ASTM C1777-20

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Designation: C1777 − 15 C1777 − 20
Standard Test Method for
Rapid Determination of the Methylene Blue Value for Fine
Aggregate or Mineral Filler Using a Colorimeter
This standard is issued under the fixed designation C1777; 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 Scope*
1.1 This test method provides a rapid test to determine the amount of methylene blue adsorbed by a specimen of fine aggregate
or mineral filler and can be used both in the laboratory and in the field.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 The text of this standard refers to notes and footnotes that provide explanatory material. These notes and footnotes
(excluding those in tables and figures) shall not be considered as requirements of this standard.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
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:
C125 Terminology Relating to Concrete and Concrete Aggregates
C702C702/C702M Practice for Reducing Samples of Aggregate to Testing Size
D75D75/D75M Practice for Sampling Aggregates
E11 Specification for Woven Wire Test Sieve Cloth and Test Sieves
2.2 Other Standards:
AASHTO T330 Standard Method of Test for the Qualitative Detection of Harmful Clays of the Smectite Group in Aggregates
Using Methylene Blue
EN 933-9 Tests for geometrical properties of aggregates. Part 9: Assessment of fines – Methylene blue test
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology C125.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 mineral filler, n—a finely divided mineral product at least 65 % of which passes the 75-μm sieve.
4. Summary of Test Method
4.1 A specimen of fine aggregate or mineral filler is combined with a methylene blue solution of known concentration and mixed
for a prescribed period of time. The specimen adsorbs some of the methylene blue from solution. The resulting mixture is filtered
This test method is under the jurisdiction of ASTM Committee C09 on Concrete and Concrete Aggregates and is the direct responsibility of Subcommittee C09.20 on
Normal Weight Aggregates.
Current edition approved Feb. 1, 2015June 1, 2020. Published April 2015July 2020. Originally approved in 2013. Last previous edition approved in 20142015 as C1777-14.
DOI: 10.1520/C1777-15. – 15. DOI: 10.1520/C1777-20.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
Available from American Association of State Highway and Transportation Officials (AASHTO), 444 N. Capitol St., NW, Suite 249, Washington, DC 20001,
http://www.transportation.org.
Available from European Committee for Standardization, Avenue Marnix 17, B-1000 Brussels, Belgium.
*A Summary of Changes section appears at the end of this standard
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C1777 − 20
and a portion of the filtered solution is diluted by a fixed amount. A colorimeter is used to determine the absorbance of the diluted
solution, from which the concentration of methylene blue prior to dilution is calculated. The change in concentration of methylene
blue before and after mixing with fine aggregate or mineral filler is converted to a methylene blue value and reported in units of
mg/g.
5. Significance and Use
5.1 This test method is used to determine rapidly the amount of methylene blue adsorbed by a specimen of fine aggregate or
mineral filler. The result is reported as a methylene blue value in units of mg of methylene blue adsorbed per g of fine aggregate
or mineral filler. The methylene blue value is a function of the amount and characteristics of clay minerals present in the test
specimen. High methylene blue values indicate increased potential for diminished fine aggregate or mineral filler performance in
a cementitious mixture due to the presence of clays.
NOTE 1—Results from this test method are not expected to be correlated with those obtained using AASHTO T 330 or EN 933-9. These three test
methods are likely to give very different numerical values even though the units are the same. The AASHTO T 330 test is performed only on the fraction
of an aggregate passing the 75 μm sieve, the EN 933-9 test is performed only on the fraction finer than 2 mm, and this test is performed on the fraction
finer than the 4.75 mm sieve. Therefore, when testing the same fine aggregate source, the AASHTO test method would give the highest methylene blue
value because any clay present in the specimen would be concentrated in the fraction finer than the 75 μm sieve. The AASHTO and EN test methods
do not take into account the amount of material passing the 75 μm sieve or 2 mm sieve, respectively. For example, a fine aggregate with high methylene
blue value measured by the AASHTO method but low percentage passing the 75 μm sieve may have less effect on concrete performance than a fine
aggregate with low methylene blue value measured by the AASHTO method but a high percentage passing the 75 μm sieve. In contrast, this test method
expresses methylene blue value based on the entire fine aggregate or mineral filler specimen. Additionally, the AASHTO and EN test methods use titration
to determine the amount of methylene blue of known concentration that is adsorbed by a specimen and require the operator to visually determine the end
point of the test. In contrast, this test method uses a colorimeter to detect the change in concentration of methylene blue solution before and after being
mixed with the fine aggregate or mineral filler specimen.
