ASTM D857-17

Standard Test Method for Aluminum in Water

SIGNIFICANCE AND USE
5.1 Although there is little information available concerning the toxicological significance of aluminum in man, the American Water Works Association has established a water quality guideline or goal of a maximum of 0.05 mg/L. Under the National Pollution Discharge Elimination System (NPDES), some permits may set aluminum discharge limits. Some evidence does exist to indicate that low levels (5 mg/L) will interfere with activated sludge processes. For the above reasons monitoring of aluminum may be desirable.  
5.2 Aluminum is monitored in boiler make-up water, where alum has been used, to determine whether aluminum is present after pretreatment. Residual aluminum may consume ion exchange capacity or consume boiler water treatment chemicals added to stoichiometrically chelate hardness ions (that is, calcium and magnesium) in boiler feed water.  
5.3 Aluminum is monitored in cooling water make-up, since its presence may result in deactivation of anionic substances in scale or corrosion inhibitor treatment chemicals, or both. Deactivation may result in decreased performance of inhibitors.  
5.4 ICP-MS may also be appropriate but at a higher instrument cost. See Test Method D5673.
SCOPE
1.1 This test method covers the direct flame atomic absorption determination of aluminum in the nitrous oxide-acetylene flame.  
1.2 This test method is applicable to waters containing dissolved and total recoverable aluminum in the range from 0.5 to 5.0 mg/L. Aluminum concentrations as high as approximately 50 mg/L can be determined using this test method without dilution. However, no precision and bias data are available for concentrations greater than 5.0 mg/L.  
1.3 This test method was tested on reagent, natural, and potable waters. It is the user's responsibility to ensure the validity of this test method for waters of untested matrices.  
1.4 The same digestion procedure may be used to determine total recoverable nickel (Test Methods D1886), chromium (Test Methods D1687), cobalt (Test Methods D3558), copper (Test Methods D1688), iron (Test Methods D1068), lead (Test Methods D3559), manganese (Test Methods D858), and zinc (Test Methods D1691).  
1.5 Precision and bias data have been obtained on reagent, natural, and potable waters. It is the responsibility of the user to ensure the validity of this test method on untested matrices.  
1.6 The values stated in SI units are to be regarded as standard. The values given in parentheses are mathematical conversion to inch-pound units that are provided for information only and are not considered standard.  
1.7 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. For specific hazard statements, see 7.5, 8.4, and Note 2.  
1.8 Former Test Methods A (Fluorometric) and B and C (Spectrophotometric) were discontinued. Refer to Appendix X1 for historical information.  
1.9 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.

General Information

• Status: Published
• Publication Date: 31-May-2017
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.05 - Inorganic Constituents in Water

Relations

• Replaces: ASTM D857-12 - Standard Test Method for Aluminum in Water
• Effective Date: 01-Jun-2017
• Refers: ASTM D3558-15(2023) - Standard Test Methods for Cobalt in Water
• Effective Date: 01-Dec-2023
• Refers: ASTM D1129-13(2020)e2 - Standard Terminology Relating to Water
• Effective Date: 01-May-2020
• Refers: ASTM D1066-18e1 - Standard Practice for Sampling Steam
• Effective Date: 01-Aug-2018
• Refers: ASTM D1066-18 - Standard Practice for Sampling Steam
• Effective Date: 01-Aug-2018
• Refers: ASTM D1691-17 - Standard Test Methods for Zinc in Water
• Effective Date: 01-Jun-2017
• Refers: ASTM D1687-17 - Standard Test Methods for Chromium in Water
• Effective Date: 01-Jun-2017
• Refers: ASTM D5673-15 - Standard Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry
• Effective Date: 01-Jul-2015
• Refers: ASTM D3559-15 - Standard Test Methods for Lead in Water (Withdrawn 2024)
• Effective Date: 01-Jun-2015
• Refers: ASTM D3558-15 - Standard Test Methods for Cobalt in Water
• Effective Date: 01-Feb-2015
• Refers: ASTM D4841-88(2013) - Standard Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents
• Effective Date: 01-Jan-2013
• Refers: ASTM D4841-88(2013)e1 - Standard Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents
• Effective Date: 01-Jan-2013
• Refers: ASTM D1691-12 - Standard Test Methods for Zinc in Water
• Effective Date: 01-Sep-2012
• Refers: ASTM D858-12 - Standard Test Methods for Manganese in Water
• Effective Date: 01-Sep-2012
• Refers: ASTM D2777-12 - Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
• Effective Date: 15-Jun-2012

