ASTM D501-03(2016)

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 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 the us...

General Information

• Status: Historical
• Publication Date: 30-Jun-2016
• ICS: 71.100.40 - Surface active agents
• Technical Committee: D12 - Soaps and Other Detergents
• Drafting Committee: D12.12 - Analysis and Specifications of Soaps, Synthetics, Detergents and their Components

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: D501 − 03 (Reapproved 2016)
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
Matter Insoluble in Water 72 and 73
1.1 These test methods cover procedures for the sampling
Tetrasodium Pyrophosphate:
and chemical analysis of inorganic alkaline detergents. Sampling 74
Tetrasodium Pyrophosphate
1.2 The procedures appear in the following order:
(Na P O ) 75 – 79
4 2 7
Matter Insoluble in Water 80 and 81
Sections
Loss on Ignition 82 and 83
Caustic Soda:
Borax:
Sampling 5
Sampling 84
Total Alkalinity as Sodium Oxide (Na O) 6 – 8
Total Borate and Excess Alkalinity or Acidity 85 – 87
Sodium Hydroxide (NaOH) 9 – 11
Matter Insoluble in Water 88 and 89
Carbonate as Sodium Carbonate (Na CO ) 12
2 3
Sodium Triphosphate:
Carbon Dioxide (CO ) by the Evolution Method 13 – 16
Sampling 90
Soda Ash:
Tritratable Na O 91 – 94
Sampling 17
Total P O :
2 5
Matter Volatile at 150 to 155°C 18 and 19
Preferred Method 95 – 97
Total Alkalinity as Sodium Carbonate (Na CO ) 20 – 22
2 3
Alternative Method 98 – 101
Sodium Bicarbonate (NaHCO ) 23 – 25
pH Titration 102 – 107
Sodium Bicarbonate (NaHCO ) by Potentiometric Titration 26 – 28
Quantitative Separation and Measurement of Various Phosphates:
Matter Insoluble in Water 29 and 30
Reverse-Flow Ion-Exchange Chromatography (Preferred
Apparent Density 31 and 32
Method) 108 – 119
Modified Soda (Sequicarbonate Type):
Paper Chromatographic Method 120 – 127
Sampling 33
pH of 1 percent Solution 128
Total Alkalinity as Sodium Oxide (Na O) 34 – 36
Turbidity 129
Sodium Bicarbonate (NaHCO ) and Sodium Carbonate (Na CO ) 37 – 39
3 2 3
Temperature Rise 130 – 134
Matter Insoluble in Water 40
Sulfate 135 – 137
Sodium Bicarbonate:
Ignition Loss 140 and
Sampling 41
Sodium Bicarbonate, Sodium Carbonate, and Free Moisture 42 – 45
Matter Insoluble in Water 142 – 144
Matter Insoluble in Water 46
Particle Size 145
Sodium Metasilicate, Sodium Sesquisilicate and Sodium Orthosil-
Orthophosphate 146 – 151
icate:
Sampling 47
1.3 The values stated in SI units are to be regarded as
Total Alkalinity as Sodium Oxide (Na O) 48 – 50
standard. No other units of measurement are included in this
Total Silica as SiO 51 – 53
standard.
Sodium Metasilicate (Na SiO ·5H O) 54
2 3 2
Sodium Sesquisilicate (3Na O·2SiO ·11H O) 55
2 2 2
1.4 This standard does not purport to address all of the
Matter Insoluble in Water 56 and 57
safety concerns, if any, associated with its use. It is the
Loss on Ignition of Sodium Sesquisilicate (3Na O·2SiO ·11H O) 58 and 59
2 2 2
Sodium Orthosilicate (Na SiO ) 60
4 4
responsibility of the user of this standard to establish appro-
Trisodium Phosphate:
priate safety and health practices and determine the applica-
Sampling 61
Trisodium Phosphate (Na PO ) Content and Phosphorus bility of regulatory limitations prior to use. Material Safety
3 4
Pentoxide (P O ) 62 – 64
2 5
Data Sheets are available for reagents and materials. Review
Trisodium Phosphate Calculated as Na PO ·12H O, Na PO ·
3 4 2 3 4
them for hazards prior to usage.
