ASTM D7359-2018 Standard Test Method for Total Fluorine Chlorine and Sulfur in Aromatic Hydrocarbons and Their Mixtures by Oxidative Pyrohydrolytic Combustion f.pdf

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1、Designation: D7359 14aD7359 18Standard Test Method forTotal Fluorine, Chlorine and Sulfur in AromaticHydrocarbons and Their Mixtures by OxidativePyrohydrolytic Combustion followed by IonChromatography Detection (Combustion IonChromatography-CIC)1This standard is issued under the fixed designation D7

2、359; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reappro

3、val.1. Scope*1.1 This test method covers the individual determination of total fluorine, chlorine and sulfur in aromatic hydrocarbons and theirmixtures. Samples containing 0.10 to 10 mg/kg of each element can be analyzed.1.2 This method can be applied to sample concentrations outside the range of th

4、e scope by dilution of the sample in anappropriate solvent to bring the total concentrations of fluorine, chlorine and sulfur within the range covered by the test method.However, it is the responsibility of the analyst to verify the solubility of the sample in the solvent and that the diluted sample

5、 resultsconform to the precision and accuracy of the method.1.2.1 Special considerations must be made in order to attain detection limits below 1.0 mg/kg in a sample. The instrument mustbe clean and properly maintained to address potential sources of contamination, or carryover, or both. Multiple se

6、quentialinjections shall be completed until a stable background is attained. A stable background is considered to be achieved when theanalysis of a minimum of three consecutive system blanks have area counts equal to or less than 5 % 5 % RSD for the anions ofinterest.1.3 In determining the conforman

7、ce of the test results using this method to applicable specifications, results shall be roundedoff in accordance with the rounding-off method of Practice E29.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standar

8、d does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine theapplicability of regulatory limitations prior to use. See

9、 Section 9.1.6 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Bar

10、riers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD3437 Practice for Sampling and Handling Liquid Cyclic ProductsD3505 Test Method for Density or Relative Density of Pure Liquid ChemicalsD6809 Guide for Quality Control and Quality Assuranc

11、e Procedures for Aromatic Hydrocarbons and Related MaterialsE29 Practice for Using Significant Digits in Test Data to Determine Conformance with SpecificationsE177 Practice for Use of the Terms Precision and Bias in ASTM Test MethodsE288 Specification for Laboratory Glass Volumetric Flasks1 This tes

12、t method is under the jurisdiction of ASTM Committee D16 on Aromatic Hydrocarbons Aromatic, Industrial, Specialty and Related Chemicals and is the directresponsibility of Subcommittee D16.04 on Instrumental Analysis.Current edition approved Dec. 1, 2014Nov. 1, 2018. Published January 2015December 20

13、18. Originally approved in 2008. Last previous edition approved in 2014 asD7359 14.14a. DOI: 10.1520/D7359-14A.10.1520/D7359-18.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information

14、, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict a

15、ll changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,

16、100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test MethodE969 Specification for Glass Volumetric (Transfer) Pipets2.2 Other Documents:OSHA Regulations, 29 CFR paragraphs 1910.1

17、000 and 1910.1200 33. Terminology3.1 Definitions:3.1.1 combustion ion chromatography, nan analytical system consisting of pyrohydrolytic combustion followed by ionchromatographic detection.3.1.2 oxidative pyrohydrolytic combustion, na process in which a sample undergoes combustion at temperatures gr

18、eater than900C in an oxygen rich environment and in the presence of excess water vapor not originating from the combustion of the sample.In oxidative pyrohydrolytic combustion, the sample is pyrolyzed into carbon dioxide, water, hydrogen halides and residual ash;typically elemental oxides.3.1.3 halo

19、gens (X), nthe elements fluorine, chlorine, bromine and iodine.3.1.4 hydrogen halide (HX), nare inorganic compounds with the formula HX where X is one of the halogens: fluorine,chlorine, bromine, and iodine. Hydrogen halides are gases that dissolve in water to give acids.3.1.5 sulfur oxide (SOx), nr

20、efers to one or more of the following compounds:3.1.5.1 sulfur dioxide (SO2)3.1.5.2 sulfur trioxide (SO3)3.1.5.3 sulfate (SO4)3.1.6 system blank, na combustion ion chromatography (CIC) analysis with no solvent or sample injection in which the samecombustion, chromatography and time protocols are use

