ASTM D1886-14(2021)e1
(Test Method)Standard Test Methods for Nickel in Water
Standard Test Methods for Nickel in Water
SIGNIFICANCE AND USE
4.1 Elemental constituents in potable water, receiving water, and wastewater need to be identified for support of effective pollution control programs. Test Methods A, B, and C provide the techniques necessary to make such measurements.
4.2 Nickel is considered to be relatively nontoxic to man and a limit for nickel is not included in the EPA National Interim Primary Drinking Water Regulations.6 The toxicity of nickel to aquatic life indicates tolerances that vary widely and that are influenced by species, pH, synergistic effects, and other factors.
4.3 Nickel is a silver-white metallic element seldom occur-ring in nature in the elemental form. Nickel salts are soluble and can occur as a leachate from nickel-bearing ores. Nickel salts are used in metal-plating and may be discharged to surface or ground waters.
SCOPE
1.1 These test methods 2, 3, 4 cover the atomic absorption determination of nickel in water and wastewaters. Three test methods are given as follows:
Concentration
Range
Sections
Test Method A—Atomic Absorption, Direct
0.1 to 10 mg/L
7 – 16
Test Method B—Atomic Absorption, Chelation-Extraction
10 to 1000 μg/L
17 – 26
Test Method C—Atomic Absorption, Graphite Furnace
5 to 100 μg/L
27 – 36
1.2 Test Methods A, B, and C have been used successfully with reagent grade water and natural waters. Evaluation of Test Method C was also made in condensate from a medium Btu coal gasification process. It is the user's responsibility to ensure the validity of these test methods for other matrices.
1.3 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.
1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazards statements, see Note 5, 11.8.1, 21.11, 23.7, and 23.10.
1.5 Two former colorimetric test methods were discontinued. Refer to Appendix X1 for historical information.
1.6 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
Relations
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.
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Designation: D1886 − 14 (Reapproved 2021)
Standard Test Methods for
Nickel in Water
This standard is issued under the fixed designation D1886; 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.
ε NOTE—The WTO caveat was editorially added in November 2021.
1. Scope 1.6 This international standard was developed in accor-
2, 3, 4 dance with internationally recognized principles on standard-
1.1 These test methods cover the atomic absorption
ization established in the Decision on Principles for the
determination of nickel in water and wastewaters. Three test
Development of International Standards, Guides and Recom-
methods are given as follows:
mendations issued by the World Trade Organization Technical
Concentration
Barriers to Trade (TBT) Committee.
Range Sections
Test Method A—Atomic Absorption,
2. Referenced Documents
Direct 0.1 to 10 mg/L 7–16
Test Method B—Atomic Absorption,
2.1 ASTM Standards:
Chelation-Extraction 10 to 1000 µg/L 17–26
Test Method C—Atomic Absorption, D858 Test Methods for Manganese in Water
Graphite Furnace 5 to 100 µg/L 27–36
D1066 Practice for Sampling Steam
1.2 Test Methods A, B, and C have been used successfully
D1068 Test Methods for Iron in Water
with reagent grade water and natural waters. Evaluation ofTest
D1129 Terminology Relating to Water
Method C was also made in condensate from a medium Btu
D1193 Specification for Reagent Water
coal gasification process. It is the user’s responsibility to
D1687 Test Methods for Chromium in Water
ensure the validity of these test methods for other matrices.
D1688 Test Methods for Copper in Water
D1691 Test Methods for Zinc in Water
1.3 The values stated in SI units are to be regarded as
D2777 Practice for Determination of Precision and Bias of
standard. The values given in parentheses are mathematical
Applicable Test Methods of Committee D19 on Water
conversion to inch-pound units that are provided for informa-
D3370 Practices for Sampling Water from Flowing Process
tion only and are not considered standard.
