Quick Start Guide for SA-9600 Series Surface Area Analyzer

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1 Quick Start Guide for SA-9600 Series Surface Area Analyzer Multi-Point Measurement HORIBA Scientific

2 SA-9603, Surface Area Analyzer, Multi-Station Outgassing station Analysis stations Liquid nitrogen bath

3 SA-9601, Surface Area Analyzer, Single-Station 2 Outgassing Stations 1 Analysis Station

4 Operation Requirements

5 Gas Requirement One nitrogen tank, % purity, output 40 psi (about 2.8atm) One helium tank, % purity, output 40 psi One DRY gas (air, N2, Ar, etc.), output 40 psi, to active the calibration loop valve Note: Shop air is not recommended due to potential moisture.

6 Gas Line Connections Three 2-stage gas regulators CGA580 for inert gases (not provided by Horiba) Three ¼ gas lines with ¼ Swage-lok compression fittings (6 of gas lines and all fittings provided by Horiba)

7 Liquid Nitrogen Daily usage depends upon number of measurements performed, but typically 2 6 liters per day

8 Analytical Balance Precision to 4 decimal places (i.e. 0.1 mg) More important for higher surface area samples Data Output HORIBA provides a Citizen CT-S4000 Thermal Printer with a Centronics communication cable------print directly from instrument HORIBA also provides Windows software, allowing to operate the instrument with computer------print from computer

9 Room Temperature Stable within ± 2 ºC Reference temp. can be updated in Diagnostic mode Atmospheric Pressure Stable within ± 10 mmhg Reference pressure can be updated in Diagnostic mode

10 Altitude versus Atmosphere Pressure

11 Altitude versus Atmosphere Pressure (con t) Altitude Above Sea Level Absolute Barometer Locations feet meter inches Hg mm Hg % air (Relative Pressure) -1, % Dead Sea, the lowest point on earth % Sea Level 5,280 1, % Denver, Mile-High City 7,355 2, % Los Alamos 12,966 3, % 玉山, 台灣 29,070 8, % Mount Everest, the highest point on earth

12 Highest Mountain in Taiwan, 玉山, 台灣

13 Setup before Power On

14 Gas can flow from gas tanks directly Gas tank with 2-stage pressure gage

15 or through building infrastructure gas lines (40psi, or 2.8bars) N 2 -He Pure N 2 Dry gas ¼ Fractional Tube OD provided by HORIBA

16 to the Horiba instrument. Pure He Pure N 2 Dry gas 6 ft of gas lines provided by HORIBA

17 6 (2 m) of tubing with ¼ Fractional Tube OD provided by

18 Insert Cell into Cell Holder Cell arms go through compression nuts, O-ring, and the ferrule

19 Install cell holders to the Analysis Stations (front 3) Cells must be installed in ALL Test locations at ALL times while power is ON If a test location is left OPEN for several minutes, the detectors may be damaged.

20 Setup after Power On

21 Turn on the instrument Press V to verify that the baseline voltage is 0±0.10 after 15 minutes of purging Adjustment might be needed if the baseline is too high

22 Verify flow meters read ; it provides 30 cc/min

23 Fine-Tuning Flowrate (diagnostic mode, 1 st time set-up) The goal is to adjust the flowrate with flowmeter until all 3 channels response within +/- 10% from each other to 1cc calibration gas, and readings are around 70, ,000. Turn on the instrument while still holding D to enter Diagnostic mode. Press Start to begin measurement. Don t worry about sample info. Instrument internally injects 1cc N 2. Detector detects calibrating gas. The second line on the screen is integrating the signals on the real time window. Once the numbers stop intergrading, stop the measurement. Adjust flowrates accordingly.

24 Sample Preparation Estimating Weight of the Sample Needed ***Total Measured Surface Area is (0.5-50)m², preferable (5-20)m² ***

25 ***Total Measured Surface Area is (0.5-50)m², preferable (5-20)m² *** TSA = SSA * W W = TSA/SSA TSA = Total Measured Surface Area (m²) *** SSA = Expected Specific Surface Area (m²/g) W = Estimated Sample Weight (g) Estimated wt, gram Estimated Max SSA,m²/g Estimated Min SSA,m²/g ** 10 1 **Large volume cells might be needed

26 Example If Expected Specific Surface Area is 5 m²/g and the estimated weight is 1 g, then TSA = SSA * W 5 m² = (5 m²/g ) * (1 g) such that, 5m² = Total Surface Area within the preferable (5-20)m² range Note: 1-4 g of sample would be within the preferable range for this sample

27 Sample Preparation Weighing Samples

28 Weight before Outgasing, i.e. W(sample+C) *This weight is not used in the final calculation* **It gives a rough idea on TSA** Estimate the sample weight Weight empty clean dry cell = W(tare) Weight cell-and-sample = W(tare)+W(sample+C) Weight of sample and contaminants = W(sample+C) C is the contamination

29 Add sample to cell using a funnel

30 Weight after Outgassing, i.e. W(sample) Degas sample to remove volatile contaminants Move to test station Take SA measurement Re-weigh cell-and-sample = W(tare)+W(sample) Calculate W(sample) = the weight of pure sample

31 Computing Specific Surface Area TSA is measured with the analyzer W(sample) is measured with analytical balance SSA=TSA / W(sample)

32 Sample Preparation Degassing to Remove Contaminants (such as moisture, VOC, etc)

33 Typically 1-2 hours at ºC Degassing stations Analysis stations Liquid nitrogen bath

34 Press T, and set up temperature and timer.

35 Starting Measurements

36 Switch cells from Preparation stations (side) to Test stations (front) Press V to verify that the baseline voltage is 0±0.10 after 15 minutes of purging Fill dewars ~ 2/3 full with LN 2 Press Start to begin measurement and follow directions on the screen to provide a Filename and Sample IDs for the measurement set

37 What Happens During Measurement?

38 Steps During Measurement 1. Purging and Internal Calibration 2. Adsorption 3. Desorption

39 1. Purging and Internal Calibration

40 2. Adsorption

41 Adsorption

42 3. Desorption

43 Amount of desorbed gas (step 10) S(desorption) is compared to acquired calibration (step4) S(calibration) to determine the total surface area Total SA TOTAL Surface Area (TSA) = Constant x (S(desorption) / S(calibration)) SSA = (TSA) / (Sample Wt)

44 Calculate, Save, and Print Data (using keypad) 1. Instrument will beep to signify the end of measurement 2. Press Enter to save current measurement to memory 3. Remove cell(s), weigh, and calculate W(sample) 4. Press Calculate and use the arrow ( ) buttons to locate the appropriate File. Press Enter to move through each field and enter W(sample) values. Once all three values have been modified the instrument automatically calculates the correct SSA. 5. Press Print with the File displayed to send the sample report to the Citizen printer.

45 Customer A, Correlation between 2 Horiba SA-9603 Material 1 Material 2 Material 3 New Analyzer Old Analyzer (New - Old)/Old X100% avg % % % % % % 4% % % % % % % % 7% % % % % 5% Data from Old Unit, m2/g Data correlation, old unit ~ new unit y = x R 2 = Date from New Unit, m2/g

46 Customer A, SA-9603 at Location 2 標樣 (Tube ID) 测试口 (Channel) B C E Avg per 测试口 (Channel) Avg per 標樣 (Tube) % 標樣 to 標樣 (Tube to Tube) variation is 1% 2% 测试口 -to- 测试口 (Channel to channel)variation is 2%

47

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