20

28. Available Lime NOTE 37—This titration can also be performed potentiometrically using
Index
28.1 Scope—The available lime index of high-calcium a suitable pH meter to a pH of 4.70.
quicklime and hydrated lime designates those constituents that
28.3.3.4
enter into the reaction under the conditions of this specified test Calculation—Calculate normality as follows:
method, otherwise known as the “rapid sugar test method.” The
interpretation of results obtained by this test method shall be
A5B/~0.1211363C!(25)
restricted by this definition.
28.2 Summary of Test Method—The sample is slaked and where:
dispersed with water. The lime is solubilized by reaction with
A 5 normality of the HCl solution,
sugar to form calcium sucrate which is then determined by B 5 Tris-(Hydroxymethyl) Amino-Methane used, g,
titration against standard acid using phenolphthalein as the C 5 HCl solution consumed, mL.
indicator. 28.3.4 Phenolphthalein Indicator (4 %)—Dissolve 4 g of
28.3 Special Solutions: dry phenolphthalein in 100 mL of 95 % alcohol.
28.3.1 Hydrochloric Acid, Standard (1.000 N)—Prepare a 28.3.5 Sucrose Solution—(40 g of pure cane sugar in solid
solution by diluting 83 mL of HCl to 1 L with CO 2-free water.
form may be used per sample in place of a sugar solution.)
Standardization of sock solution should be performed on Prepare
a a 40 % solution (w/v) using pure cane sugar and
regular basis at a minimum of once per month. For precision CO2-free water in a large beaker and stir until dissolved. Add
and bias information on standardization with Na 2CO3 or several drops of phenolphthalein indicator solution. Add 0.1 N
Tris-(Hydroxymethyl) Amino-Methane see Practice E 200. NaOH solution dropwise with stirring until a faint pink color
28.3.2 Standardization of HCl with Na2CO3: persists. Stock solution of sugar may be made for convenience;
28.3.2.1 Transfer approximately 20 g of primary standard however, it should not be stored for more than two days. As an
anhydrous sodium carbonate (Na2CO3) to a platinum dishalternative
or the acidity of each lot of sugar can be determined,
crucible, and dry at 250°C for 4 h. Cool in a desiccator. and a correction applied to the titration.
28.3.2.2 Weigh accurately 4.4 g to the nearest 0.1 mg of 28.4
the Procedure:
dried Na2CO3 and transfer to a 500-mL flask. Add 50 mL of 28.4.1 Procedure for Quicklime:
CO2-free water, swirl to dissolve the carbonate, and add two 28.4.1.1 The sample as received at the laboratory shall be
drops of a 0.1 % solution of methyl red in alcohol. Titrate thoroughly
with mixed and a representative sample with minimum
the HCl solution to the first appearance of a red color, and boil of 100 g shall be taken and pulverized to pass a No. 50
weight
the solution carefully, until the color is discharged (Note 32).
sieve for analysis. Weigh rapidly 2.804 g of the finely pulver-
Cool to room temperature, and continue the titration, alternat-
ized sample, brush carefully into a 500-mL Erlenmeyer flask
ing the addition of HCl solution and the boiling and cooling to
containing about 40 mL of CO2-free water (Note 38), and
the first appearance of a faint red color that is not discharged on
immediately stopper the flask.
further heating.
28.3.2.3 Calculation—Calculate normality as follows:
NOTE 38—Water should not be added to the sample because, especially
with quicklime, there is a tendency for the material to cake and form
A5~B318.87!/C (24) lumps difficult to completely dissolve in the sugar solution later. On the
other hand, if the lime is added to a little water, a better dispersion of the
where: fine particles occurs, leading to a more rapid dissolution of the sample. It
A 5 normality of the HCl solution, is possible that in the case of quicklime, some slaking action occurs to
facilitate the dispersion and solution.
B 5 Na2CO3 used, g, and
C 5 HCl solution consumed, mL.

