ASTM D501-03(2023)
(Test Method)Standard Test Methods of Sampling and Chemical Analysis of Alkaline Detergents
Standard Test Methods of Sampling and Chemical Analysis of Alkaline Detergents
ABSTRACT
These test methods cover procedures for the sampling and chemical analysis of inorganic alkaline detergents. These detergents include caustic soda, soda ash, modified soda (sequicarbonate type), sodium bicarbonate, sodium metasilicate, trisodium phosphate, tetrasodium pyrophosphate, borax, and sodium triphosphate. Different tests shall be conducted in order to determine the following properties of the detergents: total alkalinity, matter insoluble in water content, apparent density, ignition loss, pH level, turbidity, temperature rise, and particle size. Chemical analysis of the samples shall be performed by using either reverse-flow ion-exchange chromatography or paper chromatography.
SCOPE
1.1 These test methods cover procedures for the sampling and chemical analysis of inorganic alkaline detergents.
1.2 The procedures appear in the following order:
Sections
Caustic Soda:
Sampling
5
Total Alkalinity as Sodium Oxide (Na2O)
6 – 8
Sodium Hydroxide (NaOH)
9 – 11
Carbonate as Sodium Carbonate (Na2CO3)
12
Carbon Dioxide (CO2) by the Evolution Method
13 – 16
Soda Ash:
Sampling
17
Matter Volatile at 150 °C to 155 °C
18 and 19
Total Alkalinity as Sodium Carbonate (Na2CO3 )
20 – 22
Sodium Bicarbonate (NaHCO3)
23 – 25
Sodium Bicarbonate (NaHCO3) by Potentiometric Titration
26 – 28
Matter Insoluble in Water
29 and 30
Apparent Density
31 and 32
Modified Soda (Sequicarbonate Type):
Sampling
33
Total Alkalinity as Sodium Oxide (Na2O)
34 – 36
Sodium Bicarbonate (NaHCO3) and Sodium Carbonate (Na2CO3)
37 – 39
Matter Insoluble in Water
40
Sodium Bicarbonate:
Sampling
41
Sodium Bicarbonate, Sodium Carbonate, and Free Moisture
42 – 45
Matter Insoluble in Water
46
Sodium Metasilicate, Sodium Sesquisilicate and Sodium Orthosil- icate:
Sampling
47
Total Alkalinity as Sodium Oxide (Na2O)
48 – 50
Total Silica as SiO2
51 – 53
Sodium Metasilicate (Na2SiO3·5H2O)
54
Sodium Sesquisilicate (3Na2O·2SiO2·11H2O)
55
Matter Insoluble in Water
56 and 57
Loss on Ignition of Sodium Sesquisilicate (3Na2O·2SiO2 ·11H2O)
58 and 59
Sodium Orthosilicate (Na4SiO4)
60
Trisodium Phosphate:
Sampling
61
Trisodium Phosphate (Na3PO4) Content and Phosphorus Pentoxide (P2O5)
62 – 64
Trisodium Phosphate Calculated as Na3PO4·12H2O, Na3PO4· H2O, Na3PO4, and as P2O5
65 – 68
Total Alkalinity as Sodium Oxide (Na2O)
69 – 71
Matter Insoluble in Water
72 and 73
Tetrasodium Pyrophosphate:
Sampling
74
Tetrasodium Pyrophosphate
(Na4P2O7)
75 – 79
Matter Insoluble in Water
80 and 81
Loss on Ignition
82 and 83
Borax:
Sampling
84
Total Borate and Excess Alkalinity or Acidity
85 – 87
Matter Insoluble in Water
88 and 89
Sodium Triphosphate:
Sampling
90
Tritratable Na2O
91 – 94
Total P2O5:
Preferred Method
95 – 97
Alternative Method
98 – 101
pH Titration
102 – 107
Quantitative Separation and Measurement of Various Phosphates:
Reverse-Flow Ion-Exchange Chromatography (Preferred Method)
108 – 119
Paper Chromatographic Method
120 – 127
pH of 1 percent Solution
128
Turbidity
129
Temperature Rise
130 – 134
Sulfate
135 – 137
Ignition Loss
140 and 141
Matter Insoluble in Water
142 – 144
Particle Size
145
Orthophosphate
146 – 151
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of th...