Overview

ASTM D857-17: Standard Test Method for Aluminum in Water sets forth procedures for the determination of dissolved and total recoverable aluminum in water samples using direct flame atomic absorption spectroscopy (AAS) with a nitrous oxide-acetylene flame. This test method is applicable to reagent, natural, and potable waters, ensuring reliability in a variety of matrices. Monitoring aluminum concentrations is essential for compliance with regulatory guidelines and is critical for water treatment systems and industrial processes. The method covers a range of 0.5 to 5.0 mg/L, with the capability to handle higher concentrations (up to approximately 50 mg/L) without dilution, although precision and bias beyond 5.0 mg/L have not been established.

Key Topics

• Significance of Aluminum Monitoring: Although the toxicological impact of aluminum in humans is not fully defined, organizations such as the American Water Works Association recommend a maximum guideline of 0.05 mg/L in water. The test method supports compliance with water quality standards, particularly under regulatory frameworks such as the National Pollution Discharge Elimination System (NPDES).

• Sample Preparation and Analysis: The standard details sample collection, preservation, and preparation to ensure accuracy. Both dissolved and total recoverable aluminum can be measured, depending on filtration and acidification steps.

• Instrumentation and Technique: The direct flame AAS technique uses a nitrous oxide-acetylene flame and requires specific reagents and calibration protocols. Sodium chloride is used to suppress interferences, enhancing accuracy.

• Quality Control Measures: Stringent quality assurance procedures are outlined, including calibration verification, laboratory control samples, method blanks, matrix spikes, and duplicate analysis. Precision and bias must be regularly assessed to ensure compliance.

• Documented Range and Limitations: Applicability is confirmed primarily for waters with aluminum concentrations between 0.5 and 5.0 mg/L. For higher concentrations, users must verify accuracy, as official bias data do not extend beyond 5.0 mg/L.

Applications

• Drinking Water Quality Monitoring: Essential for utilities maintaining compliance with aluminum guidelines and ensuring the safety of potable water supplies.
• Industrial Water Systems: Used to monitor boiler make-up water, particularly where alum-based coagulants are applied during pretreatment. Ensures residual aluminum does not adversely affect boiler chemistry or ion exchange processes.
• Cooling Water Management: Monitoring aluminum prevents deactivation of anionic inhibitors, which could otherwise lead to scale formation or increased corrosion in industrial cooling circuits.
• Regulatory Reporting: Supports wastewater discharge monitoring and helps meet the requirements of environmental agencies by providing data necessary for NPDES permit reporting.

Related Standards

• ASTM D1886 – Test Methods for Nickel in Water
• ASTM D1687 – Test Methods for Chromium in Water
• ASTM D3558 – Test Methods for Cobalt in Water
• ASTM D1688 – Test Methods for Copper in Water
• ASTM D1068 – Test Methods for Iron in Water
• ASTM D3559 – Test Methods for Lead in Water
• ASTM D858 – Test Methods for Manganese in Water
• ASTM D1691 – Test Methods for Zinc in Water
• ASTM D5673 – Test Method for Elements in Water by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS), suggested as an alternative for increased sensitivity

Keywords: aluminum in water, ASTM D857, water quality, atomic absorption, drinking water standards, boiler water monitoring, cooling water, NPDES, environmental compliance

By following ASTM D857-17, laboratories and industry professionals can accurately measure aluminum in water to ensure system performance, meet regulatory requirements, and protect public health.

