Metrohm’s CIC does it: ASTM D Standard Test Method for Total Fluorine, Chlorine and Sulfur in Aromatic Hydrocarbons and Their. Significance and use according to ASTM D – 14a. ASTM D – Standard Test Method for Total Fluorine, Chlorine and Sulfur in Aromatic Hydrocarbons and Their Mixtures by Oxidative Pyrohydrolytic.
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D — 08 Standard Test Method for This standard d739 issued under the? ASTM D – A number in parentheses indicates the year of last reapproval. However, it is the responsibility of the analyst to verify the solubility of the sample in the solvent and that the diluted sample results conform to the precision and accuracy of the method.
ASTM D – 14a : Total Fluorine, Chlorine and Sulfur in Aromatic Hydrocarbons
No other units of measurement are included in this standard. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.
Current edition approved Oct. Summary of Test Method 3. There the sample is combusted in an oxygen rich pyrohydrolytic environment.
The gaseous by-products of the combusted sample are trapped in an absorption medium where the hydrogen halides HX formed during combustion disassociate into their respective ions, Xwhile the sulfur oxides SOX formed are further oxidized to SO in the presence of an oxidizing agent. An aliquot of known volume of the adsorbing solution is then automatically injected into an ion chromatograph IC by means of a sample injection valve.
The halide and sulfate anions are separated into individual elution bands on the separator column of the IC. The combined system of pyrohydrolytic combustion followed by 3 Available from U. This test method can be used to determine total sulfur and halogens aromatic hydrocarbon matrices, in? A high concentration of one anion can interfere with other constituents if their retention times are close enough to affect the resolution of their peak.
L of sample into the sample boat. The autosampler may be used as long as the accuracy and performance of the method is not degraded. These features may be used as long as they do not degrade the performance and accuracy of the method. The system is swept by a humidi? Thermoelectric coolers peltier or recirculating refrigerated liquid devices are strongly recommended.
Switching sample boats between each analysis may prove effective, provided sample size is not too large. The Gas Adsorption Unit is interfaced to the Ion Chromatograph and injects an aliquot of the adsorption solution into the Ion Chromatograph after the sample is combusted and the by-products of combustion are absorbed. L of standard or sample. The inlet end shall allow for the stepwise introduction and advancement of a sample boat into the heated zone and shall have a side arm for the introduction of the humidi?
The pyrohydrolytic combustion tube must be of ample volume, and have a heated zone with quartz wool or other suitable medium providing sufficient surface area so that the complete pyrohydrolytic combustion of the sample is ensured. S with a linearity correlation coefficient of 0. Delivery of hydronium ions for suppression by electrolysis of recycled eluent through a cation exchange membrane. Consult the manufacturer for details in setup and operation.
Other systems may be used as long as precision is shown to be as good as or better than the precision in the method.
L or mg of sample. Reagents and Materials 7. Unless otherwise indicated, it is intended that all reagents d759 conform to the speci? Correction for contaminate levels of elements of interest must be corrected for solvent blank. Alternatively, using a solvent with non-detectable contamination relative to the sample makes the blank correction unnecessary. Dilute to volume with the selected solvent described in 7.
Calculate the actual concentration of the stock standard solution s for each element by using the equation below with the actual recorded weight of the target compound used for each element. This stock standard solution can be further diluted to other desired concentrations. Other suitable materials, weights and volumes may be substituted in preparing stock calibration standards as long as the performance of the method is not degraded. Target Standard Compound s 7. NOTE 3—Other calibration standard sources and diluents may be used if precision and accuracy are not degraded.
NOTE 4—Calibration standards are typically re-mixed and re-certi? Calibration standards can have a useful life of about zstm to 12 months if properly stored in a cool, dark place. NOTE 5—A correction for chemical impurity can be used if deemed necessary. The concentration of phosphate in the absorbing solutions is used as an internal standard by the Ion Chromatograph. Use materials that are rated for containing these hydrocarbons in all sample containers and sample transfer apparatus.
Exercise extra care when using?
In contact with the skin it produces burns that may be quite d73359 unless promptly treated. Its action is insidious since it produces no immediate stinging or burning sensation and damage to the skin may result before its presence is realized.
Eyes are particularly vulnerable to severe damage from alkalis. Eyes are particularly vulnerable to severe damage. These asttm rapidly attack wool and leather. Preparation of Apparatus A typical diagram of a CIC system is d739 in Fig.
NOTE 6—It is recommended to calibrate the instrument with a minimum of three different concentration standards. Other numbers of concentration of calibration standards can be used as long as the accuracy and precision of the method is not degraded. If bubbles are present in the liquid column,?
NOTE 7—Injection of a constant or similar sample size for all materials analyzed promotes consistent combustion conditions. The difference between the two volume readings is the volume of sample injected.
Metrohm: ASTM D7359 – 14a : Total Fluorine, Chlorine and Sulfur in Aromatic Hydrocarbons
NOTE 8—An automatic sampling and injection device or autosampler can be used in place of the described manual injection procedure as long as the accuracy and performance of the method is not degraded. Calibration and Standardization Weigh the syringe before and after injection into the sample boat to determine the amount of sample injected.
The sample may also be weighed directly into a sample boat and placed into the boat drive system. This procedure can provide greater precision than the volume delivery method, provided a balance with a precision of Once the boat has returned to the home position, allow a minimum of two minutes for cooling the boat before introducing the next sample.
NOTE 10—The level of boat cooling required is directly related to the volatility of the sample analyzed. The use of a thermoelectrically cooled sample introduction area may be required to prevent premature volatilization of the sample before entering the combustion area.
After each standard concentration has been combusted, an aliquot of absorbing solution is introduced into the IC for separation and quanti? Retention times vary with operating conditions.
The standards, therefore, must be analyzed by the ion chromatograph in the same manner as the sample solutions.
NOTE 11—A typical calibration would include a series of three to ashm standards containing the elements of interest and bracketing the concentrations that are in the samples.
The calibration curve should be at least 0. Post Analysis Steps Decrease the boat drive introduction rate or hold times in the furnace, or both, if coke or soot is observed on the exit end of the combustion tube.
After any cleaning or adjustment, assemble and leak check the apparatus. Run a check standard to determine if the instrument needs to be recalibrated. The concentrations in the test specimen must be less than the concentration of the highest standard and greater than the lowest standard used in the calibration.
Asstm required a dilution x7359 concentration of the sample can be performed on the sample. NOTE 12—Samples larger than 80? L or 80 mg can be quantitatively absorbed before injecting the absorbing solution into the IC by analyzing multiple injections of sample, combusting each individually and effectively concentrating the elements of interest in the absorbing solution prior to injection into the Ion Chromatograph. The net result of larger sample sizes is an increase in sensitivity and precision of the analysis while lowering the absolute detection limit of the CIC system.
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