1、Designation:D570503 (Reapproved 2008) Designation: D5705 12Standard Test Method forMeasurement of Hydrogen Sulfide in the Vapor PhaseAbove Residual Fuel Oils1This standard is issued under the fixed designation D5705; the number immediately following the designation indicates the year oforiginal adop
2、tion 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 reapproval.1. Scope*1.1 This test method covers the field determination of hydrogen sulfide (H2
3、S) in the vapor phase (equilibrium headspace) of aresidual fuel oil sample.1.2 The test method is applicable to liquids with a viscosity range of 5.5 mm2/s at 40C to 50 mm2/s at 100C. The test methodis applicable to fuels conforming to Specification D396 Grade Nos. 4, 5 (Heavy), and 6.1.3 The applic
4、able range is from 5 to 4000 parts per million by volume (ppm v/v) (micro mole/mole).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 standard does not purport to address all of the safety concerns, if any, associa
5、ted with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D396 Specification for Fuel OilsD4057 Practice for Manual Sampl
6、ing of Petroleum and Petroleum Products Practice for Manual Sampling of Petroleum andPetroleum ProductsD6021 Test Method for Measurement of Total Hydrogen Sulfide in Residual Fuels by Multiple Headspace Extraction and SulfurSpecific DetectionD7621 Test Method for Determination of Hydrogen Sulfide in
7、 Fuel Oils by Rapid Liquid Phase Extraction3. Terminology3.1 Definitions:3.1.1 equilibrium headspace, nthe vapor space above the liquid in which all vapor components are in equilibrium with theliquid components.3.1.2 residual fuel oil, na fuel oil comprising a blend of viscous long, short, or cracke
8、d residue from a petroleum refiningprocess and lighter distillates blended to a fuel oil viscosity specification.3.1.2.1 DiscussionUnder the conditions of this test (1:1 liquid/vapor ratio, temperature, and agitation) the H2S in the vaporphase (samples headspace) will be in equilibrium with the H2S
9、in the liquid phase.4. Summary of Test Method4.1 A1-L H2S-inert test container (glass test bottle) is filled to 50 volume % with fuel oil from a filled H2S-inert container (glasssample bottle) just prior to testing. In the test container, the vapor space above the fuel oil sample is purged with nitr
10、ogen todisplace air. The test container with sample is heated in an oven to 60C, and agitated on an orbital shaker at 220 rpm for 3 min.4.2 A length-of-stain detector tube and hand-operated pump are used to measure the H2S concentration in the vapor phase ofthe test container. The length-of-stain de
11、tector tube should be close to but not in contact with the liquid surface.5. Significance and Use5.1Excessive levels of hydrogen sulfide in the vapor phase above residual fuel oils in storage tanks may result in a health hazard,OSHA limits violation, and public complaints about odors. Control measur
12、es to maintain safe levels of H1This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.E0 onBurner, Diesel, Non-Aviation Gas Turbine, and Marine Fuels.Current edition approved Dec. 1, 2008.April 15, 2
13、012. Published February 2009.May 2012. Originally approved in 1995. Last previous edition approved in 20032008 asD570503(2008). DOI: 10.1520/D5705-03R08.2For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM
14、Standardsvolume information, refer to the standards Document Summary page on the ASTM website.1This 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 pos
15、sible to adequately depict all 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 standard.C
16、opyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.1 Residual fuel oils can contain H2S in the tank atmosphere for those working in the vicinity require a consistent method forthe assessment of potentially hazardous levels of HS in the
17、liquid phase and this can result in hazardous vapor phase levels of H2S in fuel oils(WarningHS in storage tank headspaces. The vapor phase levels can vary significantly according to the headspace volume, fuel temperature and agitation. Measurement of H2Sisahighlytoxicsubstance.Useextreme care in the
18、 sampling and handling of samples that are suspected of containing high levels of HS levels in the liquid phase providesa useful indication of the residual fuel oils propensity to form high vapor phase levels, and lower levels in the residual fuel oil will directly reduce risk of H2S.).5.2This test
19、method has been developed to provide refineries, fuel terminals, and independent testing laboratories, which do nothave access to analytical instruments such as a gas chromatograph, with a simple and consistent field test method for the rapiddetermination of HS exposure. It is critical, however, tha
20、t anyone involved in handling fuel oil, such as vessel owners and operators, continue to maintain appropriatesafety practices designed to protect the crew, tank farm operators and others who can be exposed to H2S in the vapor phase of residual fuel oils. S.5.1.1 The measurement of H2S in the liquid