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D857 − 17
Standard Test Method for
Aluminum in Water
This standard is issued under the fixed designation D857; 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.
1. Scope* 1.9 This international standard was developed in accor-
dance with internationally recognized principles on standard-
1.1 This test method covers the direct flame atomic absorp-
ization established in the Decision on Principles for the
tion determination of aluminum in the nitrous oxide-acetylene
Development of International Standards, Guides and Recom-
flame.
mendations issued by the World Trade Organization Technical
1.2 This test method is applicable to waters containing
Barriers to Trade (TBT) Committee.
dissolvedandtotalrecoverablealuminumintherangefrom0.5
to 5.0 mg/L. Aluminum concentrations as high as approxi- 2. Referenced Documents
mately 50 mg/L can be determined using this test method
2.1 ASTM Standards:
without dilution. However, no precision and bias data are
D858 Test Methods for Manganese in Water
available for concentrations greater than 5.0 mg/L.
D1066 Practice for Sampling Steam
1.3 This test method was tested on reagent, natural, and D1068 Test Methods for Iron in Water
potable waters. It is the user’s responsibility to ensure the
D1129 Terminology Relating to Water
validity of this test method for waters of untested matrices. D1193 Specification for Reagent Water
D1687 Test Methods for Chromium in Water
1.4 The same digestion procedure may be used to determine
D1688 Test Methods for Copper in Water
total recoverable nickel (Test Methods D1886), chromium
D1691 Test Methods for Zinc in Water
(Test Methods D1687), cobalt (Test Methods D3558), copper
D1886 Test Methods for Nickel in Water
(Test Methods D1688), iron (Test Methods D1068), lead (Test
D2777 Practice for Determination of Precision and Bias of
Methods D3559), manganese (Test Methods D858), and zinc
Applicable Test Methods of Committee D19 on Water
(Test Methods D1691).
D3370 Practices for Sampling Water from Closed Conduits
1.5 Precision and bias data have been obtained on reagent,
D3558 Test Methods for Cobalt in Water
natural, and potable waters. It is the responsibility of the user
D3559 Test Methods for Lead in Water
to ensure the validity of this test method on untested matrices.
D4841 Practice for Estimation of Holding Time for Water
1.6 The values stated in SI units are to be regarded as Samples Containing Organic and Inorganic Constituents
standard. The values given in parentheses are mathematical D5673 Test Method for Elements in Water by Inductively
conversion to inch-pound units that are provided for informa- Coupled Plasma—Mass Spectrometry
tion only and are not considered standard. D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications
1.7 This standard does not purport to address all of the
for Standard Test Methods for Water Analysis
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3. Terminology
priate safety and health practices and determine the applica-
3.1 Definitions:
bility of regulatory limitations prior to use. For specific hazard
3.1.1 For definitions of terms used in this standard, refer to
statements, see 7.5, 8.4, and Note 2.
Terminology D1129.
1.8 Former Test Methods A (Fluorometric) and B and C
(Spectrophotometric) were discontinued. Refer to Appendix
3.2 Definitions of Terms Specific to This Standard:
X1 for historical information.
3.2.1 continuing calibration blank, n—a solution contain-
ing no analytes (of interest) which is used to verify blank
response and freedom from carryover.
These test methods are under the jurisdiction of ASTM Committee D19 on
Water and are the direct responsibility of Subcommittee D19.05 on Inorganic
Constituents in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved June 1, 2017. Published June 2017. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1945. Last previous edition approved in 2012 as D857 – 12. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D0857-17. the ASTM website.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D857 − 17
3.2.2 continuing calibration verification—a solution (or set levels recommended by the manufacturer of the spectropho-
of solutions) of known concentration used to verify freedom tometer. (Warning—The nitrous oxide-acetylene flame is
from excessive instrumental drift; the concentration is to cover hazardousduetoitsflash-backpotential.Followtheinstrument
the range of calibration curve. manufacturer’s recommended operating procedures closely.)
