ASTM D500-95(2016)
(Test Method)Standard Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils
Standard Test Methods of Chemical Analysis of Sulfonated and Sulfated Oils
ABSTRACT
These test methods cover the chemical analysis of sulfonated and sulfated oils. Water by distillation with volatile solvent and moisture and volatile matter by hot-plate shall be tested to meet the requirements prescribed. Titration test, extraction-titration test, and ash-gravimetric test shall be performed to meet the requirements specified. Total desulfated fatty matter, total active ingredients, unsaponifiable non-volatile matter, inorganic salts, total alkalinity, and total ammonia shall be tested to meet the requirements prescribed. In the absence of ammonium or triethanolamine soaps test method, brine test method, and in the presence of ammonium or triethanolamine soaps test method shall be performed to meet the requirements prescribed. Water-immiscible organic solvents volatile with steam shall be tested to meet the requirements prescribed.
SCOPE
1.1 These test methods cover the chemical analysis of sulfonated and sulfated oils. The analytical procedures appear in the following order:
Section
Moisture:
Test Method A. Water by Distillation with Volatile Solvent
4 – 9
Test Method B. Moisture and Volatile Matter by Hot-Plate Method
10 – 14
Organically Combined Sulfuric Anhydride:
Test Method A. Titration Test
15 – 19
Test Method B. Extraction-Titration Test
20 – 24
Test Method C. Ash-Gravimetric Test (in the Presence of True
Sulfonates)
25 – 28
Total Desulfated Fatty Matter
29 – 32
Total Active Ingredients
33 – 36
Unsaponifiable Nonvolatile Matter
37 – 41
Inorganic Salts
42 – 46
Total Alkalinity
47 – 49
Total Ammonia
50 – 52
Acidity as Free Fatty Acids or Acid Number:
Test Method A. In the Absence of Ammonium or Triethanolamine Soaps
53 – 56
Test Method B. In the Presence of Dark Colored Oils but in the
Absence of Ammonium or Triethanolamine Soaps (Brine Test)
57 – 60
Test Method C. In the Presence of Ammonium or Triethanolamine Soaps
61 – 63
Water-Immiscible Organic Solvents Volatile with Steam
64 – 70
1.2 The values stated in inch-pound units are to be regarded as the standard. The metric equivalents of inch-pound units may be approximate.
1.3 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 and health practices and determine the applicability of regulatory limitations prior to use. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to usage.
General Information
Buy Standard
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D500 − 95 (Reapproved 2016)
Standard Test Methods of
Chemical Analysis of Sulfonated and Sulfated Oils
This standard is issued under the fixed designation D500; 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 2. Referenced Documents
1.1 These test methods cover the chemical analysis of 2.1 ASTM Standards:
sulfonated and sulfated oils. The analytical procedures appear D1193 Specification for Reagent Water
in the following order:
3. Purity of Reagents
Section
3.1 Purity of Reagents—Reagent grade chemicals shall be
Moisture:
used in all tests. Unless otherwise indicated, it is intended that
Test Method A. Water by Distillation with Volatile Solvent 4 – 9
all reagents shall conform to the specifications of the Commit-
Test Method B. Moisture and Volatile Matter by Hot-Plate Method 10 – 14
Organically Combined Sulfuric Anhydride:
tee on Analytical Reagents of the American Chemical Society,
Test Method A. Titration Test 15 – 19
where such specifications are available. Other grades may be
Test Method B. Extraction-Titration Test 20 – 24
used, provided it is first ascertained that the reagent is of
Test Method C. Ash-Gravimetric Test (in the Presence of True 25 – 28
Sulfonates)
sufficiently high purity to permit its use without lessening the
Total Desulfated Fatty Matter 29 – 32
accuracy of the determination.
Total Active Ingredients 33 – 36
Unsaponifiable Nonvolatile Matter 37 – 41
3.2 Purity of Water—Unless otherwise indicated, references
Inorganic Salts 42 – 46
to water shall be understood to mean reagent water conforming
Total Alkalinity 47 – 49
Total Ammonia 50 – 52
to Specification D1193.
