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_____________MUESTREO Y ANÁLISIS DE JABÓN Y PRODUCTOS DE JABÓN___________

A.O.C.S. Official Method Da 17-52


Official 1961
Reapproved 1989

Borax

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_____________MUESTREO Y ANÁLISIS DE JABÓN Y PRODUCTOS DE JABÓN___________

Definition: This method determines borax in the sample.


Scope: Applicable to all soaps and soap products.

Apparatus:
1. Beakers, 250 and 400 mL.
2. Buret, 50 mL.
3. Volumetric flask, 250 mL.
4. Watch glasses.
5. Filter paper, a quantitative grade that will retain gelatinous precipitates, such as Whatman No.
1, S & S No. 589 Black Ribbon, or equivalent.
6. pH meter, standardized according to manufacturer's instructions.

Reagents:
1. Hydrochloric acid (HCl), 1:1, v/v (see Notes. Caution). Dilute 1 volume of HCl (sp. gr. 1.19)
with 1 volume of distilled water (see Notes. 1).
2. Mannitol, CP grade.
3. Methyl red indicator solution prepared by disolving 0.10 g of methyl red in 100 mL of a 1:1,
v/v solution of 95% ethyl alcohol and destiled water.
4. α-Naphtholphthalein indicator solution, prepared by dissolving 0.10g of α-Naphtholphthalein
in 100mL of 50:50. v/v solution of 95% ethyl alcohol and distilled water.
5. Sodium hydroxide (NaOH) solution 25% by weight in distilled water, carbonate free (see
Notes, Caution)
6. Sodium hydroxide (NaOH) solution, either 0.05 N or 0.10 N, accurately standardized. See
AOCS Specification H 12-52.
7. Strontium chloride (SrCl2.6H2O) solution. 33.3% by weight in distilled water, or strontium
nitrate solution (Sr(NO3)2) solution, 26.5% by weight in distilled water.

Procedure:
1. Accurately weigh a sample, conforming to the estimated borax weight noted in Table 1, into
a 250mL beaker.

Estimated borax, % Sample weight, g.


0-10 2.0
10-25 1.0
25-50 0.75
50-90 0.50
90-100 0.40________

2. Add 100 mL of distilled water (see Notes, 1) and warm on the steam bath until the sample has
dissolved.
3. Add 2 mL of 25% sodium hydroxide solution, heat the solution almost to boiling, and add,
with stirring, 10 mL of either the SrCl2.6H2O or the Sr(NO3)2 solution to precipitate the soap
and any phosphate or silicate which may be present. Heat the solution for an additional five
minutes, stirring frequently and avoiding vigorous boiling.

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_____________MUESTREO Y ANÁLISIS DE JABÓN Y PRODUCTOS DE JABÓN___________
4. Filter through the quantitative filter paper, colecting the filtrate in a 400 mL beaker. Wash the
precipitate thoroughly with hot, distilled water (about 100 mL)
5. Make the filtrate and washings just acid to methyl red indictor with 1:1 HCl and add 0.5 mL
of acid in excess. Cover the beaker with a watch glass and heat to simmering temperature for 10
min.
6. Cool the solution in a cold water bath to room temperature. Rinse the watch glass with water
and add the washings to the solution. Using the pH meter, bring the solution to a pH of
approximately 6.0 x 6.2 by the dropwise addition of 25% sodium hydroxide solution, then bring
the pH to exactly 6.3 by the dropwise addition of 0.05 N NaOH solution.
7. Add 5 g of mannitol, stir until dissolved and titrate to a pH of 8.0 with 0.05 N or 0.10 N
NaOH, depending on the amount of borax present. The tritation should be carried out in a cold
solution, room temperature or less. Record the buret reading.
8. Conduct a blank as follows: Take a volum of boiled distilled water corresponding to the
volume of solution of solution at the end of the titration (Procedure, 7). Add 0.5 mL of 1:1 HCl.
Using the pH meter, bring the pH to approximately 6.0 - 6.2 by the dropwise addition of 25%
sodium hydroxide solution, then bring the pH to exactly 6.3 by the dropwise addition of 0.05 N
NaOH solution.
9. Add 5 g of mannitol and stir until dissolved and titrate to a pH of 8.0 with the same strength
sodium hydroxide as used in Procedure, 7 Record the buret reading. The blank should not
exceed 0.1 mL and is usually less (see Notes, 2).
Calculations:
Borax, as Na2B4O7.10H2O,%=
(A-B) x N x 9.536
Weight of sample, gr

Where-
A=mL NaOH to titrate sample (Procedure, 7)
B=mL NaOH to titrate blank (Procedure, 9)
N=normality of NaOH solution

Notes:

Caution
Hydrochloric acid is a strong acid and will cause severe burns. Protective clothing should be
worn when working with this acid. It is toxic by ingestion and inhalation and a strong irritant to
eyes and skin. The use of a properly operating fume hood is recommended. When diluting the
acid, always add the acid to the water, never the reverse.
Alkalies can burn skin, eyes, respiratory tract severely. Wear heavy rubber gloves and face
shield to protect against concentrated alkali liquids. Use effective fume removal device or gas
mask to protect respiratory tract against alkali dust or vapors. When working with extremely
caustic materials like sodium, hydroxide and potassium hydroxide, always add pellets to water
and not vice versa. These alkalies are extremely exothermic when mixed with water.Take
precautions to contain the caustic solution in the event the mixing container breaks from the
extreme heat generated.

