Designation: D 1568 – 05

Standard Test Methods for

Sampling and Chemical Analysis of Alkylbenzene
Sulfonates1
This standard is issued under the fixed designation D 1568; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope SAMPLING
1.1 These test methods cover the sampling and chemical 3. General Requirements
analysis of paste, powder, or liquid detergent alkylbenzene
sulfonates. 3.1 The seller shall have the option of being represented at
1.2 The procedures for sampling and analysis appear in the the time of sampling and when he so requests shall be
following order: furnished with a duplicate sample.
Sections 4. Powders and Flakes Packed in Cans or Cartons
Sampling: 4.1 One can or carton shall be taken at random from not less
Powders and Flakes Packed in Cans or Cartons 3
Powders and Flakes in Bulk 4
than 1 % of the seller’s shipping containers, provided each
Liquids 6 package contains not less than 50 lb (22.7 kg). In the case of
Pastes 7 smaller containers, a can or carton shall be taken at random
Hazards 8
Preparation of Sample 9
from each lot of containers totaling not more than 5000 lb
Moisture: (2268 kg) or fraction thereof. The gross sample shall in all
Distillation Method 11-14 cases consist of not less than three cans or cartons taken at
Karl Fischer Method 15-20
Total Matter Insoluble in Alcohol 21-23
random from separate containers. In the case of very large lots
Neutral Oil 24-27 where the sample drawn as above will amount to more than 20
Chlorides Calculated as Sodium Chloride (NaCl) 28-31 lb (9.1 kg), the percentage of packages sampled shall be
pH 32
reduced so that the amount drawn will not exceed 20 lb (9.1
1.3 This standard does not purport to address all of the kg). The individual cans or cartons shall be tightly wrapped at
safety concerns, if any, associated with its use. It is the once in paraffined paper and sealed by rubbing the edges with
responsibility of the user of this standard to establish appro- a heated iron. The inspector shall accurately weigh each
priate safety and health practices and determine the applica- wrapped can or carton and record its weight and the date of
bility of regulatory limitations prior to use. For a specific weighing on the wrapper. The wrapped cans or cartons shall be
hazards statement, see Section 8. placed in an airtight container which should be nearly filled,
and which shall then be sealed, marked, and sent to the
2. Referenced Documents laboratory for test. Samples shall be kept cool until tested.
2.1 ASTM Standards: 2
D 1172 Test Method for pH of Aqueous Solutions of Soaps 5. Powders and Flakes in Bulk
and Detergents 5.1 A grab sample of not less than 0.5 lb (227 g) shall be
D 1193 Specification for Reagent Water taken at random from not less than 1 % of the seller’s shipping
containers, provided each package contains not less than 100 lb
(45.4 kg). In the case of smaller containers, a grab sample of
1
These test methods are under the jurisdiction of ASTM Committee D12 on not less than 0.5 lb (227 g) shall be taken at random from each
Soaps and Other Detergents and is the direct responsibility of D12.12 on Analysis
of Soaps and Synthetic Detergents. lot of containers totaling not more than 10,000 lb (4536 kg) or
Current edition approved May 1, 2005. Published June 2005. Originally fraction thereof. The gross sample shall in all cases consist of
approved in 1958. Last previous edition approved in 1997 as D 1568 – 97.
2
not less than three grab samples of 0.5 lb (227 g) each taken at
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
random from separate containers. In the case of very large lots
Standards volume information, refer to the standard’s Document Summary page on the sample drawn as above will amount to more than 20 lb (9.1
the ASTM website. kg), the percentage of packages sampled shall be reduced so

