1、Designation: F2059 06 (Reapproved 2012)1F2059 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
2、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 NOTEAn editorial change was made to Section 6 in February 2012.1. Scope1.1 This test method covers
3、 the procedure to determine the effectiveness of oil spill dispersants on various oils in the laboratory.This test method is not applicable to other chemical agents nor to the use of such products or dispersants in open waters.1.2 This test method covers the use of the swirling flask test apparatus
4、and does not cover other apparatuses nor are theanalytical procedures described in this report directly applicable to such procedures.1.3 The test results obtained using this test method are intended to provide baseline effectiveness values used to comparedispersants and oil types under conditions a
5、nalogous to those used in the test.1.4 The test results obtained using this test method are effectiveness values that should be cited as test values derived from thisstandard test. Dispersant effectiveness values do not directly relate to effectiveness at sea or in other apparatuses. Actualeffective
6、ness at sea is dependant on sea energy, oil state, temperature, salinity, actual dispersant dosage, and amount of dispersantthat enters the oil.1.5 The decision to use or not use a dispersant on an oil should not be based solely on this or any other laboratory test method.1.6 The values stated in SI
7、 units are to be regarded as standard. No other units of measurement are included in this standard.1.7 This standard 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 and healt
8、h practices and determine the applicability of regulatorylimitations prior to use.1.8 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
9、and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Summary of Test Method2.1 Dispersant is pre-mixed with oil and placed on water in a test vessel. The test vessel is agitated on a moving table shaker.At the end of the shaking period, a settling
10、period is specified and then a sample of water taken. The oil in the water column isextracted from the water using a pentane/dichloromethane mixturedichloromethane solvent and analyzed using gas chromatog-raphy.2.2 The extract is analyzed for oil using a gas chromatograph equipped with a flame ioniz
11、ation detector, (GC-FID).Quantification is by means of the internal standard method. Effectiveness values are derived by comparison with a calibrated setof effectiveness values obtained at the same time and by the same method.3. Significance and Use3.1 A standard test is necessary to establish a bas
12、eline performance parameter so that dispersants can be compared, a givendispersant can be compared for effectiveness on different oils, and at different oil weathering stages, and batches of dispersant oroils can be checked for effectiveness changes with time or other factors.1 This test method is u
13、nder the jurisdiction of ASTM Committee F20 on Hazardous Substances and Oil Spill Response and is the direct responsibility of SubcommitteeF20.13 on Treatment.Current edition approved Feb. 1, 2012April 15, 2017. Published February 2012April 2017. Originally approved in 2000. Last previous edition ap
14、proved in 20062012 asF2059 06.F2059 06(2012)1. DOI: 10.1520/F2059-06R12E01.10.1520/F2059-17This 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 possibl
15、e 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West
16、Conshohocken, PA 19428-2959. United States13.2 Dispersant effectiveness varies with oil type, sea energy, oil conditions, salinity, and many other factors. Test results fromthis test method form a baseline, but are not to be taken as the absolute measure of performance at sea. Actual field effective
17、nesscould be more or less than this value.3.3 Many dispersant tests have been developed around the world. This test has been developed over many years using findingsfrom world-wide testing to use standardized equipment, test procedures, and to overcome difficulties noted in other test procedures.4.
