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: E359 − 17

Standard Test Methods for

Analysis of Soda Ash (Sodium Carbonate)1
This standard is issued under the fixed designation E359; 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* 2. Referenced Documents

1.1 These test methods cover the analyses usually required 2.1 ASTM Standards:2
on commercial soda ash (sodium carbonate). C429 Test Method for Sieve Analysis of Raw Materials for
1.2 The analytical procedures appear in the following sec- Glass Manufacture
tions: D1193 Specification for Reagent Water
D6809 Guide for Quality Control and Quality Assurance
Sections
Procedures for Aromatic Hydrocarbons and Related Ma-
Total Alkalinity, Titrimetric 8 – 15 terials
Sodium Bicarbonate, Titrimetric 17 – 24 E11 Specification for Woven Wire Test Sieve Cloth and Test
Loss on Heating, Gravimetric 26 – 32
Moisture, Calculation 34 – 38 Sieves
Sodium Chloride, Titrimetric 40 – 46 E29 Practice for Using Significant Digits in Test Data to
Sodium Sulfate, Gravimetric 48 – 54 Determine Conformance with Specifications
Iron, Photometric 56 – 64
Sieve Analysis 66 – 72 E60 Practice for Analysis of Metals, Ores, and Related
1.3 The values stated in SI units are to be regarded as Materials by Spectrophotometry
standard. No other units of measurement are included in this E70 Test Method for pH of Aqueous Solutions With the
standard. Glass Electrode
E145 Specification for Gravity-Convection and Forced-
1.4 In determining the conformance of the test results using Ventilation Ovens
this method to applicable specifications, results shall be E180 Practice for Determining the Precision of ASTM
rounded off in accordance with the rounding-off method of Methods for Analysis and Testing of Industrial and Spe-
Practice E29. cialty Chemicals (Withdrawn 2009)3
1.5 Review the current Safety Data Sheets (SDS) for de- E200 Practice for Preparation, Standardization, and Storage
tailed information concerning toxicity, first aid procedures, of Standard and Reagent Solutions for Chemical Analysis
handling and safety precautions. E300 Practice for Sampling Industrial Chemicals
1.6 This standard does not purport to address all of the 2.2 Other Documents:
safety concerns, if any, associated with its use. It is the OSHA Regulations, 29 CFR paragraphs 19100.1000 and
responsibility of the user of this standard to establish appro- 1910.12004
priate safety, health, and environmental practices and deter-
mine the applicability of regulatory limitations prior to use. 3. Significance and Use
Specific hazards statements are given in Section 6. 3.1 Soda ash is used in a number of manufacturing pro-
1.7 This international standard was developed in accor- cesses. The procedures listed in 1.2 are suitable for specifica-
dance with internationally recognized principles on standard- tion acceptance and manufacturing control of commercial soda
ization established in the Decision on Principles for the ash.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 2
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
1
These test methods are under the jurisdiction of ASTM Committee D16 on the ASTM website.
3
Aromatic, Industrial, Specialty and Related Chemicals and are the direct responsi- The last approved version of this historical standard is referenced on
bility of Subcommittee D16.12 on Caustics and Peroxides. www.astm.org.
4
Current edition approved June 15, 2017. Published August 2017. Originally Available from U.S. Government Printing Office, Superintendent of
approved in 1968. Last previous edition approved in 2010 as E359 – 10. DOI: Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
10.1520/E0359-17. www.access.gpo.gov.