H O, Na PO , and as P O 65 – 68
2 3 4 2 5
Total Alkalinity as Sodium Oxide (Na O) 69 – 71
2. Referenced Documents
2.1 ASTM Standards:
These test methods are under the jurisdiction of ASTM Committee D12 on
D459 Terminology Relating to Soaps and Other Detergents
Soaps and Other Detergents and are the direct responsibility of Subcommittee
D12.12 on Analysis and Specifications of Soaps, Synthetics, Detergents and their
Components. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved July 1, 2016. Published August 2016. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1938. Last previous edition approved in 2009 as D501 – 03 (2009). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D0501-03R16. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D501 − 03 (2016)
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
where such specifications are available. Other grades may be
Glass Electrode
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
3. Terminology
accuracy of the determination.
3.1 Definitions:
4.2 Unless otherwise indicated, references to water shall be
3.1.1 inorganic alkaline detergent—a water soluble inor-
understood to mean reagent water conforming to Specification
ganic alkali or alkaline salt having detergent properties, but
D1193.
containing no soap or synthetics.
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.
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
4. Purity of Reagents listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
4.1 Purity of Reagents—Reagent grade chemicals shall be
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
used in all tests. Unless otherwise indicated, it is intended that MD.
CAUSTIC SODA
5. Sampling
5.1 Flake Caustic Soda—Flake caustic soda shall be 8. Calculation
sampled by removing portions from various parts of the drum.
8.1 Calculate the total alkalinity as sodium oxide (Na O) as
5.2 Powdered Caustic Soda—Powdered caustic soda shall
follows:
be sampled by inserting a sampling tube through the contents
Total alkalinity as Na O, % 5 ~A 35 3 3.1!/W (1)
of the drum in several places. The tube shall be dried by
where:
heating just before use.
A = millilitres of acid required for titration of the Na O in
5.3 Fused Caustic Soda—Fused caustic soda shall be 2
the sample, and
sampled by taking chipped samples from the center and bottom
W = grams of sample used.
of the drum and then mixing the gross sample in the approxi-
mate proportions in which the tops and bottoms occur in the
SODIUM HYDROXIDE (NaOH)
drum.
5.4 Precautions—Caustic soda shall not be sampled in a
9. Reagents
moist atmosphere. In the case of fused caustic soda the portion
9.1 Acid, Standard (1.0 N)—Prepare and standardize a 1.0 N
taken for analysis shall have the surface layer of carbonate
acid solution.
scraped off immediately before transferring to the weighing
bottle. In all cases the sample shall be transferred to a 9.2 Barium Chloride, Neutral Solution (100 g/L)—Dissolve
thoroughly dried weighing bottle immediately after it is taken; 100 g of barium chloride (BaCl ·2H O) in water and dilute to
2 2
the bottle shall be tightly stoppered at once. 1 L. Make the solution neutral to phenolphthalein.
9.3 Phenolphthalein Indicator Solution (10 g/L)—Dissolve
TOTAL ALKALINITY AS SODIUM OXIDE (Na O)
1 g of phenolphthalein in 50 mL of ethyl alcohol and then mix
6. Reagents
with 50 mL of water.
6.1 Acid, Standard (1.0 N)—Prepare and standardize a 1.0 N
10. Procedure
acid solution.
6.2 Methyl Red Indicator Solution. 10.1 Determine the NaOH on a second one-fifth aliquot
pipetted into a 250-mL Erlenmeyer flask. Add about 25 mL of
7. Procedure
BaCl solution and titrate the sample with 1.0 N acid using
7.1 Weigh 10 g of the sample, dissolve in carbon dioxide
phenolphthalein as the indicator.
(CO )-free water, wash into a 500-mL volumetric flask, and
dilute to volume with CO -free water. Protect the solution from
11. Calculation
the air as much as possible. Pipet a one-fifth aliquot into a
11.1 Calculate the percentage of sodium hydroxide (NaOH)
400-mL beaker and determine sodium oxide (Na O) by titrat-
as follows:
ing the sample against 1.0 N acid, using methyl red as the
indicator. NaOH, % 5 ~B 35 3 4.0!/C (2)
D501 − 03 (2016)
where: where:
B = millilitres of acid necessary for titration of the NaOH in A = millilitres of acid required for titration of the Na O in
the sample, and the sample,
C = grams of sample used. B = millilitres of acid required for titration of the NaOH in
the sample, and
CARBONATE AS SODIUM CARBONATE (Na CO )
2 3
W = grams of sample used.
NOTE 1—When more accurate results are desired, the evolution method
12. Calculation
for carbon dioxide as described in Sections 13 – 16 should be used.