Acidity as Free Fatty Acids or Acid Number:
Test Method A. In the Absence of Ammonium or Triethanolamine 53 – 56
MOISTURE
Soaps
Test Method B. In the Presence of Dark Colored Oils but in the 57 – 60
Method A. Water by Distillation with Volatile Solvent
Absence of Ammonium or Triethanolamine Soaps (Brine Test)
Test Method C. In the Presence of Ammonium or Triethanolamine 61 – 63
Soaps
4. Scope
Water-Immiscible Organic Solvents Volatile with Steam 64 – 70
4.1 This test method covers the determination of water
1.2 The values stated in inch-pound units are to be regarded
existing in a sample of sulfonated or sulfated oil, or both, by
as the standard. The metric equivalents of inch-pound units
distilling the sample with a volatile solvent. The method is
may be approximate.
applicable only to sulfonated and sulfated oils that do not
1.3 This standard does not purport to address all of the
contain the following: mineral acids, free sulfonic acids, or free
safety concerns, if any, associated with its use. It is the
sulfuric acid esters; or alkali hydroxides, carbonates or ac-
responsibility of the user of this standard to establish appro-
etates; or alcohol, glycerin, diethylene glycol, acetone, or other
priate safety and health practices and determine the applica-
water-miscible volatile compounds.
bility of regulatory limitations prior to use. Material Safety
Data Sheets are available for reagents and materials. Review
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
them for hazards prior to usage.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
These test methods are under the jurisdiction of ASTM Committee D12 on the ASTM website.
Soaps and Other Detergents and is the direct responsibility of Subcommittee D12.12 Reagent Chemicals, American Chemical Society Specifications, American
on Analysis and Specifications of Soaps, Synthetics, Detergents and their Compo- Chemical Society, Washington, DC. For suggestions on the testing of reagents not
nents. listed by the American Chemical Society, see Analar Standards for Laboratory
Current edition approved July 1, 2016. Published August 2016. Originally Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
approved in 1937. Last previous edition approved in 2009 as D500 – 95(2009). and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
DOI: 10.1520/D0500-95R16. MD.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D500 − 95 (2016)
5. Apparatus each 1-mL line numbered (5 mL at top). The error in any
indicated capacity may not be greater than 0.05 mL.
5.1 The apparatus required consists of a glass flask heated
by suitable means and provided with a reflux condenser
6. Reagents
discharging into a trap and connected to the flask. The
6.1 Oleic Acid, heated previous to use for 5 to 10 min over
connections between the trap and the condenser and flask shall
a free flame at a temperature of 130 to 135°C.
be interchangeable ground joints. The trap serves to collect and
6.2 Xylene.
measure the condensed water and to return the solvent to the
flask. A suitable assembly of the apparatus is illustrated in Fig.
7. Calibration
1.
7.1 To calibrate the apparatus add approximately 1 g of
5.1.1 Flask, 500-mL, of either the short-neck, round-bottom
water to a mixture of 80 g of xylene and 10 g of oleic acid.
type or the Erlenmeyer type.
Conduct the distillation as described in 8.2 – 8.4. When all the
5.1.2 Heat Source—The source of heat may be either an oil
water has distilled, cool the apparatus, add another g of water,
bath (stearic acid, paraffin wax, etc.), or an electric heater
and repeat the distillation. Continue the calibration up to the
provided with a sliding rheostat or other means of heat control.
capacity of the receiving tube.
5.1.3 Condenser—A water-cooled glass reflux condenser
(Fig. 1), having a jacket approximately 400 mm (15 ⁄4 in.) in
8. Procedure
3 1
length with an inner tube 9.5 to 12.7 mm ( ⁄8 to ⁄2 in.) in
8.1 Clean the condenser and the receiving tube thoroughly
outside diameter. The end of the condenser to be inserted in the
with soap and warm water before using. Rinse well, then treat
trap shall be ground off at an angle of 30° from the vertical axis
with hot cleaning solution (a mixture of 10 mL of saturated
of the condenser. When inserted into the trap, the tip of the
potassium dichromate (K Cr O ) and 990 mL of sulfuric acid
1 2 2 7
condenser shall be about 7 mm ( ⁄4 in.) above the surface of the
(H SO , sp gr 1.84)), and finally thoroughly wash and dry.