21、d as for the sample analysis, but without the combustion of a sample orsolvent blank. The system blank must be equal to or less than 50 % (150 %2) (1/2) the area counts of the lowest calibrationstandard used for calibration and a maximum of 50 % 50 % (1/2) of the area count of the solvent blank used

22、 in the preparationof the calibration standards for the anions of interest.3.1.7 solvent blank, na combustion ion chromatography (CIC) analysis of the solvent used for preparation of the calibrationstandards in which the same combustion, chromatography, time protocols and injection volumes are used

23、as for the sampleanalysis. The solvent blank area count must be less than or equal to two times (2) the system blank and 50 % (1/2) or less thanthe area counts of the lowest calibration standard used in the calibration of the system for the anions of interest.3.1.8 stock standard solution, nstandard

24、 prepared from primary standards and subsequently used to prepare the workingstandard.3.1.9 working standard solution, nstandard prepared from the stock standard solution and subsequently used to prepare thecalibration standards.3.1.10 calibration standard, nstandard prepared from the working standa

25、rd and subsequently used to calibrate the instrument.3.2 Abbreviations:3.2.1 CICcombustion ion chromatography3.2.2 Concconcentration3.2.3 CRMcertified reference material3.2.4 HCIhydrogen choloridechloride3.2.5 HFhydrogen fluoride3.2.6 HXhydrogen halide3.2.7 ICion chromatograph or ion chromatography3

26、.2.8 SOxsulfur oxide (SO2 and SO3)3.2.9 SO2sulfur dioxide3.2.10 SO3sulfur trioxide3.2.11 SO4sulfate3.2.12 Stdstandard3.2.13 SRMstandard reference material3 Available from U.S. Government Printing Office Superintendent of Documents, 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/

27、www.access.gpo.gov.D7359 1824. Summary of Test Method4.1 Asample of known weight or volume is placed into a sample boat and introduced at a controlled rate into a high temperaturecombustion tube. There the sample is combusted in an oxygen rich pyrohydrolytic environment. The gaseous by-products of t

28、hecombusted sample are trapped in an absorption medium where the hydrogen halides (HX) formed during combustion disassociateinto their respective ions, X- while the sulfur oxides (SOX) formed are further oxidized to SO42- in the presence of an oxidizingagent. An aliquot of known volume of the absorb

29、ing solution is then automatically injected into an ion chromatograph (IC) bymeans of a sample injection valve. The halide and sulfate anions are separated on the anion separation column of the IC. Theconductivity of the eluent is reduced with an anion suppression device prior to the ion chromatogra

30、phs conductivity detector,where the anions of interest are measured. Quantification of the fluorine, chlorine and sulfur in the original combusted sample isachieved by first calibrating the system with a series of standards containing known amounts of fluorine, chlorine and sulfur andthen analyzing

31、unknown samples under the same conditions as the standards. The combined system of pyrohydrolytic combustionfollowed by ion chromatographic detection is referred to as Combustion Ion Chromatography (CIC).5. Significance and Use5.1 The total fluorine, chlorine and sulfur contained in aromatic hydroca

32、rbon matrices can contribute to emissions, be harmfulto many catalytic chemical processes, and lead to corrosion. This test method can be used to determine total sulfur and halogensin aromatic hydrocarbons and their mixtures. The results can be used for compliance determinations when acceptable to a

33、regulatory authority using performance based criteria.6. Interferences6.1 Substances that co-elute with the anions of interest will interfere.Ahigh concentration of one anion can interfere with otherconstituents if their retention times are close enough to affect the resolution of their peak.7. Appa

34、ratus7.1 Autosampler, capable of accurately delivering a known volume of sample, typically in the range of 10 to 100 L, into thesample boat.NOTE 1The sample syringe should be rinsed with clean solvent followed by a rinse with the next sample when changing from one vial to another.Follow the manufact

35、urers recommendation to minimize carryover.7.2 Balance, analytical, with sensitivity to 0.0001 g.7.3 Boat Inlet SystemThe system provides a sampling port for the introduction of liquid samples into the sample boat and isconnected to the inlet of the combustion tube.The system is swept by a humidifie