*A Summary of Changes section appears at the end of this standard

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 E359 − 17
4. Apparatus ity of dense ash in bulk to segregate in relation to particle size
4.1 Photometers and Photometric Practice—Photometers as the result of normal transit vibrations.
and photometric practice used in these test methods shall 7.2.3 Details of good sampling depend on: (1) the type of
conform to Practice E60. shipment, whether in containers or in bulk; (2) the type of
product, whether light or dense soda ash; and (3) the type of
4.2 pH Meters—pH meters and their use shall conform to
analysis desired, whether chemical or physical.
Test Method E70.
4.3 Buret—A calibrated 50-mL buret, or any standard 7.3 Bulk Shipments:
50-mL buret calibrated by either the National Institute of 7.3.1 Although bulk shipments are normally in transit a
Standards and Technology or by the user. Alternatively, a relatively short time, there is likely to be some absorption of
100-mL calibrated buret with a 50-mL bulb at the top and a moisture and carbon dioxide in exposed surface areas. If
50-mL stem below may be used. physical tests such as screen analysis are to be included, it is
particularly important to avoid segregation that occurs on
5. Purity of Reagents and Water surface areas.
5.1 Purity of Reagents—Reagent grade chemicals shall be 7.3.2 To sample boxcar shipments, brush aside the surface
used in all tests. Unless otherwise indicated, it is intended that layer to a depth of 12 in. (305 mm) and take portions
all reagents shall conform to the specifications of the Commit- systematically from the newly exposed area to the bottom of
tee on Analytical Reagents of the American Chemical Society, the car by means of a sample thief.
where such specifications are available.5 Other grades may be 7.3.3 Hopper cars and trucks are more difficult to sample
used, provided it is first ascertained that the reagent is of adequately. Samples can be taken through the hatches with a
sufficiently high purity to permit its use without lessening the sample thief, as for boxcar sampling. Preferably, samples
accuracy of the determination. should be taken during the unloading operation at the point of
5.2 Unless otherwise indicated, references to water shall be discharge to the bin, or from any open section of the conveyor.
understood to mean Type II or Type III reagent water conform-
7.4 Bag Shipments:
ing to Specification D1193.
7.4.1 Packaged soda ash that has been in storage for some
6. Hazards time can be sampled satisfactorily only by emptying the whole
package and mixing thoroughly before taking the sample. Even
6.1 Soda ash is a primary skin irritant. Dusts or mists are such a portion is likely to represent only the package sampled
moderately irritating to the mucous membrane of the nose and rather than the stock of packages as a whole. The reason is that
eyes. The irritation is temporary and symptoms usually disap- a bag or other container taken from an outer layer of the storage
pear shortly after contact is ended. pile is subject to more air contact and consequently more
6.2 Consult current OSHA regulations, suppliers’ Safety moisture and carbon dioxide absorption than are packages
Data Sheets, and local regulations for all materials used in this buried farther back in the stock.
test method. 7.4.2 To get an idea of the quality of the soda ash as packed,
it is the usual practice to take the sample from somewhere near
7. Sampling the center of the package. This may be done by removing the
7.1 The general principles for sampling solids are covered top 6 or 8 in. (150 or 200 mm) of soda ash from the package,
in Practice E300. The following aspects of soda ash sampling then removing the sample from the center of the remaining
must be considered: portion. Such a sample carefully taken will generally be found
7.2 General: representative except in cases of long storage or unusually
7.2.1 The selection of a representative sample is a necessary damp storage conditions.
prerequisite for any accurate analysis, and this is particularly 7.5 Sample Preparation:
important with the alkalies, since they are susceptible to rapid 7.5.1 Thoroughly mix the total sample taken. Then quarter
contamination by moisture and carbon dioxide upon exposure or riffle the entire sample to obtain the required size sample for
to air. Also, some of them are not uniform in particle size and
analysis. Minimize exposure to moisture and carbon dioxide.
tend to segregate on handling.
7.2.2 The characteristics of soda ash that make proper 7.5.2 Store the sample for analysis in a glass or other
sampling difficult at times are its tendency to absorb moisture suitable container that will not contaminate the sample and that
and carbon dioxide from the air through any commercial can be sealed to prevent exposure of the sample to moisture or
container in which it is generally shipped, and the susceptibil- carbon dioxide.
TOTAL ALKALINITY
5
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
8. Scope
listed by the American Chemical Society, see Analar Standards for Laboratory 8.1 This test method covers the titrimetric determination of
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, the total alkalinity of soda ash. This alkalinity is normally
MD. expressed as percent sodium oxide (Na2O).

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 E359 − 17
9. Summary of Test Method where:
9.1 Total alkalinity is determined by titration with standard A = Na2CO3, % (see 13.2), and
hydrochloric (or sulfuric) acid using methyl orange or modified B = NaHCO3, % (see 22.1).
methyl orange indicator solution.
14. Report
10. Interferences
14.1 Report the percentage of sodium oxide to the nearest
10.1 Alkalies other than soda ash (sodium carbonate) and 0.01 %.
compounds that consume acid will affect the accuracy of this
test method. 15. Precision and Bias
11. Reagents 15.1 Precision—The following criteria should be used for
11.1 Hydrochloric (or Sulfuric) Acid (1.0 meq/mL)— judging the acceptability of results (Note 4):
Prepare in accordance with Practice E200 (record temperature 15.1.1 Repeatability (Single Analyst)—The standard devia-
of solution when standardized). tion for a single determination has been estimated to be
0.032 % absolute at 52 DF. The 95 % limit for the difference
11.2 Modified Methyl Orange Indicator Solution or Methyl
between two such runs is 0.09 % absolute.
Orange Indicator Solution—See Practice E200.
15.1.2 Laboratory Precision (Within-Laboratory, Between-
11.3 Water, carbon dioxide-free (freshly boiled and cooled). Days Variability)—The standard deviation of results (each the
average of duplicates), obtained by the same analyst on
12. Procedure
different days, has been estimated to be 0.038 % absolute at 26
12.1 Weigh, to the nearest 0.1 mg, 4.4 6 0.1 g (Note 1) of DF. The 95 % limit for the difference between two such
the sample and transfer to a 500-mL conical flask. Add 100 mL averages is 0.11 % absolute.
of water and swirl to dissolve the sample. 15.1.3 Reproducibility (Multilaboratory)—The standard de-
NOTE 1—Use of the specified weight of sample requires a 100-mL buret viation of results (each the average of duplicates), obtained by
for titration and is recommended. If a 50-mL buret is used, the sample analysts in different laboratories, has been estimated to be
weight should be halved. 0.154 % absolute at 8 DF. The 95 % limit for the difference
12.2 Add 3 drops of modified methyl orange indicator between two such averages is 0.43 % absolute.
solution (Note 2). Titrate this solution with standard 1.0
NOTE 4—These precision estimates are based on an interlaboratory
meq/mL acid to a gray end point (Note 3). Record the volume study of analyses performed in 1967 on three samples of soda ash
to the nearest 0.02 mL and temperature of the acid used. covering the range from 58.190 to 58.385 % sodium oxide. Ten labora-
Correct the acid normality for any difference from the stan- tories analyzed the three samples, with one analyst in each laboratory
dardization temperature by use of the factor ∆N/°C = 0.00035 performing duplicate determinations and repeating 1 day later.6 Practice
between 20 and 30°C. Add the correction when the temperature E180 was used for developing these precision estimates.
of use is below and subtract when above the temperature of 15.2 Bias—The bias of this test method has not been
standardization (see Practice E200). determined because of the lack of acceptable reference mate-
NOTE 2—If desired, 0.1 % methyl orange indicator solution may be
rial.
used.
NOTE 3—The analyst should end the titration at the same shade of color 16. Quality Guidelines
as was used for the end point in the standardization of the acid.
16.1 Laboratories shall have a quality control system in
13. Calculation place.
13.1 Calculate the total alkalinity as percent sodium oxide 16.1.1 Confirm the performance of the test instrument or
(Na2O) as follows: test method by analyzing a quality control sample following
the guidelines of standard statistical quality control practices.
~ A 3 B 3 0.030990! 3 100
sodium oxide, weight % 5
W
(1) 16.1.2 A quality control sample is a stable material isolated
from the production process and representative of the sample
where: being analyzed.
A = acid required for titration of the sample, mL, 16.1.3 When QA/QC protocols are already established in
B = corrected meq/mL of the acid, and the testing facility, these protocols are acceptable when they
W = sample used, g. confirm the validity of test results.
13.2 Alternatively, calculate the alkalinity as sodium car- 16.1.4 When there are no QA/QC protocols established in
bonate as follows: the testing facility, use the guidelines described in Guide
sodium carbonate, weight % 5 1.7101 3 Na 2 O, wt % (2) D6809 or similar statistical quality control practices.
13.3 If actual sodium carbonate content is desired, the
sodium bicarbonate content must be determined separately as
6
described in Sections 17 and 24. Then: Supporting data have been filed ASTM Headquarters and may be obtained by
requesting Request Research Report RR:E15-0046. Contact ASTM Customer
sodium carbonate ~ actual! , % 5 A 2 ~ B 3 0.6308! (3) Service at service @astm.org.

