ASTM D501-89(1998)

Standard Test Methods of Sampling and Chemical Analysis of Alkaline Detergents (Withdrawn 2001)

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 to 8 Sodium Hydroxide (NaOH) 9 to 11 Carbonate as Sodium Carbonate (Na CO ) 12 Carbon Dioxide (CO ) by the Evolution Method 13 to 16 Soda Ash: Sampling 17 Matter Volatile at 150 to 155C 18 and 19 Total Alkalinity as Sodium Carbonate (Na CO ) 20 to 22 Sodium Bicarbonate (NaHCO ) 23 to 25 Sodium Bicarbonate (NaHCO ) by Potentiometric Titration 26 to 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 to 36 Sodium Bicarbonate (NaHCO ) and Sodium Carbonate (Na CO ) 37 to 39 Matter Insoluble in Water 40 Sodium Bicarbonate: Sampling 41 Sodium Bicarbonate, Sodium Carbonate, and Free Moisture 42 to 45 Matter Insoluble in Water 46 Sodium Metasilicate, Sodium Sesquisilicate and Sodium Orthosilicate: Sampling 47 Total Alkalinity as Sodium Oxide (Na O) 48 to 50 Total Silica as SiO  51 to 53 Sodium Metasilicate (Na SiO  5H O) 54 Sodium Sesquisilicate (3Na O 2SiO  11H O) 55 Matter Insoluble in Water 56 and 57 Loss on Ignition of Sodium Sesquisilicate (3Na O 2SiO  11H O) 58 and 59 Sodium Orthosilicate (Na SiO ) 60 Trisodium Phosphate: Sampling 61 Trisodium Phosphate (Na PO ) Content and Phosphorus Pen- toxide (P O ) 62 to 64 Trisodium Phosphate Calculated as Na PO  12H O, Na PO  H O, Na PO , and as P O  65 to 68 Total Alkalinity as Sodium Oxide (Na O) 69 to 71 Matter Insoluble in Water 72 and 73 Tetrasodium Pyrophosphate: Sampling 74 Tetrasodium Pyrophosphate (Na P O ) 75 to 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 to 87 Matter Insoluble in Water 88 and 89 Sodium Triphosphate: Sampling 90 Tritratable Na O 91 to 94 Total P O : Preferred Method 95 to 97 Alternative Method 98 to 101 pH Titration 102 to 107 Quantitative Separation and Measurement of Various Phosphates: Reverse-Flow Ion-Exchange Chromatography (Preferred Method) 108 to 119 Paper Chromatographic Method 120 to 127 pH of 1 percent Solution 128 Turbidity 129 Temperature Rise 130 to 134 Sulfate 135 to 137 Ignition Loss 140 to 141 Matter Insoluble in Water 142 to 144 Particle Size 145 Orthophosphate 146 to 151
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

• Status: Historical
• Publication Date: 09-Jan-1998
• Withdrawal Date: 09-Aug-2001
• 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

Relations

• Replaced By: ASTM D501-03 - Standard Test Methods of Sampling and Chemical Analysis of Alkaline Detergents
• Effective Date: 01-Oct-2003

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: D 501 – 89 (Reapproved 1998)
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 (ε) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope
Sections
Tetrasodium Pyrophosphate
1.1 These test methods cover procedures for the sampling
(Na P O ) 75-79
4 2 7
and chemical analysis of inorganic alkaline detergents.