NOTE 36—This titration can also be performed potentiometrically with 28.4.1.2 Remove the stopper. Place the flask on a hot plate
the aid of a glass electrode and a calomel electrode. and immediately add 50 mL of boiling CO2-free water to the
flask. Swirl the flask and boil actively 1 min for complete
28.3.3 Standardization of HCl with TRIS (THAM)—[Tris- slaking. Remove from the hot plate, stopper the flask loosely,
(Hydroxymethyl) Amino-Methane]: and place in a cold-water bath to cool to room temperature.
28.3.3.1 Transfer an appropriate amount of primary stan- 28.4.1.3 Add 100 mL of the neutralized sugar solution (or
dard tris-(hydroxymethyl) amino-methane to suitable dish or approximately 40 g of pure cane sugar). Stopper the flask,
crucible and dry in a vacuum at 70°C for 24 h (refer to Practice
swirl, and let stand for 15 min to react. (Reaction time should
E 200). As an alternative, Tris can also be dried at 105°C not be less than 10 min nor more than 20 min.) Swirl at 5-min
(65°C) for 2 h in a regular laboratory drying oven. Cool in a intervals during reaction. Remove stopper, add 4 to 5 drops of
desiccator to room temperature. 4 % phenolphthalein indicator solution and wash down the
28.3.3.2 Preparation of Mixed Indicator—Mix 100 mg of stopper and sides of the flask with CO 2-free water.
Bromocresol Green with 2 mL 0.1 N NaOH and dilute with 28.4.1.4 When titrating (Note 39), first add about 90 % of
CO2-free water to 100 mL. Dissolve 100 mg of Alizarin Red S the acid requirement from a 100-mL buret. Finish the titration,
in 100 mL CO2-free H2O. Mix equal portions of Bromocresol more carefully at approximately one drop per second, to the
Green and Alizarin Red S solutions to form mixed indicator. first disappearance of the pink color, which persists for 3 s.
28.3.3.3 Weigh approximately 8 g of TRIS to the nearest 0.1Note the endpoint and ignore any further return of color.
mg and dissolve in 50 mL of CO 2-free water. Add 6 drops of
mixed indicator (Note 33) and titrate to a bright yellow
end-point with acid.
C 25
21

NOTE 39—A mechanical stirrer may be used during the titration if

desired. Put a clean magnetic stirrer bar into the flask and place the flask
on the magnetic stirrer. Adjust to stir as rapidly as possible without
incurring any loss by spattering. Unless the operator is familiar with
previous analyses of the lime under test, and in cases where the available
lime content varies to extremes, it is good practice to run a preliminary
test
by slow titration to determine the proper amount of acid required to
neutralize the sample.
28.4.2 Procedure for Hydrated Lime—The procedure for
determining Ca(OH)2 is the same as for CaO with the excep-
tion that cold CO2-free water is used and the boiling and
cooling steps are omitted.
28.5 Calculation:
28.5.1 Calculate for CaO as follows:

Available lime ~CaO, %=N3.V3.2,804/W

(26)

where:
N normality of acid solution,
V standard HCl used (1.000 N), mL,
W weight of sample, g, and
2.804 CaO, g, equivalent to 1 mL of standard
acid 3 100, or 1 mL of standard HCl 5 1 % CaO
if exactly 2.804 g of sample is used.
28.5.2 Calculate for Ca(OH)2 as follows:

Available lime Ca(OH)2 %=N3.V3.3,704/W

(27)

where:
N normality of acid solution,
V standard HCl (1.000 N), mL,
W weight of sample, g, and
,mdit> 3.704 Ca(OH)2, g, equivalent to 1 mL of standard
acid 3 100 or 1 mL of standard
HCl 5 1.32 % Ca(OH) 2 when exactly
2.804 g of sample is used.
28.6 Precision and Bias:
28.6.1 Twenty-four laboratories cooperated in the testing of

three high calcium quicklimes and one high calcium hydrated

lime thereby obtaining the repeatability (r) and reproducibility
(R) (Practice E 691) data contained in Table 4.
28.6.2 The user is cautioned that the repeatability and
reproducibility are considered adequate for the purposes of the
test method. However, higher levels of MgO and nonreactive
CaO increase the value of the repeatability (within lab) slightly
and the reproducibility value (between labs) noticeably.
28.6.3 Due to the lack of a recognized industry standard, the
bias of this test method has not been determined.