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 E359 − 17
SODIUM BICARBONATE 21.4 Weigh, to the nearest 1 mg, 4.0 g of the sample (or of
the primary standard) and transfer to the solution in the
17. Scope 600-mL beaker. Place the beaker on a magnetic stirrer, insert a
17.1 This test method describes the titrimetric determination stirring bar, and stir to dissolve.
of sodium bicarbonate in soda ash. The lower limit of deter- NOTE 7—The subsequent operations should be completed within 5 min
mination is 0.02 % sodium bicarbonate. to minimize absorption of atmospheric CO2.
21.5 While continuing to stir, add the 200 mL of neutralized
18. Summary of Test Method BaCl2 solution by means of a 100-mL (or 200-mL, if available)
18.1 Bicarbonate is determined titrimetrically by adding a pipet, allowing the reagent to run freely into the stirring
sample to an excess of standard sodium hydroxide solution solution.
(thus converting bicarbonate to carbonate), precipitating the 21.6 Insert the electrodes into the solution and titrate slowly
carbonate with barium chloride solutions and back-titrating the with 0.1 meq/mL HCl using a 10-mL buret, stirring continu-
excess sodium hydroxide with standard acid solution using a ously. When pH 8.8 is reached, allow the solution to stir for 1
pH meter to determine the end point. min. If the pH remains at 8.8, the end point has been reached.
18.2 A primary standard is run simultaneously to correct the If not, continue the titration until this pH is reached. Record the
titration for adsorption or occlusion of sodium hydroxide on volume of titrant to the nearest 0.05 mL.
the barium carbonate.
22. Calculation
19. Apparatus
22.1 Calculate the percentage of sodium bicarbonate as
19.1 pH Meter, with glass and calomel electrodes. Standard- follows:
ize the pH meter with commercially available pH 10 buffer
sodium bicarbonate, weight %
solution.
~B 2 A ! 3 N 3 0.084 3 100
19.2 Magnetic Stirrer, with TFE-fluorocarbon-covered stir- 5
W
(4)
ring bar.
where:
20. Reagents A = acid for sample, mL,
20.1 Barium Chloride Solution (120 g/L)—See Practice B = acid for primary standard, mL,
E200. N = meq/mL of acid, and
W = sample used, g.
20.2 Hydrochloric Acid, Standard (0.1 meq/mL)—See Prac-
tice E200. 23. Report
20.3 Sodium Carbonate, Primary Standard Na2CO3—Dry 23.1 Report the percentage of sodium bicarbonate to the
about 10 g of anhydrous primary standard sodium carbonate nearest 0.01 %.
(Na2CO3) in a platinum dish or low-form weighing bottle
(70-mm diameter) for 4 h at 250°C (minimum) but do not 24. Precision and Bias
exceed 300°C. Cool in a desiccator. Prepare fresh for use.
24.1 Precision—The following criteria should be used for
20.4 Sodium Hydroxide, Standard Solution (0.1 meq/mL)— judging the acceptability of results (Note 8):
See Practice E200. 24.1.1 Repeatability (Single Analyst)—The standard devia-
20.5 Water, carbon dioxide-free (freshly boiled and cooled). tion for a single determination has been estimated to be
0.030 % absolute at 60 DF. The 95 % limit for the difference
21. Procedure between two such runs is 0.08 % absolute.
21.1 Perform the following steps of the procedure on equal 24.1.2 Laboratory Precision (Within-Laboratory, Between-
mass of both the sample and the primary standard sodium Days Variability)—The standard deviation of results (each the
carbonate (Na2CO3) (Note 5). Make duplicate determinations. average of duplicates), obtained by the same analyst on
different days, has been estimated to be 0.078 % absolute at 30
NOTE 5—To compensate for the adsorption or occlusion of NaOH by
the precipitated BaCO3 (21.5), the use of primary standard Na2CO3 as a
DF. The 95 % limit for the difference between two such
blank is required. averages is 0.22 % absolute.
24.1.3 Reproducibility (Multilaboratory)—The standard de-
21.2 Place 200 mL of BaCl2 solution in a 400-mL beaker.
viation of results (each the average of duplicates), obtained by
Using a pH meter, adjust the solution to pH 8.8 by addition of
analysts in different laboratories, has been estimated to be
0.1 meq/mL NaOH solution (or HCl) as required.
0.084 % absolute at 9 DF. The 95 % limit for the difference
21.3 Into a 600-mL beaker place 150 mL of CO2-free water. between two such averages is 0.24 % absolute.
Add by pipet 5.0 mL of 0.1 meq/mL NaOH solution.
NOTE 8—These precision estimates are based on an interlaboratory
NOTE 6—If, in 21.6, the pH of the sample solution is below 8.8 before study of analyses performed in 1967 on three samples covering the range
titrating with 0.1 meq/mL HCl, repeat the test adding by pipet 10.0 mL of from 0.23 to 0.98 % sodium bicarbonate. One analyst in ten laboratories
0.1 meq/mL NaOH solution to the beakers being prepared for both the performed duplicate determinations and repeated 1 day later.6 Practice
sample and the primary standard Na2CO3. E180 was used in developing these precision estimates.

