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4、555 FAX, or 610.832.9585 PHONE. Soxhlet Extraction of Catalyst UOP Method 602-15 Scope This method is for separating hydrocarbons from catalyst samples by extraction with a volatile solvent. This extraction is used to obtain a hydrocarbon and water free catalyst sample for carbon determination by UO
5、P Method 703, “Carbon on Catalysts by Induction Furnace Combustion and Infrared Detection.” It can also be used to determine the non-volatile hydrocarbon content of the sample, or to provide an extract for subsequent analysis. The use of an automated system is described in the Appendix. For self-hea
6、ting samples, refer to the drying procedure in the Appendix. References ASTM Method G120, “Determination of Soluble Residual Contamination by Soxhlet Extraction,” www.astm.org UOP Method 703, “Carbon on Catalysts by Induction Furnace Combustion and Infrared Detection,” www.astm.org UOP Method 918, “
7、Collection and Grinding of Adsorbents and Catalysts for Analysis,” www.astm.org Outline of Method A ground sample is placed in an extraction thimble and Soxhlet extracted with methylene chloride for four hours, or until the solvent in the thimble chamber is clear. The thimble with sample is then dra
8、ined and dried at 105C in a nitrogen-purged oven for four hours. If quantitative results for hydrocarbon separated by this method are required, the thimble must be dried and weighed with the sample before and after extraction. To obtain a sample of the non-volatile hydrocarbons for subsequent organi
9、c type identification, the extracted material is made up to a specified volume with the extraction solvent. When the mass of the non-volatile residue is desired, the solvent is volatilized in a tared beaker and reweighed. The Appendix contains an alternative procedure using an automated extraction s
10、ystem. 2 of 9 602-15 Apparatus Reference to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. Balance, readability 0.0001 g Beaker, 250-mL, borosilicate glass, Fisher Scientific, Cat. No. FB-100-250 Clamps, high pressure, 6- to 11-mm, Fisher
11、 Scientific, Cat. No. 14-198-5B Cylinder, graduated, borosilicate glass, 250-mL, Fisher Scientific, Cat. No. 08-554F Desiccator, borosilicate glass, large diameter, Fisher Scientific, Cat. No. 08-595E Dessicator plate, polypropylene, 230-mm, Fisher Scientific, Cat. No. 08-643-2C Extraction heater, 6
12、-unit, 28-cm long x 76-cm wide x 23-cm high, includes brackets and rods, Fisher Scientific, Cat. No. 09-678-1 Flask, volumetric, 250-mL, Fisher Scientific, Cat. No. 10-208J Forceps, extra long, 300-mm, Fisher Scientific, Cat. No. 10-316C Hotplate, laboratory Mortar and pestle, porcelain, 130-mm OD,
13、Fisher Scientific, Cat. Nos. 12-961C and 12-961-5C, respectively Oven, drying, capable of operation at 105C, Fisher Scientific, Cat. No. 13-247-637G or 13-247-737G. The oven requires proper ventilation for the solvent vapors. Purging the oven with nitrogen is required and placing the oven inside of
14、a fume hood is recommended. Regulator, gas, two-stage, Matheson Tri-Gas, Cat. No. 81-580 Soxhlet extraction assembly, borosilicate glass, comprised of a 40-mm ID extraction tube with top sT 40/50 joint, 250-mL flask and condenser, Fisher Scientific, Cat. No. 09-556B (see Note) Tubing, tygon, 7.9-mm
15、ID, 15-m long, Fisher Scientific, Cat. No. 14-169-1M Vials with caps, 22.2-mL Fisher Scientific, Cat. No. 03-338-H Reagents and Materials References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. References to water mean deionized or d
16、istilled. Calcium chloride, anhydrous, dessicant, 4-20 mesh, Fisher Scientific, Cat. No. C614 Methylene chloride, 99.8% minimum purity, Fisher Scientific, Cat. No. D37 Nitrogen, 99.99% minimum purity Pencil, soft lead (F or 2) Thimbles, Whatman, pure cellulose, 33- x 80-mm, Fisher Scientific, Cat. N
17、o. 09-656B Water, deionized or distilled 3 of 9 602-15 Procedure The analyst is expected to be familiar with general laboratory practices, the technique of Soxhlet extraction, and the equipment being used. Additional information on the technique of Soxhlet extraction, including a diagram of the appa
18、ratus, can be found in ASTM Method G120, “Determination of Soluble Residual Contamination by Soxhlet Extraction.” Qualitative Extraction Preceding Carbon Determination 1. Grind the catalyst according to UOP Method 918, “Collection and Grinding of Adsorbents and Catalysts for Analysis,” or with a mor
19、tar and pestle to a fine mesh size. 2. Place approximately 5 g of catalyst into the extraction thimble. Close the thimble by folding over the top 1.5 cm and pressing it shut with the forceps. Use a pencil to identify the contents of the thimble. Do not use an ink pen. Place the thimble in the extrac