3.2.3 total recoverable aluminum, n—a descriptive term
8. Reagents and Materials
relating to the forms of aluminum recovered in the acid
8.1 Purity of Reagents—Reagent grade chemicals shall be
digestion procedure specified in this standard.
used in all tests. Unless otherwise indicated, it is intended that
4. Summary of Test Method all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society
4.1 Aluminum is determined by direct atomic absorption
where such specifications are available. Other grades may be
with only the addition of an ionization suppressor and sensi-
used, provided it is first ascertained that the reagent is of
tivity enhancer (optional).
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
5. Significance and Use
8.2 Purity of Water—Unless otherwise indicated, references
5.1 Although there is little information available concerning
towatershallbeunderstoodtomeanreagentwaterconforming
the toxicological significance of aluminum in man, theAmeri-
to Specification D1193, Type I. Other reagent water types may
can Water Works Association has established a water quality
be used, provided it is first ascertained that the water is of
guideline or goal of a maximum of 0.05 mg/L. Under the
sufficiently high purity to permit its use without lessening the
National Pollution Discharge Elimination System (NPDES),
bias and precision of the determination. Type II water was
some permits may set aluminum discharge limits. Some
specified at the time of round-robin testing of this test method.
evidence does exist to indicate that low levels (5 mg/L) will
interfere with activated sludge processes. For the above rea- 8.3 Aluminum Solution, Standard (1 mL = 0.1 mg Al)—
sons monitoring of aluminum may be desirable. Dissolve 1.758 g of aluminum potassium sulfate
(AlK(SO ) ·12H O) in water. Add 1 mL of nitric acid and
4 2 2
5.2 Aluminum is monitored in boiler make-up water, where
dilute to 1 L. A purchased aluminum stock solution of
alum has been used, to determine whether aluminum is present
appropriate known purity is also acceptable.
after pretreatment. Residual aluminum may consume ion
exchange capacity or consume boiler water treatment chemi- 8.4 Bis-(2-Ethoxyethyl) Ether. (Warning—Avoid inhala-
cals added to stoichiometrically chelate hardness ions (that is, tion. Perform all manipulation in a well-ventilated hood. This
calcium and magnesium) in boiler feed water. ether can form dangerous peroxides and should be inspected
regularly for their presence.)
5.3 Aluminumismonitoredincoolingwatermake-up,since
its presence may result in deactivation of anionic substances in 8.5 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
scale or corrosion inhibitor treatment chemicals, or both. chloric acid (HCl).
Deactivation may result in decreased performance of inhibi-
8.6 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
tors.
(HNO ).
5.4 ICP-MS may also be appropriate but at a higher instru-
8.7 Sodium Chloride Solution (25.4 g/L)—Dissolve 25.4 g
ment cost. See Test Method D5673.
of sodium chloride (NaCl) in water and dilute to 1 L.
8.8 Oxidant:
6. Interferences
8.8.1 Air, which has been suitably dried and filtered, is used
6.1 Aluminum ionizes slightly in the nitrous oxide-
to support combustion before switching to nitrous oxide.
acetylene flame, but the addition of sodium chloride described
8.8.2 Nitrous Oxide is the required oxidant.
in this test method suppresses this interference. By this
8.9 Fuel—Standard commercially available acetylene is the
technique, a maximum concentration of 9000 mg/L sodium,
required fuel. The cylinder should be replaced at a gage
9000 mg/L potassium, 4000 mg/L calcium, 4000 mg/L
pressure of 517 kPa (75 psi) to minimize the carry-over of
magnesium, 9000 mg/L sulfate, 9000 mg/L chloride, 9000
acetone. Since “purified” grades contain a solvent that softens
mg/L nitrate, and 9000 mg/L iron may be tolerated.
poly(vinyl chloride) tubing, its use constitutes a safety hazard
and is not recommended.
7. Apparatus
8.10 Filter Paper—Purchase suitable filter paper. Typically
7.1 Atomic Absorption Spectrophotometer, for use at 309.3
the filter papers have a pore size of 0.45-µm membrane.
nm.
Material such as fine-textured, acid-washed, ashless paper, or
7.2 Aluminum Hollow-Cathode Lamp—Multielement lamps
are not recommended.
Reagent Chemicals, American Chemical Society Specifications, American
7.3 Oxidant—See 8.8.
Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