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 E359 − 17
24.2 Bias—The bias of this test method has not been W = sample used, g.
determined because of the lack of acceptable reference mate-
rial. 31. Report
25. Quality Guidelines 31.1 Report the percentage loss in mass to the nearest
0.01 %.
25.1 Laboratories shall have a quality control system in
place. 32. Precision and Bias
25.1.1 Confirm the performance of the test instrument or
32.1 Precision—The following criteria should be used for
test method by analyzing a quality control sample following
judging the acceptability of results (Note 9):
the guidelines of standard statistical quality control practices.
32.1.1 Repeatability (Single Analyst)—The standard devia-
25.1.2 A quality control sample is a stable material isolated
tion for a single determination has been estimated to be
from the production process and representative of the sample
0.016 % absolute at 54 DF. The 95 % limit for the difference
being analyzed.
between two such runs is 0.04 % absolute.
25.1.3 When QA/QC protocols are already established in
32.1.2 Laboratory Precision (Within-Laboratory, Between-
the testing facility, these protocols are acceptable when they
Days Variability)—The standard deviation of results (each the
confirm the validity of test results.
average of duplicates), obtained by the same analyst on
25.1.4 When there are no QA/QC protocols established in
different days, has been estimated to be 0.015 % absolute at 27
the testing facility, use the guidelines described in Guide
DF. The 95 % limit for the difference between two such
D6809 or similar statistical quality control practices.
averages is 0.04 % absolute.
LOSS ON HEATING 32.1.3 Reproducibility (Multilaboratory)—The standard de-
viation of results (each the average of duplicates), obtained by
26. Scope analysts in different laboratories, has been estimated to be
26.1 This test method covers the gravimetric determination 0.030 % absolute at 8 DF. The 95 % limit for the difference
of loss on heating of soda ash. between two such averages is 0.08 % absolute.
NOTE 9—These precision estimates are based on an interlaboratory
27. Summary of Test Method study of analyses performed in 1967 on three samples covering the range
from 0.35 to 0.55 % loss on heating. One analyst in each of ten
27.1 Loss on heating is determined gravimetrically by laboratories performed duplicate determinations and repeated 1 day later.6
heating a weighed sample under controlled conditions to expel Practice E180 was used in developing these precision estimates.
moisture and thermally convert sodium bicarbonate to sodium
32.2 Bias—The bias of this test method has not been
carbonate by elimination of water and carbon dioxide.
determined because of the lack of acceptable reference mate-
28. Apparatus rial.
28.1 Drying Oven, gravity-convection, Type IB. See Speci- 33. Quality Guidelines
fication E145.
33.1 Laboratories shall have a quality control system in
28.2 Weighing Bottle, 70-mm diameter, low-form, glass, place.
with cover. 33.1.1 1 Confirm the performance of the test instrument or
test method by analyzing a quality control sample following
29. Procedure
the guidelines of standard statistical quality control practices.
29.1 Dry the weighing bottle at 250°C minimum (270°C 33.1.2 A quality control sample is a stable material isolated
max) for 30 min. Cool in a desiccator and weigh to the nearest from the production process and representative of the sample
0.1 mg. being analyzed.
29.2 Place 5 6 0.1 g of the sample in the weighing bottle, 33.1.3 When QA/QC protocols are already established in
cover and weigh to the nearest 0.1 mg. Determine the sample the testing facility, these protocols are acceptable when they
weight by difference. confirm the validity of test results.
33.1.4 When there are no QA/QC protocols established in
29.3 Dry with the cover ajar for 4 h at 250°C minimum the testing facility, use the guidelines described in Guide
(270°C maximum). Cool in a desiccator with the cover ajar. D6809 or similar statistical quality control practices.
Weigh to the nearest 0.1 mg with the cover closed.
MOISTURE
30. Calculation
30.1 Calculate the percentage loss in weight as follows: 34. Scope
~ A 2 B ! 3 100 34.1 This test method covers the calculation of moisture in
loss in weight, weight % 5 (5) soda ash.
W

where: 35. Summary of Test Method

A = mass of bottle and sample before heating, g, 35.1 Moisture is determined by calculation. The percent of
B = mass of bottle and sample after heating, g, and volatile products resulting from decomposition of sodium

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 E359 − 17
bicarbonate, 22.1, is subtracted from the percent loss on 39.1.4 When there are no QA/QC protocols established in
heating, 30.1, and the difference is reported as moisture. the testing facility, use the guidelines described in Guide
D6809 or similar statistical quality control practices.
NOTE 10—The test method makes the assumption that in commercial
soda ash, nonvolatile matter other than moisture and products of sodium
bicarbonate decomposition will not be evolved at 250 to 270°C.
SODIUM CHLORIDE

40. Scope
36. Calculation
40.1 This test method covers the titrimetric determination of
36.1 Calculate the percentage of moisture as follows: sodium chloride in soda ash. The lower limit of detection is
moisture, weight % 5 A 2 ~ B 3 0.369! (6) 0.005 % sodium chloride.
where:
41. Summary of Test Method
A = loss on heating, % (see 30.1), and
B = sodium bicarbonate, % (see 22.1). 41.1 Chloride is determined titrimetrically by the Volhard
method. A sample is dissolved, acidified, and treated with a
37. Report small excess of standard silver nitrate solution. The precipi-
tated silver chloride is removed by filtration and the excess
37.1 Report the percentage of moisture to the nearest silver nitrate is titrated with standard ammonium thiocyanate
0.01 %. solution using ferric ammonium sulfate indicator solution.