2 4
liquid in the trap after the distillation conditions have been
established. Fig. 1 shows a conventional sealed-in type of 8.2 Take enough of the sample to be tested for analysis to
yield about 4 mL of water. Introduce the approximate quantity
condenser, but any other condenser fulfilling the detailed
requirements above may be used. into a weighing bottle and make the weighings from the bottle
into the flask, taking care that after removal of the sample no
5.1.4 Trap—A trap made of well-annealed glass constructed
in accordance with Fig. 1 and graduated as shown to contain 5 drops of oil are left on the outside of the weighing bottle. Add
80 g of xylene and oleic acid equivalent to about two and
mL at 20°C. It shall be subdivided into 0.1-mL divisions, with
one-half times the weight of the bone-dry sample to prevent
foaming and jellying of the contents of the flask. Introduce
glass beads to prevent bumping and mix the contents of the
flask thoroughly by swirling, taking care to avoid any loss of
material. Fill the trap with xylene and immediately connect the
flask with the distillation apparatus. Insert a loose cotton plug
in the top of the condenser tube to prevent condensation of
atmospheric moisture in the condenser tube.
8.3 Heat the flask and regulate the heating so that the
condenser tube immediately below the water jacket is just
barely hot. In this way a minimum of water will condense
farther up the condenser where it may be difficult to volatilize
any moisture condensed on the walls.
8.4 Continue the distillation at the specified rate until
practically no water is visible on any part of the apparatus
except within the graduations of the trap. This operation
usually requires less than 1 h. Increase the rate of distillation in
order to remove all traces of condensed water in the condenser
tube, and continue the distillation until the water level in the
trap remains unchanged after a 10-min interval. Dislodge any
droplets adhering to the side of the receiver with a thin copper
wire twisted into a loop. Immerse the receiving tube in warm
A = 45 to 55 mm water at about 40°C for 15 min or until the xylene layer
B = 22 to 24 mm in inside diameter
becomes clear, then read and record the temperature and the
C = 9 to 11 mm in inside diameter
exact volume of the water in the trap.
D = 235 to 240 mm
E = 146 to 156 mm
9. Calibration
F and G are interchangeable joints, standard taper 24/40.
9.1 The volume of condensed water measured in the trap
may be converted into its equivalent weight in grams by means
FIG. 1 Apparatus for Water Determination by Distillation with
Volatile Solvent, Method A of Table 1. Calculate the percentage of water as follows:
D500 − 95 (2016)
A
TABLE 1 Specific Gravity of Water
13. Procedure
Temperature, °C Specific Gravity
13.1 Weigh approximately 5 g of oleic acid into the beaker
4 1.00000
and insert the thermometer. Heat the oleic acid gradually, while
35 0.99406
36 0.99371 stirring with the thermometer, until the temperature reaches
37 0.99336
130°C. Place the beaker in an oven at 105 to 110°C for 15 min,
38 0.99299
cool in a desiccator, and weigh. Repeat the heating over the hot
39 0.99262
40 0.99224 plate and in the oven until two successive weighings differ by
41 0.99186
less than 1.5 mg.
42 0.99147
43 0.99107
13.2 Place about 6 g of the sample in the weighing flask and
44 0.99066
determine the weight accurately. Transfer the sample to the
45 0.99025
beaker (containing the oleic acid and the thermometer) and
A
This table is taken from Smithsonian Tables, compiled from various authors.
weigh the flask again. Heat the mixture exactly as in the taring
of the beaker as described in 13.1. The loss in weight is
equivalent to the moisture in the sample.
14. Calculation
Water, % 5 ~A/B! 3 100 (1)
14.1 Calculate the percentage of moisture and volatile
where:
matter in the sample as follows:
A = weight of water, g, and
Moisture and volatile matter, % 5 A/B 3 100 (2)
~ !
B = weight of sample, g.
where:
Method B. Moisture and Volatile Matter by Hot-Plate
A = loss of weight, g, and
Method
B = weight of sample, g.
