ASTM F2059-17 Standard Test Method for Laboratory Oil Spill Dispersant Effectiveness Using the Swirling Flask.pdf

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1、Designation: F2059 17Standard Test Method forLaboratory Oil Spill Dispersant Effectiveness Using theSwirling Flask1This standard is issued under the fixed designation F2059; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year

2、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. Scope1.1 This test method covers the procedure to determine theeffectiveness of oil spill dispersants on various oils in the

3、laboratory. This test method is not applicable to other chemicalagents nor to the use of such products or dispersants in openwaters.1.2 This test method covers the use of the swirling flask testapparatus and does not cover other apparatuses nor are theanalytical procedures described in this report d

4、irectly appli-cable to such procedures.1.3 The test results obtained using this test method areintended to provide baseline effectiveness values used tocompare dispersants and oil types under conditions analogousto those used in the test.1.4 The test results obtained using this test method areeffect

5、iveness values that should be cited as test values derivedfrom this standard test. Dispersant effectiveness values do notdirectly relate to effectiveness at sea or in other apparatuses.Actual effectiveness at sea is dependant on sea energy, oil state,temperature, salinity, actual dispersant dosage,

6、and amount ofdispersant that enters the oil.1.5 The decision to use or not use a dispersant on an oilshould not be based solely on this or any other laboratory testmethod.1.6 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.7 T

7、his standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.1.8 This internation

8、al standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committ

9、ee.2. Summary of Test Method2.1 Dispersant is pre-mixed with oil and placed on water ina test vessel. The test vessel is agitated on a moving tableshaker. At the end of the shaking period, a settling period isspecified and then a sample of water taken. The oil in the watercolumn is extracted from th

10、e water using a dichloromethanesolvent and analyzed using gas chromatography.2.2 The extract is analyzed for oil using a gas chromato-graph equipped with a flame ionization detector, (GC-FID).Quantification is by means of the internal standard method.Effectiveness values are derived by comparison wi

11、th a cali-brated set of effectiveness values obtained at the same time andby the same method.3. Significance and Use3.1 A standard test is necessary to establish a baselineperformance parameter so that dispersants can be compared, agiven dispersant can be compared for effectiveness on differentoils,

12、 and at different oil weathering stages, and batches ofdispersant or oils can be checked for effectiveness changeswith time or other factors.3.2 Dispersant effectiveness varies with oil type, sea energy,oil conditions, salinity, and many other factors. Test resultsfrom this test method form a baseli

13、ne, but are not to be takenas the absolute measure of performance at sea. Actual fieldeffectiveness could be more or less than this value.3.3 Many dispersant tests have been developed around theworld. This test has been developed over many years usingfindings from world-wide testing to use standardi

14、zedequipment, test procedures, and to overcome difficulties notedin other test procedures.4. Interferences and Sources of Error4.1 Interferences can be caused by contaminants, particu-larly residual oil or surfactants in solvents, on glassware, andother sample processing apparatus that lead to discr

15、ete artifacts1This test method is under the jurisdiction of ASTM Committee F20 onHazardous Substances and Oil Spill Response and is the direct responsibility ofSubcommittee F20.13 on Treatment.Current edition approved April 15, 2017. Published April 2017. Originallyapproved in 2000. Last previous ed

16、ition approved in 2012 as F2059 06(2012)1.DOI: 10.1520/F2059-17Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization establ

17、ished in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1or elevated baselines in gas chromatograms. All glasswaremust be thoroughly cleaned. The cleaning process

18、includesrinsing with dichloromethane to remove the oil, followed byrinsing three times each with tap water, purified water (reverseosmosis), and acetone. Once cleaned, precautions must betaken to minimize contact of the glassware with surfactants toprevent undesired interferences.4.2 Dispersant effe

19、ctiveness is very susceptible to energylevels. Table top shakers generally start and stop slowly.Shakers that start motion rapidly and stop suddenly impart ahigh energy to the system and thus cause more dispersion thanwould be the case with a normal shaker. Furthermore, thisvariation would not be re

20、peatable. The shaker table usedshould be observed for rapid movements or stops to ensure thatit is usable for these tests. The rotational speed of the shakershould be checked with a tachometer every week.4.3 The Erlenmeyer flasks used in this test are tapered andthe energy level varies with the amou

