Optimizing Ultra Fast Simulated Distillation with a Low Thermal Mass (LTM) GC System. Jim McCurry Roger Firor Agilent Technologies Wilmington, DE

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1 Optimizing Ultra Fast Simulated Distillation with a Low Thermal Mass (LTM) GC System Jim McCurry Roger Firor Agilent Technologies Wilmington, DE Page 1

2 Scope of the Analyzer Designed for ASTM D7798 For the determination of boiling range distribution of petroleum products and biodiesel (B5,B10,B20) Applicable to petroleum distillates having a final boiling point not greater than 538 C Difference between initial BP and final BP must be greater than 55 C Not applicable to naphthas, reformates, gasolines or full range crude oils Page 2

3 Basic System Structure G3440B, 7890B #211, Capillary FID #112 Split/splitless Inlet or #150 MMI with CO2 cooling , 5 meter 0.25 mm fused silica deactivated Used for connecting column unions to inlet and detector G , Calibration Mix C5-C , Reference Gas Oil Page 3

4 LTM Configuration Options G6678A/79A/80A: 5-inch format Bundle Choose option: 78A 1-channel, 5 inch format, 1 power supply G : ULM Union kit w/ferrules Note: Supported as a single channel system only Page 4

5 Auto Injector Options Auto Injector required G4513A: 7693A with 16 sample module G4514A: 7693A Tray G4520A: 7693A Tray with heater/mixer and barcode reader G4520A is highly recommended 5uL syringe required: G Page 5

6 Software Requires the following: OpenLab CDS ChemStation Addition C 1.05 or greater Simulated Distillation Software Add on: G Note: Not supported on any other software platform Page 6

7 Column Investigation Three columns were considered for D7798: 5 m x 0.32mm x 0.52 um DB-1 4 m x 0.25 mm x 0.50 um DB-1 4m x 0.25 mm x 0.25 um DB-1 The focus here will be on the two 0.25 um ID columns Page 7

8 New Columns for Ultra Fast Simulated Distillation 5 inch LTM Format Dimensions: 4 m x 0.25 mm I.D. x 0.50 um DB-1 4 m x 0.25 mm I.D. x 0.25 um DB-1 Temp limits are: -60ºC to 360ºC Part Number: G (0.50 um column) Part Number: G (0.25 um column) Column should be installed with unions Column shipped with unions attached in special packaging Page 8

9 LTM Column Technology Page 9

10 LTM Column Heating and Cooling Characteristics Page 10

11 LTM Ultra Fast Simulated Distillation Configuration for D B with helium carrier gas 0.5 m x 0.25mm deactivated fused silica MMI or S/S Inlet 5 Inch LTM Module FID Page 11

12 Working with Flexible Metal Ferrules Page 12

13 Sample Preparation: General Guidelines Calibration Mix:C5-C44 Reference Gas Oil Viscous Oil Samples Dilute approx. 3:1 with Carbon disulfide Inject 0.1 ul Inject 0.1 ul neat Dilute as needed with Carbon disulfide, Typically 5 to 1. Heat 3 min. in tray at 80 C if required Inject from 0.1 to 0.5 ul Page 13

14 Parameters for Split/Splitless/LTM System Inlet: Split/Splitless, 355 C Liner: Single taper w/glass wool, # or # Split ratio: 30:1, helium carrier Column: 4 m x 0.25 mm x 0.25 um DB1 inseg: 0.5 m x 0.25 mm fused silica outseg: 0.5 m x 0.25 mm fused silica Flow: 8 ml/min, C, constant flow LTM Oven Program: 35 C (0.1 min) to 355 C ( C/min FID: 355 C Data Rate: 10 Hz or 20 Hz 7890B oven temp: 320 C isothermal Page 14