18、Interferences and Sources of Error4.1 Interferences can be caused by contaminants, particularly residual oil or surfactants in solvents, on glassware, and othersample processing apparatus that lead to discrete artifacts or elevated baselines in gas chromatograms. All glassware must bethoroughly clea
19、ned. The cleaning process includes rinsing with dichloromethane to remove the oil, followed by rinsing three timeseach with tap water, purified water (reverse osmosis), and acetone. Once cleaned, precautions must be taken to minimize contactof the glassware with surfactants to prevent undesired inte
20、rferences.4.2 Dispersant effectiveness is very susceptible to energy levels. Table top shakers generally start and stop slowly. Shakers thatstart motion rapidly and stop suddenly impart a high energy to the system and thus cause more dispersion than would be the casewith a normal shaker. Furthermore
21、, this variation would not be repeatable. The shaker table used should be observed for rapidmovements or stops to ensure that it is usable for these tests. The rotational speed of the shaker should be checked with atachometer every week.4.3 The Erlenmeyer flasks used in this test are tapered and the
22、 energy level varies with the amount of fill.4.4 The output is highly sensitive to the volume of oil, water, and extractant delivered. All pipets and dispensers should becalibrated frequently and verified daily.4.5 The use of positive displacement pipets is mandatory for all controlled volumes of mi
23、crolitre quantities. Use of volumedisplacement pipets will result in erroneous results due to the viscosity of the dispersants and oils, the variable viscosity of the oilsto be tested (some semi-solid), and the density of dichloromethane.4.6 The order of addition of the dispersant and oil has effect
24、s on the accuracy of results, as the dispersant may interact with thevessel walls if added first, thereby reducing the quantity available in the premix. It is therefore important to add oil to the vesselfirst, and add the dispersant directly to the oil. A second addition of oil is suggested simply b
25、ecause it is easier to control a largevolume of oil than a minute volume of dispersant when attempting to achieve a specific ratio of 25:1.4.7 Following surfactant addition, vigorous mixing is required to thoroughly homogenize the sample. Sharp, manual strokes aresuggested for light oils, while very
26、 heavy oils may require stirring with a clean glass rod or spatula.4.8 There are indications that the results for some premixed dispersant/oil combinations change over time. It is necessary to takeprecautions against this potential source of variation. The testing should be concluded as soon as poss
27、ible after the premix isprepared, generally within a few hours. Results from samples stored for periods as long as a week should not be considered reliable.4.9 Since the performance of the dispersant is affected by salinity, thorough mixing of the salt water is required. Care shouldalso be observed
28、to avoid evaporation from open containers of salt water. Over a period of days and weeks, the loss of water cansignificantly increase the salinity. An airtight closure is recommended to maintain salinity levels at 3.3 %.should be thoroughlymixed, stored in airtight containers, and checked with a sal
29、inity meter prior to use. Salinity should be 3.3 6 .1%.4.10 Temperature is a factor in dispersion, so it is important that all components (salt water, pre-mix, and temperature controlledchamber) are stable at 20C2 (or the chosen operating temperature) before starting.4.11 Extreme care should be take
30、n when applying the oil to the surface so that mixing does not occur. The oil should gentlyglide across the water to form a slick. If the oil streams out into the water, the agitation can disperse the oil, increasing the amountof oil dispersed and erroneously raising the final dispersion result.4.12
31、 A slick may form at the water surface in the spout of the swirling flask during mixing and settling. It is important this oildoes not enter the water sampled for analysis. Therefore it is important to drain the contents of the spout (about 3 mL) prior tosampling, and ensure any adhering droplets do
32、 not enter the sample.4.13 The procedure is time critical for the elements of mixing, settling, and sampling. Care should be taken to adhere to thetimes indicated in the procedure for both the mixing and settling element, as variations in energy input, and especially time allowedfor droplet creaming
33、, can impact results. Since the water samples cannot be sampled simultaneously, this step must be performedwith as much careful haste as possible, to reduce the difference in settling times experienced by the samples in the test run.4.14 Analysis of the gas chromatograph-detectable Total Petroleum H