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 D 1568 – 05
that the amount drawn shall not exceed 20 lb (9.1 kg). The two or three times, and upon removal a core of the material being sampled
inspector shall rapidly mix the gross sample and place it in an is obtained.
airtight container which shall be filled, sealed, marked, accu- 8. Hazards
rately weighed, with its weight and the date of weighing
recorded on the package, and be sent to the laboratory for test. 8.1 All reagents and chemicals should be handled with care.
Samples shall be kept cool until tested. Before using any chemical, read and follow all safety precau-
tions and instructions on the manufacturer’s label or MSDS
6. Liquids (Material Safety Data Sheet).
6.1 A sample of not less than 0.5 pt (236.6 mL) shall be 9. Preparation of Sample
taken at random from not less than 1 % of the seller’s shipping
9.1 Powders and Flakes—Minimizing exposure to air, rap-
containers, provided each package contains not less than 10 gal
idly disintegrate and mix the sample of powdered, flake, or
(37.9 L). In the case of smaller containers, a sample of not less
chip product. If desired, quarter down to about 1 lb (453.6 g).
than 0.5 pt (236.6 mL) shall be taken at random from each lot
Weigh at once all portions for analysis, preserving the remain-
of containers totaling not more than 1000 gal (3785.4 L) or
der in an airtight container in a cool place.
fraction thereof. The gross sample shall in all cases consist of
9.2 Liquids—No preparation of the sample of liquid, other
not less than three samples of 0.5 pt (236.6 mL) each taken at
than a thorough mixing, is necessary unless it is received
random from separate containers. Before drawing the sample
during very cold weather, when it should be allowed to stand
from the container selected, the contents of the container shall
at least 1 h after it has warmed to room temperature (20 to
be thoroughly agitated. The inspector shall thoroughly mix the
30°C) before it is tested, particularly for its lathering qualities.
gross sample, place it in clean, dry cans or bottles, which shall
be completely filled and securely stoppered with clean corks or NOTE 2—If pastes or liquids are known to be acidic, and decomposition
caps, then sealed, marked, and sent to the laboratory for test. of sample can result from heating, the samples shall be adequately labeled
for precautionary treatment and warmed to room temperature or other
maximum temperature as agreed upon for mixing and sampling.
7. Pastes
9.3 Pastes—Store preferably in glass. If crystals separate,
7.1 Pastes Packed in Cans or Cartons of 5 lb (2.27 kg) or
melt on water bath (Note 1).
Less—One can or carton shall be taken at random from not less
than 1 % of the seller’s shipping containers, provided each
METHODS OF CHEMICAL ANALYSIS
package contains not less than 50 lb (22.7 kg). In the case of
smaller containers, a can or carton shall be taken at random 10. Purity of Reagents
from each lot of containers totaling not more than 5000 lb
(2268 kg) or fraction thereof. The gross sample shall in all 10.1 Reagent grade chemicals shall be used in all tests.
cases consist of not less than three cans or cartons taken at Unless otherwise indicated, it is intended that all reagents shall
random from separate containers. In the case of very large lots conform to the specifications of the Committee on Analytical
where the sample drawn as above will amount to more than 20 Reagents of the American Chemical Society, where such
lb (9.1 kg), the percentage of packages sampled shall be specifications are available.3 Other grades may be used, pro-
reduced so that the amount drawn shall not exceed 20 lb (9.1 vided it is first ascertained that the reagent is of sufficiently
kg). The samples shall be wrapped, sealed, marked, and sent to high purity to permit its use without lessening the accuracy of
the laboratory for test. the determination.
7.2 Pastes Packed in Bulk—A “trier” sample (Note 1) of not 10.2 Unless otherwise indicated, references to water shall be
less than 0.5 lb (227 g) shall be taken at random from not less understood to mean reagent water conforming to Specification
than 1 % of the seller’s shipping containers, provided each D 1193.
package contains not less than 50 lb (22.7 kg). In the case of
MOISTURE BY THE DISTILLATION METHOD
smaller containers, a “trier” sample of not less than 0.5 lb (227
(Preferred Method)
g) shall be taken at random from each lot of containers totaling
not more than 5000 lb (2268 kg) or fraction thereof. The gross
11. Apparatus
sample shall in all cases consist of not less than three 0.5-lb
(227-g) samples, each taken at random from separate contain- 11.1 The apparatus required shall consist of a glass flask
ers. With very large lots where the sample drawn as above will heated by suitable means and provided with a reflux condenser
amount to more than 10 lb (4.5 kg), the percentage of packages discharging into a trap and connected to the flask. The
sampled shall be reduced so that the amount drawn shall not connections between the trap and the condenser and flask shall
exceed 10 lb (4.5 kg). The inspector shall promptly place the be interchangeable ground joints. The trap serves to collect and
gross sample in a clean, dry, airtight and watertight container,
which shall be filled, sealed, marked, and sent to the laboratory
for test. 3
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
NOTE 1—A trier sample is obtained by inserting a “trier” into the listed by the American Chemical Society, see Analar Standards for Laboratory
material. A trier is a halfround steel cylinder 1⁄2 to 3⁄4 in. (12.7 to 19 mm) Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
in diameter, 6 to 36 in. (152 to 914 mm) in length, pointed on one end and and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
having a grip handle on the other end. After insertion, the trier is turned MD.