15 Parameters for MMI/LTM System Inlet: MMI, 355 C Liner: Single taper w/glass wool, # or # Split ratio: 30:1, helium carrier Column: 4 m x 0.25 mm x 0.25 um DB1 inseg: 0.5 m x 0.25 mm fused silica outseg: 0.5 m x 0.25 mm fused silica Flow: 8 ml/min, C, constant flow LTM Oven Program: 35 C (0.1 min) to 355 C ( C/min FID: 355 C Data Rate: 10 Hz or 20 Hz 7890B oven temp: 320 C isothermal Page 15

16 C5-C40 Calibration Mix: 160 C/min, MMI 4 m x 0.25 mm x 0.50 um DB-1 C40 Page 16

17 C44 Elution on the Thicker Film Column 4 m x 0.25 mm x 0.50 um DB C/min, MMI C44 elutes on final isothermal section Parameters not optimized: All calibration hydrocarbons should elute during the temperature program ramp Page 17

18 C5-C44 Calibration: 150 C/min Column: 4 m x 0.25 mm x 0.25 um DB-1 C44 elutes during oven ramp Page 18

19 Comparison of Thin and Thick Film Columns for C5-C6 Separation C5 C6 4 m x 0.25 mm x 0.50 um DB-1 C5 4 m x 0.25 mm x 0.25 um DB-1 C6 Both provide adequate separation Page 19

20 The MMI Shows Minimal Discrimination Over a Wide Boiling Point Range Page 20

21 The S/S Discrimination Test Hydrocarbon Conc. (ppm) Area nc12/ncx nc10/ncx 100 ppm HC's 200 ppm HC's C C C C C C C C C C C C C C C C Page 21

22 RGO: 150 C/min Column: 4 m x 0.25 mm x 0.25 um DB-1 Page 22

23 Column Flow vs. LTM Oven Program Rate As the column ramp rate increases, flow rates must increase to maintain separation, speed and elution Column flow ml/min Program rate C/min Starting with a flow of C/min Page 23

24 Method Translation for 2X Speed Gain Page 24

25 Programmed at 300 C/min: C5 - C44 Column: 4 m x 0.25 mm x 0.25 um DB-1 Column Flow Rate: 21.7 ml/min C44 elutes at less than 1.10 min.- Faster rates not recommended Page 25

26 RGO: MMI, 160 C/min Column: 4 m x 0.25 mm x 0.25 um DB-1 Page 26

27 RGO Setup in the Software Page 27

28 RGO Engineering Report 160 C/min S/S Inlet Yield table meets method specifications for RGO No. 1 Batch 2 n-butanol n-butanol Page 28

29 RGO Overlay of 5 runs: S/S Inlet 160 C/min Page 29

30 RGO Overlay of 5 Runs: 160 C/min, MMI Page 30

31 Repeatability: RGO with 160 C/min Temperatures in F % OFF AVG RSD %RSD ASTM DIFF F ASTM DIFF = Allowable difference (+ or -) from last column Page 31

32 Repeatability: RGO with 160 C/min Temperatures in F % OFF AVG RSD %RSD ASTM DIFF F ASTM DIFF = Allowable difference (+ or -) from last column Page 32

33 Cracked Gas Oil Setup Pane: Split/Splitless Inlet Page 33

34 Cracked Gas Oil Engineering Report Page 34

35 Blanks Following 10 runs of a Gas Oil Showing Absence of Carryover blanks runs Page 35

36 Summary: Simulated Distillation Solutions Two Configurations are available 7890B/FID 7890B/LTM II/FID Auto Injector with Tray provides sample heating to reduce viscosity prior to injection Simulated Distillation Software is partially integrated into the OpenLab ChemStation for calculation and report automation Page 36

37 Summary A 4 m x 0.25 mm x 0.25 um column proved optimal for elution of C44 while maintaining C5/C6 separation An LTM program rate of 150 C/min offers speed while eluting C44 easily during the temperature ramp LTM program rates above 300 C/min are not recommended as higher boiling hydrocarbons may will not elute during the temperature program ramp and little speed advantage is obtained Discrimination is nearly absent with the Multimode Inlet (MMI) and Split/Splitless over a C10 to C44 range Rapid cool down of the LTM oven greatly reduces cycle time Page 37

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