20、tion apparatus. Less than 5 grams may be used if a limited supply of sample is available and the amount is sufficient for subsequent analyses. 3. Transfer 150 mL of methylene chloride with a graduated cylinder into the solvent flask. 4. Lubricate the ground glass joints by marking them liberally wit
21、h a soft lead pencil. 5. Assemble the apparatus in a fume hood according to manufacturers specification and turn on the cooling water to the condensers. 6. Turn on and increase heat to obtain a gentle reflux of the solvent. 7. Continue to reflux for a minimum of four hours, or until the solvent in t
22、he thimble is visibly clear when nearly full. 8. When the extraction is complete, turn off the heat and allow the apparatus to cool for 30 minutes. 9. Turn off the water to the condensers. 10. Disconnect the condenser from the thimble chamber and, with the forceps, lift the thimble, set it in the op
23、ening of the thimble chamber, and allow it to drain for approximately 15 minutes to remove excess solvent. 11. Discard the solvent, unless it is required for organic type identification. 12. Place the thimble in a clean beaker and dry in the nitrogen-purged, vented oven at 105C for a minimum of 4 ho
24、urs. The thimble may be left in the oven at 105C overnight. 13. Remove the beaker with the thimble from oven, place in a desiccator, and allow to cool. 14. Transfer the sample to a vial and cap immediately. Quantitative Extraction to Determine Hydrocarbon Content 1. Place a new extraction thimble in
25、 a 250 mL beaker and dry it for 30 1 minutes in a nitrogen-purged, vented oven at 105C. 2. Grind the catalyst according to UOP Method 918, “Collection and Grinding of Adsorbents and Catalysts for Analysis,” or with a mortar and pestle to a fine mesh size. 3. Remove the beaker and thimble from the ov
26、en, place in a desiccator, and allow to cool for 15 1 minutes. 4. Weigh the beaker and thimble to the nearest 0.0001 g to obtain a tare weight. 4 of 9 602-15 5. Transfer a sufficient quantity of the ground catalyst to fill the thimble approximately 2/3 full. 6. Weigh and record the gross weight of t
27、he sample, thimble and beaker. 7. Follow the extraction procedure as described under Qualitative Extraction Preceding Carbon Determination, Steps 3 through 11. 8. Put the thimble in the tared beaker originally used and place in the drying oven at 105C for four hours. 9. Remove the beaker with the th
28、imble from oven, place in a desiccator, and allow to cool for 15 1 minutes. 10. Weigh the beaker containing the thimble and extracted sample to the nearest 0.1 mg. Record the weight. Extracts for Other Analysis If subsequent analysis of the extracted material is required, the hydrocarbon can be prov
29、ided as a solution in the extraction solvent or as a quantitative, non-volatile residue. When a solution is required: 1. Quantitatively transfer the solvent solution resulting from either of the preceding sections to a 250-mL volumetric flask. 2. Rinse the apparatus, collecting the rinsings in the v
30、olumetric flask and dilute to the mark with additional solvent. When a quantitative non-volatile residue is required: 1. Extract the sample as described under Quantitative Extraction to Determine Hydrocarbon Content. 2. Transfer all of the solvent from the extraction apparatus to a tared beaker. 3.
31、In a hood, carefully evaporate to 5-10 mL on a hot plate at a low temperature. 4. Place the beaker in the nitrogen-purged, vented oven at 105C for one hour. 5. Remove the beaker with the thimble from oven, place in a desiccator, and allow to cool. 6. Weigh the beaker and residue to the nearest 0.1 m
32、g. Calculations If a quantitative extraction to determine hydrocarbon content is performed, use the following calculations to determine extractable hydrocarbons and/or non-volatile extracted materials. Calculate the mass-% extractable hydrocarbon content of the catalyst sample using Equation 1. Any
33、water present in the catalyst sample that is removed during the four-hour drying procedure will be included in the extractable hydrocarbons value. Report to the nearest 0.1 mass-%. Extractable hydrocarbons, mass-% = C )BA(100 (1) where: A = mass of beaker, thimble and sample before extraction, g B =
34、 mass of beaker, thimble and sample after extraction and oven drying, g C = mass of sample before extraction, g 100 = factor to convert from g/g to mass-% 5 of 9 602-15 Calculate the mass-% non-volatile extracted materials after oven drying at 105C using Equation 2. Report to the nearest 0.1 mass-%.