2
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 D 1568 – 05
measure the condensed water and to return the solvent to the 11.1.4.3 25-mL Trap—Subdivided from 0 to 1 mL in
flask. A suitable assembly of the apparatus is illustrated in Fig. 0.1-mL divisions and from 1 to 25 mL in 0.2-mL divisions.
1. NOTE 3—The condenser and trap should be thoroughly cleaned before
11.1.1 Flask—A 1000-mL flask of either the short-neck, use.
round-bottom type or the Erlenmeyer type.
11.1.2 Heat Source—Either an oil bath (stearic acid, paraffin 12. Solvent
wax, etc.), or an electric heater provided with a sliding rheostat 12.1 Xylene (or Toluene)—Saturate xylene (or toluene) with
or other means of heat control. water by shaking with a small quantity of water and distill. Use
11.1.3 Condenser—A water-cooled glass reflux condenser the distillate for the determination.
(Fig. 1), having a jacket approximately 153⁄4 in. (400 mm) in
length, with an inner tube 3⁄8 to 1⁄2 in. (9.5 to 12.7 mm) in 13. Procedure
outside diameter, and not less than 1⁄4 in. (6.35 mm) in inside 13.1 Transfer to the 1000-mL flask, equipped with the size
diameter, shall be used. The end of the condenser to be inserted of the trap specified in 11.1.4, an amount of sample according
in the trap may be ground off at an angle of 30° from the to the percentage of moisture expected, as follows:
vertical axis of the condenser. When inserted into the trap, the Moisture Expected, % Weight of Sample to be Used, gA
tip of the condenser shall be about 1⁄4 in. (7 mm) above the
surface of the liquid in the trap after the distillation conditions 0 to 5, incl 50 6 5
Over 5 to 17, incl 50 6 5
have been established. Fig. 1 shows a conventional sealed-in Over 17 to 30, incl 406 4
type of condenser, but any other condenser fulfilling the Over 30 to 50, incl 30 6 3
detailed requirements of this paragraph may be used. Over 50 to 70, incl 30 6 3
Over 70 to 85, incl 25 6 2
11.1.4 Trap—For greatest accuracy several trap sizes are _______________
allowable, depending upon the percentage of moisture ex- A
Weighed to the nearest 0.25 g.
pected: Add immediately about 100 mL of xylene or toluene. Place
Moisture Expected, percent Size of Trap, mL a small, thin sheet of long-fiber, chemical-resistant glass4 wool
0 to 5, incl 5 on the surface of the toluene. The glass wool should be
Over 5 to 17, incl 10 thoroughly dried in the oven and held in the desiccator before
Over 17 to 30, incl 10 use.
Over 30 to 50, incl 25
Over 50 to 70, incl 25 13.2 Connect the flask and receiver to the condenser and
Over 70 to 85, incl 25 pour sufficient xylene or toluene down the condenser tube to
Traps made of well-annealed glass, constructed essentially cause a slight overflow through the side tube. Wrap the flask
as shown in Fig. 1, and graduated to contain one of the and tube leading to the receiver with an insulating cloth, so that
following specified volumes at 20°C shall be used: refluxing will be under better control.
11.1.4.1 5-mL Trap—Subdivided into 0.1-mL divisions with 13.3 Heat the oil bath with a gas burner or other source of
each 1 mL line numbered (5 mL at top). The error in any heat, or apply heat directly to the flask with an electric heater
indicated capacity may not be greater than 0.05 mL. and distill slowly. The rate at the start should be approximately
11.1.4.2 10-mL Trap—Subdivided from 0 to 1 mL in 100 drops/min. When the greater part of the water has distilled
0.1-mL divisions and from 1 to 10 mL in 0.2-mL divisions. over, increase the distillation rate to 200 drops/min until no
more water is collected. Purge the reflux condenser during the
distillation with 5-mL portions of xylene (or toluene) to wash
down any moisture adhering to the walls of the condenser. The
water in the receiver may be made to separate from the xylene
(or toluene) by using a spiral copper or nichrome wire. Move
the wire up and down in the condenser occasionally, thus
causing the water to settle at the bottom of the receiver. Reflux
for at least 2 h, and shut off the heat at the end of this period.
13.4 Wash down condenser with 1 mL of absolute ethanol
(CH3CH2OH). Adjust the temperature of the distillate to 20°C
and read the volume of water.

