ASTM E2664-22

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. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E2664 − 16 E2664 − 22
Standard Test Method Practice for
Methanol Wall Wash of Marine Vessels Handling Polyester
Grade Monoethylene Glycol
This standard is issued under the fixed designation E2664; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope*
1.1 This test method covers the methanol wall wash procedure and the chemical and physical analysis of the wall wash sampling
for cargo tanks of marine vessels handling polyester grade monoethylene glycol. The key sections for the wall wash procedure and
test methods appear in the following order:
Sections
Wall Wash Procedure 7 and 8
Appearance 9 – 11
Color 12 – 14
Hydrocarbons 15 – 17
Chloride 18 – 21
1.2 The values given in SI units are to be considered as the standard. No other units of measurement are included in this standard.
1.3 Review the current Safety Data Sheet (SDS) for detailed information concerning toxicity, first aid procedures and safety
precautions.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. For specific hazard statements, see Section 6.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D1209 Test Method for Color of Clear Liquids (Platinum-Cobalt Scale)
D1722 Test Method for Water Miscibility of Water-Soluble Solvents
D4176 Test Method for Free Water and Particulate Contamination in Distillate Fuels (Visual Inspection Procedures)
D5386 Test Method for Color of Liquids Using Tristimulus Colorimetry
This test method practice is under the jurisdiction of ASTM Committee D16 on Aromatic, Industrial, Specialty and Related Chemicals and is the direct responsibility
of Subcommittee D16.14 on Alcohols & Glycols.
Current edition approved Jan. 1, 2016July 15, 2022. Published February 2016July 2022. Originally approved in 2009. Last previous edition approved in 20092016 as E2664
– 09a.16. DOI: 10.1520/E2664-16.10.1520/E2664-22.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2664 − 22
E180 Practice for Determining the Precision of ASTM Methods for Analysis and Testing of Industrial and Specialty Chemicals
(Withdrawn 2009)
E2469 Test Method for Chloride in Mono-, Di- and Tri-ethylene Glycol by Ion Chromatography
E2680 Test Method for Appearance of Clear, Transparent Liquids (Visual Inspection Procedure)
3. Significance and Use
3.1 The methanol wall wash test is performed to determine the cleanliness and suitability of cargo tanks or compartments on a
marine vessel prior to loading polyester grade monoethylene glycol. Polyester grade monoethylene glycol has very high quality
requirements and must be handled with care, as it is adversely affected by oxygen, hydrocarbons, water and chloride. It is especially
susceptible to aromatic contamination, which degrades UV transmittance. Possible sources of contamination are the prior cargoes
and cleaning agents. The methanol wall wash procedure provides a representative sampling of the impurities and contamination
present on the sides of the cargo tank.
3.2 The test methods used for analysis of the methanol wall wash samples are capable of determining low levels of impurities or
contamination in methanol. These tests include appearance, color, hydrocarbons and chloride. The producers of polyester grade
monoethylene glycol need confirmation of the cleanliness and suitability of the marine vessel’s tanks prior to loading with
in-specification material. Cargo tanks that do not pass the wall wash test should not be loaded.
3.3 Alternative test methods and technology for several of the methods can be found in the Appendix. The alternative test methods
do not have precision data for the application of these methods in analyzing methanol. Use of these methods is optional and
individuals using the alternative methods should assure themselves that the method is sufficiently precise. Precision data is only
for the original test methods listed.
4. Purity of Reagents
4.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society (ACS) where
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
4.2 High-Purity Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by
Type II of Specification D1193. It is recommended that all water be filtered through a 0.2-μm filter.
4.3 Methanol, ACS reagent grade with very low concentrations of chloride.
NOTE 1—Chloride in high purity methanol used for preparation of the chloride working standards should not exceed 0.01 mg/kg. This information should
be provided by the supplier or determined by the analyst before use.
5. Quality Control
5.1 It is recommended that a control chart for the concentration of chloride in a methanol wall wash quality control sample be
established and maintained according to common guidelines. Measure the control sample each time a test sample(s) is tested. If
the measured value exceeds the action limit of the control chart, take appropriate action before proceeding with sample tests.
6. Hazards
6.1 Each analyst must be acquainted with the potential hazards of the equipment, reagents, products, solvents and procedures
before beginning laboratory work. Sources of information include: operation manuals, SDS, literature, and other related data.
Safety information should be requested from the supplier. Disposal of waste materials, reagents, reactants, and solvents must be
in compliance with laws and regulations from all applicable governmental agencies.
6.2 Methanol is a flammable and toxic substance. Methanol is absorbed through the skin and by breathing the vapors. Be careful
when handling a flammable solvent and work in a well-ventilated area away from sources of ignition. Use the proper Personal
Protective Equipment (PPE) to minimize exposure.
E2664 − 22
METHANOL WALL WASH
7. Procedure
7.1 All equipment must be clean and rinsed with reagent grade, low chloride methanol to prevent chloride contamination of the
sample.
7.2 Pour approximately 1 L of reagent grade, low chloride methanol into a 1-L plastic squeeze bottle.
7.3 Use a plastic funnel that has been cut flat on one side to catch the methanol. The funnel and 1-L sample bottle should be rinsed
with reagent grade, low chloride methanol immediately before sampling.
7.4 Clean, chemical resistant gloves and eye protection should be worn for personal protection and to prevent contamination of
the samples.
7.5 Do not test wet areas of a cargo tank. The tank must be dry before conducting the wall wash tests. The tank is not acceptable
for testing if wet areas are more than a few spots.