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D501 − 03 (Reapproved 2023)
Standard Test Methods of
Sampling and Chemical Analysis of Alkaline Detergents
This standard is issued under the fixed designation D501; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope
Sections
Total Alkalinity as Sodium Oxide (Na O) 69 – 71
1.1 These test methods cover procedures for the sampling
Matter Insoluble in Water 72 and 73
and chemical analysis of inorganic alkaline detergents. Tetrasodium Pyrophosphate:
Sampling 74
1.2 The procedures appear in the following order:
Tetrasodium Pyrophosphate
(Na P O ) 75 – 79
4 2 7
Sections
Matter Insoluble in Water 80 and 81
Caustic Soda:
Loss on Ignition 82 and 83
Sampling 5
Borax:
Total Alkalinity as Sodium Oxide (Na O) 6 – 8
Sampling 84
Sodium Hydroxide (NaOH) 9 – 11
Total Borate and Excess Alkalinity or Acidity 85 – 87
Carbonate as Sodium Carbonate (Na CO ) 12
2 3
Matter Insoluble in Water 88 and 89
Carbon Dioxide (CO ) by the Evolution Method 13 – 16
Sodium Triphosphate:
Soda Ash:
Sampling 90
Sampling 17
Tritratable Na O 91 – 94
Matter Volatile at 150 °C to 155 °C 18 and 19
Total P O :
2 5
Total Alkalinity as Sodium Carbonate (Na CO ) 20 – 22
2 3
Preferred Method 95 – 97
Sodium Bicarbonate (NaHCO ) 23 – 25
Alternative Method 98 – 101
Sodium Bicarbonate (NaHCO ) by Potentiometric Titration 26 – 28
pH Titration 102 – 107
Matter Insoluble in Water 29 and 30
Quantitative Separation and Measurement of Various Phosphates:
Apparent Density 31 and 32
Reverse-Flow Ion-Exchange Chromatography (Preferred
Modified Soda (Sequicarbonate Type):
Method) 108 – 119
Sampling 33
Paper Chromatographic Method 120 – 127
Total Alkalinity as Sodium Oxide (Na O) 34 – 36
pH of 1 percent Solution 128
Sodium Bicarbonate (NaHCO ) and Sodium Carbonate (Na CO ) 37 – 39
3 2 3
Turbidity 129
Matter Insoluble in Water 40
Temperature Rise 130 – 134
Sodium Bicarbonate:
Sulfate 135 – 137
Sampling 41
Ignition Loss 140 and
Sodium Bicarbonate, Sodium Carbonate, and Free Moisture 42 – 45
Matter Insoluble in Water 46
Matter Insoluble in Water 142 – 144
Sodium Metasilicate, Sodium Sesquisilicate and Sodium Orthosil-
Particle Size 145
icate:
Orthophosphate 146 – 151
Sampling 47
Total Alkalinity as Sodium Oxide (Na O) 48 – 50
1.3 The values stated in SI units are to be regarded as
Total Silica as SiO 51 – 53
standard. No other units of measurement are included in this
Sodium Metasilicate (Na SiO ·5H O) 54
2 3 2
Sodium Sesquisilicate (3Na O·2SiO ·11H O) 55
2 2 2 standard.
