ASTM D501-03(2009)
(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:
General Information
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 2009)
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.Anumber 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
bility of regulatory limitations prior to use. Material Safety
Trisodium Phosphate (Na PO ) Content and Phosphorus
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
D459Terminology 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 Oct. 1, 2009. Published December 2009. Originally contactASTM Customer Service at service@astm.org. ForAnnual Book ofASTM
approved in 1938. Discontinued August 2001 and reinstated as D501–03. Last Standards volume information, refer to the standard’s Document Summary page on
previous edition approved in 2003 as D501–03. DOI: 10.1520/D0501-03R09. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D501 − 03 (2009)
D1193Specification for Reagent Water all reagents shall conform to the specifications of the Commit-
E1Specification for ASTM Liquid-in-Glass Thermometers tee onAnalytical Reagents of theAmerican Chemical Society,
E70Test 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
TotalalkalinityasNa O,% 5 A 35 33.1 /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 NaOin
5.3 Fused Caustic Soda—Fused caustic soda shall be 2
the sample, and
sampledbytakingchippedsamplesfromthecenterandbottom
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(1.0N)—Prepareandstandardizea1.0N
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 mLof ethyl alcohol and then mix
6. Reagents
with 50 mL of water.
6.1 Acid,Standard(1.0N)—Prepareandstandardizea1.0N
acid solution. 10. Procedure
6.2 Methyl Red Indicator Solution.
10.1 Determine the NaOH on a second one-fifth aliquot
pipetted into a 250-mLErlenmeyer flask.Add about 25 mLof
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
dilutetovolumewithCO -freewater.Protectthesolutionfrom
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 34.0 /C (2)
~ !
D501 − 03 (2009)
where: where:
B = millilitres of acid necessary for titration of the NaOH in A = millilitres of acid required for titration of the NaOin
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.
NOTE1—Whenmoreaccurateresultsaredesired,theevolutionmethod
12. Calculation
for carbon dioxide as described in Sections13–16 should be used.
12.1 Calculatethecarbonateassodiumcarbonate(Na CO )
2 3
as follows:
Na CO ,% 5 A 2 B 35 35.3 /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 Aspiratewithastreamofcarbondioxide(CO )-freeair
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 twoway
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.
thirdtocarryatubefortheintroductionofacontinuousstream
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
placetheminthestoppersothatthepointsareveryclosetothe
apparatuswiththetraininplace.Starttheaspirationatarateof
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
sufficientH SO (2+9)toneutralizetheNaOHandasufficient
2 4
the flask will be free from CO .
excesstoensurethefinalacidityofthemixtureasindicatedby
the methyl orange. Always leave some acid in the thistle tube
13.2 Preparation of Absorption Train—Attach to the top of
asanairseal.Heatgentlyandcontinueuntilthecontentsofthe
the reflux condenser a train consisting of the following:
flask have boiled for 5 min; remove the source of heat, and
13.2.1 AU-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
first half and the same drying agent in the second half as used 16. Calculation
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 32.409 /W 3100 (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 (2009)
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.Ifthesodaashiscaked,thesampleshallbeobtained
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 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 approximately2gofthe sample in a tared
24. Procedure
weighing bottle and weigh to the nearest 0.1 mg. Remove the
stopperanddryinanovenat150to155°Cfor1h.Replacethe
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-mLbeaker. Dissolve in 100 mLof 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
Volatilematter,% 5 L/W 3100 (5)
~ !
25.1 Calculate the percentage of sodium bicarbonate
where:
(NaHCO ) as follows:
L = grams loss in weight, and
NaHCO ,% 5mLof1.0 N NaOHsolution (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 ,% 30.6309 (8)
~ !
2 3 3
20. Reagents
where:
20.1 Methyl Orange Indicator Solution (1 g/L)—Dissolve A = total alkalinity as Na CO , in percent.
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 shall be used.
standardize 0.5 N hydrochloric acid (HCl).
SODIUM BICARBONATE (NaHCO )BY
POTENTIOMETRIC TITRATION
21. Procedure
21.1 Transfer approximately 1.2 g of sample into a tared
26. Reagents
weighing bottle. Weigh to
...
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