Streams
1.4 This standard does not purport to address all of the
D3557 Test Methods for Cadmium in Water
safety concerns, if any, associated with its use. It is the
D3558 Test Methods for Cobalt in Water
responsibility of the user of this standard to establish appro-
D3559 Test Methods for Lead in Water
priate safety, health, and environmental practices and deter-
D3919 Practice for Measuring Trace Elements in Water by
mine the applicability of regulatory limitations prior to use.
Graphite Furnace Atomic Absorption Spectrophotometry
Forspecifichazardsstatements,seeNote5,11.8.1,21.11,23.7,
D4841 Practice for Estimation of Holding Time for Water
and 23.10.
Samples Containing Organic and Inorganic Constituents
1.5 Two former colorimetric test methods were discontin-
D5673 Test Method for Elements in Water by Inductively
ued. Refer to Appendix X1 for historical information.
Coupled Plasma—Mass Spectrometry
D5810 Guide for Spiking into Aqueous Samples
D5847 Practice for Writing Quality Control Specifications
These test methods are under the jurisdiction of ASTM Committee D19 on
for Standard Test Methods for Water Analysis
Water and are the direct responsibility of Subcommittee D19.05 on Inorganic
Constituents in Water.
3. Terminology
Current edition approved Nov. 1, 2021. Published November 2021. Originally
approved in 1961. Last previous edition approved in 2014 as D1886 – 14. DOI:
3.1 Definitions:
10.1520/D1886-14R21E01.
3.1.1 For definitions of terms used in this standard, refer to
Chilton, J. M., “Simultaneous Colorimetric Determination of Copper, Cobalt,
and Nickel as Diethyldithiocarbamates,” Analytical Chemistry, Vol 25, 1953, pp.
Terminology D1129.
1274–1275.
Platte, J.A., and Marcy,V. M., “ANewTool for theWater Chemist,” Industrial
Water Engineering, May 1965. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Brown,E.,Skougstad,M.W.,andFishman,M.J.,“MethodsforCollectionand contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Analysis of Water Samples for Dissolved Minerals and Gases,” Techniques of Standards volume information, refer to the standard’s Document Summary page on
Water-ResourcesInvestigationsoftheU.S.GeologicalSurvey,Book5,1970,p.115. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D1886 − 14 (2021)
3.2 Definitions of Terms Specific to This Standard: before acidification. The holding time for samples may be
3.2.1 total recoverable nickel, n—adescriptivetermrelating calculated in accordance with Practice D4841.
to the nickel forms recovered in the acid-digestion procedure
NOTE 1—Alternatively, the pH may be adjusted in the laboratory if the
specified in these test methods.
sample is returned within 14 days. However, acid must be added at least
24hoursbeforeanalysistodissolveanymetalsthatadsorbtothecontainer
4. Significance and Use walls. This could reduce hazards of working with acids in the field when
appropriate.
4.1 Elementalconstituentsinpotablewater,receivingwater,
and wastewater need to be identified for support of effective
TEST METHOD A—ATOMIC ABSORPTION, DIRECT
pollution control programs. Test MethodsA, B, and C provide
7. Scope
the techniques necessary to make such measurements.
7.1 This test method covers the determination of dissolved
4.2 Nickel is considered to be relatively nontoxic to man
and total recoverable nickel and has been used successfully
and a limit for nickel is not included in the EPA National
6 with reagent water, tap water, river water, lake water, ground
Interim Primary Drinking Water Regulations. The toxicity of
water, a refinery effluent, and a wastewater.
nickel to aquatic life indicates tolerances that vary widely and
thatareinfluencedbyspecies,pH,synergisticeffects,andother 7.2 This test method is applicable in the range from 0.1 to
factors. 10 mg/L of nickel. The range may be extended upward by
dilution of the sample.