Matter Insoluble in Water 80 and 81
Loss on Ignition 82 and 83
1.2 The procedures appear in the following order:
Borax:
Sections
Sampling 84
Caustic Soda:
Total Borate and Excess Alkalinity or Acidity 85-87
Sampling 5
Matter Insoluble in Water 88 and 89
Total Alkalinity as Sodium Oxide (Na O) 6-8
Sodium Triphosphate:
Sodium Hydroxide (NaOH) 9-11
Sampling 90
Carbonate as Sodium Carbonate (Na CO)12
2 3
Tritratable Na O 91-94
Carbon Dioxide (CO ) by the Evolution Method 13-16
Total P O :
2 5
Soda Ash:
Preferred Method 95-97
Sampling 17
Alternative Method 98-101
Matter Volatile at 150 to 155°C 18 and 19
pH Titration 102-107
Total Alkalinity as Sodium Carbonate (Na CO ) 20-22
2 3
Quantitative Separation and Measurement of Various Phosphates:
Sodium Bicarbonate (NaHCO ) 23-25
3 Reverse-Flow Ion-Exchange Chromatography (Preferred
Sodium Bicarbonate (NaHCO ) by Potentiometric Titration 26-28
Method) 108-119
Matter Insoluble in Water 29 and 30
Paper Chromatographic Method 120-127
Apparent Density 31 and 32
pH of 1 percent Solution 128
Modified Soda (Sequicarbonate Type):
Turbidity 129
Sampling 33
Temperature Rise 130-134
Total Alkalinity as Sodium Oxide (Na O) 34-36
Sulfate 135-137
Sodium Bicarbonate (NaHCO ) and Sodium Carbonate (Na CO ) 37-39
3 2 3 Ignition Loss 140 and
Matter Insoluble in Water 40
Sodium Bicarbonate:
Matter Insoluble in Water 142-144
Sampling 41
Particle Size 145
Sodium Bicarbonate, Sodium Carbonate, and Free Moisture 42-45
Orthophosphate 146-151
Matter Insoluble in Water 46
Sodium Metasilicate, Sodium Sesquisilicate and Sodium Orthosil-
1.3 This standard does not purport to address all of the
icate:
safety concerns, if any, associated with its use. It is the
Sampling 47
responsibility of the user of this standard to establish appro-
Total Alkalinity as Sodium Oxide (Na O) 48-50
Total Silica as SiO 51-53
2 priate safety and health practices and determine the applica-
Sodium Metasilicate (Na SiO ·5H O) 54
2 3 2
bility of regulatory limitations prior to use. Material Safety
Sodium Sesquisilicate (3Na O·2SiO ·11H O) 55
2 2 2
Data Sheets are available for reagents and materials. Review
Matter Insoluble in Water 56 and 57
Loss on Ignition of Sodium Sesquisilicate (3Na O·2SiO ·11H O) 58 and 59
2 2 2 them for hazards prior to usage.
Sodium Orthosilicate (Na SiO)60
4 4
Trisodium Phosphate:
2. Referenced Documents
Sampling 61
2.1 ASTM Standards:
Trisodium Phosphate (Na PO ) Content and Phosphorus
3 4
Pentoxide (P O ) 62-64
2 5 D459 Terminology Relating to Soaps and Other Deter-
Trisodium Phosphate Calculated as Na PO ·12H O, Na PO ·
3 4 2 3 4
gents
H O, Na PO , and as P O 65-68
2 3 4 2 5
D1193 Specification for Reagent Water
Total Alkalinity as Sodium Oxide (Na O) 69-71
Matter Insoluble in Water 72 and 73
E1 Specification for ASTM Thermometers
Tetrasodium Pyrophosphate:
E70 Test Method for pH of Aqueous Solutions with the
Sampling 74
Glass Electrode
These test methods are under the jurisdiction of ASTM Committee D-12 on
Soaps and Other Detergents and are the direct responsibility of Subcommittee Annual Book of ASTM Standards, Vol 15.04.
D12.14 on Analysis of Inorganic Alkaline Detergents. Annual Book of ASTM Standards, Vol 11.01.
Current edition approved May 26, 1989. Published July 1989. Originally pub- Annual Book of ASTM Standards, Vol 14.03.
1 5
lished as D501–38. Last previous edition D501–85ε . Annual Book of ASTM Standards, Vol 15.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 501 – 89 (1998)
3. Terminology tee onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
3.1 Definitions:
used, provided it is first ascertained that the reagent is of
3.1.1 inorganic alkaline detergent—a water soluble inor-
sufficiently high purity to permit its use without lessening the
ganic alkali or alkaline salt having detergent properties, but
accuracy of the determination.
containing no soap or synthetics.
4.2 Unless otherwise indicated, references to water shall be
3.1.2 For definitions of other terms used in these test
understood to mean reagent water conforming to Specification
methods, refer to Terminology D459.
D1193.
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
4. Purity of Reagents
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
4.1 Purity of Reagents—Reagent grade chemicals shall be
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
used in all tests. Unless otherwise indicated, it is intended that
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
all reagents shall conform to the specifications of the Commit- MD.
CAUSTIC SODA
TotalalkalinityasNa O,% 5 ~A 35 33.1!/W (1)
5. Sampling
5.1 Flake Caustic Soda—Flake caustic soda shall be
where:
sampled by removing portions from various parts of the drum.
