1、Designation: E2664 09aStandard Test Method forMethanol Wall Wash of Marine Vessels Handling PolyesterGrade Monoethylene Glycol1This standard is issued under the fixed designation E2664; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revisio
2、n, 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 methanol wall wash proce-dure and the chemical and physical analysis of th
3、e wall washsampling for cargo tanks of marine vessels handling polyestergrade monoethylene glycol. The key sections for the wall washprocedure and test methods appear in the following order:SectionsWall Wash Procedure 7 and 8Appearance 9-11Color 12-14Hydrocarbons 15-17Chloride 18-211.2 The values gi
4、ven in SI units are to be considered as thestandard. No other units of measurement are included in thisstandard.1.3 Review the current Material Safety Data Sheet (MSDS)for detailed information concerning toxicity, first aid proce-dures and safety precautions.1.4 This standard does not purport to add
5、ress 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. For specific hazardstatements, see Section 6.2. Referen
6、ced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)D1722 Test Method for Water Miscibility of Water-SolubleSolventsD4176 Test Method for Free Water and Particulate Con-tamination in Distillate Fuels (Visual Inspec
7、tion Proce-dures)D5386 Test Method for Color of Liquids Using TristimulusColorimetryE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty ChemicalsE2469 Test Method for Chloride in Mono-, Di- and Tri-ethylene Glycol by Ion ChromatographyE268
8、0 Test Method for Appearance of Clear, TransparentLiquids (Visual Inspection Procedure)3. Significance and Use3.1 The methanol wall wash test is performed to determinethe cleanliness and suitability of cargo tanks or compartmentson a marine vessel prior to loading polyester grade monoeth-ylene glyco
9、l. Polyester grade monoethylene glycol has veryhigh quality requirements and must be handled with care, as itis adversely affected by oxygen, hydrocarbons, water andchloride. It is especially susceptible to aromatic contamination,which degrades UV transmittance. Possible sources of con-tamination ar
10、e the prior cargoes and cleaning agents. Themethanol wall wash procedure provides a representative sam-pling of the impurities and contamination present on the sidesof the cargo tank.3.2 The test methods used for analysis of the methanol wallwash samples are capable of determining low levels ofimpur
11、ities or contamination in methanol. These tests includeappearance, color, hydrocarbons and chloride. The producersof polyester grade monoethylene glycol need confirmation ofthe cleanliness and suitability of the marine vessels tanks priorto loading with in-specification material. Cargo tanks that do
12、not pass the wall wash test should not be loaded.3.3 Alternative test methods and technology for several ofthe methods can be found in the Appendix. The alternative testmethods do not have precision data for the application of thesemethods in analyzing methanol. Use of these methods is1This test met
13、hod is under the jurisdiction of ASTM Committee E15 onIndustrial and Specialty Chemicals and is the direct responsibility of SubcommitteeE15.02 on Product Standards.Current edition approved Oct. 1, 2009. Published November 2009. Originallyapproved in 2009. Last previous edition approved in 2009 as E
14、2664-09. DOI:10.1520/E2664-09A.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section
15、 appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.optional and individuals using the alternative methods shouldassure themselves that the method is sufficiently precise.Precision data is only for the
16、 original test methods listed.4. Purity of Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society (ACS)where suc
17、h specifications are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.4.2 High-Purity WaterUnless otherwise indicated, refer-ences to water shall be understood to m
18、ean reagent water asdefined by Type II of Specification D1193. It is recommendedthat all water be filtered through a 0.2-m filter.4.3 Methanol, ACS reagent grade with very low concentra-tions of chloride.NOTE 1Chloride in high purity methanol used for preparation of thechloride working standards sho
19、uld not exceed 0.01 mg/kg. This informa-tion should be provided by the supplier or determined by the analystbefore use.5. Quality Control5.1 It is recommended that a control chart for the concen-tration of chloride in a methanol wall wash quality controlsample be established and maintained according