4.3 Nickel is a silver-white metallic element seldom occur-
ring in nature in the elemental form. Nickel salts are soluble
8. Summary of Test Method
and can occur as a leachate from nickel-bearing ores. Nickel
8.1 Nickel is determined by atomic absorption spectropho-
salts are used in metal-plating and may be discharged to
tometry. Dissolved nickel is determined by aspirating the
surface or ground waters.
filtered sample directly with no pretreatment.Total recoverable
nickel is determined by aspirating the sample following
5. Purity of Reagents
hydrochloric-nitric acid digestion and filtration. The same
5.1 Reagent grade chemicals shall be used in all tests.
digestion procedure is used for cadmium (Test Methods
Unless otherwise indicated, it is intended that all reagents shall
D3557), chromium (Test Methods D1687), cobalt (Test Meth-
conform to the specifications of the Committee on Analytical
odsD3558),copper(TestMethodsD1688),iron(TestMethods
Reagents of the American Chemical Society where such
D1068), lead (Test Methods D3559), manganese (Test Meth-
specifications are available. Other grades may be used, pro-
ods D858), and zinc (Test Methods D1691).
vided it is first ascertained that the reagent is of sufficiently
9. Interferences
high purity to permit its use without lessening the accuracy of
the determination.
9.1 Sodium, potassium, sulfate, and chloride (9000 mg/L
each), calcium, magnesium and iron (4000 mg/L each), nitrate
5.2 Purity of Water—Unless otherwise indicated, references
(2000 mg/L), and cadmium, lead, copper, zinc, cobalt, and
towatershallbeunderstoodtomeanreagentwaterconforming
chromium (10 mg/L each) do not interfere.
to Specification D1193, Type I. Other reagent water types may
be used, provided it is first ascertained that the water is of
NOTE 2—Background correction by techniques such as a continuum
sufficiently high purity to permit its use without lessening the
source, nonabsorbing lines, or chelation-extraction, may be necessary for
bias and precision of the determination. Type II water was low levels of nickel for some types of water. Instrument manufacturer’s
instructions for use of the specific correction technique should be
specified at the time of the round-robin testing of this test
followed.
method.
10. Apparatus
6. Sampling
10.1 Atomic Absorption Spectrophotometer, for use at 232.0
6.1 Collect the sample in accordance with Practice D1066
nm.
or Practices D3370, as applicable.
NOTE 3—The manufacturer’s instructions should be followed for all
6.2 Samples shall be preserved with HNO (sp gr 1.42) to a
instrumental parameters.Wavelengths other than 232.0 nm may be used if
they have been determined to be equally suitable.
pH of 2 or less immediately at the time of collection, normally
about 2 mL/L. If only dissolved nickel is to be determined, the
10.2 Nickel Hollow-Cathode Lamp—Multielement hollow-
sample shall be filtered through a 0.45-µm membrane filter
cathode lamps are available and also have been found satis-
factory.
10.3 Pressure-Reducing Valves—The supplies of fuel and
EPAPublication No. EPA-570/9-76-003 was originally published in 1976, and
oxidant shall be maintained at pressures somewhat higher than
amended in 1980. Contact the Environmental Protection Agency, 401 “M” ST.,
the controlled operating pressure of the instrument by suitable
S.W., Washington, DC 20406 for availability.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and valves.
Standard-Grade Reference Materials, American Chemical Society, Washington,
DC. For suggestions on the testing of reagents not listed by theAmerican Chemical 11. Reagents and Materials
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
11.1 Filter Paper—Purchase suitable filter paper. Typically
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
copeial Convention, Inc. (USPC), Rockville, MD. the filter papers have a pore size of 0.45-µm membrane.
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D1886 − 14 (2021)
TABLE 1 Precision and Concentration, Direct Aspiration
Material such as fine-textured, acid-washed, ashless paper, or
(Test Method A)
glass fiber paper are acceptable. The user must first ascertain
Reagent Water:
that the filter paper is of sufficient purity to use without
¯
Concentration (X), mg/L 7.74 0.84 3.93
adversely affecting the bias and precision of the test method.
S 0.502 0.102 0.383
T
S 0.261 0.045 0.324
O
11.2 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
Natural Water:
chloric acid (HCl).
