Live Crude Oil Volatility
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1 Live Crude Oil Volatility Dan Wispinski : Alberta Innovates Technology Futures Bob Falkiner : Imperial Oil Engineering Services CCQTA/COQA October 31, 2014
2 Food-Agriculture Environment Health Pipeline Oil and Gas
3 Vapor Pressure Light Ends Determination by GC
4 ASTM Definition for Live Crude Live crude oil,n crude oil with sufficiently high vapor pressure that it would boil if exposed to normal atmospheric pressure at room temperature. Discussion - Sampling and handling of live crude oils requires a pressurized sample system and pressurized sample containers to ensure sample integrity and prevent loss of volatile components.
5 Need no method for Live Crude Oil ASTM D7169 HTSD Crude sample is diluted with CS ambient temperature & pressure Light ends lost Light ends not reported Light ends are quenched by CS 2
6 Need no method for Live Crude Oil ASTM D7900 Merge Internal Standard is added to crude sample at ambient Temperature & Pressure Light ends lost Light ends are reported (usually to nc10 DHA) and remainder of crude is backflushed Data used to correct CS 2 quenching in distillation curve by combination with D7169
7 Need no method for Live Crude Oil ASTM D7900 / ASTM D7169 Samples are collected under atmospheric conditions Use of sealed sample collection cylinders not mentioned
8 High Vapor Pressure Live Crude Oil Transportation Environment, Health, & Safety Economic
9 Transportation & EH&S TVP Impacts of Crude Oil Fugitive emissions Storage tanks floating roof, tank integrity Rail cars design, safety Pipelines
10 Economic Crude Oil Valuation Custody transfer Refinery impacts Compliance
11 High Vapor Pressure Live Crude Oil Analysis Issues Sampling Vapor Pressure Direct analysis of TVP via field method and ASTM D6377 lab method Light end composition HPLIS/GC with EOS TVP
12 Sampling Sealed container (FPC) is required
13 Sampling Sealed container (FPC) required
14 Sampling HPLIS/GC includes procedures and instructions for pressurized cylinders D3700 FPC or D1265 ullage tube
15 Measuring Vapor Pressure Crude Oil ASTM D323 Reid Vapor Pressure 100 F & V\L 4:1 The extreme sensitivity of vapor pressure measurements to losses through evaporation and the resulting changes in composition is such as to require the utmost precaution and the most meticulous care in the handling of samples yet sampling in open container is specified ASTM D6377 VPCR x, t where x = V/L ratio of 0.02 to 4 and t = 0 to 100 C
16 Measuring Vapor Pressure Crude Oil ASTM D6377 VPCR x, Industry norm Sampling in sealed sample container (FPC) required Automated instrument temp & VL ratios Regulatory EPA allows method but silent on how to apply it
17 c2 and c2 and Mass % Mass % Small amounts of C1-C4 have a Huge VP Impact IOL0011 Cut Points IOL0010 Cut Points Acceptable Stabilization Not Acceptable Stabilization Small Mass% = Large Mole% for C1 to C4 due to low MW x large component VP C1~ 2500 psi C2 ~ 800 psi C3 ~ 200 psi C4 ~ 65 psi
18 Experimental Values
19 Pressure, kpa EOS SRK Modeling of Binary Mixtures Calculated VP of gases in isooctane, 37.8C AIR Methane Ethane Propane Butane Volume Ratio, V/L initial
20 Determination of Light Hydrocarbons and Hydrocarbon Boiling Point Distribution and Cut Point Intervals in Live Crude Oils and Condensates by Gas Chromatography ASTM WK45458 Alberta Innovates Technology Futures CCQTA/COQA October 2014
21 Scope This test method covers the determination of light hydrocarbons, their boiling point distribution and cut point intervals via gas chromatography in live crude oils and condensates with VPCR 4 up to 200 kpa at 37.8 C as described in Test Method D6377 Methane (nc 1 ) to hexane (nc 6 ) including ic5, benzene, and benzene precursors are speciated and quantitated.
22 HPLIS Method Summary Liquid sample valve connected to pressurized sample Theoretical mass response factors Cut point fractions generalized physical properties External std calibration with density correction determination of residue similar to RefOil 5010 in D7169 Primary purpose is light end quant BP distribution can be determined
23 Component Molecular Weight of Component (g/mol) Density of 20 C (g/ml) Generalized Boiling Point of Cut Point Fraction Interval C Generalized Molecular Weight of Cut Point Fraction Interval (g/mol) Generalized Density of Cut Point Fraction 20 C (g/ml) Theoretical Mass Response Factor C C C ic n-c ic n-c n-c Benzene n-c n-c n-c n-c n-c n-c n-c n-c n-c n-c n-c n-c n-c n-c n-c n-c n-c n-c Residue
24 Instrument Set-up Hydrogen Carrier GC HPLIS heated stem injection (200 C) Split/splitless injector MXT1 15m x 0.280mm, 3um film column. FID detector
25 HPLIS with heated collar
26 HPLIS Load and Inject Positions
27 Heated STEM of HPLIS
28 Discrimination Check Relative Response Std Component RRF (nc20 reference) nc nc nc nc nc nc nc
29 C1-C7 peaks resolution pa 3000 FID1 A, (SEPT05\BAC_7.D) nc3 Component Wt% nc1 nc2 ic4 nc4 ic5 nc5 nc nc nc ic nc ic nc nc6 nc7 nc34 nc32 nc31 nc30 nc29 nc28 nc10 nc27 nc26 nc25 nc21 nc20 nc23 nc18 nc24 nc19 nc17 nc8 nc16 nc9 nc14 nc12 nc13 nc min
30 Enlivened Bakken Crude pa *FID1 A, (SEPT05\BAC_3.D - SEPT05\BAC_BLK.D) nc2 ic4 nc1 nc4 nc3 ic5 nc5 nc6 nc7 nc8 nc9 nc10 Enlivened Bakken Crude C1, propane and C4 added 6runs Component Average Std Dev % Relative Wt % Std Dev nc nc nc ic nc ic nc nc nc C7 plus nc1 nc12 nc13 nc14 nc15 nc16 nc17 nc18 nc19 nc20 nc21 nc2 nc23 nc24 nc25 nc26 nc27 nc28 nc min nc30 nc31
31 Calibration Standards Gasoline/Jet A1mix spiked with methane, ethane, and n-paraffin's betweenc16 and C24. Seven D1265 cylinders were made and run multiple times on the HPLIS to get precision data, and verify the ability to make homogeneous samples in cylinders of this type.