12.1 Calculate the carbonate as sodium carbonate (Na CO )
2 3
as follows:
Na CO , % 5 @~A 2 B! 35 3 5.3#/W (3)
2 3
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 to 30 mL/min until the train is
condenser, the second to carry a thistle tube with a two-way
free from CO as determined by no further change in weight
stopcock for the introduction of acid into the flask, and the
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 to 30 mL/min, and slowly add through the thistle tube
containing soda-asbestos (Ascarite) so that the air admitted to
sufficient H SO (2 + 9) to neutralize the NaOH and a sufficient
2 4
the flask will be free from CO .
excess to ensure the final acidity of the mixture as indicated by
the methyl orange. Always leave some acid in the thistle tube
13.2 Preparation of Absorption Train—Attach to the top of
as an air seal. Heat gently and continue until the contents of the
the reflux condenser a train consisting of the following:
flask have boiled for 5 min; remove the source of heat, and
13.2.1 A U-tube containing granulated zinc for the removal
continue aspirating until the flask has cooled, or for about 30
of acid gases,
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
13.2.4 A protective U-tube containing any of the above percentage of carbon dioxide (CO ) as sodium carbonate
mentioned drying agents. (Na CO ) as follows:
2 3
13.2.5 Attach the final tube to an aspirator.
Na CO , % 5 @~C 3 2.409!/W# 3 100 (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 (2016)
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. 3
solution fresh before use.
MATTER VOLATILE AT 150 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 to 155°C for 1 h. Replace the
24.1 Weigh 8.4 g of the sample to the nearest 0.05 g and
stopper and allow to cool to room temperature in a desiccator
transfer to a 250-mL beaker. Dissolve in 100 mL of water, and
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! 3 100 (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 percentage of sodium carbonate (Na CO ) as
2 3
TOTAL ALKALINITY AS SODIUM CARBONATE
follows:
(Na CO )
2 3
Na CO , % 5 A 2 ~NaHCO , % 3 0.6309! (8)
2 3 3
20. Reagents
where:
A = total alkalinity as Na CO , in percent.
20.1 Methyl Orange Indicator Solution (1 g/L)—Dissolve
2 3
NOTE 3—For referee purposes, or when more accurate results are
0.1 g of methyl orange in water and dilute to 100 mL.
required than are yielded by the procedure described in Section 25, the
20.2 Hydrochloric Acid, Standard (0.5 N)—Prepare and
method described in Section 28 sh
...

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: D501 − 03 (Reapproved 2009) D501 − 03 (Reapproved 2016)
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
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 (Na O) 6 – 8
Sodium Hydroxide (NaOH) 9 – 11
Carbonate as Sodium Carbonate (Na CO ) 12
2 3
Carbon Dioxide (CO ) by the Evolution Method 13 – 16
Soda Ash:
Sampling 17
Matter Volatile at 150 to 155°C 18 and 19
Total Alkalinity as Sodium Carbonate (Na CO ) 20 – 22
2 3
Sodium Bicarbonate (NaHCO ) 23 – 25
Sodium Bicarbonate (NaHCO ) 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 (Na O) 34 – 36
Sodium Bicarbonate (NaHCO ) and Sodium Carbonate (Na CO ) 37 – 39
3 2 3
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 (Na O) 48 – 50
Total Silica as SiO 51 – 53
Sodium Metasilicate (Na SiO ·5H O) 54
2 3 2
Sodium Sesquisilicate (3Na O·2SiO ·11H O) 55
2 2 2
Matter Insoluble in Water 56 and 57
Loss on Ignition of Sodium Sesquisilicate (3Na O·2SiO ·11H O) 58 and 59
2 2 2
Sodium Orthosilicate (Na SiO ) 60
4 4
Trisodium Phosphate:
Sampling 61
Trisodium Phosphate (Na PO ) Content and Phosphorus
3 4
Pentoxide (P O ) 62 – 64
2 5
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
2 3 4 2 5
Total Alkalinity as Sodium Oxide (Na O) 69 – 71
Matter Insoluble in Water 72 and 73
Tetrasodium Pyrophosphate:
Sampling 74
Tetrasodium Pyrophosphate
(Na P O ) 75 – 79
4 2 7
These test methods are under the jurisdiction of ASTM Committee D12 on Soaps and Other Detergents and are 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 1938. Discontinued August 2001 and reinstated as
D501 – 03.Last previous edition approved in 20032009 as D501 – 03.D501 – 03 (2009). DOI: 10.1520/D0501-03R09.10.1520/D0501-03R16.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D501 − 03 (2016)
Sections
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 Na O 91 – 94
Total P O :
2 5
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
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 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:
D459 Terminology Relating to Soaps and Other Detergents
D1193 Specification for Reagent Water
E1 Specification for ASTM Liquid-in-Glass Thermometers
E70 Test Method for pH of Aqueous Solutions With the Glass Electrode
3. Terminology
3.1 Definitions:
3.1.1 inorganic alkaline detergent—a water soluble inorganic alkali or alkaline salt having detergent properties, but containing
no soap or synthetics.