38. Precision and Bias 42. Reagents

38.1 Precision—The following criteria should be used for 42.1 Ammonium Thiocyanate, Standard Solution (0.1 meq/
judging the acceptability of results (Note 11): mL)—See Practice E200.
38.1.1 Repeatability (Single Analyst)—The standard devia- 42.2 Ferric Ammonium Sulfate Indicator Solution—See
tion for a single determination has been estimated to be Practice E200.
0.014 % absolute at 54 DF. The 95 % limit for the difference
between two such runs is 0.04 % absolute. 42.3 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
38.1.2 Laboratory Precision (Within-Laboratory, Between- (HNO3).
Days Variability)—The standard deviation of results (each the 42.4 Silver Nitrate, Standard Solution (0.1 meq/mL)—See
average of duplicates), obtained by the same analyst on Practice E200.
different days, has been estimated to be 0.031 % absolute at 27
DF. The 95 % limit for the difference between two such 43. Procedure
averages is 0.09 % absolute. 43.1 Weigh, to the nearest 1 mg, 10 g of sample (Note 12)
38.1.3 Reproducibility (Multilaboratory)—The standard de- and transfer to a 500 mL glass-stoppered conical flask, using
viation of results (each the average of duplicates), obtained by about 100 mL of water to effect the transfer. Add 1 mL of ferric
analysts in different laboratories, has been estimated to be ammonium sulfate indicator solution and sufficient HNO3 (sp
0.044 % absolute at 8 DF. The 95 % limit for the difference gr 1.42) slowly to dissolve the reddish-brown ferric hydroxide
between two such averages is 0.12 % absolute. precipitate. Then add 1 to 2 mL excess HNO3 and cool to room
NOTE 11—These precision estimates are based on an interlaboratory temperature.
study of analyses performed in 1967 on three samples covering the range NOTE 12—If the sodium chloride content is less than 0.1 % use a 20-g
from 0.18 to 0.34 % moisture in soda ash. One analyst in each of ten sample.
laboratories performed duplicate determinations and repeated 1 day later.6
Practice E180 was used in developing these precision estimates. 43.2 Add, from a buret, 1 mL of 0.1 meq/mL NH4CNS
38.2 Bias—The bias of this test method has not been solution. Titrate the solution with 0.1 meq/mL AgNO3 solution
determined because of the lack of acceptable reference mate- to the disappearance of the reddish-brown color. Then add 2
rial. mL of 0.1 meq/mL AgNO3 solution in excess. Stopper the flask
and shake the solution vigorously.
39. Quality Guidelines 43.3 Filter off the precipitated silver chloride using semi-
quantitative paper. Wash the paper with three 5-mL portions of
39.1 Laboratories shall have a quality control system in
water. Titrate the filtrate and washings with 0.1 meq/mL
place.
NH4SCN solution until the first permanent reddish-brown
39.1.1 Confirm the performance of the test instrument or
color appears and persists after shaking for a minimum of 15 s.
test method by analyzing a quality control sample following
the guidelines of standard statistical quality control practices. 43.4 Record the volumes of titrants used to the nearest 0.02
39.1.2 A quality control sample is a stable material isolated mL. Include the initial volume of 0.1 meq/mL NH4SCN
from the production process and representative of the sample solution used in 43.2.
being analyzed.
39.1.3 When QA/QC protocols are already established in 44. Calculation
the testing facility, these protocols are acceptable when they 44.1 Calculate the percentage of sodium chloride as fol-
confirm the validity of test results. lows:

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 E359 − 17
sodium chloride,weight %5 (7) SODIUM SULFATE
@ ~ A 3 N 1 ! 2 ~ B 3 N 2 ! # 3 0.05844 3 100 48. Scope
W
48.1 This test method covers the gravimetric determination
where: of sulfate present in soda ash. The lower limit of detection is
A = AgNO3 solution added, mL, 0.005 % sodium sulfate.
B = NH4CNS solution added, mL,
N1 = meq/mL of AgNO3 solution used, 49. Summary of Test Method
N2 = meq/mL of NH4 CNS solution used, and
W = sample used, g. 49.1 Sulfate is determined gravimetrically by precipitation
with barium chloride solution, filtering, washing, igniting, and
45. Report weighing as barium sulfate.