Matter Insoluble in Water 56 and 57
Loss on Ignition of Sodium Sesquisilicate (3Na O·2SiO ·11H O) 58 and 59
2 2 2 1.4 This standard does not purport to address all of the
Sodium Orthosilicate (Na SiO ) 60
4 4
safety concerns, if any, associated with its use. It is the
Trisodium Phosphate:
Sampling 61 responsibility of the user of this standard to establish appro-
Trisodium Phosphate (Na PO ) Content and Phosphorus
3 4
priate safety, health, and environmental practices and deter-
Pentoxide (P O ) 62 – 64
2 5
mine the applicability of regulatory limitations prior to use.
Trisodium Phosphate Calculated as Na PO ·12H O, Na PO ·
3 4 2 3 4
H O, Na PO , and as P O 65 – 68
Material Safety Data Sheets are available for reagents and
2 3 4 2 5
materials. Review them for hazards prior to usage.
1.5 This international standard was developed in accor-
These test methods are under the jurisdiction of ASTM Committee D12 on
dance with internationally recognized principles on standard-
Soaps and Other Detergents and are the direct responsibility of Subcommittee
D12.12 on Analysis and Specifications of Soaps, Synthetics, Detergents and their
ization established in the Decision on Principles for the
Components.
Development of International Standards, Guides and Recom-
Current edition approved July 1, 2023. Published July 2023. Originally approved
mendations issued by the World Trade Organization Technical
in 1938. Last previous edition approved in 2016 as D501 – 03 (2016). DOI:
10.1520/D0501-03R23. Barriers to Trade (TBT) Committee.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D501 − 03 (2023)
2. Referenced Documents 4. Purity of Reagents
2.1 ASTM Standards:
4.1 Purity of Reagents—Reagent grade chemicals shall be
D459 Terminology Relating to Soaps and Other Detergents
used in all tests. Unless otherwise indicated, it is intended that
D1193 Specification for Reagent Water
all reagents shall conform to the specifications of the Commit-
E1 Specification for ASTM Liquid-in-Glass Thermometers
tee on Analytical Reagents of the American Chemical Society,
E70 Test Method for pH of Aqueous Solutions With the 3
where such specifications are available. Other grades may be
Glass Electrode
used, provided it is first ascertained that the reagent is of
3. Terminology sufficiently high purity to permit its use without lessening the
accuracy of the determination.
3.1 Definitions:
3.1.1 inorganic alkaline detergent—a water soluble inor-
4.2 Unless otherwise indicated, references to water shall be
ganic alkali or alkaline salt having detergent properties, but
understood to mean reagent water conforming to Specification
containing no soap or synthetics.
D1193.
3.1.2 For definitions of other terms used in these test
methods, refer to Terminology D459.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 The term “inorganic alkaline detergent” in these test
methods is defined in accordance with Terminology D459.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
For referenced ASTM standards, visit the ASTM website, www.astm.org, or DC. For suggestions on the testing of reagents not listed by the American Chemical
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
Standards volume information, refer to the standard’s Document Summary page on U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
the ASTM website. copeial Convention, Inc. (USPC), Rockville, MD.
CAUSTIC SODA
5. Sampling
5.1 Flake Caustic Soda—Flake caustic soda shall be the air as much as possible. Pipet a one-fifth aliquot into a
sampled by removing portions from various parts of the drum. 400 mL beaker and determine sodium oxide (Na O) by titrat-
ing the sample against 1.0 N acid, using methyl red as the
5.2 Powdered Caustic Soda—Powdered caustic soda shall
indicator.
be sampled by inserting a sampling tube through the contents
of the drum in several places. The tube shall be dried by
8. Calculation
heating just before use.
8.1 Calculate the total alkalinity as sodium oxide (Na O) as
5.3 Fused Caustic Soda—Fused caustic soda shall be
follows:
sampled by taking chipped samples from the center and bottom
Total alkalinity as Na O, % 5 ~A × 5 × 3.1!/W (1)
of the drum and then mixing the gross sample in the approxi- 2
mate proportions in which the tops and bottoms occur in the
where:
drum.
