D Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Standard + Redline PDF Bundle ASTM License Agreement . D - 14 Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Format, Pages, Price. PDF ASTM License Agreement. Astm Astm d - Download as PDF File .pdf), Text File .txt) or read online.
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An Agilent Simulated Distillation (SIMDIS) system is described for quality control and monitoring of refinery processes. The system uses an Agilent N gas. ASTM D • 80 Seconds. Analysis. Introduction. Simulated distillation is a GC method used to characterize petroleum fractions and products, since it permits. Introduction. ASTM method D describes the gas chromatography. (GC) conditions for simulated distillation of petroleum fractions in the boiling point range.
Table 2 represents the current normal paraffin boiling point values accepted by Subcommittee D B Test Method D has traditionally used n-paraffin boiling points rounded to the nearest whole degree for calibration.
The boiling points listed in Table 2 are correct to the nearest whole number in both degrees Celsius and degrees Fahrenheit. However, if a conversion is made from one unit to the other and then rounded to a whole number, the result will not agree with the table value for a few carbon numbers.
For example, the boiling point of n-heptane is However, converting Carbon numbers 2, 4, 7, 8, 9, 13, 14, 15, 16, 25, 27, and 32 are affected by rounding. Warningn-octane is ammable and harmful if inhaled.
The calibration mixture specied in 7. For open tubular columns, use the mixture specied in 7. WarningCarbon disulde is extremely volatile, ammable, and toxic. The mixture shall cover the boiling range from n-C5 to n-C44, but does not need to include every carbon number see Note 5. Boiling points of n-paraffins are listed in Table 2. Connect the free end of the column to the detector. These columns have much lower column bleed than packed columns.
Column conditioning is less critical with these columns but some conditioning may be necessary. The column can be conditioned very rapidly and effectively using the following procedure. Before heating the column, allow the system to purge with carrier gas at ambient temperature for at least 30 min. Resolution is therefore specied to maintain equivalence between different systems laboratories employing this test method. This must be veried when the system is put in service, and whenever any changes are made to the system or operational parameters.
Analyze the calibration mixture using the identical procedure to be used for the analysis of samples see Section If stationary phases other than those referenced in 7. Calibration and Standardization The schedule will include cooling the column oven to the initial starting temperature, equilibration time, sample injection and system start, analysis, and nal upper temperature hold time. Following the analysis sequence protocol, cool the column to the initial starting temperature.
If a retention time or detector response calibration is being performed, use the peak detection mode. For samples and baseline compensation determinations, use the area slice mode of integration. The recommended slice rate for this test method is 1. Other slice rates may be used if within the limits of 0.
Larger slice rates may be used, as may be required for other reasons, if provision is made to accumulate bunch the slice data to within these limits prior to determination of the boiling range distribution. Follow the analysis sequence protocol for all subsequent repetitive analyses or calibrations.
Since complete resolution of sample peaks is not expected, do not change the detector sensitivity setting during the analysis.
Simulated Distillation of Petroleum Products (ASTM D2887) by GC in
A blank analysis must be performed at least once per day. The blank analysis is necessary due to the usual occurrence of chromatographic baseline instability and is subtracted from sample analyses to remove any nonsample slice area from the chromatographic data.
The blank analysis is typically performed prior to sample analyses, but may be useful if determined between samples or at the end of a sample sequence to provide additional data regarding instrument operation or residual sample carryover from previous sample analyses.
Attention must be given to all factors that inuence baseline stability, such as column bleed, septum bleed, detector temperature control, constancy of carrier gas ow, leaks, instrument drift, and so forth. Periodic baseline blank analyses should be made, following the analysis sequence protocol, to give an indication of baseline stability.
NOTE 6If automatic baseline correction see Note 4 is provided by the gas chromatograph, further correction of area slices may not be required.
ASTM Standards on Rubber Products
However, if an electronic offset is added to the signal after baseline compensation, additional area slice correction may be required in the form of offset subtraction. Consult the specic instrumentation instructions to determine if an offset is applied to the signal. If the algorithm used is unclear, the slice area data can be examined to determine if further correction is necessary. Determine if any offset has been added to the compensated signal by examining the corrected area slices of those time slices that precede the elution of any chromatographic unretained substance.
If these corrected area slices representing the true baseline deviate from zero, subtract the average of these corrected area slices from each corrected area slice in the analysis. Inject an appropriate aliquot 0. Obtain a normal peak detection data record in order to determine the peak retention times and the peak areas for each component.