20、 to commonguidelines.4Measure the control sample each time a testsample(s) is tested. If the measured value exceeds the actionlimit of the control chart, take appropriate action beforeproceeding with sample tests.6. Hazards6.1 Each analyst must be acquainted with the potentialhazards of the equipmen
21、t, reagents, products, solvents andprocedures before beginning laboratory work. Sources ofinformation include: operation manuals, MSDS, literature, andother related data. Safety information should be requested fromthe supplier. Disposal of waste materials, reagents, reactants,and solvents must be in
22、 compliance with laws and regulationsfrom all applicable governmental agencies.6.2 Methanol is a flammable and toxic substance. Methanolis absorbed through the skin and by breathing the vapors. Becareful when handling a flammable solvent and work in awell-ventilated area away from sources of ignitio
23、n. Use theproper Personal Protective Equipment (PPE) to minimizeexposure.METHANOL WALL WASH7. Procedure7.1 All equipment must be clean and rinsed with reagentgrade, low chloride methanol to prevent chloride contamina-tion of the sample.7.2 Pour approximately 1 L of reagent grade, low chloridemethano
24、l into a 1-L plastic squeeze bottle.7.3 Use a plastic funnel that has been cut flat on one side tocatch the methanol. The funnel and 1-Lsample bottle should berinsed with reagent grade, low chloride methanol immediatelybefore sampling.7.4 Clean, chemical resistant gloves and eye protectionshould be
25、worn for personal protection and to prevent contami-nation of the samples.7.5 Do not test wet areas of a cargo tank. The tank must bedry before conducting the wall wash tests. The tank is notacceptable for testing if wet areas are more than a few spots.7.6 Choose two sites on each tank wall (bulkhea
26、d) approxi-mately 15 to 20 cm wide and as high as possible (approxi-mately 2 m high). Start spraying methanol on the wall at the1.83 m height with the spray bottle approximately 15 cm fromthe wall. Collect the methanol with the special funnel into aclean 1-L glass bottle with the funnel placed at le
27、ast 0.3 to 0.6m below the spray. Continue spraying methanol while movingdown the wall until approximately 0.6 m from the bottom. Useapproximately 200 mL of methanol on each of the four sides ofthe tank. Be consistent with the spraying and collecting of themethanol. Do not scrap the tank wall with th
28、e funnel whencollecting the methanol.7.7 Include “non-typical” areas, such as discolored patches,lining breaks and exposed metal. If the “non-typical” areas areless than 20 % of the tank surface, include them in the fourareas normally tested. If they are more than 20 % of the tanksurface, test them
29、separately.7.8 Test separately any areas having crystalline deposits.7.9 Collect the methanol from the four sides of a tank intothe same sample bottle. Cap the bottle, label from which cargotank it was taken and transport to the laboratory for analysis.7.10 Include a sample of the methanol used in t
30、he wall washprocedure. This is the analytical “blank”. This methanol will beanalyzed with the tank samples and the results of the “blank”will be subtracted from each tanks wall wash samples results.8. Analysis8.1 The methanol wall wash samples shall be analyzed forthe following:1. Appearance Clear a
31、nd bright (pass)2. Color 10 Pt/Co, maximum3. Hydrocarbons None by test (pass)4. Chloride 0.549 mg/kg, maximum8.2 If the result found for chloride lies between 0.5 and 1mg/kg, the wall wash procedure should be repeated. If a secondwall wash sample is not acceptable for chloride, the cargo tankshould
32、not be loaded.8.3 If the container needs to be cleaned further, a sample ofthe water used to do the cleaning may be sampled for chlorides.The water should contain less than 0.2 mg/kg chlorides.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For
33、 suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.4ASTM Manual on Presenta
34、tion of Data and Control Chart Analysis, 7thEdition, ASTM Services MNL 7A (revision of Special Technical Publication (STP)15D).E2664 09a2APPEARANCE9. Procedure9.1 Determine the appearance of the sample in accordancewith Test Method E2680 for visual clarity and particulatecontamination.9.2 Allow the
35、sample to equilibrate to room temperature (orto the storage temperature or the temperature at which thesample is used) prior to visual inspection. A temperature-controlled water bath can be used to bring the sample to thedesired temperature if measurements must be made at aspecific temperature accor