21、nt of fill.4.4 The output is highly sensitive to the volume of oil,water, and extractant delivered. All pipets and dispensersshould be calibrated frequently and verified daily.4.5 The use of positive displacement pipets is mandatory forall controlled volumes of microlitre quantities. Use of volumedi

22、splacement pipets will result in erroneous results due to theviscosity of the dispersants and oils, the variable viscosity ofthe oils to be tested (some semi-solid), and the density ofdichloromethane.4.6 The order of addition of the dispersant and oil haseffects on the accuracy of results, as the di

23、spersant may interactwith the vessel walls if added first, thereby reducing thequantity available in the premix. It is therefore important to addoil to the vessel first, and add the dispersant directly to the oil.Asecond addition of oil is suggested simply because it is easierto control a large volu

24、me of oil than a minute volume ofdispersant when attempting to achieve a specific ratio of 25:1.4.7 Following surfactant addition, vigorous mixing is re-quired to thoroughly homogenize the sample. Sharp, manualstrokes are suggested for light oils, while very heavy oils mayrequire stirring with a cle

25、an glass rod or spatula.4.8 There are indications that the results for some premixeddispersant/oil combinations change over time. It is necessary totake precautions against this potential source of variation. Thetesting should be concluded as soon as possible after thepremix is prepared, generally w

26、ithin a few hours. Results fromsamples stored for periods as long as a week should not beconsidered reliable.4.9 Since the performance of the dispersant is affected bysalinity, the salt water should be thoroughly mixed, stored inairtight containers, and checked with a salinity meter prior touse. Sal

27、inity should be 3.3 6 .1%.4.10 Temperature is a factor in dispersion, so it is importantthat all components (salt water, pre-mix, and temperaturecontrolled chamber) are stable at 20C2(or the chosen operat-ing temperature) before starting.4.11 Extreme care should be taken when applying the oil tothe

28、surface so that mixing does not occur. The oil should gentlyglide across the water to form a slick. If the oil streams out intothe water, the agitation can disperse the oil, increasing theamount of oil dispersed and erroneously raising the finaldispersion result.4.12 A slick may form at the water su

29、rface in the spout ofthe swirling flask during mixing and settling. It is importantthis oil does not enter the water sampled for analysis. Thereforeit is important to drain the contents of the spout (about 3 mL)prior to sampling, and ensure any adhering droplets do notenter the sample.4.13 The proce

30、dure is time critical for the elements ofmixing, settling, and sampling. Care should be taken to adhereto the times indicated in the procedure for both the mixing andsettling element, as variations in energy input, and especiallytime allowed for droplet creaming, can impact results. Sincethe water s

31、amples cannot be sampled simultaneously, this stepmust be performed with as much careful haste as possible, toreduce the difference in settling times experienced by thesamples in the test run.4.14 Analysis of the gas chromatograph-detectable TotalPetroleum Hydrocarbon (TPH) content is subject to var

32、iabilityin GC operation and repeatability. Therefore, it is imperativethat a rigorous quality assurance program is in place to ensurethe GC is functioning properly and valid results are obtained.4.15 Care should be taken to determine the baseline in avalid and repeatable manner for both samples and

33、calibrationsets.4.16 The accuracy and repeatability of the test can beverified and compared using standard oil and dispersantsamples5. Apparatus5.1 Modified 120-mL Erlenmeyer Flask, used as the testvessel. A side spout is added to a standard Erlenmeyer flask toenable sampling from the water column w

34、ith minimal distur-bance of resurfaced oil. This vessel is illustrated in Fig. 1.5.2 Moving-Table Shaker, with an orbital motion of 1 in.(25.4 mm) and fitted with flask holders. Ideally such shakersshould be constructed inside temperature-controlled chambers.If such an enclosed chamber is not used,

35、the measurement mustbe conducted inside temperature-controlled rooms.5.3 Gas Chromatograph (GC), equipped with a flame ion-ization detector is used for analysis. The column is a fusedsilica column.2The normal operating temperature is 20C (6 1C). An alternate temperaturemay be selected based on test

36、requirements.F2059 1725.4 The following is a list of other necessary supplies.Suppliers of suitable units are footnoted. Equivalent suppliesare acceptable in every case. Quantities of supplies are given toconduct a full set of six samples and calibration set:5.4.1 Eighteen Crimp Style Vials, with al