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.
4. Purity of Reagents
4.1 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
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.
4.2 Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to Specification
D1193.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
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.
D501 − 03 (2016)
CAUSTIC SODA
5. Sampling
5.1 Flake Caustic Soda—Flake caustic soda shall be sampled by removing portions from various parts of the drum.
5.2 Powdered Caustic Soda—Powdered caustic soda shall be sampled by inserting a sampling tube through the contents of the
drum in several places. The tube shall be dried by heating just before use.
5.3 Fused Caustic Soda—Fused caustic soda shall be sampled by taking chipped samples from the center and bottom of the
drum and then mixing the gross sample in the approximate proportions in which the tops and bottoms occur in the drum.
5.4 Precautions—Caustic soda shall not be sampled in a moist atmosphere. In the case of fused caustic soda the portion taken
for analysis shall have the surface layer of carbonate scraped off immediately before transferring to the weighing bottle. In all cases
the sample shall be transferred to a thoroughly dried weighing bottle immediately after it is taken; the bottle shall be tightly
stoppered at once.
TOTAL ALKALINITY AS SODIUM OXIDE (Na O)
6. Reagents
6.1 Acid, Standard (1.0 N)—Prepare and standardize a 1.0 N acid solution.
6.2 Methyl Red Indicator Solution.
7. Procedure
7.1 Weigh 10 g of the sample, dissolve in carbon dioxide (CO )-free water, wash into a 500-mL volumetric flask, and dilute
to volume with CO -free water. Protect the solution from the air as much as possible. Pipet a one-fifth aliquot into a 400-mL beaker
and determine sodium oxide (Na O) by titrating the sample against 1.0 N acid, using methyl red as the indicator.
8. Calculation
8.1 Calculate the total alkalinity as sodium oxide (Na O) as follows:
Total alkalinity as Na O,%5 A 3533.1 /W (1)
~ !
where:
A = millilitres of acid required for titration of the Na O in the sample, and
W = grams of sample used.
SODIUM HYDROXIDE (NaOH)
9. Reagents
9.1 Acid, Standard (1.0 N)—Prepare and standardize a 1.0 N acid solution.
9.2 Barium Chloride, Neutral Solution (100 g/L)—Dissolve 100 g of barium chloride (BaCl ·2H O) in water and dilute to 1 L.
2 2
Make the solution neutral to phenolphthalein.
9.3 Phenolphthalein Indicator Solution (10 g/L)—Dissolve 1 g of phenolphthalein in 50 mL of ethyl alcohol and then mix with
50 mL of water.
10. Procedure
10.1 Determine the NaOH on a second one-fifth aliquot pipetted into a 250-mL Erlenmeyer flask. Add about 25 mL of BaCl
solution and titrate the sample with 1.0 N acid using phenolphthalein as the indicator.
11. Calculation
11.1 Calculate the percentage of sodium hydroxide (NaOH) as follows:
NaOH,%5 ~B 3534.0!/C (2)
where:
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 ) as follows:
2 3
Na CO ,%5 A 2 B 3535.3 /W (3)
@~ ! #
2 3
D501 − 03 (2016)
where:
A = millilitres of acid required for titration of the Na O in the sample,
B = millilitres of acid required for titration of the NaOH in the sample, and
W = grams of sample used.
NOTE 1—When more accurate results are desired, the evolution method for carbon dioxide as described in Sections 13 – 16 should be used.
CARBON DIOXIDE (CO ) BY THE EVOLUTION METHOD
13. Apparatus
13.1 Apparatus Assembly—Place a 150-mL wide-neck extraction flask on a gauze over a burner. Fit the flask with a three-hole
rubber stopper, one opening to carry a 25-cm reflux condenser, the second to carry a thistle tube with a twowaytwo-way stopcock
for the introduction of acid into the flask, and the third to carry a tube for the introduction of a continuous stream of carbon dioxide
(CO )-free air into the flask. Draw out the ends of the thistle and air supply tubes to a small point, and place them in the stopper
so that the points are very close to the bottom of the flask. Attach to the air supply tube, a U-tube containing soda-asbestos
(Ascarite) so that the air admitted to the flask will be free from CO .