NOTE 2—Recommendations for maximum methylene blue values for specific applications are not provided in this test method. Maximum methylene
blue values should be established based on successful performance of fine aggregate or mineral filler in the applications under consideration.
6. Interferences
6.1 Methylene blue will degrade when exposed to light. Store in darkness. No appreciable degradation occurs during the time
it takes to complete the test method.
6.2 Methylene blue will stain glassware and plastic ware. Therefore, do not reuse such apparatus.
7. Apparatus
7.1 4.75-mm sieve conforming to Specification E11.
7.2 Mass Balancebalance having a capacity of 50 g or more and capable of measuring to the nearest 0.1 g or less.
7.3 Micropipette capable of measuring to the nearest 1 μL.
7.4 Colorimeter capable of reading absorbance of a specimen at a wavelength of 610 6 1 nm at operating temperatures of at
least 0 to 50ºC. The colorimeter shall be able to read absorbance between zero and the absorbance associated with a 0.144 % mass
concentration of methylene blue solution.
7.5 Disposable items for each test—two plastic 50-mL test tubes, one plastic 1-mL vial, one 3-mL syringe with Luer-Lok
adapter, one 0.2-μm syringe filter, one colorimeter glass cuvette (or sample cell), one micropipette tip, and two transfer pipettes.
7.6 Additional disposable items for confirming methylene blue starting concentration—plastic 50-mL test tube, colorimeter
glass cuvette, micropipette tip, and transfer pipette.
7.7 Additional disposable items for standardizing the colorimeter—plastic 50-mL test tube, colorimeter glass cuvette,
micropipette tip, and transfer pipette.
7.8 Drying Apparatus—apparatus—A ventilated oven capable of maintaining a uniform temperature of 110 6 5°C. Other
suitable drying apparatuses shall be permitted, such as an electric hot plate or heat lamp. The temperature of the specimen shall
not exceed 150°C. In cases where the fine aggregate or mineral filler itself is altered by temperature greater than 115°C, use a
ventilated, controlled-temperature oven at 110 6 5°C.
NOTE 3—Drying by means other than a ventilated oven may be appropriate for field use.
8. Reagents and Materials
8.1 Purity of Reagents—reagents—reagent grade methylene blue shall be used in all tests.
8.2 Purity of water—references to water shall be understood to mean distilled or deionized water.
8.3 Methylene blue test solution—a 0.50 % mass concentration methylene blue solution based on mass of trihydrate methylene
blue in water.
NOTE 4—Methylene blue is available in both anhydrous and trihydrate form and can also be obtained in solution form. This test is based on the mass
of the trihydrate form.
C1777 − 20
9. Sampling, Test Specimens, and Test Units
9.1 Sample fine aggregate in accordance to Practice D75D75/D75M.
9.2 Thoroughly mix the sample and reduce it as necessary using the applicable procedures in Practice C702C702/C702M.
9.3 If it appears necessary, dampen the material to avoid segregation or loss of fines during specimen preparation.
9.4 Obtain at least 30 g of material passing the 4.75-mm sieve in the following manner:
9.4.1 Separate the sample on the 4.75-mm sieve by means of a lateral and vertical motion of the sieve, accompanied by a jarring
action so as to keep the sample moving continuously over the surface of the sieve. Continue the sieving until not more than 1 mass
% of the residue passes the sieve during th
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