21、phase is appropriate for product quality control, while the measurement of H2Sinthe vapor phase is appropriate for health and safety purposes.5.2 This test method was developed to provide refineries, fuel terminals and independent testing laboratories, which do not haveaccess to analytical instrumen
22、ts such as a gas chromatograph, with a simple and consistent field test method for the rapiddetermination of H2S in the vapor phase above residual fuel oils.NOTE 1D5705 is one of three test methods for quantitatively measuring H2S in residual fuels:1) Test Method D6021 is an analytical test method t
23、o determine H2S levels in the liquid phase.2) Test Method D7621 is a rapid test method to determine H2S levels in the liquid phase.NOTE 2Because of the reactivity, absorptivity and volatility of H2S, any measurement method only provides an H2S concentration at a given momentin time.5.3 This test met
24、hod does not necessarily simulate the vapor phase H2S concentration ofin a fuel storage tank. It does, however,provide a level of consistency so that the test result is only a function of the residual fuel oil sample and not the test method,operator, or location. No general correlation can be establ
25、ished between this field test and actual vapor phase concentrations of H2Sin residual fuel oil storage or transports. However, a facility that produces fuel oil from the same crude source under essentiallyconstant conditions might be able to develop a correlation for its individual case.6. Interfere
26、nces6.1 Typically, sulfur dioxide and mercaptans may cause positive interferences. In some cases, nitrogen dioxide can cause anegative interference. Most detector tubes will have a precleanse layer designed to remove certain interferences up to somemaximum interferant level. Consult the manufacturer
27、s instructions for specific interference information.7. Apparatus7.1 Shaker, a bench-top orbital shaker and platform equipped with a four-prong clamp to hold 1-L Boston round-bottom glassbottles and capable of operation at 220 rpm.7.2 Timer, capable of measuring from1sto30minatsecond intervals.7.3 S
28、topper with Temperature Measuring Device, a No. 2 cork stopper with a temperature measuring devices inserted throughit that is capable of accurately measuring the temperature of the sample at 60 6 1C as required in the procedure and extendingat least 25 mm into the residual fuel but no closer than 2
29、5 mm from the bottom of a test bottle (see Fig. 1(a). A dial thermometerhaving a range of 18 to 82C and a 200mm stem has been found suitable to use.7.4 Oven or Water Bath, capable of heating the fuel oil samples to 60 6 1C.7.5 Detector Tube Pump, a hand-operated piston or bellows-type (Fig. 1(b) pum
30、p with a capacity of 100 cm36 5cm3perstroke.3It must be specifically designed for use with detector tubes. (WarningA detector tube and pump together form a unitand must be used as such. Each manufacturer calibrates detector tubes to match the flow characteristics of its specific pump.Crossing brands
31、 of pumps and tubes is not permitted, as considerable loss of system accuracy is likely to occur.)8. Reagents and Materials8.1 ContainersBoth sample and test containers are composed of H2S-inert material such as 1-L size (clear Bostonround-bottom) glass bottles with screw caps. The bottles are clean
32、 and dry. Mark test containers at the 50 % volume level by usinga ruler. (WarningHydrogen sulfide reacts with metal surfaces and is easily oxidized, which depletes its concentration and givesfalse low test results. Containers such as epoxy-lacquered cans are suitable for sample collection. Alternati
33、ve containers must giveequivalent results to those obtained by using glass.)8.2 Length-of-Stain Detector Tube and Calibration Scale, a sealed glass tube with breakoff tips sized to fit the tube holder ofthe detector tube pump. The reagent layer inside the tube, typically a silica gel substrate coate
34、d with the active chemicals, mustbe specific for hydrogen sulfide and must produce a distinct color change when exposed to a sample of gas containing hydrogensulfide. Any substances known to interfere must be listed in the instructions accompanying the tubes. A calibration scale shouldbe marked dire
35、ctly on the tube, or other markings that provide for easy interpretation (reading) of hydrogen sulfide content froma separate calibration scale should be supplied with the tubes. The calibration scale shall correlate H2S concentration to the length3Direct Reading Colorimetric Indicator Tubes Manual,
36、 First Edition, American Industrial Hygiene Association, Akron, OH 44311, 1976.D5705 122of the color stain.AnnexA1 provides additional information. Shelf life of the detector tubes must be a minimum of two years fromthe date of manufacture, when stored according to the manufacturers recommendations.