A = millilitres of acid required for titration of the Na O in
5.4 Precautions—Caustic soda shall not be sampled in a
the sample, and
moist atmosphere. In the case of fused caustic soda the portion W = grams of sample used.
taken for analysis shall have the surface layer of carbonate
SODIUM HYDROXIDE (NaOH)
scraped off immediately before transferring to the weighing
bottle. In all cases the sample shall be transferred to a
9. Reagents
thoroughly dried weighing bottle immediately after it is taken;
the bottle shall be tightly stoppered at once. 9.1 Acid, Standard (1.0 N)—Prepare and standardize a 1.0 N
acid solution.
TOTAL ALKALINITY AS SODIUM OXIDE (Na O)
9.2 Barium Chloride, Neutral Solution (100 g/L)—Dissolve
6. Reagents 100 g of barium chloride (BaCl ·2H O) in water and dilute to
2 2
1 L. Make the solution neutral to phenolphthalein.
6.1 Acid, Standard (1.0 N)—Prepare and standardize a 1.0 N
acid solution.
9.3 Phenolphthalein Indicator Solution (10 g/L)—Dissolve
1 g of phenolphthalein in 50 mL of ethyl alcohol and then mix
6.2 Methyl Red Indicator Solution.
with 50 mL of water.
7. Procedure
10. Procedure
7.1 Weigh 10 g of the sample, dissolve in carbon dioxide
(CO )-free water, wash into a 500 mL volumetric flask, and 10.1 Determine the NaOH on a second one-fifth aliquot
dilute to volume with CO -free water. Protect the solution from pipetted into a 250 mL Erlenmeyer flask. Add about 25 mL of
D501 − 03 (2023)
BaCl solution and titrate the sample with 1.0 N acid using Na CO , % 5 A 2 B × 5 × 5.3 /W (3)
@~ ! #
2 3
phenolphthalein as the indicator.
where:
11. Calculation
A = millilitres of acid required for titration of the Na O in
the sample,
11.1 Calculate the percentage of sodium hydroxide (NaOH)
B = millilitres of acid required for titration of the NaOH in
as follows:
the sample, and
NaOH, % 5 ~B × 5 × 4.0!/C (2)
W = grams of sample used.
where:
NOTE 1—When more accurate results are desired, the evolution method
for carbon dioxide as described in Sections 13 – 16 should be used.
B = millilitres of acid necessary for titration of the NaOH in
the sample, and
C = grams of sample used.
CARBONATE AS SODIUM CARBONATE (Na CO )
2 3
12. Calculation
12.1 Calculate the carbonate as sodium carbonate (Na CO )
2 3
as follows:
CARBON DIOXIDE (CO ) BY THE EVOLUTION METHOD
13. Apparatus
13.1 Apparatus Assembly—Place a 150 mL wide-neck ex- 15. Procedure
traction flask on a gauze over a burner. Fit the flask with a
15.1 Aspirate with a stream of carbon dioxide (CO )-free air
three-hole rubber stopper, one opening to carry a 25 cm reflux
at a rate of approximately 20 mL ⁄min to 30 mL ⁄min until the
condenser, the second to carry a thistle tube with a two-way
train is free from CO as determined by no further change in
stopcock for the introduction of acid into the flask, and the
weight greater than 0.3 mg in the U-tube.
third to carry a tube for the introduction of a continuous stream
15.2 Weigh 10 g of the sample to the nearest 0.01 g directly
of carbon dioxide (CO )-free air into the flask. Draw out the
into the extraction flask, cover with 50 mL of freshly boiled
ends of the thistle and air supply tubes to a small point, and
water, add 2 drops of methyl orange solution, and close the
place them in the stopper so that the points are very close to the
apparatus with the train in place. Start the aspiration at a rate of
bottom of the flask. Attach to the air supply tube, a U-tube
20 mL ⁄min to 30 mL ⁄min, and slowly add through the thistle
containing soda-asbestos (Ascarite) so that the air admitted to
tube sufficient H SO (2 + 9) to neutralize the NaOH and a
2 4
the flask will be free from CO .