7.4 Fuel—See 8.9. listed by the American Chemical Society, see Annual Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
7.5 Pressure-Reducing Regulators—The supplies of fuel
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
and oxidant should be reduced by suitable regulators to the MD.
D857 − 17
TABLE 1 Overall (S ) and Single-Operator (S ) Interlaboratory
glass fiber paper are acceptable. The user must first ascertain
T o
Precision for Aluminum by Direct AAS
that the filter paper is of sufficient purity to use without
Reagent Water:
adversely affecting the bias and precision of the test method.
Concentration (X), mg/L 0.848 2.54 4.11
S 0.167 0.19 0.19
T
9. Sampling
S 0.128 0.18 0.23
o
Natural Water:
9.1 Collect samples in accordance with Practices D1066 or
Concentration (X), mg/L 0.772 2.48 4.07
D3370, as applicable. For dissolved aluminum, filter the
S 0.194 0.19 0.21
T
S 0.166 0.16 0.28
o
samples at the time of collection through a 0.45-µm filter
(8.10).Acidify the filtrate to pH 2 or less with nitric acid (8.6).
For total recoverable aluminum, acidify the unfiltered sample
to pH 2 or less at the time of collection. The holding time for
NOTE 2—For brines and samples with high levels of suspended matter,
samples may be calculated in accordance with Practice D4841.
the amount of reduction in volume is left to the discretion of the analyst.
NOTE 3—Many laboratories have found block digestion systems a
NOTE 1—Alternatively, the pH may be adjusted in the laboratory within
useful way to digest samples for trace metals analysis. Systems typically
14 days of collection. However, acid must be added at least 24 hours
consist of either a metal or graphite block with wells to hold digestion
before analysis to dissolve any metals that adsorb to the container walls.
tubes. The block temperature controller must be able to maintain unifor-
This could reduce hazards of working with acids in the field when
mity of temperature across all positions of the block. The digestion block
appropriate.
must be capable of maintaining a temperature between 65°C and 95°C.
For trace metals analysis, the digestion tubes should be constructed of
9.2 An effective way to clean glassware is to soak all
polypropylene and have a volume accuracy of at least 0.5 %. All lots of
glasswareinhotHCl(1 + 1)for2h.Drainandrinsewithwater
tubes should come with a certificate of analysis to demonstrate suitability
or reagent.
for their intended purpose.
12.5 Cool and, if necessary, filter the samples through a
10. Preparation of Apparatus
filter (fine-texture, acid-washed, ashless paper) into a 100-mL
10.1 An effective way to clean glassware is to soak all
volumetric flask. Wash the paper several times and bring the
glasswareinhotHCl(1 + 1)for2h.Drainandrinsewithwater
volume to 100-mL.
or reagent.
12.6 To a 10-mLaliquot of sample add 1.0 mLof NaCl and
mix thoroughly. If 1 mL of bis–(2–ethoxyethyl) ether was
11. Calibration and Standardization
added to the blank and standards as a sensitivity enhancer
11.1 Prepare aluminum standards in the range from 0.0 to
(11.2), an equal amount must be added to each sample.
5.0 mg/L by dilution of the aluminum standard solution (see
12.7 Atomize each of the standards, samples, and blank and
8.3) with water. It is the responsibility of the user to ensure the
determine its absorbance or concentration. Atomize water
validity of this test method for concentrations if the range is
between samples.
extended.
11.2 Add 1.0 mL of NaCl solution (8.7) to 10.0 mL of
13. Calculation
standard and mix thoroughly. If very low concentrations of
13.1 Determine the concentration of aluminum in each
aluminum are anticipated in the samples, 1 mL of bis-
sample by referring to the calibration curve in 13.3.
(2–ethoxyethyl)(8.4)ethermaybeaddedtotheblankandeach
Alternatively,calibratethespectrophotometerandreaddirectly
standard, which will act as a sensitivity enhancer. If this
in concentration mode.
sensitivity enhancer is used, it must also be added to each
13.2 Calculate the concentration of total recoverable alumi-
sample (12.6).
num in milligrams per litre using Eq 1:
11.3 Read directly in concentration if this capability is
Aluminum, mg/L 5 C 3 100/V (1)
provided with the instrument or measure the absorbance of the ~ !
standards and construct an analytical curve by plotting the
where:
absorbance of the standards versus the concentration of alumi-
C = concentration from curve, mg/L, and
num.
V = volume of aliquot, mL.
12. Procedure 13.3 Calculate the concentration of d
...