14. Calculations
14.1 Calculate the percentage of moisture as follows:
Moisture, % 5 [~V3 0.998!/W] 3 100 (1)

where:

4
FIG. 1 Assembly of Distillation Apparatus Borosilicate glass has been found satisfactory for this purpose.

3
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 D 1568 – 05

V = volume of water, mL at 20°C, and yellow to reddish yellow. Continue to titrate in 0.1 to 0.2-mL
W = weight of the sample, g. increments until the red-brown color of iodine persists.
18.4 Blank—Run a blank determination on 50 mL of methyl
WATER BY THE KARL FISCHER TITRATION alcohol, using the procedure described in 18.2 and 18.3.
METHOD 18.5 Repeat the procedure described in 18.1-18.3 using 0.3
(Alternative Method) to 0.7 g of sodium tartrate dihydrate in place of the sample.
15. Application 19. Calculations
15.1 This method is intended to be used where the amount 19.1 Calculate the water equivalent of the Karl Fischer
of moisture is low. reagent as follows:
16. Apparatus C 5 ~A3 0.1566!/B (2)

16.1 Automatic Buret (Machlett Type), 50-mL capacity,

1000-mL reservoir of amber glass with a straight tip. The buret where:
should also be equipped with a drying tube containing a C = grams of water equivalent to 1 mL of Karl Fischer
suitable drying agent such as anhydrous calcium sulfate reagent,
(Drierite)5 to protect the Karl Fischer reagent from moisture in A = grams of sodium tartrate used (18.5), and
the air. Calcium chloride also is satisfactory. Magnesium B = millilitres of Karl Fischer reagent required for titration
perchlorate (Dehydrite) must not be used, due to the possible of the sodium tartrate.
danger of explosion in contact with organic vapors.6 19.2 Calculate the percentage of water in the sample as
follows:
NOTE 4—Instead of the described and recommended buret there are a
number of other practical arrangements of titration apparatus. Water, % 5 [~A 2 B! 3 C/D] 3 100 (3)