A = millilitres of acid required for titration of the NaOin
5.2 Powdered Caustic Soda—Powdered caustic soda shall
the sample, and
be sampled by inserting a sampling tube through the contents
W = grams of sample used.
of the drum in several places. The tube shall be dried by
heating just before use. SODIUM HYDROXIDE (NaOH)
5.3 Fused Caustic Soda—Fused caustic soda shall be
9. Reagents
sampledbytakingchippedsamplesfromthecenterandbottom
of the drum and then mixing the gross sample in the approxi-
9.1 Acid, Standard (1.0 N)—Prepare and standardize a 1.0
mate proportions in which the tops and bottoms occur in the
N acid solution.
drum.
9.2 Barium Chloride, Neutral Solution(100g/L)—Dissolve
5.4 Precautions—Caustic soda shall not be sampled in a
100 g of barium chloride (BaCl ·2H O) in water and dilute to
2 2
moist atmosphere. In the case of fused caustic soda the portion
1 L. Make the solution neutral to phenolphthalein.
taken for analysis shall have the surface layer of carbonate
9.3 Phenolphthalein Indicator Solution (10 g/L)—Dissolve
scraped off immediately before transferring to the weighing
1 g of phenolphthalein in 50 mLof ethyl alcohol and then mix
bottle. In all cases the sample shall be transferred to a
with 50 mL of water.
thoroughly dried weighing bottle immediately after it is taken;
10. Procedure
the bottle shall be tightly stoppered at once.
10.1 Determine the NaOH on a second one-fifth aliquot
TOTALALKALINITYAS SODIUM OXIDE (Na O)
pipetted into a 250-mLErlenmeyer flask.Add about 25 mLof
BaCl solution and titrate the sample with 1.0 N acid using
6. Reagents
phenolphthalein as the indicator.
6.1 Acid, Standard (1.0 N)—Prepare and standardize a 1.0
N acid solution.
11. Calculation
6.2 Methyl Red Indicator Solution.
11.1 Calculate the percentage of sodium hydroxide (NaOH)
as follows:
7. Procedure
NaOH,% 5 B 35 34.0 /C (2)
~ !
7.1 Weigh 10 g of the sample, dissolve in carbon dioxide
(CO )-free water, wash into a 500-mL volumetric flask, and
2 where:
dilutetovolumewithCO -freewater.Protectthesolutionfrom
2 B = millilitresofacidnecessaryfortitrationoftheNaOHin
the air as much as possible. Pipet a one-fifth aliquot into a
the sample, and
400-mL beaker and determine sodium oxide (Na O) by titrat-
C = grams of sample used.
ing the sample against 1.0 N acid, using methyl red as the
CARBONATE AS SODIUM CARBONATE (Na CO )
indicator.
2 3
8. Calculation 12. Calculation
8.1 Calculate the total alkalinity as sodium oxide (Na O) as 12.1 Calculatethecarbonateassodiumcarbonate(Na CO )
2 2 3
follows: as follows:
D 501 – 89 (1998)
Na CO,% 5[~A 2 B! 35 35.3]/W (3)
2 3 W = grams of sample used.
where:
NOTE 1—Whenmoreaccurateresultsaredesired,theevolutionmethod
A = millilitres of acid required for titration of the NaOin
2 for carbon dioxide as described in Sections 13-16 should be used.
the sample,
B = millilitresofacidrequiredfortitrationoftheNaOHin
the sample, and
CARBON DIOXIDE (CO ) BY THE EVOLUTION METHOD
13. Apparatus 15. Procedure
13.1 Apparatus Assembly—Place a 150-mL wide-neck ex- 15.1 Aspiratewithastreamofcarbondioxide(CO )-freeair
traction flask on a gauze over a burner. Fit the flask with a at a rate of approximately 20 to 30 mL/min until the train is
three-hole rubber stopper, one opening to carry a 25-cm reflux free from CO as determined by no further change in weight
condenser, the second to carry a thistle tube with a twoway greater than 0.3 mg in the U-tube.
stopcock for the introduction of acid into the flask, and the 15.2 Weigh 10 g of the sample to the nearest 0.01 g directly
thirdtocarryatubefortheintroductionofacontinuousstream into the extraction flask, cover with 50 mL of freshly boiled
of carbon dioxide (CO )-free air into the flask. Draw out the water, add 2 drops of methyl orange solution, and close the
ends of the thistle and air supply tubes to a small point, and apparatuswiththetraininplace.Starttheaspirationatarateof
placetheminthestoppersothatthepointsareveryclosetothe 20 to 30 mL/min, and slowly add through the thistle tube
bottom of the flask. Attach to the air supply tube, a U-tube sufficientH SO (2+9)toneutralizetheNaOHandasufficient
2 4
containing soda-asbestos (Ascarite) so that the air admitted to excesstoensurethefinalacidityofthemixtureasindicatedby
the flask will be free from CO . 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
16. Calculation
first half and the same drying agent in the second half as used
16.1 From the increase in weight of the tube calculate the
in 13.2.2, and
13.2.4 A protective U-tube containing any of the above percentage of carbon dioxide (CO ) as sodium carbonate
(Na CO ) as follows:
mentioned drying agents.