37、9. Sampling9.1 The sampling of residual fuel oils is done according to Practice D4057 for the sampling of storage tanks, ships, or barges.Composite sampling or running samples can be taken; spot samples should be taken from the midpoint or below midpoint of thefuel oil in a storage tank by first suf
38、ficiently purging sample transfer lines and then taking single samples where each samplecomprises one and only one test. (WarningSamples taken for this test method shall be dedicated to a single H2S determinationand not used for any other purpose, as any additional handling can lead to loss of H2S a
39、nd thus low results.)NOTE1Liquid 3Liquid samples taken well into the fuel oil have had less H2S lost by degassing as compared with a fuel oils surface. Samples takenfrom well within the fuel oil storage provide material that represents the greatest potential for H2S exposure during fuel oil movement
40、s. Hydrogen sulfideis lost by degassing (elevated temperature and mechanical agitation increases H2S degassing), oxidation, and absorption on water-wet surfaces.9.2 Fill at least two 1-L size sample containers with fuel oil. Minimize the headspace of the sample container. Cap immediatelyand deliver
41、to the testing facility. Test each sample within one to four hours from the time of sampling.9.3 Sample integrity is extremely important; therefore, sample containers must be composed of inert materials, filled nearlycompletely with liquid, and capped tightly until tested. Sample handling should be
42、minimized, and rapid testing for H2S is required.Samples can not be stored for later testing as H2S loss may occur by the mechanism described in Note 1Note 3.10. Procedure10.1 Let each filled sample container sit at room temperature for at least 1 h, transfer part of its contents to an empty 1-L tes
43、tbottle such that it is filled 50 % 6 5 volume % with the sample. Discard the remaining contents of the sample container incompliance with applicable laws. A single test is to be performed on material from an individual sample container.10.2 Insert a nitrogen purge line outlet to within about 13 mm
44、above the fuel surface. Nitrogen purge at 2 L/min for 30 s theheadspace above the test sample to displace air and water vapor. Minimize the time the bottle is open to avoid further loss of sampleFIG. 1 Measurement of H2S in the Vapor Phase of Residual FuelOilD5705 123vapors. Close the test bottle op
45、ening (gas tight) with a cork stopper fitted with a dial thermometer (Fig. 1(a) immediately afternitrogen purging.10.3 Place each test bottle with sample in an oven or a water bath, set at 60 6 1C, until the sample temperature reaches 606 1C. Keep the sample in the oven or bath for a minimum of 30 m
46、in, which includes the time for the sample to reach 60C.NOTE2If 4If the sample temperature does not reach 60C, low results will be obtained for the H2S concentration. If the temperature exceeds 60C,high results will be obtained for the H2S concentration.10.4 While the sample is heating, place an unb
47、roken length-of-stain detector tube in the hand-operated pump and test the pumpfor leaks. Consult the manufacturers instructions for leak check procedure details and for maintenance instructions if leaks aredetected. The leak check typically takes 1 min.10.5 Remove the test bottle from the oven and
48、place it in the four-prong clamp of the shaker. Shake at 220 rpm for 3 min 61sto achieve H2S equilibrium between the liquid and the vapor phase.10.6 Rest the test bottle on a flat surface, remove the stopper with the dial thermometer, and immediately seal the top of thebottle with aluminum foil.10.7
49、 Select a detector tube with a range that best encompasses the expected H2S concentration. Reading accuracy is improvedwhen the stain length extends into the upper half of the calibration scale.10.8 Break off the tube tips and insert the tube into the pump, observing the flow direction indication on the tube. Insert the tubethrough the aluminum foil on the test bottle. Rest the pump on top of the test bottle with the detector tube only contacting thesamples vapor phase. Do not allow the detector tube to contact the liquid, see Fig. 1(b). Use on
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