13.2 Preparation of Absorption Train—Attach to the top of the reflux condenser a train consisting of the following:
13.2.1 A U-tube containing granulated zinc for the removal of acid gases,
13.2.2 A drying tube containing magnesium perchlorate, anhydrous calcium sulfate (Drierite), or anhydrous calcium chloride,
13.2.3 A weighed U-tube containing soda-asbestos in the first half and the same drying agent in the second half as used in
13.2.2, and
13.2.4 A protective U-tube containing any of the above mentioned drying agents.
13.2.5 Attach the final tube to an aspirator.
14. Reagents
14.1 Methyl Orange Indicator Solution (1 g/L)—Dissolve 0.1 g of methyl orange in water and dilute to 100 mL.
14.2 Sulfuric Acid (2 + 9) —Mix 2 volumes of concentrated sulfuric acid (H SO , sp gr 1.84) carefully with stirring into 9
2 4
volumes of water.
15. Procedure
15.1 Aspirate with a stream of carbon dioxide (CO )-free air at a rate of approximately 20 to 30 mL/min until the train is free
from CO as determined by no further change in weight greater than 0.3 mg in the U-tube.
15.2 Weigh 10 g of the sample to the nearest 0.01 g directly into the extraction flask, cover with 50 mL of freshly boiled water,
add 2 drops of methyl orange solution, and close the apparatus with the train in place. Start the aspiration at a rate of 20 to 30
mL/min, and slowly add through the thistle tube sufficient H SO (2 + 9) to neutralize the NaOH and a sufficient excess to ensure
2 4
the final acidity of the mixture as indicated by the methyl orange. Always leave some acid in the thistle tube as an air seal. Heat
gently and continue until the contents of the flask have boiled for 5 min; remove the source of heat, and continue aspirating until
the flask has cooled, or for about 30 min.
15.3 Remove the U-tube containing soda-asbestos and weigh using a tared U-tube as a counterpoise. The increase in weight
represents CO .
16. Calculation
16.1 From the increase in weight of the tube calculate the percentage of carbon dioxide (CO ) as sodium carbonate (Na CO )
2 2 3
as follows:
Na CO , %5 @~C 32.409!/W# 3100 (4)
2 3
where:
C = grams of CO , and
W = grams of sample used.
NOTE 2—This test method for the determination of Na CO as CO is to be preferred when a procedure more accurate than that described in Section
2 3 2
12 is required.
SODA ASH
D501 − 03 (2016)
17. Sampling
17.1 Soda ash shall be sampled by removing portions from various parts of the container. Samples shall not be taken from those
portions of the soda ash where caking is noticeable due to the absorption of moisture and carbon dioxide through the container.
If the soda ash is caked, the sample shall be obtained by thoroughly mixing and quartering the entire contents of the package.
MATTER VOLATILE AT 150 TO 155°C
18. Procedure
18.1 Place approximately 2 g of the sample in a tared weighing bottle and weigh to the nearest 0.1 mg. Remove the stopper
and dry in an oven at 150 to 155°C for 1 h. Replace the stopper and allow to cool to room temperature in a desiccator containing
no desiccant and reweigh.
19. Calculation
19.1 Calculate the percentage of volatile matter as follows:
Volatile matter,%5 ~L/W! 3100 (5)
where:
L = grams loss in weight, and
W = grams of sample used.
TOTAL ALKALINITY AS SODIUM CARBONATE (Na CO )
2 3
20. Reagents
20.1 Methyl Orange Indicator Solution (1 g/L)—Dissolve 0.1 g of methyl orange in water and dilute to 100 mL.
20.2 Hydrochloric Acid, Standard (0.5 N)—Prepare and standardize 0.5 N hydrochloric acid (HCl).
21. Procedure
21.1 Transfer approximately 1.2 g of sample into a tared weighing bottle. Weigh to the nearest 0.1 mg, protecting the sample
at all times, as much as possible, from moisture in the air during weighing. Dissolve the sample in about 50 mL of water in a
400-mL beaker and add 2 drops of methyl orange indicator solution. Run in, while stirring, 0.5 N HCl until 1 drop establishes the
first appearance of a pink color in the solution. Remove the beaker, heat to boiling, and boil for 1min to remove most of the CO .
Cool and finish the titration to the first appearance of a pink color in the soluti
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