum peak height respon
13、se of 10 times the background noise for 1 mg/kg n-octane when operated at the recommended conditions, Agilent Technologies, Model 7890 Data system, electronic, for obtaining peak areas. This device must integrate areas at a sufficiently fast rate so that narrow peaks typically resulting from use of
14、a capillary column can be accurately measured. Agilent Technologies, ChemStation. Hood, fume Leak detector, gas, Alltech Associates, Cat. No. 21-250 Refrigerator, flammable storage or explosion proof Regulator, air, two-stage, high purity, delivery pressure range 30-700 kPa (4-100 psi), Matheson Tri
15、-Gas, Model 3122-590 Regulator, hydrogen, two-stage, high purity, delivery pressure range 30-700 kPa (4-100 psi), Matheson Tri-Gas, Model 3122-350 Regulator, nitrogen, two-stage, high purity, delivery pressure range 30-700 kPa (4-100 psi), Matheson Tri-Gas, Model 3122-580 Sample injector, any syring
16、e or injector capable of injecting a repeatable 0.5-L volume of sample. The use of an automatic injection device is required to achieve necessary repeatable injection volumes. See Note and Appendix. Agilent Technologies, Model 7683. Reagent and Materials References to catalog numbers and suppliers a
17、re included as a convenience to the method user. Other suppliers may be used. Air, zero gas, total hydrocarbons less than 2.0 ppm as methane, local supply Benzene, 99.9% minimum purity, Sigma-Aldrich, Cat. No. 270709. CAUTION: Benzene is especially hazardous. Perform all work with benzene in a fume
18、hood, using appropriate personal protection equipment, as directed by local regulations and the MSDS. Gas purifier, for hydrogen, to remove oxygen and moisture from carrier gas, VICI Mat/Sen, Cat. No. P200-1 3 of 11 555-10 Hydrogen, zero gas, 99.99% minimum purity, total hydrocarbons less than 0.5 p
19、pm as methane, local supply Nitrogen, zero gas, 99.99% minimum purity, total hydrocarbons less than 0.5 ppm as methane, local supply n-Octane, 99.0% minimum purity, Sigma-Aldrich, Cat. No. 74821 Pipets, disposable, Pasteur, VWR, Cat. No. 14673-043 Pipet bulbs, VWR, Cat. No. 15001-362 Syringe, replac
20、ement, for recommended sample injector, 5-L, Agilent Technologies, Cat. No. 5181-1273 Vials, 22-mL, with polyseal-lined caps, VWR, Cat. No. 16087-068 Vials, autosampler, for recommended sample injector, with caps, Agilent Technologies, Cat. No. 5182-0864 Calibration Preparation of Calibration Blend
21、Quantitative results are based on the injection of repeatable volumes of both the calibration blend and the sample. Absolute response factors, derived from the calibration blend, are used to relate the peak areas of each known component to mg/kg. 1. Prepare a stock solution as described in ASTM Meth
22、od D4307 to contain approximately 1.5 mass-% n-octane in benzene. Thoroughly mix the solution by shaking. Record all weights to the nearest 0.1 mg. Obtain the purest benzene possible to prepare the blend. Analyze it, looking for impurities that elute at the n-octane site. If impurities in the benzen
23、e are present at this site, the concentration must be accounted for in the calculation of the respective concentrations of the octane in the blend. This blend will be used as the stock solution in the preparation of the actual calibration blend. Label this mixture as the stock solution. 2. Prepare t
24、he calibration blend to contain approximately 1.5 mass-% of the stock solution in benzene. Thoroughly mix the calibration blend by shaking. Record all weights to the nearest 0.1 mg. If refrigerated, the stock solution and calibration blend should remain stable for five months. The benzene solutions
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