UOP 99-2007 PENTANE-INSOLUBLE MATTER IN PETROLEUM OILS USING A MEMBRANE FILTER.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 1947, 1963, 1982, 2007 UOP LLC. All ri
3、ghts 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, 610.832.9555 FA
4、X, or 610.832.9585 PHONE. Pentane-Insoluble Matter in Petroleum Oils Using a Membrane Filter UOP Method 99-07 Scope This method is for the determination of pentane-insolubles in petroleum oils and is applicable to samples that are fluid at about 37C or lower temperatures. This method covers the rang
5、e of 0.01 to about 20 mass-% pentane-insolubles. Solid particulate materials interfere. The data provided by this method may be used as an index to coking tendency of petroleum oils when considering their suitability as charge stocks to cracking or other processes. More viscous or solid materials su
6、ch as asphalts may be handled by using the modification described in the Appendix. A similar test method for heptane-insolubles, for samples that are fluid at 80C, is UOP Method 614, “Heptane-Insoluble Matter in Petroleum Oils by Membrane Filtration,” which also mentions toluene-insolubles in a Note
7、. ASTM Method D 4055, “Pentane Insolubles by Membrane Filtration,” is also similar in technique, but is written for particulates in lubricating oils rather than asphaltenes. References ASTM Method D 56, “Flash Point by Tag Closed Cup Tester,” www.astm.org ASTM Method D 4055, “Pentane Insolubles by M
8、embrane Filtration,” www.astm.org UOP Method 614, “Heptane-Insoluble Matter in Petroleum Oils by Membrane Filtration,” www.astm.org Outline of Method A weighed sample is dispersed at ambient temperature in n-pentane, digested at 37C, and filtered through a weighed membrane filter. Samples that canno
9、t be completely dispersed cannot be analyzed. The membrane filter is dried and reweighed to obtain the weight of insoluble matter. 2 of 10 99-07 Definition Asphaltenes are defined as the material present in oil fractions that is not soluble in light paraffinic solvents. They are fine, powdery, black
10、-brown solids which are polymeric materials spanning a wide range of molecular weights. Their chemical composition is quite complicated. They appear to be closely associated with high molecular weight semi-polar naphthenic materials. The terms “pentane- insolubles” and “asphaltenes” are often used s
11、ynonymously. Apparatus References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used, unless stated otherwise. Balance, readability 0.1-mg, capacity 200-g Clamps, for 250-mL flasks in shaker bath, Fisher Scientific, Cat. No. 15-455-15E Cyli
12、nder, graduated, 250-mL, Fisher Scientific, Cat. No. 08-557E Desiccator, with plate, to hold Petri dishes, Fisher Scientific, Cat. No. 08-615A Dishes, Petri, borosilicate glass, 60-mm diameter Filter holder, stainless steel, “Millipore Hydrosol“ filter holder, Millipore Corp., Cat. No. XX 20 047 20
13、Flask, filtering, with sidearm, 2-L, Fisher Scientific, Cat No. K953760-2000 Flask, Erlenmeyer, narrow neck, 250-mL, with pennyhead, ground-glass, standard taper stopper, Fisher Scientific, Cat. No. 10-100E Forceps, stainless steel, with flat, polished tips for handling filters, Millipore Corp., Cat
14、. No. XX62 000 06 Gloves, thermal resistant, Fisher Scientific, Cat No. 11-462-56 Oven, capable of operation at 95C, Fisher Scientific, Cat No. 13-247-637G Pipet, volumetric transfer, 2-mL, Fisher Scientific, Cat. No. 13-650-2C. Cut 4-5 mm off the tip to obtain a large-bore tip. Pipet, 25-mL graduat
15、ed serological, large tip opening, Fisher Scientific, Cat. No. 13-671-108E Pipet filler, Fisher Scientific, Cat. No. 03-692-35 Pump, vacuum, Welch Rotovap, Fisher Scientific, Cat. No. 01-129-19. If the pump is to be located in the hood, or anywhere near the warmed pentane, an explosion proof model s
16、uch as Fisher Scientific, Cat. No. 01-182-003 must be used. Shaker water bath, Precision Scientific Model 50, Fisher Scientific, Cat. No. 15-455-5 Thermometer, for oven, without mercury, Fisher Scientific, Cat. No. 15-041-6C Ultrasonic bath, 9-L capacity, 185 watt, Fisher Scientific, Cat. No. 15-335
17、-110 Wash Bottle, 500-mL, fluorinated HDPE, Fisher Scientific, Cat. No. 03-409-17B Reagents and Materials References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used, unless stated otherwise. 3 of 10 99-07 Depth filter disc, 35-mm diamete
18、r, Millipore Corp., Cat. No. AP2503500, if needed, see Procedure, Step 10 Dessicant, indicating Drierite, Fisher Scientific, Cat. No. 07-578-3A n-pentane, 99% minimum purity, residue after evaporation 0.001%, Acros Organics, Cat. No. 16787 0025, Fisher Scientific Membrane filter discs, 0.8 m and 5.0
19、 m pore sizes, 47-mm diameter, white, plain, MF, Millipore Corp., Cat. Nos. AAWP04700 and SMWP04700, respectively Sampling Samples for this test should be taken in clean containers under a blanket of nitrogen or other inert gas. The container should be filled only about 3/4 full so that the sample c
20、an be shaken vigorously before testing. No other tests or analyses should be made on this sample until after the pentane-insoluble content is determined. Samples under an inert gas blanket can usually be kept a few days at room temperature. However, for best results, test the sample the same day it
21、is taken. Sample Preparation The sampling procedure varies according to two conditions: the expected pentane-insoluble matter content, and the fluidity of the sample. If the sample is sufficiently fluid to withdraw into a pipet, take the sample from the container at room temperature. If the sample i
22、s too viscous, or is waxy, it must be heated. 1. Loosen the cap or stopper of the sample container to vent it and place it in the 95C oven along with the appropriate pipet. CAUTION: If there is any possibility of the sample containing light ends, or if it is of unknown origin, test it for flash poin
23、t by ASTM Method D 56, “Flash Point by Tag Closed Cup Tester,” before placing it in the oven. If it flashes, do not use the oven to heat the sample. 2. Heat small bottles (pint or less) 30 minutes before sampling. Allow one hour of heating for a gallon container. Never heat for more than about 2 hou
24、rs, because some oils can form additional insoluble compounds on prolonged heating (see Note 1). Very high boiling samples, such as asphalts, should be sampled as described in the Appendix. The size of the sample taken for the test and the size of the pores of the membrane filter disc to be used are
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