sufficient excess to ensure the final acidity of the mixture as
indicated by the methyl orange. Always leave some acid in the
13.2 Preparation of Absorption Train—Attach to the top of
thistle tube as an air seal. Heat gently and continue until the
the reflux condenser a train consisting of the following:
contents of the flask have boiled for 5 min; remove the source
13.2.1 A U-tube containing granulated zinc for the removal
of heat, and continue aspirating until the flask has cooled, or for
of acid gases,
about 30 min.
13.2.2 A drying tube containing magnesium perchlorate,
15.3 Remove the U-tube containing soda-asbestos and
anhydrous calcium sulfate (Drierite), or anhydrous calcium
weigh using a tared U-tube as a counterpoise. The increase in
chloride,
weight represents CO .
13.2.3 A weighed U-tube containing soda-asbestos in the
16. Calculation
first half and the same drying agent in the second half as used
in 13.2.2, and
16.1 From the increase in weight of the tube calculate the
percentage of carbon dioxide (CO ) as sodium carbonate
13.2.4 A protective U-tube containing any of the above
mentioned drying agents. (Na CO ) as follows:
2 3
13.2.5 Attach the final tube to an aspirator.
Na CO , % 5 @~C × 2.409!/W# × 100 (4)
2 3
where:
14. Reagents
C = grams of CO , and
14.1 Methyl Orange Indicator Solution (1 g/L)—Dissolve
W = grams of sample used.
0.1 g of methyl orange in water and dilute to 100 mL. NOTE 2—This test method for the determination of Na CO as CO is
2 3 2
to be preferred when a procedure more accurate than that described in
14.2 Sulfuric Acid (2 + 9) —Mix 2 volumes of concentrated
Section 12 is required.
sulfuric acid (H SO , sp gr 1.84) carefully with stirring into 9
2 4
volumes of water.
D501 − 03 (2023)
SODA ASH
17. Sampling
17.1 Soda ash shall be sampled by removing portions from
W = grams of sample used.
various parts of the container. Samples shall not be taken from
SODIUM BICARBONATE (NaHCO )
those portions of the soda ash where caking is noticeable due
to the absorption of moisture and carbon dioxide through the
23. Reagents
container. If the soda ash is caked, the sample shall be obtained
23.1 Silver Nitrate Solution (100 g/L)—Dissolve 100 g of
by thoroughly mixing and quartering the entire contents of the
silver nitrate (AgNO ) in water and dilute to 1 L. Prepare this
package.
solution fresh before use.
MATTER VOLATILE AT 150 °C TO 155 °C
23.2 Sodium Hydroxide, Standard Solution (1.0 N)—
Prepare and standardize a 1.0 N sodium hydroxide (NaOH)
18. Procedure
solution.
18.1 Place approximately 2 g of the sample in a tared
24. Procedure
weighing bottle and weigh to the nearest 0.1 mg. Remove the
stopper and dry in an oven at 150 °C to 155 °C for 1 h. Replace
24.1 Weigh 8.4 g of the sample to the nearest 0.05 g and
the stopper and allow to cool to room temperature in a
transfer to a 250 mL beaker. Dissolve in 100 mL of water, and
desiccator containing no desiccant and reweigh.
titrate with 1.0 N NaOH solution until a drop of the test
solution added to a drop of AgNO solution on a spot plate
19. Calculation
gives a dark color instantly.
19.1 Calculate the percentage of volatile matter as follows:
25. Calculation
Volatile matter, % 5 L/W × 100 (5)
~ !
25.1 Calculate the percentage of sodium bicarbonate
where:
(NaHCO ) as follows:
L = grams loss in weight, and
NaHCO , % 5 mL of 1.0 N NaOH solution (7)
W = grams of sample used.
Calculate the pe
...
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