UOP 377-2013 Free Sulfur in LPG by Mercury Number.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 1959, 1990, 2013 UOP LLC. All rights r
3、eserved. 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, 610.832.9555 FAX, or
4、610.832.9585 PHONE. Free Sulfur in LPG by Mercury Number UOP Method 377-13 Scope This is a semi-quantitative method for determining free sulfur in liquefied petroleum gases. Peroxide is an interference that increases the apparent elemental sulfur value. The lower limit of detection is a mercury numb
5、er of 1.0, which is equivalent to approximately 2.0 mg/kg (mass-ppm). References ASTM Method D1657, “Density or Relative Density of Light Hydrocarbons by Pressure Hydrometer,” www.astm.org UOP Method 999, “Precision Statements in UOP Methods,” www.astm.org Outline of Method A known mass of liquefied
6、 petroleum gas (LPG) is dissolved in toluene and then the LPG is evaporated. The remaining toluene, which contains the elemental sulfur, is placed in a bottle to which oleic acid and mercury are added and the mixture is shaken vigorously. The resulting mercuric sulfide suspension is visually compare
7、d to a set of previously prepared standards containing known amounts of elemental sulfur. A relative density of the LPG is determined and the mercury number is calculated. The sulfur concentration can also be calculated in mass-ppm. Definition Mercury Number is defined as milligrams of free sulfur p
8、er liter. Apparatus References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. Balance, 8000-g capacity, readable to 0.l g Balance, readable to 0.0001 g Bottles, clear oil sample, 118-mL, with cork stopper, Fisher Scientific, Cat. No. 0
9、2-911-472. Mark each bottle at the 100-mL point by filling the bottle with a measured 100 mL of water, and marking with a marker or scriber. Cylinders, graduated, 5- and 50-mL, Fisher Scientific, Cat. Nos. 08-550A and -550D, respectively 2 of 4 377-13 Delivery tube, stainless steel, 6.35-mm OD, for
10、LPG sample cylinder, 100-mm length with a connection on one end that corresponds with the outlet connection of the sample cylinder and the other end plain. Flask, Erlenmeyer, 500-mL, Fisher Scientific, Cat. No. FB-500-500 Flask, volumetric, 1000-mL, Fisher Scientific, Cat. No. 10-212-5L Hood, labora
11、tory fume Marker, diamond point, Fisher Scientific, Cat. No. 75-0 Pipet, Mohr, 1-mL, 0.1-mL sub-divisions, Fisher Scientific, Cat. No. 13-665-G Pipets, volumetric, Class A, 2- and 100-mL, Fisher Scientific, Cat. Nos. 13-650-2C and -2U, respectively Timer, laboratory, Fisher Scientific, Cat. No. 14-6
12、48-35 Reagents and Materials References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. Boiling chips, carbon, Fisher Scientific, Cat. No. 09-191-12 Mercury, triple distilled, Fisher Scientific, Cat. No. 7439-97-6 Oleic acid, Fisher Sci
13、entific, Cat. No. A195 Sulfur, precipitated, Fisher Scientific, Cat. No. 7704-34-9. Flowers of sulfur cannot be used. Toluene, 99.8% minimum purity, Fisher Scientific, Cat. No. 108-88-3 Procedure The analyst is expected to be familiar with general laboratory practices and the equipment being used. D
14、ispose of used reagents, materials, and samples in an environmentally safe manner according to local regulations. Perform all activities except weighing in a laboratory hood. Preparation of Standards Prepare a standard sulfur stock solution as follows: 1. Place 1.0 g 0.001 g of precipitated sulfur i
15、n a 1000-mL volumetric flask. Do not use flowers of sulfur. 2. Add toluene to dissolve the sulfur. 3. Fill to the mark with toluene and shake to mix. This standard sulfur stock solution contains 1.0 mg of elemental sulfur per mL. Standard Mercuric Sulfide Suspensions 1. Add by pipet 100 mL of toluen
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