36、d inert carrier gas and shall be capable of allowingthe quantitative delivery of the material to be analyzed into the oxidation zone at a controlled rate.7.4 Boat Inlet CoolerSample volatility requires an apparatus capable of cooling the sample boat prior to sample injection intothe boat.7.5 Gas Flo

37、w ControlThe apparatus must be equipped with flow controllers capable of maintaining a constant flow of oxygenand argon or helium carrier gas.7.6 FurnaceAn electric furnace which can maintain a minimum temperature of 900C.7.7 Gas Absorption Unit, having an absorption tube with sufficient capacity to

38、 hold a minimum of 5 mL which is automaticallyfilled with a known volume of absorption solution by a built-in burette or other similar device. The gas absorption unit is interfacedto the IC and injects an aliquot of the absorption solution into the IC after the sample is combusted and the by-product

39、s ofcombustion are absorbed. The gas absorption unit rinses the absorption tube and the transfer lines from the combustion tube to thegas absorption unit with Type I reagent water (8.2) or other appropriate absorption solution prior to sample combustion and afterthe absorption solution is injected i

40、nto the IC to minimize cross contamination.7.8 Gas-Tight Sampling Syringe, of 10, 25, 50, 100, or 250- L capacity and capable of accurately delivering microliterquantities.7.9 Pyrohydrolytic Combustion Tube made of quartz and capable of withstanding temperatures up to 1100C. The combustiontube must

41、be of ample volume and may include quartz wool or other suitable medium to provide sufficient mixing and surface areato ensure complete combustion of the sample.7.10 Humidifier Delivery System, capable of delivering Type 1 reagent water (8.2) to the combustion tube at a controlled ratesufficient to

42、provide a pyrohydrolytic environment.7.11 Ion Chromatograph (IC),4an analytical system with all required accessories including columns, suppressor and detector.4 Many different companies manufacture automatic ion chromatographs. Consult the specific manufacturer instruction manuals for details regar

43、ding setup and operation.D7359 1837.11.1 Injection System, capable of delivering 20 to 500 L with a precision better than 1 % 1 % or as recommended for thisdetermination by the manufacturer. Larger volumes can be used as long as the performance criteria of the method are not degraded.7.11.2 Pumping

44、System, capable of delivering mobile phase flows between 0.2 and 2.5 mL/min with a precision better than 2 %,2 %, or as recommended for this determination by the manufacturer.7.11.3 Continuous Eluent Generation (optional), to automatically prepare and purify the eluent used in the ion chromatography

45、.Electrolytic eluent generation and auto-buret preparation of eluent by means of in-line dilution of a stock solution have been foundsatisfactory for this method. Other continuous eluent generation devices may be used if the precision and accuracy of the methodare not degraded.7.11.4 Anion Pre-conce

46、ntration Column (optional), used for anion pre-concentration and matrix elimination. Pre-concentrationenables larger volumes of absorbing solution (1 to 3 mL) to be analyzed without the associated water dip. Matrix elimination refersto the elimination of any unreacted hydrogen peroxide in the absorb

47、ing solution prior to injection onto the guard and anionseparator columns and potentially interfere with the fluoride peak resolution.7.11.5 Guard Column, for protection of the analytical column from strongly retained constituents. Improved separation isobtained with additional theoretical plates.7.

48、11.6 Anion Separator Column, capable of producing satisfactory baseline separations of the anion peaks of interest as shownin Fig. 1.7.11.7 Anion Suppressor Device, reduces the background conductivity of the eluent after separation by the anion separatorcolumn. Both chemical and continuous electroly

49、tic suppressors have been found satisfactory for this method. Other anionsuppressor devices may be used as long as the precision and accuracy of the method are not degraded.7.11.8 Conductivity Detector, temperature controlled to 0.01C, capable of at least 0 to 1000 S/cm on a linear scale.7.11.8 Data Acquisition System, an integrator or computer data handling system capable of integrating the peak areas of ionchromatograph7.12 Quartz or Ceramic Sample Boats of sufficient size to hold 10 to 100 L.The boat is filled with quartz wool or othe