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: D857 − 12 D857 − 17
Standard Test Method for
Aluminum in Water
This standard is issued under the fixed designation D857; 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.
1. Scope*
1.1 This test method covers the direct flame atomic absorption determination of aluminum in the nitrous oxide-acetylene flame.
1.2 This test method is applicable to waters containing dissolved and total recoverable aluminum in the range from 0.5 to 5.0
mg/L. Aluminum concentrations as high as approximately 50 mg/L can be determined using this test method without dilution.
However, no precision and bias data are available for concentrations greater than 5.0 mg/L.
1.3 This test method was tested on reagent, natural, and potable waters. It is the user’s responsibility to ensure the validity of
this test method for waters of untested matrices.
1.4 The same digestion procedure may be used to determine total recoverable nickel (Test Methods D1886), chromium (Test
Methods D1687), cobalt (Test Methods D3558), copper (Test Methods D1688), iron (Test Methods D1068), lead (Test
MethodMethods D3559), manganese (Test MethodMethods D858), and zinc (Test Methods D1691).
1.5 Precision and bias data have been obtained on reagent, natural, and potable waters. It is the responsibility of the user to
ensure the validity of this test method on untested matrices.
1.6 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values statedgiven
in each system are mathematical conversions and may not be exact equivalents; therefore, each system shall be used independently
of the other.parentheses are mathematical conversion to inch-pound units that are provided for information only and are not
considered standard.
1.7 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. For specific hazard statements, see Note 17.5, Note 28.4, and Note 42.
1.8 Former Test Methods A (Fluorometric) and B and C (Spectrophotometric) were discontinued. Refer to Appendix X1 for
historical information.
1.9 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.
2. Referenced Documents
2.1 ASTM Standards:
D858 Test Methods for Manganese in Water
D1066 Practice for Sampling Steam
D1068 Test Methods for Iron in Water
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D1687 Test Methods for Chromium in Water
D1688 Test Methods for Copper in Water
D1691 Test Methods for Zinc in Water
D1886 Test Methods for Nickel in Water
These test methods are under the jurisdiction of ASTM Committee D19 on Water and are the direct responsibility of Subcommittee D19.05 on Inorganic Constituents
in Water.
Current edition approved Sept. 1, 2012June 1, 2017. Published September 2012June 2017. Originally approved in 1945. Last previous edition approved in 20072012 as
ε1
D857 – 07D857 – 12. . DOI: 10.1520/D0857-12.10.1520/D0857-17.
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.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D857 − 17
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Closed Conduits
D3558 Test Methods for Cobalt in Water
D3559 Test Methods for Lead in Water
D4841 Practice for Estimation of Holding Time for Water Samples Containing Organic and Inorganic Constituents
D5673 Test Method for Elements in Water by Inductively Coupled Plasma—Mass Spectrometry
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications for Standard Test Methods for Water Analysis
3. Terminology
3.1 Definitions— For definitions of terms used in these test methods, refer to Terminology D1129.
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 continuing calibration blank, n—a solution containing no analytes (of interest) which is used to verify blank response and
freedom from carryover.
3.2.2 continuing calibration verification—a solution (or set of solutions) of known concentration used to verify freedom from
excessive instrumental drift; the concentration is to cover the range of calibration curve.
3.2.3 total recoverable aluminum, n—an arbitrarya descriptive term relating to the forms of aluminum recovered in the acid
digestion procedure specified in this test method.standard.
4. Summary of Test Method
4.1 Aluminum is determined by direct atomic absorption with only the addition of an ionization suppressor and sensitivity
enhancer (optional).
5. Significance and Use
5.1 Although there is little information available concerning the toxicological significance of aluminum in man, the American