10. Scope
ORGANICALLY COMBINED SULFURIC
ANHYDRIDE
10.1 This test method covers the determination of the
Method A. Titration Test (For Sulfated Oils)
percentage of water and other compounds volatile at about
100°C existing in a sample of sulfonated or sulfated oil, or
15. Scope
both, by rapid evaporation. The test method is applicable only
15.1 This test method covers the determination of the
to sulfonated and sulfated oils that do not contain the follow-
ing: mineral acids, free sulfonic acids or free sulfuric acid organically combined sulfuric anhydride existing in a sample
of sulfated oil by boiling the sample with sulfuric acid and
esters, ammonia, acetic acid or similar volatile acids, alkali
hydroxides, carbonates, acetates or similar salts that may react determining the acidity of the reaction mixture. This method is
applicable only to oils that split off their combined SO upon
with oleic acid at elevated temperatures liberating volatile
acids, or glycerin, diethylene glycol, xylene, or other com- boiling with mineral acids and that do not contain compounds
that cannot be accurately titrated in water solution with methyl
pounds of similar volatility.
orange as the indicator.
11. Apparatus
16. Apparatus
11.1 The apparatus required consists of a glass-stoppered
16.1 The apparatus required consists of a glass flask pro-
weighing flask, a glass beaker, and a suitable thermometer.
vided with a glass stopper and an air condenser. The connection
11.1.1 Weighing Flasks—Any suitable glass-stoppered
between the flask and the condenser shall be a ground joint.
weighing flask of 10 to 15-mL capacity.
Perforated glass beads shall be used to prevent bumping.
11.1.2 Beaker—A Griffin low-form glass beaker with an
16.1.1 Flask—An Erlenmeyer flask (Fig. 2) made of a
approximate capacity of 150 mL and a diameter of about 5 cm.
borosilicate glass, having a capacity of approximately 300 mL
11.1.3 Heat Source—The source of heat may be either an
and provided with a glass stopper.
electric hot plate with or without asbestos paper or board cover,
16.1.2 Condenser—The condenser required consists of a
or an open flame under a suitable asbestos board and a wire
glass tube, 915 mm (36 in.) in length, and 8 mm ( ⁄16 in.) in
gauze (to spread the heat).
outside diameter. The lower end of the tube shall be flared and
11.1.4 Thermometer, graduated from 90 to 150°C, about 3
ground to fit the mouth of the Erlenmeyer flask.
in. in length, and substantially constructed.
16.1.3 Glass Beads—Perforated glass beads, made of
chemically-resistant glass, approximately 4 mm ( ⁄32 in.) in
12. Reagents
diameter. Before using, the glass beads shall be boiled thor-
12.1 Desiccating Agent—Any suitable desiccating agent
oughly in several portions of water or until the wash water
may be used.
reacts neutral to methyl orange indicator.
NOTE 1—Recent investigations seem to indicate that calcium chloride is
17. Reagents
unreliable as a laboratory desiccating agent.
12.2 Oleic Acid. 17.1 Ethyl Ether.
D500 − 95 (2016)
after each addition of reagent. Drain burets for 3 min before
taking readings. Calculate the alkalinity, A, as follows:
A 5 B 3D 2 C 3E /W (3)
@~ ! ~ !#
where:
A = total alkalinity, mg of KOH/g,
B = millilitres of H SO required for titration of the sample,
2 4
C = millilitres of NaOH solution required for titration of the
sample,
D = strength of H SO , mg of KOH/mL,
2 4
E = strength of NaOH solution, mg of KOH/mL, and
W = weight of sample, g.