7.6 Choose two sites on each tank wall (bulkhead) approximately 15 to 20 cm wide and as high as possible (approximately 2 m
high). Start spraying methanol on the wall with the spray bottle approximately 15 cm from the wall. Collect the methanol with
the special funnel into a clean 1-L glass bottle with the funnel placed at least 0.3 to 0.6 m below the spray. Continue spraying
methanol while moving down the wall until approximately 0.6 m from the bottom. Use approximately 200 mL of methanol on each
of the four sides of the tank. Be consistent with the spraying and collecting of the methanol. Do not scrap the tank wall with the
funnel when collecting the methanol.
7.7 Include “non-typical” areas, such as discolored patches, lining breaks and exposed metal. If the “non-typical” areas are less
than 20 % of the tank surface, include them in the four areas normally tested. If they are more than 20 % of the tank surface, test
them separately.
7.8 Test separately any areas having crystalline deposits.
7.9 Collect the methanol from the four sides of a tank into the same sample bottle. Cap the bottle, label from which cargo tank
it was taken and transport to the laboratory for analysis.
7.10 Include a sample of the methanol used in the wall wash procedure. This is the analytical “blank”. This methanol will be
analyzed with the tank samples and the results of the “blank” will be subtracted from each tank’s wall wash sample’s results.
8. Analysis
8.1 The methanol wall wash samples shall be analyzed for the following:
1. Appearance Clear and bright (pass)
2. Color 10 Pt/Co, maximum
3. Hydrocarbons None by test (pass)
4. Chloride 0.5 mg/kg, maximum
8.2 If the container needs to be cleaned further, a sample of the water used to do the cleaning may be sampled for chlorides. The
water should contain less than 0.2 mg/kg chlorides.
E2664 − 22
APPEARANCE
9. Procedure
9.1 Determine the appearance of the sample in accordance with Test Method E2680 for visual clarity and particulate
contamination.
9.2 Allow the sample to equilibrate to room temperature (or to the storage temperature or the temperature at which the sample
is used) prior to visual inspection. A temperature-controlled water bath can be used to bring the sample to the desired temperature
if measurements must be made at a specific temperature according to product specifications.
9.3 When using a water bath, replace the sample container’s cap with an airtight closure through which a calibrated
temperature-sensing device is immersed in the sample. Periodically agitate the sample in a manner sufficient to homogenzide the
bulk of the sample. Remove the sample container from the water bath and wipe dry. Remove the temperature-sensing device and
replace the original cap before proceeding with the visual inspection.
9.4 Hold the sample up to a bright light source and visually examine the sample at arm’s length for clarity, suspended matter (any
foreign matter that does not float or settle to the bottom of the bottle) and any free water (or oil) droplets or layers.
9.5 Swirl the sample gently to form a vortex and avoid formation of bubbles. Examine the bottom of the vortex at arm’s length
for particulate matter (any foreign material that settles to the bottom of the bottle) and free water (or oil).
10. Report
10.1 Report the following information:
10.1.1 Report the appearance as “Pass” if the visual clarity was found to be “Clear and Bright” with no more than the maximum
number of particles of suspended matter no greater than 1 mm in diameter and no free water (or oil) were found and the particulate
matter had no particulates of sufficient size and quantity to be easily noted at the bottom of the vortex. See Table 1.
10.1.2 Report the appearance as “Fail” if the visual clarity as found to be “Not Clear and Bright” with more than the maximum
number of particles of suspended matter greater than 1 mm in diameter and/or free water (or oil) were found and/or particulate
matter was found with particulates of sufficient size and quantity to be easily noted at the bottom of the vortex. See Table 1.
11. Precision and Bias
11.1 No information is presented about either the precision or bias of Test Method E2680 since the test result is nonquantitative.
COLOR
12. Procedure
12.1 Determine the color of the sample in accordance with Test Method D5386 for near clear liquids using an instrument with
color measurements converted to the platinum-cobalt system (Pt-Co).
13. Report
13.1 Report the following information:
13.1.1 Report the color for an instrumental Pt-Co measurement to the nearest whole unit.
14. Precision and Bias
14.1 The following criteria should be used to judge the acceptability of results (see Note 2):
E2664 − 22
14.1.1 Repeatability (Single Analyst)—The precision of the procedure for measuring color will be determined.
14.1.2 Laboratory Precision (Within-Laboratory, Between-Days Variability)—The precision of the procedure for measuring color
will be determined.
14.1.3 Reproducibility (Multi-Laboratory)—The precision of the procedure for measuring color will be determined.
NOTE 2—The equations in Practice E180 will be used in developing the precision estimates.
14.2 Bias—The bias of this test method cannot be determined because no referee method or reference standard is available to
determine the true value.
HYDROCARBONS
15. Procedure
15.1 Determine the presence of water-immiscible materials (hydrocarbons) in the sample in accordance with Test Method D1722.
This is a qualitative test.
16. Report
16.1 Report the following information:
16.1.1 If the sample water mixture has no hydrocarbon layer and is as free of cloudiness or turbidity as the blank, report the sample
as “passes” test. If any cloudiness, turbidity or a hydrocarbon layer is detected after 30 min, report as “fails” test.
17. Precision and Bias
17.1 No information is presented about either precision or bias of this test method since the test result is non-quantitative and is
reported as pass or fail.
CHLORIDE
18. Procedure
18.1 Determine the concentration of chloride in the sample in accordance with Test Method E2469 by ion chromatography (IC).
An IC system with Carbonate-Based Eluent should produce a separation of chloride equivalent to or better than that shown in Fig.
1.
18.1.1 The chloride working standards should be prepared in methanol. The methanol used to prepare the chloride working
standards should not exceed 0.01 mg/kg of chloride (see 4.3).
18.1.2 The methanol wall wash sample should be analyzed without dilution. It is recommended that each sample be analyzed in
duplicate and the average result reported.
19. Report
19.1 Report the following information:
19.1.1 Report the concent
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