Water Works Association has established a water quality guideline or goal of a maximum of 0.05 mg/L. Under the National
Pollution Discharge Elimination System (NPDES), some permits may set aluminum discharge limits. Some evidence does exist
to indicate that low levels (5 mg/L) will interfere with activated sludge processes. For the above reasons monitoring of aluminum
may be desirable.
5.2 Aluminum is monitored in boiler make-up water, where alum has been used, to determine whether aluminum is present after
pretreatment. Residual aluminum may consume ion exchange capacity or consume boiler water treatment chemicals added to
stoichiometrically chelate hardness ions (that is, calcium and magnesium) in boiler feed water.
5.3 Aluminum is monitored in cooling water make-up, since its presence may result in deactivation of anionic substances in
scale or corrosion inhibitor treatment chemicals, or both. Deactivation may result in decreased performance of inhibitors.
5.4 ICP-MS may also be appropriate but at a higher instrument cost. See Test Method D5673.
6. Interferences
6.1 Aluminum ionizes slightly in the nitrous oxide-acetylene flame, but the addition of sodium chloride described in this test
method suppresses this interference. By this technique, a maximum concentration of 9000 mg/L sodium, 9000 mg/L potassium,
4000 mg/L calcium, 4000 mg/L magnesium, 9000 mg/L sulfate, 9000 mg/L chloride, 9000 mg/L nitrate, and 9000 mg/L iron may
be tolerated.
7. Apparatus
7.1 Atomic Absorption Spectrophotometer, for use at 309.3 nm.
7.2 Aluminum Hollow-Cathode Lamp—Multielement lamps are not recommended.
7.3 Oxidant—See 8.8.
7.4 Fuel—See 8.9.
7.5 Pressure-Reducing Regulators—The supplies of fuel and oxidant should be reduced by suitable regulators to the levels
recommended by the manufacturer of the spectrophotometer. (Warning—The nitrous oxide-acetylene flame is hazardous due to
its flash-back potential. Follow the instrument manufacturer’s recommended operating procedures closely.)
NOTE 1—Warning: The nitrous oxide-acetylene flame is hazardous due to its flash-back potential. Follow the instrument manufacturer’s recommended
operating procedures closely.
D857 − 17
8. Reagents and Materials
8.1 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.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Specification D1193, Type I. Other reagent water types may be used, provided it is first ascertained that the water is of sufficiently
high purity to permit its use without lessening the bias and precision of the determination. Type II water was specified at the time
of round-robin testing of this test method.
8.3 Aluminum Solution, Standard (1 mL = 0.1 mg Al)—Dissolve 1.758 g of aluminum potassium sulfate (AlK(SO ) ·12H O)
4 2 2
in water. Add 1 mL of nitric acid and dilute to 1 L. A purchased aluminum stock solution of appropriate known purity is also
acceptable.
8.4 Bis-(2-Ethoxyethyl) Ether.
NOTE 2—Warning: Avoid inhalation. Perform all manipulation in a well-ventilated hood. This ether can form dangerous peroxides and should be
inspected regularly for their presence.(Warning—Avoid inhalation. Perform all manipulation in a well-ventilated hood. This ether can
form dangerous peroxides and should be inspected regularly for their presence.)
8.5 Hydrochloric Acid (sp gr 1.19)—Concentrated hydrochloric acid (HCl).
8.6 Nitric Acid (sp gr 1.42)—Concentrated nitric acid (HNO ).
8.7 Sodium Chloride Solution (25.4 g/L)—Dissolve 25.4 g of sodium chloride (NaCl) in water and dilute to 1 L.
8.8 Oxidant:
8.8.1 Air, which has been suitably dried and filtered, is used to support combustion before switching to nitrous oxide.
8.8.2 Nitrous Oxide is the required oxidant.
8.9 Fuel—Standard commercially available acetylene is the required fuel. The cylinder should be replaced at a gage pressure
of 517 kPa (75 psi) to minimize the carry-over of acetone. Since “purified” grades contain a solvent that softens poly(vinyl
chloride) tubing, its use constitutes a safety hazard and is not recommended.
8.10 Filter Paper—Purchase suitable filter paper. Typically the filter papers have a pore size of 0.45-μm membrane. Material
such as fine-textured, acid-washed, ashless paper, or glass fiber paper are acceptable. The user must first ascertain that the filter
paper is of sufficient purity to use without adversely affecting the bias and precision of the test method.
9. Sampling