45.1 Report the percentage of sodium chloride to the nearest 50. Reagents
0.001 %.
50.1 Barium Chloride Solution (120 g BaCl2·2H2O/L)—See
46. Precision and Bias Practice E200.
50.2 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
46.1 Precision—The following criteria should be used for
chloric acid (HCl).
judging the acceptability of results (Note 13):
46.1.1 Repeatability (Single Analyst)—The standard devia- 50.3 Methyl Orange Indicator Solution (1 g/L)—See Prac-
tion for a single determination has been estimated to be tice E200.
0.0026 % absolute at 50 DF. The 95 % limit for the difference 50.4 Silver Nitrate Solution (17 g/100 mL)—See Practice
between two such runs is 0.007 % absolute. E200.
46.1.2 Laboratory Precision (Within-Laboratory, Between-
Days Variability)—The standard deviation of results (each the 51. Procedure
average of duplicates), obtained by the same analyst on
different days, has been estimated to be 0.0058 % absolute at 51.1 Weigh 25 g of the sample to the nearest 0.1 g into a
25 DF. The 95 % limit for the difference between two such 600-mL beaker and dissolve with about 200 mL of water. Add
averages is 0.016 % absolute. 2 to 4 drops of methyl orange indicator solution and acidify
carefully with HCl, adding 1 mL in excess of that required to
46.1.3 Reproducibility (Multilaboratory)—The standard de-
neutralize the sample.
viation of results (each the average of duplicates), obtained by
analysts in different laboratories, has been estimated to be 51.2 Examine the solution at this point. If it contains any
0.0068 % absolute at 7 DF. The 95 % limit for the difference insoluble matter, filter off same on a retentive filter paper
between two such averages is 0.019 % absolute. washing the paper once with water.
NOTE 13—These precision estimates are based on an interlaboratory 51.3 Heat the solution (or filtrate) to boiling. Add slowly to
study of analyses performed in 1967 on three samples covering the range the boiling solution 25 mL of BaCl2 solution with constant
from 0.08 to 0.18 % sodium chloride. One analyst in each of ten stirring. Digest for 30 min on a steam bath and allow the
laboratories performed duplicate determinations and repeated 1 day later.6 precipitate to settle overnight at room temperature.
Practice E180 was used in developing these precision estimates.
51.4 Filter on ashless, fine quantitative paper and transfer
46.2 Bias—The bias of this test method has not been
the precipitate to the paper with a fine stream of hot water from
determined because of the lack of acceptable reference mate-
a wash bottle. Wash the precipitate with successive small
rial.
portions of hot water until the washings are free of chloride on
testing with 3 to 4 drops of AgNO3 solution.
47. Quality Guidelines
51.5 Heat a platinum or porcelain crucible 850 to 900°C for
47.1 Laboratories shall have a quality control system in
15 min, cool in a desiccator, and weigh to the nearest 0.0001 g.
place.
Fold the washed filter paper with precipitate and place in the
47.1.1 Confirm the performance of the test instrument or tared crucible. Dry and char carefully without flaming over a
test method by analyzing a quality control sample following low flame, and then more strongly until the paper is burned off.
the guidelines of standard statistical quality control practices. Ignite at 850 to 900°C for a minimum of 30 min. Remove the
47.1.2 A quality control sample is a stable material isolated crucible from the furnace, cool partially, place in a desiccator,
from the production process and representative of the sample and cool to room temperature. Reweigh to the nearest 0.0001
being analyzed. g.
47.1.3 When QA/QC protocols are already established in
the testing facility, these protocols are acceptable when they 52. Calculation
confirm the validity of test results.
47.1.4 When there are no QA/QC protocols established in 52.1 Calculate the percentage of sodium sulfate as follows:
the testing facility, use the guidelines described in Guide ~ A 2 B ! 3 0.60854 3 100
sodium sulfate, weight % 5 (8)
D6809 or similar statistical quality control practices. W

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 E359 − 17
where: 57. Summary of Test Method
A = mass of crucible and precipitate after ignition, g, 57.1 Iron is determined photometrically as the orange-red
B = mass of empty crucible, g, and complex of the ferrous form with 1,10-phenanthroline (ortho-
W = sample used, g. phenanthroline) in an acetate-buffered solution at pH 5. The
color develops within 15 min, is very stable, and follows
53. Report Beer’s law. Intensity of the color formed is measured at 510 nm
53.1 Report the percentage of sodium sulfate to the nearest in a photometer calibrated with standard iron solutions.
0.001 %.
58. Interferences
54. Precision and Bias 58.1 Impurities normally found in soda ash do not cause any
54.1 Precision—The following criteria should be used for interference. Copper, if present to the extent of 0.5 mg/100 mL
judging the acceptability of results (Note 14): of final solution, changes the hue of the solution, but interferes
54.1.1 Repeatability (Single Analyst)—The standard devia- only slightly when excess reagent is present. Zinc, cadmium,
tion for a single determination has been estimated to be and nickel form complexes and consume reagent but do not
0.0031 % absolute at 60 DF. The 95 % limit for the difference interfere when sufficient reagent is present.
between two such runs is 0.009 % absolute.
54.1.2 Laboratory Precision (Within-Laboratory, Between- 59. Reagents
Days Variability)—The standard deviation of results (each the 59.1 Ammonium Acetate-Acetic Acid Solution—See Practice
average of duplicates), obtained by the same analyst on E200.
different days, has been estimated to be 0.0043 % absolute at
59.2 Ammonium Hydroxide (1 + 1)—See Practice E200.
30 DF. The 95 % limit for the difference between two such
averages is 0.012 % absolute. 59.3 Congo Red Indicator Paper.
54.1.3 Reproducibility (Multilaboratory)—The standard de- 59.4 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
viation of results (each the average of duplicates), obtained by chloric acid (HCl).
analysts in different laboratories, has been estimated to be
59.5 Hydroxylamine Hydrochloride Solution (100 g/L)—
0.0070 % absolute at 9 DF. The 95 % limit for the difference
See Practice E200.
between two such averages is 0.020 % absolute.
59.6 Iron, Standard Solution (1 mL = 0.010 mg Fe)—See
NOTE 14—These precision estimates are based on an interlaboratory
study of analyses performed in 1967 on three samples covering the range
Practice E200.
from 0.013 to 0.23 % sodium sulfate. One analyst in each of ten 59.7 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
laboratories performed duplicate determinations and repeated 1 day later.6 (HNO3).
Practice E180 was used in developing these precision estimates.
59.8 1,10-Phenanthroline (Orthophenanthroline) Solution
54.2 Bias—The bias of this test method has not been
(3 g/L)—See Practice E200.
determined because of the lack of acceptable reference mate-
rial. 60. Preparation of Standard Curve
55. Quality Guidelines 60.1 Calibration Solutions—Transfer 0.5, 1.0, 2.0, 3.0, and
5.0 mL of the standard iron solution (1 mL = 0.010 mg Fe) into
55.1 Laboratories shall have a quality control system in
a series of 100-mL volumetric flasks. Dilute the contents of
place.
each flask to about 50 mL with water. Proceed as directed in
55.1.1 Confirm the performance of the test instrument or
60.3.
test method by analyzing a quality control sample following
the guidelines of standard statistical quality control practices. 60.2 Reference Solution—Transfer 50 mL of water to a
55.1.2 A quality control sample is a stable material isolated 100-mL volumetric flask and proceed in accordance with 60.3.
from the production process and representative of the sample 60.3 Color Development—To each flask add in order, with
being analyzed. mixing after each addition, 5 mL of hydroxylamine hydrochlo-
55.1.3 When QA/QC protocols are already established in ride solution, NH4OH (1 + 1) as required to make the solution
the testing facility, these protocols are acceptable when they just alkaline to congo red paper used as external indicator, 5
confirm the validity of test results. mL of the acetate buffer solution, and 5 mL of the phenanthro-
55.1.4 When there are no QA/QC protocols established in line solution. Dilute to volume with water and mix thoroughly.
the testing facility, use the guidelines described in Guide Allow to stand for 15 min for complete color development.
D6809 or similar statistical quality control practices.
60.4 Photometry—Transfer a suitable portion of the refer-
IRON ence solution to an absorption cell with a 5-cm light path (Note
15) and adjust the photometer (see 4.1) to the initial setting
56. Scope using a light band centered at approximately 510 nm. While
maintaining this adjustment, take the photometric readings
56.1 This test method covers the photometric determination
(absorbances) of the calibration solutions.
of iron in soda ash. The lower limit of detection is 0.1 µg/g as
Fe. NOTE 15—This test method has been written for cells having a 5-cm