36、ding to product specifications.9.3 When using a water bath, replace the sample containerscap with an airtight closure through which a calibratedtemperature-sensing device is immersed in the sample. Peri-odically agitate the sample in a manner sufficient to homoge-nzide the bulk of the sample. Remove
37、 the sample containerfrom the water bath and wipe dry. Remove the temperature-sensing device and replace the original cap before proceedingwith the visual inspection.9.4 Hold the sample up to a bright light source and visuallyexamine the sample at arms length for clarity, suspendedmatter (any foreig
38、n matter that does not float or settle to thebottom of the bottle) and any free water (or oil) droplets orlayers.9.5 Swirl the sample gently to form a vortex and avoidformation of bubbles. Examine the bottom of the vortex atarms length for particulate matter (any foreign material thatsettles to the
39、bottom of the bottle) and free water (or oil).10. Report10.1 Report the appearance as “Pass” if the visual claritywas found to be “Clear and Bright” with no more than themaximum number of particles of suspended matter no greaterthan 1 mm in diameter and no free water (or oil) were foundand the parti
40、culate matter had no particulates of sufficient sizeand quantity to be easily noted at the bottom of the vortex. SeeTable 1.10.2 Report the appearance as “Fail” if the visual clarity asfound to be “Not Clear and Bright” with more than themaximum number of particles of suspended matter greater than1
41、mm in diameter and/or free water (or oil) were found and/orparticulate matter was found with particulates of sufficient sizeand quantity to be easily noted at the bottom of the vortex. SeeTable 1.11. Precision and Bias11.1 No information is presented about either the precisionor bias of Test Method
42、E2680 since the test result is nonquan-titative.COLOR12. Procedure12.1 Determine the color of the sample in accordance withTest Method D5386 for near clear liquids using an instrumentwith color measurements converted to the platinum-cobaltsystem (Pt-Co).13. Report13.1 Report the color for an instrum
43、ental Pt-Co measure-ment to the nearest whole unit.14. Precision and Bias14.1 The following criteria should be used to judge theacceptability of results (see Note 2):14.1.1 Repeatability (Single Analyst)The precision of theprocedure for measuring color will be determined.14.1.2 Laboratory Precision
44、(Within-Laboratory, Between-Days Variability)The precision of the procedure for measur-ing color will be determined.14.1.3 Reproducibility (Multi-Laboratory)The precisionof the procedure for measuring color will be determined.NOTE 2The equations in Practice E180 will be used in developing theprecisi
45、on estimates.14.2 BiasThe bias of this test method cannot be deter-mined because no referee method or reference standard isavailable to determine the true value.HYDROCARBONS15. Procedure15.1 Determine the presence of water-immiscible materials(hydrocarbons) in the sample in accordance with Test Meth
46、odD1722. This is a qualitative test.16. Report16.1 If the sample water mixture has no hydrocarbon layerand is as free of cloudiness or turbidity as the blank, report thesample as “passes” test. If any cloudiness, turbidity or ahydrocarbon layer is detected after 30 min, report as “fails”test.17. Pre
47、cision and Bias17.1 No information is presented about either precision orbias of this test method since the test result is non-quantitativeand is reported as pass or fail.CHLORIDE18. Procedure18.1 Determine the concentration of chloride in the samplein accordance with Test Method E2469 by ion chroma
48、tography(IC). An IC system with Carbonate-Based Eluent shouldproduce a separation of chloride equivalent to or better thanthat shown in Fig. 1.18.1.1 The chloride working standards should be preparedin methanol. The methanol used to prepare the chlorideworking standards should not exceed 0.01 mg/kg
49、of chloride(see 4.3).TABLE 1 Recommended Maximum Number of SuspendedParticles Allowed for a Sample to PassSample TypeRecommended Numberof Particles AllowedTypical SampleVolume (mL)Methanol Wall Wash 0 20 400E2664 09a318.1.2 The methanol wall wash sample should be analyzedwithout dilution. It is recommended that each sample beanalyzed in duplicate and the average result reported.19. Report19.1 Report the concentration of chloride in the methanolwall wash sample to the nearest 0.01 mg/kg.19.2 A correction should be made to each wall wash sampleif chloride is found in