17. Reagents
where:
17.1 Karl Fischer Reagent—Purchase as separate stable A = millilitres of Karl Fischer reagent required to titrate the
solutions of iodine in methanol and sulfur dioxide in pyridine sample,
with directions for mixing prior to use.7 Alternatively, stable B = millilitres of Karl Fischer reagent required to titrate the
single-solution, pyridine-free reagent solutions are available blank,
from laboratory supply houses.8 C = grams of water equivalent to 1 mL of Karl Fischer
17.2 Methyl Alcohol, Anhydrous—The water content of the reagent, and
methyl alcohol (CH3OH) shall not be more than 0.1 weight D = grams of sample used.
percent. Run a blank on each new container of methyl alcohol
to establish the water content. 20. Precision
17.3 Sodium Tartrate Dihydrate (Na2C4·H4O6·2H2O)— 20.1 Based on experimental results, the intralaboratory
The water content of the sodium tartrate should be 15.66 6 precision (95 % limits) for simultaneous duplicate determina-
0.05 %. This value can be checked by heating a sample at tions by one analyst is 6 0.22 % at a moisture level of 70 %.
150°C for 3 h. 20.2 The over-all precision (intralaboratory) is statistically
estimated (95 % limits) to be 6 0.17 % at a moisture level of
18. Procedure 70 %.
18.1 Weigh to the nearest 0.1 mg a portion of the sample,
containing from 50 to 200 mg of water, into a dry, 125-mL TOTAL MATTER INSOLUBLE IN ALCOHOL
Erlenmeyer flask and stopper immediately.
18.2 Add 50 mL of methyl alcohol and immediately cover 21. Reagent
the flask aperture with a rubber dam.9 Allow to stand for a few 21.1 Ethyl Alcohol, Neutral (95 %)—Freshly boiled ethyl
minutes with occasional swirling. alcohol (95 % or higher) and neutral to phenolphthalein indi-
18.3 Pierce the rubber dam, insert the tip of the buret, and cator, conforming to either Formula No. 3A or No. 30 of the
titrate with the Karl Fischer reagent. Approach of the end point U.S. Bureau of Internal Revenue.
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 22. Procedure
22.1 Transfer 2 g of the sample, weighed to nearest 0.001 g,
to a 250-mL beaker. Add 100 mL of neutral ethyl alcohol
5
Drierite, which is a special indicating type of anhydrous calcium sulfate, is (95 %), cover the beaker, and heat on the steam bath with
obtainable from the W. A. Hammond Co., Yellow Springs, Ohio. frequent stirring and maceration of the sample until completely
6
A suitable buret can be obtained from the Precision Scientific Co., 3737
Cortland St., Chicago, Ill. 60647. disintegrated. Let settle and filter the supernatant liquid
7
Instructions for laboratory preparation of the Karl Fischer Reagent are given in through a tared Gooch crucible, with suction, into a 300-mL
Section 2(1.1) of ASTM Method D 890, Test for Water in Liquid Naval Stores, 1983 Erlenmeyer flask, retaining as much of the residue as possible
Annual Book of ASTM Standards, Vol 06.03.
8
Examples of brands available are Hydranalt of Riedel-de Faën AG, and
in the beaker. Repeat this extraction three times with 25-mL
Aquastart of EM Science, Inc. portions of hot neutral ethyl alcohol (95 %), each time retain-
9
Davol “Sani Tab” caps have been found suitable for this purpose. ing as much of the residue as possible in the beaker. Finally,