34、ydrocarbon (TPH) content is subject to variability in GCoperation and repeatability. Therefore, it is imperative that a rigorous quality assurance program is in place to ensure the GC isfunctioning properly and valid results are obtained.2 The normal operating temperature is 20C (6 1C). An alternate
35、 temperature may be selected based on test requirements.F2059 1724.15 Care should be taken to determine the baseline in a valid and repeatable manner for both samples and calibration sets.4.16 The accuracy and repeatability of the test can be verified and compared using standard oil and dispersant s
36、amples5. Apparatus5.1 Modified 120-mL Erlenmeyer Flask, used as the test vessel. A side spout is added to a standard Erlenmeyer flask to enablesampling from the water column with minimal disturbance of resurfaced oil. This vessel is illustrated in Fig. 1.5.2 Moving-Table Shaker, with an orbital moti
37、on of 1 in. (25.4 mm) and fitted with flask holders. Ideally such shakers shouldbe constructed inside temperature-controlled chambers. If such an enclosed chamber is not used, the measurement must beconducted inside temperature-controlled rooms.5.3 Gas Chromatograph (GC), equipped with a flame ioniz
38、ation detector is used for analysis. The column is a fused silicacolumn.5.4 The following is a list of other necessary supplies. Suppliers of suitable units are footnoted. Equivalent supplies areacceptable in every case. Quantities of supplies are given to conduct a full set of six samples and calib
39、ration set:5.4.1 Eighteen Crimp Style Vials, with aluminum/PTFE (polytetrafluoroethylene) seals, 12 by 32 mm,5.4.2 Twelve Erlenmeyer Flasks, 125 mL Glass, modified with the addition of a drain spout attached to base,35.4.3 Six Graduated Mixing Cylinders and Stoppers, 25 mL glass,5.4.4 Six Separatory
40、 Funnels and Stoppers, glass, 125 mL,5.4.5 Six Graduated 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, 5 to 25 mL,5.4.9 Positive Displacement Pipet, 1
41、0 to 100 L,5.4.10 Positive Displacement Pipet, variable volume, 1 mL,5.4.11 Two Digital Timers,5.4.12 Dispenser or Graduated Cylinders, 20 mL to 100 mL, and5.4.13 One Plastic Carboy, 20 L.3 The sole source of supply of the apparatus known to the committee at this time is Pro Science, Inc., 770 Birch
42、mount Road, Unit 25, Scarborough, Ontario M1K5H3.If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consideration at a meetingof the responsible technical committee,1 which you may attend.FIG. 1 Flask with
43、Side SpoutF2059 1736. Reagents6.1 ReagentsWater purified by reverse osmosis or equivalent means is used for the test water. Dichloromethane and pentaneare distilled-in-glass grades.is distilled-in-glass grade. Fine granular sodium chloride or table salt, non-iodized, is used for makingthe salt water
44、. The chemical dispersant is used as supplied by the manufacturer. Oil is used as received.7. Procedure7.1 Crude Oil and Dispersant Sample Collection and StorageThe bulk oil is mechanically mixed for 2 to 4 h prior to obtaininga working sample. Working samples are stored in 2-L high-density polyethy
45、lene bottles with polypropylene screw closures. Theworking sample is mechanically shaken for 30 min at 20C (or the chosen operating temperature) prior to removing a sub-samplefor testing. When not in use, all samples should be stored in a temperature controlled room at 5C. The dispersant is manually
46、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 vial withPTFE-lined cap. Approximately 100 mg of dispersant is added to the oil. Oil is added until a 1:25 ratio (by weight) of dispersantto oil is achieved. T
47、his is added to achieve the 1:25 ratio within 1% by weight. The sample is well mixed by manual shaking orstirring.7.3 Salt-Water PreparationGranular salt is weighed and added to water from reverse osmosis (RO) filtration to obtain a 3.3 %(w/v) solution. The water temperature is stabilized to 20C (or
48、 the chosen operating temperature) before use.7.4 Swirling Flask PreparationThe 120 mL of salt water is placed into a 125-mL modified Erlenmeyer flask. The flask isinserted into the flask holders on the oscillating table of the shaker.A100-L volume of pre-mix solution is carefully applied ontothe su
49、rface of the water using a positive displacement pipet. The tip of the pipet is placed at the water surface and the dispersant/oilmixture gently expelled. Extreme care should be taken when applying the oil to the surface such that mixing does not occur. Theoil should gently glide across the water to form a slick. If the oil streams out into the water, the agitation can disperse the oil,increasing the amount of oil dispersed and erroneously raising the final dispersion result. Herding of the oil and some creeping ofthe mixture up the vessel wall is normal but can