32 Calibration Standard 7 cylinders -24 runs Average, mass% StdDev Max Min r estimate %RSD Methane Ethane Propane Isobutane Butane C4+ to C c c c c c c TOTAL AREA
33 Calibration Standard Norm. FID1A, (FL_SAMPLES\HPLISSTDFL \FL D) Propane isobutane Methane Ethane butane pentane Isopentane hexane C7 C8 C9 C10 C11 C12 C13 C14 C15 C16 C17 C19 C20 C22 C min
34 Validation standards accumulator (FPC) Five samples prepared from a dead oil, with different target mass% concentrations of light ends. Sample VP (kpa) C1 C2 C3 ic4 nc4 ic at 4:1 Vapor-toliquid volume nc5 nc6 5 ratio at 37.8 C Sample 1 High Sample 2 Typical Sample 3 typical repeat Sample 4 typical high c1,c2,c Sample 5 Low sample Not calculated
35 Dead Oil Analysis Component HPLIS GC, mass% METHANE 0.00 ETHANE 0.00 PROPANE 0.00 IC NC IC NC NC NC NC NC NC NC Total 100
36 Sample 1 Component HPLIS GC, mass% Actual, mass% METHANE ETHANE PROPANE IC NC IC NC NC NC NC NC NC NC Total
37 Sample 2 & 3 Components HPLIS GC Actual HPLIS GC Actual METHANE ETHANE PROPANE IC NC IC NC NC NC NC NC NC NC Total
38 Sample 4 Component HPLIS GC, mass% Actual, mass% METHANE ETHANE PROPANE IC NC IC NC NC NC NC NC NC NC Total
39 Sample 5 Component HPLIS GC, mass% Actual, mass% METHANE ETHANE PROPANE IC NC IC NC NC NC NC NC NC NC Total
40 Predicted Vapor Pressure (kpa) EOS SRK HPLIS GC mass% vs VPCR 25,37.8,50,65 C Samples 2,3,4, y = 0.76x R² = V/L=1 Linear (V/L=1) Measured Vapor Pressure (kpa)
41 Predicted Vapor Pressure (kpa) EOS SRK HPLIS GC mass% vs VPCR 25,37.8,50,65 C Samples 2,3,4, y = 0.79x R² = V/L=4 Linear (V/L=4) Measured Vapor Pressure (kpa)
42 EOS Calculations Predictions for sample#1 appears to be an outlier. R 2 = 0.89 VPCR 25,37.8,50,65 C and R 2 = 0.93 VPCR 25,37.8,50,65 C Sample #1 methane = 0.25mass% HPLIS vs actual 0.29mass% (highest light ends) D6377 will be repeated EOS may be improved if the molecular weight of the crude becomes available. If the crude has a lower molecular weight than the molecular weight actually used, the errors will be lower.
43 EOS Calculations The maximum error between the results predicted by the simulation with that observed experimentally is within -21.6% for the V/L ratios measurements made where the effect of air saturation in the dead oil is reduced.
44 Current Status Several labs showing interest one other lab set up (CANMET Devon) will do comparisons Calibration sample shows excellent precision Validation sample results between GC and actual values very good D6377 measurements vs EOS D6377 measurements affected by air at low VL D6377 VP vs VL curve can indicate light dissolved gases but air vs C1,C2 can only be discerned by alternate techniques (GC HPLIS, etc)
45 Current Status Characterizing wide variety of samples - condensates, conventional oil, shale oil, dilbits, synbits - Method is on ASTM D02.04 Subcommittee ballot closing Oct 30, 2014
46 Thank you AITF Chris Goss, Trevor Lockyer, Deepyaman Seth CCQTA, ASTM Bob Falkiner Imperial Oil Engineering Services Dan Wispinski Alberta Innovates
Live Crude Oil Volatility
Live Crude Oil Volatility Dan Wispinski : Alberta Innovates Technology Futures Bob Falkiner : Imperial Oil Engineering Services October 16/15 PerkinElmer Corpus Christi Any and all implied or statutory
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