4
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 D 1568 – 05
evaporate any remaining alcohol and dissolve the residue in the siphon up and away from the liquid in the cylinder. Gently
smallest possible quantity of hot water (5 mL is sufficient). blow the ether remaining in the siphon into the Erlenmeyer
Reprecipitate the alcohol-insoluble matter by slowly adding, flask. Rinse the exit end of the siphon with a small volume of
while stirring vigorously, 50 mL of neutral ethyl alcohol. ether.
25.4 Remove the ether by distillation in a controlled tem-
NOTE 5—Solution and reprecipitation of alcohol-insoluble matter is
necessary for complete separation from alcohol-soluble matter. perature water bath held at 60 to 70°C.
22.2 Transfer the precipitate quantitatively to the tared NOTE 7—The use of a regulated, steam-heated water bath is recom-
Gooch crucible, washing well with 95 % alcohol. Dry 2 h or mended. An electrically-heated sand bath may be used in place of the
water bath, provided certain safety measures are carried out. The switch
longer at 105 6 2°C. Cool in a desiccator and weigh. Repeat
control should be some distance away from the hot plate and place of
heating until constant weight is attained. work. A sand bath of such size as to fit on top of the hot plate should be
provided. The temperature of the sand bath should be automatically
23. Calculation maintained between 60 and 70°C by a suitable regulator.10
23.1 Calculate the percentage of total matter insoluble in 25.5 Repeat the procedure described in 25.2-25.4 four
alcohol as follows: additional times, making a total of five extractions.
T 5 ~M/W! 3 100 (4)
NOTE 8—The same siphon must be used throughout the determination.
NOTE 9—The ether should be evaporated to a small volume after each
where: extraction, permitting the total volume of ether from the next extraction to
be held conveniently in the 250-mL flask. Do not attempt to evaporate
T = percentage of total matter insoluble in alcohol,
more than 125 mL of ether at one time, as losses due to foaming may
M = grams of insoluble matter, and occur.
W = grams of sample used.
25.6 Evaporate as much as possible of the petroleum ether
NEUTRAL OIL from the combined extracts on the water bath. Remove the
flask from the water bath when the ether no longer distills from
24. Reagents the flask.
24.1 Acetone. 25.7 Place the flask on a sheet of asbestos 1⁄8 in. (3 mm)
24.2 Ethyl Alcohol, Neutral (95 %)—Freshly boiled ethyl thick on a boiling water bath and remove the last traces of ether
alcohol, 95 % or higher and neutral to phenolphthalein indica- with the aid of a stream of clean, dry air. Do not leave on the
tor, conforming to either Formula No. 3A or No. 30 of the U.S. water bath for any time longer than absolutely necessary to
Bureau of Internal Revenue.. volatilize the petroleum ether. This should take no more than 5
24.3 Petroleum Ether, having a distillation range between min.
30 and 60°C, or n-pentane having a distillation range between NOTE 10—If the operation described in 25.7 requires more than 5 min,
33 and 41°C. either too great a volume of ether remained in the flask in the procedure
described in 25.6, or the stream of air is of insufficient volume, or both
25. Procedure conditions are abnormal. Take the proper steps to correct either or both
25.1 Accurately weigh a sample equivalent to 3 to 5 g of sources of error.
active ingredient and transfer to a 250-mL extraction cylinder. 25.8 Add 2 mL of acetone and repeat the procedure de-
Add 50 mL of neutral ethyl alcohol and 50 mL of water. Shake scribed in 25.7. Wipe the flask with a clean cloth, cool in a
to disperse. desiccator, and weigh.
25.2 Add 50 mL of petroleum ether (or n-pentane), stopper
the cylinder, and shake up and down vigorously for 1 min 26. Calculation
(Note 6). Remove the stopper and wash it and the internal walls 26.1 Calculate the results as follows:
of the cylinder with a small volume of petroleum ether. Allow
Neutral oil, ~unsulfonated material! % 5 ~A/B! 3 100 (5)
to stand until the emulsion breaks and both layers are perfectly
clear.
NOTE 6—Use of ethyl ether yields higher values because of increased
where:
solubility of sulfones, etc. A = grams of residue, and
B = grams of sample used.
25.3 Siphon off the ether layer into a dry, tared 250-mL
wide-mouth Erlenmeyer flask. Care should be taken not to 27. Precision
siphon off any of the bottom alcohol-water layer with the ether
27.1 Based on experimental results, the intralaboratory
extract. The end of the siphon tube should be near the top of the
precision of this method is statistically estimated (95 % limits)
ether layer at the start of the siphoning operation and away
to be 6 0.03 %.
from the cylinder wall. During the siphoning, push the tube
27.2 For simultaneous duplicate determinations by one
down gradually as far as possible without contamination to
analyst, the estimated precision is 6 0.01 %.
within 1⁄8 to 1⁄4 in. (3 to 6 mm) of the boundary between the
ether and water layers. If the operation of siphoning off the
ether extract is carefully carried out, no water will be siphoned
off with the ether layer. After the siphoning step, slide the 10
The Foxboro regulator has been found satisfactory for this purpose.