18.1.2 Increase in Acidity upon Boiling, F—Weigh 10 g of
the sample into the Erlenmeyer flask and boil under the air
condenser with H SO (1+19) for 1 ⁄2 h or until both the oil and
2 4
water layers are perfectly clear, using glass beads to prevent
bumping. The volume of H SO added shall be sufficient to
2 4
neutralize the total alkalinity, A, of the sample plus 25 mL in
FIG. 2 Apparatus for Determination of Organically Combined
excess. Reg
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D500 − 95 (Reapproved 2009) D500 − 95 (Reapproved 2016)
Standard Test Methods of
Chemical Analysis of Sulfonated and Sulfated Oils
This standard is issued under the fixed designation D500; 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
1.1 These test methods cover the chemical analysis of sulfonated and sulfated oils. The analytical procedures appear in the
following order:
Section
Moisture:
Test Method A. Water by Distillation with Volatile Solvent 4 – 9
Test Method B. Moisture and Volatile Matter by Hot-Plate Method 10 – 14
Organically Combined Sulfuric Anhydride:
Test Method A. Titration Test 15 – 19
Test Method B. Extraction-Titration Test 20 – 24
Test Method C. Ash-Gravimetric Test (in the Presence of True 25 – 28
Sulfonates)
Total Desulfated Fatty Matter 29 – 32
Total Active Ingredients 33 – 36
Unsaponifiable Nonvolatile Matter 37 – 41
Inorganic Salts 42 – 46
Total Alkalinity 47 – 49
Total Ammonia 50 – 52
Acidity as Free Fatty Acids or Acid Number:
Test Method A. In the Absence of Ammonium or Triethanolamine 53 – 56
Soaps
Test Method B. In the Presence of Dark Colored Oils but in the 57 – 60
Absence of Ammonium or Triethanolamine Soaps (Brine Test)
Test Method C. In the Presence of Ammonium or Triethanolamine 61 – 63
Soaps
Water-Immiscible Organic Solvents Volatile with Steam 64 – 70
1.2 The values stated in inch-pound units are to be regarded as the standard. The metric equivalents of inch-pound units may
be approximate.
1.3 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 and health practices and determine the applicability of regulatory
limitations prior to use. Material Safety Data Sheets are available for reagents and materials. Review them for hazards prior to
usage.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
3. Purity of Reagents
3.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
These test methods are under the jurisdiction of ASTM Committee D12 on Soaps and Other Detergents and is the direct responsibility of Subcommittee D12.12 on
Analysis and Specifications of Soaps, Synthetics, Detergents and their Components.
Current edition approved Oct. 1, 2009July 1, 2016. Published December 2009August 2016. Originally approved in 1937. Last previous edition approved in 20032009 as
D500 – 95(2003).(2009). DOI: 10.1520/D0500-95R09.10.1520/D0500-95R16.
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’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D500 − 95 (2016)
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination.
3.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Specification D1193.
MOISTURE
Method A. Water by Distillation with Volatile Solvent
4. Scope
4.1 This test method covers the determination of water existing in a sample of sulfonated or sulfated oil, or both, by distilling
the sample with a volatile solvent. The method is applicable only to sulfonated and sulfated oils that do not contain the following:
mineral acids, free sulfonic acids, or free sulfuric acid esters; or alkali hydroxides, carbonates or acetates; or alcohol, glycerin,
diethylene glycol, acetone, or other water-miscible volatile compounds.
5. Apparatus
5.1 The apparatus required consists of a glass flask heated by suitable means and provided with a reflux condenser discharging
into a trap and connected to the flask. The connections between the trap and the condenser and flask shall be interchangeable
ground joints. The trap serves to collect and measure the condensed water and to return the solvent to the flask. A suitable assembly
of the apparatus is illustrated in Fig. 1.
5.1.1 Flask, 500-mL, of either the short-neck, round-bottom type or the Erlenmeyer type.
5.1.2 Heat Source—The source of heat may be either an oil bath (stearic acid, paraffin wax, etc.), or an electric heater provided
with a sliding rheostat or other means of heat control.
5.1.3 Condenser—A water-cooled glass reflux condenser (Fig. 1), having a jacket approximately 400 mm (15 ⁄4 in.) in length
3 1
with an inner tube 9.5 to 12.7 mm ( ⁄8 to ⁄2 in.) in outside diameter. The end of the condenser to be inserted in the trap shall be
ground off at an angle of 30° from the vertical axis of the condenser. When inserted into the trap, the tip of the condenser shall
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For suggestions on the testing of reagents not listed by
the American Chemical Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD.
A = 45 to 55 mm
B = 22 to 24 mm in inside diameter
C = 9 to 11 mm in inside diameter
D = 235 to 240 mm
E = 146 to 156 mm
F and G are interchangeable joints, standard taper 24/40.
