ASTM-D – Download as PDF File .pdf), Text File .txt) or read online. Find the most up-to-date version of ASTM D at Engineering This application note demonstrates detemination of sulfur in hydrocarbon fuels by LECO CHN with Sulfur Add-On Module (S) in accordance with ASTM.
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Sulfur with the chemical symbol S is the chemical element that is in the sixth and third groups of the periodic table of elements. Sulfur is a non-metallic, multi-volume, most commonly known as yellow crystals in sulfide and sulfate minerals.
Two of the three procedures use iodate detection ; one employing an induction furnace for pyrolysis, the other a resistance furnace. The third procedure uses IR detection following pyrolysis in a resistance furnace. A standardization factor is employed to obtain accurate results. The combustion products astn passed into an absorber containing an acid solution of potassium iodide and starch indicator.
A faint blue color is developed in the absorber solution by the addition of standard potassium iodate solution. As combustion proceeds, bleaching the blue color, more iodate is added. The amount of standard iodate consumed during the combustion is a measure of the sulfur content of the sample.
Most sulfur present is combusted to SO2 which is then measured with an infrared detector after moisture and dust are removed by traps. A microprocessor calculates the mass percent sulfur from the sample weight, the integrated detector signal and a predetermined calibration factor. Both the sample identification number and mass percent sulfur are then printed out.
The calibration asgm is determined using standards approximating the material to be analyzed. The IR system can tolerate somewhat higher concentrations. Nitrogen when present in excess of 0. Nitrogen d152 not interfere with the IR system.
The alkali and alkaline earth metals, as well as zinc, phosphorus, and lead, do not interfere with either system. Two major types are available, the primary difference being the manner in which the necessary high temperatures are obtained.
These two types are as follows: The furnace work coil should have a minimum output of W; the minimum input rating of the furnace must be W. With the correct amount of iron chips, weighed to Absorber, as described in Test Method D Beret, standard mL or automatic types available from the manufacturers of the specific combustion units, are suitable. Specific combustion assemblies require additional equipment such as crucibles, combustion boats, crucible lids, boat pushers, separator disks, combustion tubes, sample inverters, oxygen flow indicator, and oxygen drying trains.
The additional equipment required is dependent on the type of furnace used and is available from the manufacturer of the specific combustion unit. Take samples in accordance with the instructions in Practice D Preparation of Apparatus Induction-Type Furnace Assemble the apparatus according to the instructions furnished by the manufacturer. Purify the oxygen by passing it through 1 H2SO4 relative density 1. Connect a rotameter between the purifying train and the furnace.
Insert a small glass-wool plug in the upper end of the glass tubing connecting the furnace with the absorber to catch oxides of tin. Connect the exit end of the combustion tube to the absorber with glass tubing, using gum rubber tubing to make connections. Position the absorber so as to make this delivery line as short as possible.
Adjust the oxygen flow to 1 6 0. Add a sufficient amount of the appropriate standard KIO3 solution Table 1 to produce a faint blue color.
ASTM D|Gilsonite sulfur|Gilsonite sulfur content
This color will serve as the end point for the titration. Adjust the buret to zero. Turn on the furnace filament switch and allow at astk 1 min warm-up before running samples. Assemble the apparatus according to the instructions furnished by the manufacturer. Adjust the oxygen flow rate to 2 6 0. Add 65 mL of HCl 3 6 and 2 mL of starch-iodide solution to the absorber.
Add a few drops of the appropriate standard KIO3 solution Table 2 to produce a faint blue color. Determination of Alum Factor: To assure that the furnace is in proper adjustment and that its operation produces acceptably high temperature, potassium alum is employed for standardizing the apparatus. Depending on the type of combustion equipment used, proceed as described in Sections to determine the alum factor.
Use 15 mg weighed to Use the same materials in the determination of the alum and standardization factors as for the unknown samples. For example, V2O5 has a definite effect and should be included if used for unknowns as recommended in the procedure with the resistance-type furnace.
Calculate the alum factor as follows: The alum factor should be in the range from 1. If values smaller than 1. If values larger than 1. Determination of Standardization Factor: Because effects such as sample volatility can also affect the relative recovery as SO2 of the sulfur originally present in the sample, it is necessary to determine a standardization factor. Proceed as described in Sectionsusing an oil sample asym similar type to the unknown sample and of accurately known sulfur content.
For S1552 detectiondetermine and load the microprocessor with the calibration factor for the particular type of sample to be analyzed lubricating oil, petroleum coke, residual fuel as recommended by the manufacturer.
Calculate the standardization factor as follows: Run a suitable analytical quality control sample several times daily. When the observed value lies between acceptable limits on a quality control chart, proceed with sample determinations.
Standard Test Method for Sulfur in Petroleum Products High-Temperature Method About sulfur Sulfur with the chemical symbol S is the chemical element that is in the sixth and third groups of the periodic table of elements.
Induction Type, which depends upon the high frequency electrical induction aztm of heating. Miscellaneous Apparatus Specific combustion assemblies require additional equipment such as crucibles, combustion boats, crucible lids, boat pushers, separator disks, combustion tubes, sample inverters, oxygen flow indicator, and oxygen drying trains. Potassium Alum Aluminum Potassium Sulfate.
(Lamp method) sulfur content analyzer astm d1552 sulfur content tester
Potassium Iodate, Standard Solution 0. Thoroughly mix the solution. Ascarite, 8 to 20 mesh. Special Materials for Induction-Type Furnaces: Tin 20 to mesh. Iron-Chip Accelerator having a sulfur content of notmore than 0. Starch-Iodide Solution—Make a paste by adding 9 g of soluble starch to 15 mL of water. Add this mixture, with stirring, to mL of boiling water. Cool the mixture, add 15g of potassium iodide KIand dilute to 1 L with water. Sulfuric Acid relative density 1.
Vanadium Pentoxide, anhydrous, powdered V2O5.
Sampling Take samples in accordance with the instructions in Practice D Resistance—Type Furnace Assemble the apparatus according to the instructions furnished by the manufacturer. Standardization For Iodate Methods: