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This test method is under the jurisdiction of ASTM Committee D-1 on Paint
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and Related Coatings, Materials, and Applicationsand is the direct responsibility of Reagent Chemicals, American Chemical Society Specifications, American
Subcommittee D01.33on Polymers and Resins. Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Current edition approved May 25, 1990. Published July 1990. Originally listed by the American Chemical Society, see Analar Standards for Laboratory
published as D 1726 – 60. Last previous edition D 1726 – 87. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
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Annual Book of ASTM Standards, Vol 06.04. and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
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Annual Book of ASTM Standards, Vol 11.01. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D 1726
7.5 Toluene (Warning—See Section 8.), conforming to 12.2 Hot Plate, with variable heat control.
Specification D 841. 12.3 Magnetic Stirrer, with polytetrafluoroethylene (PTFE)-
coated stirring bar.
8. Hazards 12.4 Buret or Automatic Titrator.
8.1 Hydrochloric acid and potassium hydroxide are corro- 12.5 Silver Electrode or equivalent.
sive. Toluene and methyl ethyl ketone are flammable and their 12.6 Boiling Chips.
vapors can be harmful. Precautions should be taken to avoid
inhalation and skin or eye contact with these chemicals. All 13. Reagents and Material
sample preparations should be done in a well ventilated area, 13.1 Acetone.
such as a fume hood. 13.2 Bromcresol Green Indicator Solution (0.1 %)—
9. Procedure Dissolve 0.1 g of bromcresol green in 100 mL of water.
13.3 Nitric acid, (HNO3) (1 + 1), diluted with water.
9.1 Weigh to the nearest 1 mg, 6 to 8 g of neutral specimen
13.4 Potassium Hydroxide, alcohol solution (0.1 N)—
into a 250-mL glass-stoppered Erlenmeyer flask. By means of
Dissolve 5.6 g of potassium hydroxide (KOH) in 1 mL of
a pipet, transfer 50.0 mL of 0.1 N alcoholic KOH solution into
methanol (99 %) or ethanol conforming to Formula No. SD-30
the flask and add 15 mL of toluene. Stopper the flask and swirl
of the US Bureau of Internal Revenue. No standardization of
to mix. Add a few boiling aids and attach to the reflux
the solution is necessary.
condenser on the hot plate.
13.5 Silver Nitrate, alcohol solution (0.0025 N)—Dissolve
9.2 Allow the solution to reflux gently for 15 6 1 min. At
0.425 g of silver nitrate (AgNO3), weighed to the nearest 1 mg,
the end of the reflux period, remove the flask from the hot plate
in 1 L of methanol (99 %) or ethanol conforming to Formula
and cool to room temperature with the condenser in place.
No. SD-30 of the US Bureau of Internal Revenue. Standardize
9.3 Remove the condenser, add 3 drops of phenolphthalein
against hydrochloric acid or sodium chloride solution (with
indicator solution to the specimen, and titrate with 0.1 N HCl.
traceability to an NIST standard).
The end point is taken when 1 drop changes the solution from
13.6 Toluene.
pink to colorless.
NOTE 1—Add 100 mL of methyl ketone to the specimen if required to 14. Hazards
ensure a homogeneous solution during titration of the excess KOH
solution.
14.1 Nitric acid, potassium hydroxide, and silver nitrate are
corrosive. Acetone and toluene are flammable and their vapors
9.4 Make a blank determination on the reagents following can be harmful. Precautions should be taken to avoid inhalation
the same procedure but omitting the specimen. and skin or eye contact with these chemicals. All sample
10. Calculation preparations should be done in a well ventilated area, such as
a fume hood.
10.1 Calculate the weight percent hydrolyzable chloride
content, H, of the specimen as follows: 15. Procedure
H 5 @~V 2 B!N 3 3.55#/W (1) 15.1 Weigh 2 to 3 g of specimen, to the nearest 0.005 g, into
where: a 250-mL Erlenmeyer flask. Add 20 mL of toluene, 20 mL of
B 5 HCl required for titration of the blank, mL, acetone, and 50 mL of 0.1 N alcoholic KOH. Swirl or mix until
V 5 HCl required for titration of the hydrolyzed speci- dissolution is complete.
men, mL, 15.2 Add several boiling chips, connect the flask to the
N 5 normality of the HCl, reflux condenser, and gently reflux for 15 6 1 min on a hot
3.55 5 grams of chlorine per milliequivalent multiplied by plate.
the percentage factor of 100, and 15.3 Remove the hot plate from under the flask and allow
W 5 specimen weight, g. the flask and contents to cool to room temperature. Rinse down
the condenser with acetone then remove from the flask.
11. Precision 15.4 Quantitatively transfer the contents of the flask to a
11.1 The following criteria should be used for judging the 250-mL beaker using acetone as wash solution. Dilute the
acceptability of results at the 95 % confidence level: solution to about 125 mL with acetone, insert a stirring bar, and
11.1.1 Repeatability—Two results obtained by the same place on a magnetic stirrer.
operator should be considered suspect if they differ by more 15.5 Add five drops of bromcresol green indicator. While
than 0.02 % absolute. stirring add 1 + 1 nitric acid dropwise just until the permanent
11.1.2 Reproducibility—Two results obtained by operators color changes from blue to yellow.
in different laboratories should be considered suspect if they
NOTE 2—Caution—Do not add excess nitric acid. Do not acidify the
differ by more than 0.05 weight %.
solution until ready to begin the titration. Make certain that the solution is
TEST METHOD B at room temperature before acidifying. These cautions are necessary to
prevent the chloride results from being low due to recombination with the
12. Apparatus resin.
12.1 Reflux Apparatus, consisting of a 250-mL Erlenmeyer 15.6 Titrate with 0.0025 N silver nitrate using the combina-
flask attached to a reflux condensor. tion silver electrode and the automatic titrator or buret.
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D 1726
15.7 Reflux a blank, which includes all components except 17. Precision
the sample, and titrate with 0.0025 N silver nitrate.
17.1 A liquid epoxy resin of approximately 150 ppm hydro-
16. Calculation lyzable chloride was sampled to five laboratories and seven
16.1 Calculate the parts per million hydrolyzable chloride analysts obtained the following results.
content, H, of the specimen as follows: 17.1.1 Repeatability—The difference between two results
obtained by the same analyst should not vary by more than
H 5 @~V 2 B!N 3 35.5 3 103#/W
8.32 % at the 95 % confidence level.
where: 17.1.2 Reproducibility—The difference between two re-
B 5 AgNO3 required for the titration of the blank, sults, each the mean of two determinations, obtained by
mL, analysts in different laboratories should not vary by more than
V 5 AgNO3 required for the titration of the hy- 15.88 % relative at the 95 % confidence level.
drolyzed specimen, mL,
N 5 Normality of the AgNO3,
18. Keywords
35.5 3 103 5 grams of chlorine per milliequivalent multi-
plied by the ppm conversion of 1 3 106, and 18.1 hydrolyzable chloride; liquid epoxy resin; saponifiable
W 5 specimen weight, g. chloride
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