9.1 Collect samples in accordance with Practices D1066 or D3370, as applicable. For dissolved aluminum, filter the samples
at the time of collection through a 0.45-μm filter. filter (8.10). Acidify the filtrate to pH 2 or less with nitric acid. acid (8.6). For
total recoverable aluminum, acidify the unfiltered sample to pH 2 or less at the time of collection. The holding time for samples
may be calculated in accordance with Practice D4841.
NOTE 1—Alternatively, the pH may be adjusted in the laboratory if the sample is returned within 14 days. within 14 days of collection. However, acid
must be added at least 24 hours before analysis to dissolve any metals that adsorb to the container walls. This could reduce hazards of working with acids
in the field when appropriate.
9.2 Soak An effective way to clean glassware is to soak all glassware in hot HCl (1 + 1) for 2 h. Drain and rinse at least five
times with water. Drain and flush with methyl alcohol, ethyl alcohol, or isopropyl alcohol.with water or reagent.
10. Preparation of Apparatus
10.1 Soak An effective way to clean glassware is to soak all glassware in hot HCl (1 + 1) for 2 h. Drain and rinse at least five
times with water. Drain and flush with methyl alcohol, ethyl alcohol, or isopropyl alcohol.with water or reagent.
11. Calibration and Standardization
11.1 Prepare aluminum standards in the range from 0.0 to 5.0 mg/L by dilution of the aluminum standard solution (see 8.3) with
water. It is the responsibility of the user to ensure the validity of this test method for concentrations if the range is extended.
11.2 Add 1.0 mL of NaCl solution (8.7) to 10.0 mL of standard and mix thoroughly. If very low concentrations of aluminum
are anticipated in the samples, 1 mL of bis-(2–ethoxyethyl) (8.4) ether may be added to the blank and each standard, which will
act as a sensitivity enhancer. If this sensitivity enhancer is used, it must also be added to each sample (12.6).
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 Annual 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.
D857 − 17
TABLE 1 Overall (S ) and Single-Operator (S ) Interlaboratory
T o
Precision for Aluminum by Direct AAS
Reagent Water:
Concentration (X), mg/L 0.848 2.54 4.11
S 0.167 0.19 0.19
T
S 0.128 0.18 0.23
o
Natural Water:
Concentration (X), mg/L 0.772 2.48 4.07
S 0.194 0.19 0.21
T
S 0.166 0.16 0.28
o
11.3 Measure the Read directly in concentration if this capability is provided with the instrument or measure the absorbance of
the standards and construct an analytical curve by plotting the absorbance of the standards versus the concentration of aluminum.
Alternatively, calibrate the spectrophotometer and read directly in concentration.
12. Procedure
12.1 If dissolved aluminum is to be determined proceed to 12.6.
12.2 Measure a volume of well-mixed acidified sample containing less than 0.5 mg of aluminum (100 mL maximum) into a
125-mL beaker.
12.3 Add 0.5 mL of HNO and 5 mL of HCl.
12.4 Heat the samples (between 65°C and 95°C) on a hot plate below boiling in a well-ventilated hood until the volume has
been reduced to 10 to 15 mL, making certain the samples do not boil.
NOTE 2—For brines and samples with high levels of suspended matter, the amount of reduction in volume is left to the discretion of the analyst.
NOTE 3—Many laboratories have found block digestion systems a useful way to digest samples for trace metals analysis. Systems typically consist of
either a metal or graphite block with wells to hold digestion tubes. The block temperature controller must be able to maintain uniformity of temperature
across all positions of the block. The digestion block must be capable of maintaining a temperature between 65°C and 95°C. For trace metals analysis,
the digestion tubes should be constructed of polypropylene and have a volume accuracy of at least 0.5%. 0.5 %. All lots of tubes should come with a
certificate of analysis to demonstrate suitability for their intended purpose.
12.5 Cool and, if necessary, filter the samples through a filter (fine-texture, acid-washed, ashless paper) into a 100-mL
volumetric flask. Wash the paper several times and bring the volume to 100-mL.
12.6 To a 10-mL aliquot of sample add 1.0 mL of NaCl and mix thoroughly. If 1 mL of bis–(2–ethoxyethyl) ether was added
to the blank and standards as a sensitivity enhancer (11.2),(11.2), an equal am
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