Collect a time slice area record if a boiling range distribution report is desired. Distortion in retention time measurement and hence errors in boiling point temperature determination will be likely if column overloading occurs. The column liquid phase loading has a direct bearing on acceptable sample size.
Reanalyze the calibration mixture using a smaller sample size or a more dilute solution to avoid peak distortion. The greatest potential for deviation from linearity will be associated with the lower boiling point paraffins.
In general, the lower the sample IBP, the lower will be the starting temperature of the analysis. Although extrapolation of the curve at the upper end is more accurate, calibration points must bracket the boiling range of the sample at both the low and high ends.
Perform an analysis of the gas oil following the analysis sequence protocol. Collect the area slice data and provide a boiling point distribution report as in Sections 12 and If it does not meet the criteria in Table 3, check that all hardware is operating properly and all instrument settings are as recommended by the manufacturer.
Rerun the retention boiling point calibration as described in Procedure A narrow boiling range sample will require a smaller amount injected than a wider boiling range sample. Different volumes of the calibration standard can be injected to nd the maximum amount of a component that the stationary phase can tolerate without overloading see Note the peak height for this amount of sample. The maximum sample signal intensity should not exceed this peak height.
This type of sample may also be diluted with CS2 to control the amount of sample injected to comply with Thus, the most satisfactory procedure is to inspect the chromatogram and the area counts at each interval near the end of the run to determine the point at which the rate of change per second of the chromatographic signal has reached a constant low value of no greater than 0.
In some rather unusual cases, a sample may have individual peaks, separated at the end of the run, which return to baseline between the peaks. In such cases, the total area point of the sample obviously is somewhere beyond the last detectable peak.
Mark this point as the IBP of the sample. This will give the cumulative percent of the sample recovered at each time interval. Using linear interpolation where necessary, determine the retention time associated with each percent between 1 and Report NOTE 9If a plot of the boiling point distribution curve is desired, use graph paper with uniform subdivisions and use either retention time or temperature as the horizontal axis. Plot each boiling temperature against its corresponding normalized percent.
Draw a smooth curve connecting the points. Collect a contiguous time slice area record of the entire analysis. Also see Note 6 regarding automatic baseline correction.
Sum the corrected area slices to obtain the cumulative corrected areas for each time interval during the run. Move back along the chromatogram until a cumulative area equals Mark this point as the FBP.
Some samples have extremely long tailing end portions due to gradually decreasing quantities of heavy materials. This fact, coupled with the natural tendency of the chromatographic baseline to rise at the end of the run due to septum or column bleed or elution of traces of heavy Precision and Bias 6 NOTE 10This precision estimate is based on the analysis of nine samples by 19 laboratories using both packed and open tubular columns.
The range of results found in the round robin are listed in Table 6. Any other means used to dene the distribution would require the use of a physical process, such as a conventional distillation or gas chromatographic characterization. This would therefore result in a method-dependent denition and would not constitute a true value from which bias can be calculated.
Keywords When the retention times of these compounds are compared with n-paraffins of equivalent atmospheric boiling point, these ring compounds appear to be eluted early from methyl silicone rubber columns. A plot showing 36 compounds other than n-paraffins plotted along the calibration curve for n-paraffins alone is shown in Fig. The numbered dots are identied in Table X1. In this gure, the atmospheric boiling points are plotted against the observed retention times. If columns containing different percentages of stationary phase or different temperature programming rates were used, the slope and curvature of the n-paraffin curve solid line would change, but the relative relationships would remain essentially the same.
Deviations of simulated distillation boiling points, as estimated from the curve, from actual boiling points for a few compounds are shown in Table X1. The deviations obtained by plotting boiling points at 10 mm rather than mm are tabulated also.
It is apparent that the deviation is much less at 10 mm pressure. This indicates that the distillation data produced by gas chromatography closely approximates those obtained in reduced pressure distillation. Since the vapor-pressure-temperature curves for multiple-ring type compounds do not have the same slope or curvature as those of n-paraffins, an apparent discrepancy would exist when n-paraffin boiling points at atmospheric pressure are used.
Thus, distillation data are subject to the same deviations experienced in simulated distillation by gas chromatography. A comparison of data obtained from TBP distillation with those obtained from simulated distillation of three high boiling petroleum fractions is shown in Table X1. The TBP distillations were made on theoretical plate spinning band columns at 1 mm Hg pressure.