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 E359 − 17
light path. Cells of other dimensions may be used, provided suitable the average of duplicates), obtained by the same analyst on
adjustments can be made in the amounts of samples and reagents used. different days, has been estimated to be 3.60 % relative at 27
60.5 Calibration Curve—Plot on coordinate paper the pho- DF. The 95 % limit for the difference between two such
tometric readings (absorbances) of the calibration solutions averages is 10 % relative.
versus milligrams of iron per 100 mL of solution. 64.1.3 Reproducibility (Multilaboratory)—The coefficient
of variation of results (each the average of duplicates), ob-
61. Procedure tained by analysts in different laboratories, has been estimated
61.1 Test Solutions—Weigh 50 6 0.1 g of sample and to be 13.3 % relative at 8 DF. The 95 % limit for the difference
transfer to a 600-mL beaker. Add 100 mL of water and stir to between two such averages is 37 % relative.
dissolve. Acidify with HCl (sp gr 1.19) in increments until 100 NOTE 17—These precision estimates are based on an interlaboratory
mL have been added. Cover with a watch glass, heat to boiling study of analyses performed in 1967 on three samples covering the range
and boil for 1 min. Remove from the heat and examine the from 10 to 30 µg/g iron in soda ash. One analyst in each of ten laboratories
bottom of the beaker for the presence of “mill scale” or other performed duplicate determinations and repeated 1 day later.6 Practice
E180 was used in developing these precision estimates.
insoluble particles (Note 16). If present, decant the clear
solution to a 500-mL volumetric flask. To the residue in the 64.2 Bias—The bias of this test method has not been
beaker add 5 mL of HCl and 2 mL of HNO3 (sp gr 1.42), heat determined because of the lack of acceptable reference mate-
to boiling in a hood, and evaporate nearly to dryness. Cool and rial.
transfer the residual solution to the 500-mL volumetric flask,
carefully rinsing the beaker. Cool the solution in the flask and 65. Quality Guidelines
make up to the mark with water and mix well. Pipet an aliquot 65.1 Laboratories shall have a quality control system in
containing 0.005 to 0.05 mg of iron into a 100-mL volumetric place.
flask. 65.1.1 Confirm the performance of the test instrument or
NOTE 16—The presence of such “mill scale” affects the precision of test method by analyzing a quality control sample following
results obtainable by the test method because of the difficulty of obtaining the guidelines of standard statistical quality control practices.
a representative sample. 65.1.2 A quality control sample is a stable material isolated
61.2 Reference Solution—Transfer 50 mL of water to a from the production process and representative of the sample
100-mL volumetric flask, and add 1 mL of HCl. being analyzed.
65.1.3 When QA/QC protocols are already established in
61.3 Color Development—Develop the color of the test the testing facility, these protocols are acceptable when they
solution, 61.1, and the reference solution 61.2, as described in confirm the validity of test results.
60.3. 65.1.4 When there are no QA/QC protocols established in
61.4 Photometry—Take the photometric reading of the test the testing facility, use the guidelines described in Guide
and reference solutions as described in 60.4. D6809 or similar statistical quality control practices.