Numbered Notes
1. Distilled carbon dioxide free water should be used throughout this procedure.

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_____________MUESTREO Y ANÁLISIS DE JABÓN Y PRODUCTOS DE JABÓN___________
2. An indicator endpoint may be employed when a pH meter is not available. The procedure is
as follows: Starting with Step 6 in the Procedure above, cool the solution in a cold water bath to
room temperature. Rinse the watch glass with water and add the washings to the solution. Add
several drops of methyl red indicator. Titrate with 0.05 N NaOH to the methyl red end point
(yellow). Record the buret reading. Add 5 g of mannitol and stir until dissolved. Add 3mL of α-
naphtholphthalein indicator solution, and tritate the boric acid complex with 0.05 N or 0.10 N
NaOH to a greenyellow endpoint. The tritation should be carried out in cold solution (room
temperature orless). A blank should be run on the amount of mannitol used in the tritation. The
blank should not exceed 0.1 mL and is usually less Methyl purple can be used in place of
methyl red.

References:
1. Bernstein and Haftel, The Determination of Borax in Soap, JAOCS 27:45 (1950).

MOISTURE

Definition: This method determines the water content of alkylbenzene sulfonate products when
the moisture is low.
Scope: Applicable to samples with moisture contents less than 2%.

Apparatus:
1. Automatic Buret (Machlett Type), 50 mL capacity. 1000 mL reservoil of amber glass with a
straight tip. The buret should also be equipped with a drying tube containing a suitable drying
agent such as anhydrous calcium sulfate, to protect the Karl Fischer reagent from moisture in
the air. Calcium chloride also is satisfactory.
Magnesium perchlorate must not be used, due to the possible danger of explosion in contact
with organic vapors.

Note-In place of the described buret, there are the number of other titration apparatus, including
automatic Karl Fisher titrators, available. These may be used, provided proper standardization
procedures are followed.

2. Erlenmeyer flask, 125mL, with ground glass stopper

Reagents:
1. Karl Fischer Reagent. This reagent is comercially available from a number of laboratory
suply companies.

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_____________MUESTREO Y ANÁLISIS DE JABÓN Y PRODUCTOS DE JABÓN___________
2. Methyl alcohol (CHOH), anhydrous. The water content of the CH3OH shall not be more than
0.1 per cent by weight. Run a blank on each new container of methyl alcohol to make certain it
meets this specification.
3. Sodium trartrate dihydrate (Na2C1H4O6.2H2O).
The water content of the sodium tratrate should be 15.66% ± 0.05%. This value can be checked
by heating sample at 150 C for 3 hr and determining the moisture loss.
Procedure:
1. Weigh to the nearest 0.1 mg a portion of the test sample, containing from 50 to 200 mg of
water, into a dry, 125 mL Erlenmeyer flask and stopper immediately.

2. Add 50 mL of anhydrous methyl alcohol and immediately cover the flask aperture with a
rubber dam (see Notes, 1). Allow to stand for a few minutes with occasional swirling.

3. Pierce the rubber dam, insert the tip of the buret, and titrate with the Karl Fischer reagent.
Approach of the end point is shown by a decrease in speed of discharge of the brown color of
the reagent and a slight change in color of the sample from yellow to reddish yellow. Continue
to titrate in 0.1 to 0.2 mL increments until the red-brown color of iodine persists.

4. Run a blank determination on 50mL of methyl alcohol, using the procedure described in
paragraphs 2 and 3.

5. Repeat the procedure described in Paragraphs 1 to 3 using 0.3 to 0.7 g of sodium tartrate
dihydrate in place of the sample.

Calculations: 1. Calculate the water equivalent of the Karl


Fischer reagent as follows-

F= A x 0.1566
T–B

Where-

F= grams of water equivalent to 1 mL, of Karl Fischer reagent

A= grams of sodium tartrate used (Procedure, paragraph 5)

T= milliliters of Karl Fischer reagent required for titration of the sodium tartrate

2. Calculate the percentage of water in the sample as follows-

Water, % = (S - B) x F x 100 ……D

Where-

S= milliliters of Karl Fischer reagent required to titrate the sample

B= mililiters of Karl Fischer reagent required to titrate the blank

F= grams of water equivalent to 1 mL of Karl Fischer reagent (from Calculations, 1)

D= grams of sample used

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_____________MUESTREO Y ANÁLISIS DE JABÓN Y PRODUCTOS DE JABÓN___________

Precision: 1. Based on experimental results, the


intralaboratory precision (95% limits) for simultaneous duplicate determinations by one analyst
is ± 0.22% at a moisture level of 70%.

2. The over-all precision (interlaboratory) is statistically estimated (95% limits) to be ± 0.17% at


a moisture level of 70%.

Notes:

Caution Methanol (methyl alcohol) is


flammable and toxic.
Avoid contact with eyes. Avoid breathing vapors.
Use effective fume removal device (an react vigorouly) with sodium hydroxide + chloroform,
potasium hydroxide - chloroform, and perchloric acid.

Numbered Notes
1. Coments automated Karl Fischer units are equipped with appropirate closures.

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