2 3
13.2.5 Attach the final tube to an aspirator.
Na CO,% 5[~C 32.409!/W] 3100 (4)
2 3
14. Reagents
where:
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.
14.2 Sulfuric Acid (2+9)—Mix 2 volumes of concentrated
NOTE 2—This test method for the determination of Na CO as CO is
2 3 2
sulfuric acid (H SO , sp gr 1.84) carefully with stirring into 9
to be preferred when a procedure more accurate than that described in
2 4
volumes of water. Section 12 is required.
D 501 – 89 (1998)
SODAASH
17. Sampling SODIUM BICARBONATE (NaHCO )
17.1 Soda ash shall be sampled by removing portions from
23. Reagents
various parts of the container. Samples shall not be taken from
those portions of the soda ash where caking is noticeable due
23.1 Silver Nitrate Solution (100 g/L)—Dissolve 100 g of
to the absorption of moisture and carbon dioxide through the silver nitrate (AgNO ) in water and dilute to 1 L. Prepare this
container.Ifthesodaashiscaked,thesampleshallbeobtained
solution fresh before use.
by thoroughly mixing and quartering the entire contents of the 23.2 Sodium Hydroxide, Standard Solution (1.0 N)—
package.
Prepare and standardize a 1.0 N sodium hydroxide (NaOH)
solution.
MATTER VOLATILE AT 150 TO 155°C
24. Procedure
18. Procedure
24.1 Weigh 8.4 g of the sample to the nearest 0.05 g and
18.1 Place approximately2gofthe sample in a tared
transfer to a 250-mLbeaker. Dissolve in 100 mLof water, and
weighing bottle and weigh to the nearest 0.1 mg. Remove the
titrate with 1.0 N NaOH solution until a drop of the test
stopperanddryinanovenat150to155°Cfor1h.Replacethe
solution added to a drop of AgNO solution on a spot plate
stopper and allow to cool to room temperature in a desiccator
gives a dark color instantly.
containing no desiccant and reweigh.
25. Calculation
19. Calculation
25.1 Calculate the percentage of sodium bicarbonate
19.1 Calculate the percentage of volatile matter as follows:
(NaHCO ) as follows:
Volatilematter,% 5 ~L/W! 3100 (5)
NaHCO,% 5mLof1.0 NNaOHsolution (7)
where:
Calculate the percentage of sodium carbonate (Na CO)as
2 3
L = grams loss in weight, and
follows:
W = grams of sample used.
Na CO,% 5 A 2 ~NaHCO,% 30.6309! (8)
2 3 3
TOTALALKALINITYAS SODIUM CARBONATE
where:
(Na CO )
2 3 A = total alkalinity as Na CO , in percent.
2 3
NOTE 3—For referee purposes, or when more accurate results are
20. Reagents
required than are yielded by the procedure described in Section 25, the
20.1 Methyl Orange Indicator Solution (1 g/L)—Dissolve
method described in Section 28 shall be used.
0.1 g of methyl orange in water and dilute to 100 mL.
SODIUM BICARBONATE (NaHCO)BY
20.2 Hydrochloric Acid, Standard (0.5 N)—Prepare and
POTENTIOMETRIC TITRATION
standardize 0.5 N hydrochloric acid (HCl).
21. Procedure 26. Reagents
21.1 Transfer approximately 1.2 g of sample into a tared
26.1 Barium Chloride, Neutral Solution (122 g/L)—
weighing bottle. Weigh to the nearest 0.1 mg, protecting the Dissolve 122 g of barium chloride (BaCl ·2H O) in water and
2 2
sample at all times, as much as possible, from moisture in the
dilute to 1 L. Make the solution neutral to phenolphthalein.
air during weighing. Dissolve the sample in about 50 mL of 26.2 Hydrochloric Acid, Standard (0.1 N)—Prepare and
water in a 400-mL
...