SD, C F Decanted Oil TBP, C F Discussion The protocol described here utilizes cyclic operation of a single reactor containing a batch of fluidized catalyst particles to simulate feed oil cracking and catalyst regeneration. The oil to be cracked is preheated and fed from the top through an injector tube with its tip close to the bottom of the fluid bed.
The vapor generated after catalytic cracking is condensed and collected in a receiver, and the liquid product collected is subsequently analyzed for simulated distillation to determine yields of fractions in different boiling ranges.
The noncondensable gaseous product is sent to an on-line gas chromatograph for analysis to determine yields of dry gas and liquefied petroleum gas.
The volume of the gaseous product is measured by the water displacement method.
Chemistry and Technology of Lubricants
Levels of CO2 are measured quantitatively via an IR cell and are converted to coke yield. Any water formed is recovered and determined by Karl Fischer titration.
One benefit to this procedure is the use of the automated sequence carried out by the LTU during the reaction process. After initiating the test sequence in step 3. If there is spent catalyst remaining in the reactor from previous runs, it is discharged into the waste vessel, and fresh catalyst from the specified hopper is loaded into the reactor.
The syringe is then filled at a feed rate of 1. Finally, N2 flow to the IR gas analyzer is started and the system records the initial mass on the scale used to weigh displaced water and the pressure of the initial product gas which should be zero.
Following priming, the syringe pump is set in motion and feed is first diverted back to the feed bottle for 10 sec first slop time followed by feed injection into the reactor for a preset time after switching back the three-way valve ahead of the syringe pump. Upon completion of injection, feed is diverted back again to the feed bottle for another 10 sec second slop time. At the end of feed injection, counts begin for both liquid strip time and catalyst strip time.
The former is chosen as 7 liquid strip multiplier times the feed injection time while the latter equals liquid strip time less 10 sec with a maximum sec. The product flows are sent to the gas collection vessel through liquid receivers where high-boiling products are condensed. Catalyst regeneration starts with valve switches at the end of the catalyst stripping cycle.
The CO2 concentration is continuously monitored by the IR gas analyzer until it is below 0. The air is turned off and the N2 flow to the reactor is re-established at the end of regeneration.
At this stage, the liquid receiver for the run can be removed manually from the system for subsequent handling if desired. The line between the collection vessel and the GC is purged with product gas, and the loop is filled for the subsequent GC analysis.
Return the unit to the first step of the test sequence for a new run, or discharge the spent catalyst to the waste vessel if it is the last run. The established protocol proves successful in production of transportation fuels from canola oil in a blend.
Good material balances mass recoveries are obtained in this study with a mean of The conversions and yields from duplicate runs at The protocol is largely based on the LTU operating manual.
The procedures in the manual must be strictly followed, except as noted. Critical steps within the protocol include preparation of equilibrium catalyst must be on-size and coke-free ; reactor preparation using a feed line that yields a constant injector height, either 1. One modification in the protocol that deviates from the LTU operating manual and ASTM D is that in the final step of weighing the liquid receiver, the stopper is quickly removed from and put back in the receiver to equalize the pressure before weighing.
This allows release of excess N2, which is trapped at coolant temperature. However, it may also risk the chance of losing some gaseous product. Theoretically, this step may reduce the mass balance by 2. The result agrees with experimental values versus decreases in mass balance by 3.
The high rapeseed oil concentration appears to be harmful to the system, requiring more frequent changes of the injector than normal, especially when pure canola oil is cracked. At low concentrations such as the one presented in this study, fouling did not occur.For some of the runs using the said LTU, the simulated distillation results show significant amounts of dissolved gases in the liquid products due to the waxy nature of the feeds, resulting in overestimated gasoline yields and conversions.
The schedule will include cooling the column oven to the initial starting temperature, equilibration time, sample injection and system start, analysis, and nal upper temperature hold time. For example, the boiling point of n-heptane is This correlation model is only valid for diesel and jet fuels, excluding biodiesels.
About this book
Our innovative detection, imaging, informatics and service capabilities, combined with deep market knowledge and expertise, help customers gain earlier and more accurate insights to improve lives and the world around us. Color code — black for base oil, pink for blend; thin lines — before feed injection; thick lines — after feed injection. These solutions are designed for commercial, government, product quality, and academic research professionals running high-sensitivity GC analyses on a wide range of food, environmental, pharmaceutical, and petrochemical samples for compliance with safety and regulatory standards.
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