FIG. 1 Apparatus for Water Determination by Distillation with Volatile Solvent, Method A
D500 − 95 (2016)
be about 7 mm ( ⁄4 in.) above the surface of the liquid in the trap after the distillation conditions have been established. Fig. 1 shows
a conventional sealed-in type of condenser, but any other condenser fulfilling the detailed requirements above may be used.
5.1.4 Trap—A trap made of well-annealed glass constructed in accordance with Fig. 1 and graduated as shown to contain 5 mL
at 20°C. It shall be subdivided into 0.1-mL divisions, with each 1-mL line numbered (5 mL at top). The error in any indicated
capacity may not be greater than 0.05 mL.
6. Reagents
6.1 Oleic Acid, heated previous to use for 5 to 10 min over a free flame at a temperature of 130 to 135°C.
6.2 Xylene.
7. Calibration
7.1 To calibrate the apparatus add approximately 1 g of water to a mixture of 80 g of xylene and 10 g of oleic acid. Conduct
the distillation as described in 8.2 – 8.4. When all the water has distilled, cool the apparatus, add another g of water, and repeat
the distillation. Continue the calibration up to the capacity of the receiving tube.
8. Procedure
8.1 Clean the condenser and the receiving tube thoroughly with soap and warm water before using. Rinse well, then treat with
hot cleaning solution (a mixture of 10 mL of saturated potassium dichromate (K Cr O ) and 990 mL of sulfuric acid (H SO , sp
2 2 7 2 4
gr 1.84)), and finally thoroughly wash and dry.
8.2 Take enough of the sample to be tested for analysis to yield about 4 mL of water. Introduce the approximate quantity into
a weighing bottle and make the weighings from the bottle into the flask, taking care that after removal of the sample no drops of
oil are left on the outside of the weighing bottle. Add 80 g of xylene and oleic acid equivalent to about two and one-half times
the weight of the bone-dry sample to prevent foaming and jellying of the contents of the flask. Introduce glass beads to prevent
bumping and mix the contents of the flask thoroughly by swirling, taking care to avoid any loss of material. Fill the trap with xylene
and immediately connect the flask with the distillation apparatus. Insert a loose cotton plug in the top of the condenser tube to
prevent condensation of atmospheric moisture in the condenser tube.
8.3 Heat the flask and regulate the heating so that the condenser tube immediately below the water jacket is just barely hot. In
this way a minimum of water will condense farther up the condenser where it may be difficult to volatilize any moisture condensed
on the walls.
8.4 Continue the distillation at the specified rate until practically no water is visible on any part of the apparatus except within
the graduations of the trap. This operation usually requires less than 1 h. Increase the rate of distillation in order to remove all traces
of condensed water in the condenser tube, and continue the distillation until the water level in the trap remains unchanged after
a 10-min interval. Dislodge any droplets adhering to the side of the receiver with a thin copper wire twisted into a loop. Immerse
the receiving tube in warm water at about 40°C for 15 min or until the xylene layer becomes clear, then read and record the
temperature and the exact volume of the water in the trap.
9. Calibration
9.1 The volume of condensed water measured in the trap may be converted into its equivalent weight in grams by means of
Table 1. Calculate the percentage of water as follows:
Water,%5 ~A/B! 3100 (1)
A
TABLE 1 Specific Gravity of Water
Temperature, °C Specific Gravity
4 1.00000
35 0.99406
36 0.99371
37 0.99336
38 0.99299
39 0.99262
40 0.99224
41 0.99186
42 0.99147
43 0.99107
44 0.99066
45 0.99025
A
This table is taken from Smithsonian Tables, compiled from various authors.
D500 − 95 (2016)
where:
A = weight of water, g, and
B = weight of sample, g.
Method B. Moisture and Volatile Matter by Hot-Plate Method
10. Scope
10.1 This test method covers the determination of the percentage of water and other compounds volatile at about 100°C existing
in a sample of sulfonated or sulfated oil, or both, by rapid evaporation. The test method is applicable only to sulfonated and sulfated
oils that do not contain the following: mineral acids, free sulfonic acids or free sulfuric acid esters, ammonia, acetic acid or similar
volatile acids, alkali hydroxides, carbonates, acetates or similar salts that may react with oleic acid at elevated temperatures
liberating volatile acids, or glycerin, diethylene glycol, xylene, or other compounds of similar volatility.