5
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 D 1568 – 05
CHLORIDES CALCULATED AS SODIUM 30.4 Clean the silver electrode in the HNO3(1+1) containing
CHLORIDE (NaCl) NaNO2. Set up the titration cell with the silver electrode
connected to the top terminal and the saturated calomel cell
28. Apparatus connected to the bottom terminal. Set the pH meter on + mV.
28.1 Stirrer Motor and Small Glass Rod Stirrer. Start the stirring and titrate the solution potentiometrically as
28.2 Potentiometer.11 follows:
28.3 Calomel Reference Electrode, saturated. 30.4.1 Add 0.5 mL of AgNO3 solution and measure the emf.
28.4 Silver Wire Electrode, 1 mm in diameter by 120 mm in If appreciable chloride is present, the emf should be in the
length. range of 100 mV.
30.4.2 Add AgNO3 solution slowly in 2 to 3-mL portions
29. Reagents and Materials until the emf reaches 200 mV. Stir well.
29.1 Acetone. 30.4.3 Add AgNO3 solution in 0.1-mL portions, allowing
29.2 Ethyl Alcohol—Freshly boiled ethyl alcohol conform- sufficient time after each addition for the solution to reach
ing to Formula No. 3A or No. 30 of the U.S. Bureau of Internal equilibrium (60 to 80 s). Measure the emf (stirrer off) at each
Revenue. 0.1-mL point.
29.3 Methyl Orange Indicator Solution. 30.4.4 Calculate the end point by the rate of change method
29.4 Nitric Acid (1+1)—Mix 1 volume of concentrated (Note 11). The end point is usually in the range of 260 to 270
nitric acid (HNO3, sp gr 1.42) containing 0.3 % sodium nitrite mV.
(NaNO2) with 1 volume of water. NOTE 11—Example—The method for determining the maximum rate of
29.5 Nitric Acid (1+4)—Mix 1 volume of HNO3 (sp gr change is as follows:
1.42) with 4 volumes of water.
29.6 Silver Nitrate, Standard Solution (0.2 N)—Prepare and mL emf DE† DE8
21.20 210
standardize a 0.2 N silver nitrate (AgNO3) solution as follows: 21.30 220 10 10
Weigh 17 g of AgNO3 to the nearest 0.001 g. Dissolve in water 21.40 240 20 17A
and transfer to a 500-mL volumetric flask. Dilute to the mark. 21.50 277 37
21.60 302 25 12
Standardize as follows: Dry about 10 g of NaCl at 110°C to _________________
constant weight. Weigh about 2.00 g of the dried NaCl to the A
Maximum rate of change.
nearest 0.001 g. Dissolve in a solvent consisting of 60 % water
and 40 % alcohol. Transfer to a 100-mL volumetric flask and End point 5 21.4 1 ~@17/~17 1 21!# 3 0.1! (7)
dilute to the mark with solvent. Pipet 100 mL of the NaCl 5 21.46 mL (7)
solution to a beaker and titrate with the AgNO3 solution as
described in Section 30. 30.5 Run a blank and subtract the value obtained from the
29.6.1 Calculate the normality of the AgNO3 solution as value calculated in 30.4.4.
follows:
Normality 5 ~A 3 10!/~B 3 58.45! (6) 31. Calculations
31.1 Calculate as sodium chloride (NaCl) the percentage of
chlorides present, as follows:
where:
A = grams of NaCl used, and A 5 [~S 2 B!N 3 5.85]/C (8)
B = millilitres of AgNO3 solution required for titration of
the NaCl.
where:
A = percentage of chlorides present, calculated as NaCl,
30. Procedure S = millilitres of AgNO3 solution required for titration of
30.1 Chlorides may be determined on the original sample, the sample,
the alcohol-insoluble portion, or on the alcohol-soluble matter, B = millilitres of AgNO3 solution required for titration of
and should be reported on these bases, the total chlorides the blank,
calculated as NaCl being reported for the analysis of the N = normality of the AgNO3 solution, and
original sample. C = grams of sample used.
30.2 Weigh to 6 0.001 g a portion of the sample approxi-
mately equal to 30 g divided by the percentage of NaCl pH
expected, but the sample should not exceed 10 g.
30.3 Dissolve in 250 mL of hot water, add 2 drops of methyl 32. Procedure
orange indicator solution, and acidify to the acid color by 32.1 Determine the pH in accordance with Test Method
adding HNO3(1+4). Warm slightly and stir to effect maximum D 1172, except measure 10 min after adjusting the solution of
solution. Add 50 mL of acetone. the sample to volume.

33. Keywords
11
The Beckman Model G pH meter has been found satisfactory for this purpose. 33.1 alkylbenzene sulfonates; chemical analysis; sampling

6
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 D 1568 – 05
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