37、uminum/PTFE(polytetrafluoroethylene) seals, 12 by 32 mm,5.4.2 Twelve Erlenmeyer Flasks, 125 mL Glass, modifiedwith the addition of a drain spout attached to base,35.4.3 Six Graduated Mixing Cylinders and Stoppers, 25 mLglass,5.4.4 Six Separatory Funnels and Stoppers, glass, 125 mL,5.4.5 Six Graduate

38、d Mixing Cylinders and Stoppers, glass,100 mL,5.4.6 Six Separatory Funnels and Stoppers, glass, 250 mL,5.4.7 Six Graduated Cylinders, glass, 50 mL,5.4.8 Six Dispenser or Glass Graduated Cylinders, 5to25mL,5.4.9 Positive Displacement Pipet, 10 to 100 L,5.4.10 Positive Displacement Pipet, variable vol

39、ume, 1 mL,5.4.11 Two Digital Timers,5.4.12 Dispenser or Graduated Cylinders, 20 mL to 100mL, and5.4.13 One Plastic Carboy, 20 L.6. Reagents6.1 ReagentsWater purified by reverse osmosis or equiva-lent means is used for the test water. Dichloromethane isdistilled-in-glass grade. Fine granular sodium c

40、hloride or tablesalt, non-iodized, is used for making the salt water. Thechemical dispersant is used as supplied by the manufacturer.Oil is used as received.7. Procedure7.1 Crude Oil and Dispersant Sample Collection andStorageThe bulk oil is mechanically mixed prior to obtaininga working sample. Wor

41、king samples are stored in high-densitypolyethylene bottles with polypropylene screw closures. Theworking sample is mechanically shaken for 30 min at 20C (orthe chosen operating temperature) prior to removing a sub-sample for testing. When not in use, all samples should bestored in a temperature con

42、trolled room at 5C. The dispersantis manually shaken, vigorously, prior to sampling.7.2 Premix Sample PreparationA small amount of oil(approximately 1.0 mL) is weighed into a 5-mL amber vialwith PTFE-lined cap. Approximately 100 mg of dispersant isadded to the oil. Oil is added until a 1:25 ratio (b

43、y weight) ofdispersant to oil is achieved. This is added to achieve the 1:25ratio within 1% by weight. The sample is well mixed bymanual shaking or stirring.7.3 Salt-Water PreparationGranular salt is weighed andadded to water from reverse osmosis (RO) filtration to obtaina 3.3 % (w/v) solution. The

44、water temperature is stabilized to20C (or the chosen operating temperature) before use.7.4 Swirling Flask PreparationThe 120 mL of salt wateris placed into a 125-mL modified Erlenmeyer flask. The flaskis inserted into the flask holders on the oscillating table of theshaker. A 100-L volume of pre-mix

45、 solution is carefullyapplied onto the surface of the water using a positive displace-ment pipet. The tip of the pipet is placed at the water surfaceand the dispersant/oil mixture gently expelled. Extreme careshould be taken when applying the oil to the surface such thatmixing does not occur. The oi

46、l should gently glide across thewater to form a slick. If the oil streams out into the water, theagitation can disperse the oil, increasing the amount of oildispersed and erroneously raising the final dispersion result.Herding of the oil and some creeping of the mixture up thevessel wall is normal b

47、ut can be minimized.7.5 Shaking of Swirling FlasksThe flask and contents aremechanically mixed on the shaker in a temperature controlledchamber at 20C (or the chosen operating temperature), im-mediately after applying the oil to the surface of the water. Arotation speed of 150 r/min and a mixing tim

48、e of 20 min areused to agitate the samples followed by a 10-min settlingperiod. The flasks should be removed from the table-mountedholders prior to the settling period to limit the agitationbetween settling and sampling.7.6 Sample CollectionAfter the settling time is complete,3 mL of oil-in-water ph

49、ase from the spout of the flask aredrained and disposed of to remove any oil residing in the spoutand to obtain a representative sample. A 30-mL aliquot of thedispersed oil in water sample is collected in a graduatedcylinder and transferred to a 125-mL separatory funnel. The oilis extracted three times with 5 mL of the dichloromethanesolvent, shaken vigorously for at least 1 min, and the extract3The sole source of supply of the apparatus known to the committee at this timeis Pro Science, Inc., 770 Birchmount Road, Unit 25, Scarborough, OntarioM1K5H3. If you