¯
Concentration (X), mg/L 7.74 0.84 3.87
S 0.629 0.108 0.401
T
NOTE 4—If a high reagent blank is obtained, distill the HCl or use a
S 0.420 0.067 0.192
O
spectrograde acid.
NOTE 5—When HCl is distilled, an azeotropic mixture is formed (;6N
HCl). Therefore, whenever concentrated HCl is used in the preparation of
reagents or in the procedure, use twice the volume of the distilled HCl.
12.4 Read directly in concentration if this capability is
11.3 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
provided with the instrument or prepare an analytical curve by
(HNO ).
plotting the absorbance versus the concentration for each
standard on linear graph paper or use a computer.
NOTE 6—If a high reagent blank is obtained, distill the HNO or use a
spectrograde acid.
13. Procedure
11.4 Nitric Acid (1 + 499)—Add 1 volume HNO (sp gr
13.1 Measure 100.0 mL of a well-mixed acidified sample
1.42) to 499 volumes of water.
into a 125-mL beaker or flask.
11.5 Nickel Solution, Stock (1.0 mL = 1.0 mg Ni)—
Commerciallypurchaseordissolve4.953gofnickelousnitrate NOTE 7—If only dissolved nickel is to be determined, start with 13.5.
[Ni(NO ) ·6H O] in a mixture of 10 mL of HNO (sp gr 1.42)
3 2 2 3
13.2 Add 5 mL of HCl (sp gr 1.19) (11.2) to each sample.
and 100 mL of water. Dilute to 1 L with water. A purchased
13.3 Heat the samples on a steam bath or hotplate in a
nickelstocksolutionofappropriateknownpurityisacceptable.
well-ventilated fume hood until the volume has been reduced
11.6 Nickel Solution, Standard (1 mL = 0.1 mg Ni)—Dilute
to 15 to 20 mL, making certain that the samples do not boil.
100.0 mL of the stock nickel solution and 1 mL of HNO to 1
NOTE8—Forsampleswithhighlevelsofsuspendedmatterordissolved
L with water.
solids, the amount of reduction in volume is left to the discretion of the
analyst.
11.7 Oxidant:
NOTE 9—Many laboratories have found block digestion systems a
11.7.1 Air, which has been passed through a suitable filter to
useful way to digest samples for trace metals analysis. Systems typically
remove oil, water, and other foreign substances is the usual
consist of either a metal or graphite block with wells to hold digestion
oxidant.
tubes. The block temperature controller must be able to maintain unifor-
mity of temperature (65°C to 85°C) across all positions of the block. For
11.8 Fuel:
trace metals analysis, the digestion tubes should be constructed of
11.8.1 Acetylene—Standard, commercially available acety-
polypropylene and have a volume accuracy of at least 0.5 %. All lots of
lene is the usual fuel. Acetone, always present in acetylene tubes should come with a certificate of analysis to demonstrate suitability
for their intended purpose.
cylinders, can affect analytical results. The cylinder should be
replaced at 345 kPa (50 psig). (Warning—“Purified” grade
13.4 Cool and filter the samples through a suitable filter
acetylene containing a special proprietary solvent rather than
(11.1), such as fine-textured, acid-washed, ashless paper, into
acetone should not be used with poly(vinyl chloride) tubing as
100-mL volumetric flasks. Wash the filter paper two or three
weakening of the walls can cause a potentially hazardous
times with water and bring filtrate to volume.
situation.)
13.5 Atomize each filtered and acidified sample and deter-
mineitsabsorbanceorconcentration.AtomizeHNO (1 + 499)
12. Standardization
between samples.
12.1 Prepare a blank and at least four standard solutions to
14. Calculation
bracket the expected nickel concentration range of the samples
to be analyzed by diluting the standard nickel solution with
14.1 Calculatetheconcentrationofnickelineachsample,in
HNO (1 + 499) as described in 11.6. Prepare the standards
milligrams per litre, using 12.4.
(100mL)eachtimethetestistobeperformedorasdetermined
by Practice D4841.
15. Precision and Bias
12.2
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