11. Apparatus
11.1 The apparatus required consists of a glass-stoppered weighing flask, a glass beaker, and a suitable thermometer.
11.1.1 Weighing Flasks—Any suitable glass-stoppered weighing flask of 10 to 15-mL capacity.
11.1.2 Beaker—A Griffin low-form glass beaker with an approximate capacity of 150 mL and a diameter of about 5 cm.
11.1.3 Heat Source—The source of heat may be either an electric hot plate with or without asbestos paper or board cover, or
an open flame under a suitable asbestos board and a wire gauze (to spread the heat).
11.1.4 Thermometer, graduated from 90 to 150°C, about 3 in. in length, and substantially constructed.
12. Reagents
12.1 Desiccating Agent—Any suitable desiccating agent may be used.
NOTE 1—Recent investigations seem to indicate that calcium chloride is unreliable as a laboratory desiccating agent.
12.2 Oleic Acid.
13. Procedure
13.1 Weigh approximately 5 g of oleic acid into the beaker and insert the thermometer. Heat the oleic acid gradually, while
stirring with the thermometer, until the temperature reaches 130°C. Place the beaker in an oven at 105 to 110°C for 15 min, cool
in a desiccator, and weigh. Repeat the heating over the hot plate and in the oven until two successive weighings differ by less than
1.5 mg.
13.2 Place about 6 g of the sample in the weighing flask and determine the weight accurately. Transfer the sample to the beaker
(containing the oleic acid and the thermometer) and weigh the flask again. Heat the mixture exactly as in the taring of the beaker
as described in 13.1. The loss in weight is equivalent to the moisture in the sample.
14. Calculation
14.1 Calculate the percentage of moisture and volatile matter in the sample as follows:
Moisture and volatile matter,%5 ~A/B! 3100 (2)
where:
A = loss of weight, g, and
B = weight of sample, g.
ORGANICALLY COMBINED SULFURIC ANHYDRIDE
Method A. Titration Test (For Sulfated Oils)
15. Scope
15.1 This test method covers the determination of the organically combined sulfuric anhydride existing in a sample of sulfated
oil by boiling the sample with sulfuric acid and determining the acidity of the reaction mixture. This method is applicable only
to oils that split off their combined SO upon boiling with mineral acids and that do not contain compounds that cannot be
accurately titrated in water solution with methyl orange as the indicator.
16. Apparatus
16.1 The apparatus required consists of a glass flask provided with a glass stopper and an air condenser. The connection between
the flask and the condenser shall be a ground joint. Perforated glass beads shall be used to prevent bumping.
16.1.1 Flask—An Erlenmeyer flask (Fig. 2) made of a borosilicate glass, having a capacity of approximately 300 mL and
provided with a glass stopper.
D500 − 95 (2016)
FIG. 2 Apparatus for Determination of Organically Combined Sulfuric Anhydride, Method A
16.1.2 Condenser—The condenser required consists of a glass tube, 915 mm (36 in.) in length, and 8 mm ( ⁄16 in.) in outside
diameter. The lower end of the tube shall be flared and ground to fit the mouth of the Erlenmeyer flask.
16.1.3 Glass Beads—Perforated glass beads, made of chemically-resistant glass, approximately 4 mm ( ⁄32 in.) in diameter.
Before using, the glass beads shall be boiled thoroughly in several portions of water or until the wash water reacts neutral to methyl
orange indicator.
17. Reagents
17.1 Ethyl Ether.
17.2 Methyl Orange Indicator Solution (1 g/L)—Dissolve 0.1 g of methyl orange in 100 mL of water.
17.3 Sodium Chloride (NaCl), solid.
17.4 Sodium Hydroxide, Standard Solution (1 N)—Accurately prepare and standardize a 1 N sodium hydroxide (NaOH)
solution. Express the strength or concentration of the solution as milligrams of KOH per millilitre; 1 mL of 1 N NaOH solution
is equivalent to 56.1 mg of KOH.
17.5 Sodium Hydroxide,
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.