62. Calculation SIEVE ANALYSIS

62.1 Convert the photometric reading (absorbance) of the
66. Scope
test solution to milligrams of iron by means of the calibration
curve. Calculate the parts per million of iron as follows: 66.1 This test method covers the sieve analysis of soda ash
(sodium carbonate) to measure the particle size. ASTM STP
A 3 1000
iron, µg/g 5 (9) 447A7 may also be useful to obtain guidelines for sieve
B
analysis in general.
where:
A = iron found in 100 mL of final solution, mg, and 67. Summary of Test Method
B = sample represented in the aliquot taken, g. 67.1 The particle size distribution of soda ash is determined
by passing the material through a series of sieves arranged in
63. Report order of increasing fineness and calculating the cumulative
63.1 Report the micrograms per gram of iron to the nearest percentage of each screen fraction.
0.1 µg/g.
68. Apparatus
64. Precision and Bias 68.1 Testing Sieves—Sieves shall conform to Specification
64.1 Precision—The following criteria should be used for E11, with particular reference to Table 1 and Section 4. Sieves
judging the acceptability of results (Note 17): shall be designated by the U.S. standard sieves and consist of
64.1.1 Repeatability (Single Analyst)—The coefficient of the following sieves stacked from coarsest on top to pan on the
variation for a single determination has been estimated to be bottom: 20, 30, 40, 50, 70, 80, 100, 140 200, 235 pan.
4.98 % relative at 54 DF. The 95 % limit for the difference
between two such runs is 14 % relative.
64.1.2 Laboratory Precision (Within-Laboratory, Between- 7
Manual on Test Sieving Methods, ASTM STP 447A, ASTM, West
Days Variability)—The coefficient of variation of results (each Conshohocken, PA, 1969.

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 E359 − 17
TABLE 1 Precision for Sieve Analysis 72.1.1 Laboratory Precision (Within-Laboratory, Between-
Laboratory Precision Reproducibility Days Variability)—The coefficient of variation of results,
Cumu- Coefficient
Degrees 95 %
Coefficient
Degrees 95 %
obtained by the same analyst on different days, has been
lative of of
% Variation,
of Range (%
Variation,
of Range (% estimated to be the values shown in Table 1 for the indicated
Freedom Relative) Freedom Relative) cumulative percent levels at the associated degrees of freedom.
% %
<1 20 10 56.0 31 5 86.8 The 95 % limit for the difference between two such results is
1 to 25 7.5 102 21.1 12.1 5 33.9 also shown in the table.
25 to 95 2.1 79 5.9 3.9 5 10.9
>95 0.29 60 0.8 0.33 5 0.9 72.1.2 Reproducibility (Multilaboratory)—The coefficient
of variation of results, obtained by analysts in different
laboratories has been estimated to be the values shown in Table
68.2 Sieve Shaker—A mechanically operated sieve shaker 1 for the indicated cumulative percent levels at the associated
that imparts to the set of sieves a rotary motion and tapping degrees of freedom. The 95 % limit for the difference between
action of uniform speed shall be provided. Shaker shall two such results is also shown in the table.
conform to specifications of 4.2 provided in Test Method C429.
NOTE 18—These above precision estimates are based upon an inter-
68.3 Balance—Properly calibrated and capable of 0.1 g laboratory study on two samples of soda ash (typical product and a coarser
accuracy. than normal material). One analyst in each of six laboratories performed
single determinations on three different days for a total of 36 determina-
69. Procedure tions using 10 sieves each. Practice E180 was used as a general guide in
69.1 Weigh 100 g of sample to the nearest 0.1 g, and transfer developing these precision estimates. The research report for the sieve
analysis is not on file at ASTM Headquarters and is considered missing.
it onto the top of the stacked sieves. Cover the top sieve and Because replicate determinations were not made on a single day, no
place the entire assembly on the sieve shaker. Shake the nest of estimate of repeatability is possible.
sieves for 10 min.
72.2 Bias—The bias of the test method has not been
69.2 Carefully remove the top sieve from the stack and pour determined because of the lack of acceptable reference mate-
its contents into a weighing pan. Tap the sieve or use a small rial.
stiff brush to gather the remaining sample particles into the
weighing pan. 73. Quality Guidelines
69.3 Record the weight to the nearest 0.1 g. Weigh the
contents of the remaining sieves in the same manner. 73.1 Laboratories shall have a quality control system in
place.
70. Calculation 73.1.1 Confirm the performance of the test instrument or
70.1 Calculate the cumulative percentage of each screen test method by analyzing a quality control sample following
fraction as follows: the guidelines of standard statistical quality control practices.
A 73.1.2 A quality control sample is a stable material isolated
cumulative weight % 5 3 100 (10) from the production process and representative of the sample
B
being analyzed.
where: 73.1.3 When QA/QC protocols are already established in
A = mass of screen fraction plus the combined mass of the the testing facility, these protocols are acceptable when they
previous screen fractions in the sample, g, and confirm the validity of test results.
B = mass of sample, g.
73.1.4 When there are no QA/QC protocols established in
71. Report the testing facility, use the guidelines described in Guide
D6809 or similar statistical quality control practices.
71.1 Report the cumulative percentage to the nearest 0.1 %.
72. Precision and Bias 74. Keywords
72.1 Precision—The following criteria should be used for 74.1 bicarbonate; chloride; iron; loss on heating; moisture;
judging the acceptability of results (Note 18): sieve analysis; soda ash; sodium carbonate; sulfate

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 E359 − 17
SUMMARY OF CHANGES

Subcommittee D16.16 has identified the location of selected changes to this standard since the last issue
(E359 – 10) that may impact the use of this standard. (Approved June 15, 2017.)

(1) Changed % mass (mm) to weight %. (4) Updated footnote 1 to read “This test method is under the
(2) Added Quality Guidelines after Precision and Bias for each jurisdiction of ASTM Committee D16 on Aromatic, Industrial,
test. Specialty and Related Chemicals and is the direct responsibil-
(3) Added Guide D6809 to Referenced Documents, section ity of Subcommittee D16.16 on Industrial and Specialty
2.1. Product Standards.”

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