35、 Non-volatile extracted materials, mass-% = C )ED(100 (2) where: C = mass of sample before extraction, g D = mass of beaker and extracted material, g E = mass of empty beaker, g 100 = factor to convert from g/g to mass-% Note Several vendors offer complete automated systems that are satisfactory alt
36、ernatives. The use of one such system is described in the Appendix. Precision Repeatability and Reproducibility Because this method is primarily used for the qualitative removal of hydrocarbons from catalysts prior to carbon determination, the repeatability and reproducibility of the test are not ca
37、lculated. Time for Analysis Table 1 shows the labor requirements and elapsed times for the various extraction procedures. Table 1 Times for Analysis Labor Requirement, Hours Elapsed Time, Hours Qualitative extraction preceding carbon determination 0.2 10 Quantitative extraction to determine hydrocar
38、bon content 1.5 12 Extracts for other analysis 0.4 5 Suggested Suppliers Fisher Scientific, 711 Forbes Ave., Pittsburgh, PA 15219-4785, USA (412-490-8300) Matheson Tri-Gas, 166 Keystone Dr., Montgomeryville, PA 18936, USA (215-641-2700) 6 of 9 602-15 Appendix Soxhlet Extraction Using an Automated
39、System Scope This procedure is for separating hydrocarbons from catalyst samples by extraction with a volatile solvent using an automated extraction system. This extraction is used to obtain a hydrocarbon and water free catalyst sample for carbon determination by UOP Method 703. It can also be used
40、to determine the non-volatile hydrocarbon content of the sample, or to provide an extract for subsequent organic types analysis. Up to four samples can be extracted simultaneously in the four-position extraction system specified. Outline of Method A ground sample is placed in an extraction thimble a
41、nd Soxhlet extracted with methylene chloride for two hours. The thimble with sample is then drained and dried at 105C in a nitrogen-purged oven for four hours. If quantitative results for hydrocarbon separated by this method are required, the thimble must be dried and weighed with the sample before
42、and after extraction. To obtain a sample of the non-volatile hydrocarbons for subsequent organic type identification, the extracted material is made up to a specified volume with the extraction solvent. When the mass of the non-volatile residue is desired, the solvent is volatilized in a tared beake
43、r and reweighed. Apparatus Reference to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. The following items are required in addition to items in the body of the method. Extraction system, Model B-811, Buchi Glass collars, for 27mm O.D. ext
44、raction thimbles, Buchi, Cat. No. 037277 Solvent beakers, Buchi, Cat. No. 037276. Reagents and Materials References to catalog numbers and suppliers are included as a convenience to the method user. Other suppliers may be used. References to water mean deionized or distilled. The following item is r
45、equired in addition to items in the body of the method. Thimbles, Whatman, pure cellulose, 25-mm I.D. x 100-mm, Fisher Scientific, Cat. No. 09-656L Procedure The Buchi B-811 extraction system is configured for the “Soxhlet Warm” extraction type. This reduces the required extraction time from 4 hours
46、 to 2 hours by heating the extraction chamber. Set the upper and lower heat settings to those recommended by the manufacturer for the solvent used. See Table A1 for an example. 7 of 9 602-15 Table A1 Recommended Settings For Buchi B-811 Extraction System Extraction type Soxhlet Warm Solvent methylen
47、e chloride Lower heater temperature 9 Upper heater temperature 2 Extraction time 2 hours Rinse time 10 minutes Dry time 0 Inert gas purge optional Qualitative Extraction Preceding Carbon Determination 1. Grind the catalyst according to UOP Method 918, “Collection and Grinding of Adsorbents and Catal
48、ysts for Analysis,” or with a mortar and pestle to a fine mesh size. 2. Place approximately 5 g of catalyst into the extraction thimble. Use a pencil to identify the contents of the thimble. Do not use an ink pen. Less than 5 grams may be used if a limited supply of sample is available and the amoun
49、t is sufficient for subsequent analyses. 3. Insert the extraction thimble into the glass collar such that all but 2-3 mm of the thimble extends from the bottom of the collar. The notches must be at the top. 4. Mount the collar to the sample holder at the end of the condensation tube. 5. Repeat steps 2 - 4 for all remaining samples, then lower the condensers and turn clockwise to seal the system. 6. Transfer 100 mL of methylene chloride with a graduated cylinder into each solvent beaker. 7. Lift the solvent beakers into th
