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1、1 ASAP 2020 PHYSISORPTION LABORATORY PRACTICAL EXERCISE GUIDE 2 Table of Contents ASAP 2020 PHYSISORPTION . 1 DAY 1 - INTRODUCTION TO SAMPLE FILE USAGE AND SAMPLE PREP . 3 LAB Session 1 - Intro to sample prep and sample files . 3 LAB Session 3 - Initiating carbon analysis . 24 LAB Session 5 - Prepar
2、ing Y-Zeolite for analysis . 28 LAB Session 6 - Initiating Silica Alumina analysis . 31 DAY 2 - MICROPOROUS SAMPLES AND SAMPLE PREP . 31 LAB Session 1 - Building Y-Zeolite Sample file . 31 LAB Session 3 -Y-Zeolite second degas . 35 LAB Session 4 - Creating entire Alumina sample file . 36 DAY 3 - IND
3、EPENDENT ALUMINA ANALYSIS . 39 LAB Session 1 - Analyzing an Alumina sample . 39 3 DAY 1 - INTRODUCTION TO SAMPLE FILE USAGE AND SAMPLE PREP LAB Session 1 - Intro to sample prep and sample files Physi Sample Prep Sample preparation is the foundation upon which any good, reliable, reproducible analysi
4、s is built. With the ASAP 2020 very few things can go wrong in sample preparation. In this section we will examine these critical aspects. Sample Quantity The ASAP 2020 measures pressure and then computes volume adsorbed as a result of changes in pressure. Very slight errors in measurement may be ca
5、used by minute, inherent transducer error. There is a sacrifice of accuracy when the total amount of sample in the test tube is very low. For the highest accuracy possible, greater amounts of sample should be used. Total surface area amounts approaching 50 m2 are not uncommon for highly accurate ana
6、lyses. Remember, however, that the greater the amount of total surface area present for analysis the more time must be allowed for the analysis. You should develop your own standards as you discover the best methods for your needs. Of course, any weighing errors, no matter how small, are magnified w
7、hen low sample masses are used. This is why a minimum of 0.1 g is specified. When analyzing a light or fluffy material, the entire area of the test tube within the heating mantle can be filled with sample in an attempt to attain sufficient sample mass. Remember that the sample mass initially placed
8、in the sample tube will be reduced as a result of the removal of trapped moisture (degassing). It is usually a good idea to use 5 - 20% excess sample mass than required so a sufficient mass will remain after the sample has been cleaned. The seal frit is a convenient method to insure sample material
9、is not contaminated as it is transferred from the degas port to the analysis port. It is simpler to use than a rubber stopper and we recommend its use as part of standard sample preparation. 4 LAB Initial Sample Preparation Please use the following items , an analytical balance, and the sample data
10、sheet (below)to perform the steps below. Clean Sample Tube Filler Rod Seal Frit Weighing Support 5 Reference Material (Carbon) 1. Tare the balance with weighing support in place. 2. Weigh the assembled sample tube (including filler rod and seal frit ) using the weighing support for stability. 3. Rec
11、ord this mass on the sample data sheet. 4. Tare balance with weighing dish. 5. Weigh approximately 0.60 grams of Carbon reference material. 6. Load the sample into the sample tube. 7. Insert the seal frit into the top of the sample tube. 8. Prepare a second sample tube, this time using about 0.25 gr
12、ams of the Silica- Alumina reference material. 6 ASAP Series Sample Data Record ASAP Series Sample Data Record Sample tube:_ Sample: _ Carbon_ Before Degas: 1. Mass of empty sample tube assembly (sample tube, seal frit and filler rod) _ g 2. Mass of sample tube assembly plus sample _ g 3. Mass of sa
13、mple (Step 2) (Step 1) _ g After Degas: 4. Mass of sample tube assembly plus sample _ g 5. Mass of sample (Step 4) (Step 1) _ g After Analysis: 6. Mass of sample tube assembly plus sample _ g 7. Mass of sample (Step 6) (Step 1) _ g You may use the After Degas value (Step 5) or the After Analysis value (Step 7), provided they are close to the same value. Compare the sample mass obtained after analysis (Step 7) with the sample mass after degas (Step 5). These two values should be close in ra
