ASTM D1886-14(2021)e1

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

• Status: Published
• Publication Date: 31-Oct-2021
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.05 - Inorganic Constituents in Water

Relations

• 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 D1066-18 - Standard Practice for Sampling Steam
• Effective Date: 01-Aug-2018
• Refers: ASTM D1066-18e1 - Standard Practice for Sampling Steam
• Effective Date: 01-Aug-2018
• Refers: ASTM D1687-17 - Standard Test Methods for Chromium in Water
• Effective Date: 01-Jun-2017
• Refers: ASTM D1691-17 - Standard Test Methods for Zinc in Water
• Effective Date: 01-Jun-2017
• Refers: ASTM D3557-17 - Standard Test Methods for Cadmium 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)e1 - 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) - 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 D3557-12 - Standard Test Methods for Cadmium in Water
• Effective Date: 01-Sep-2012

Overview

ASTM D1886-14(2021)e1 details standard test methods for determining nickel content in potable water, receiving water, and wastewater. Developed by ASTM International, this standard outlines three atomic absorption spectrophotometry methods, crucial for environmental monitoring and water quality compliance. By accurately quantifying nickel, stakeholders ensure effective pollution control and safety for aquatic life, supporting regulatory frameworks and environmental management.

Nickel, a silver-white metal, typically occurs in water as dissolved salts and can enter water systems through natural leaching from ores or industrial processes such as metal plating. While considered relatively nontoxic to humans, nickel’s toxicity varies among aquatic species, making reliable detection methodologies in water critical for ecological risk assessments.

Key Topics

• Test Methods

  • Test Method A: Atomic Absorption, Direct
    Suitable for nickel concentrations ranging from 0.1 to 10 mg/L.
  • Test Method B: Atomic Absorption, Chelation-Extraction
    Detects lower concentrations (10 to 1,000 μg/L) using a chelating extraction step.
  • Test Method C: Atomic Absorption, Graphite Furnace
    Highly sensitive, covering 5 to 100 μg/L; evaluated successfully in various water matrices.

• Application Ranges
  These methods are effective for reagent-grade water, natural waters, and select industrial samples, emphasizing their versatility for routine water analysis.

• Nickel in Water

  • Found as dissolved or total recoverable forms.
  • Origins include leaching from soils, corrosion of pipes, and direct industrial discharges.

• Environmental Significance

  • Essential for pollution control and compliance with environmental programs.
  • Nickel standards are not included in some national drinking water regulations but remain important for tracking aquatic toxicity and industrial discharge.

• Sample Handling and Quality Control
  The standard stresses rigorous sampling, preservation, and quality control practices to ensure accuracy, including:

  • Use of reagent-grade chemicals and high-purity water.
  • Preservation of acidified samples and filtration protocols.
  • Method validation, calibration, blanks, laboratory control samples, and matrix spike recoveries.

Applications

• Regulatory Compliance

  • Used by laboratories and environmental agencies to support compliance with water quality regulations and industry permits.
  • Enables municipalities and utilities to monitor trace metal contaminants, supporting safe public water supplies and environmental stewardship.

• Industrial and Environmental Monitoring

  • Applicable in effluent monitoring for facilities such as metal plating plants and industries discharging nickel-bearing waste.
  • Supports assessment of environmental impacts in surface and groundwater studies.

• Research and Risk Assessment

  • Facilitates studies on nickel’s ecological effects, bioavailability, and toxicity in diverse aquatic systems.
  • Used in academic, governmental, and private research settings for data collection and analysis.

Related Standards

• ASTM D858 - Test Methods for Manganese in Water
• ASTM D1068 - Test Methods for Iron in Water
• ASTM D1687 - Test Methods for Chromium in Water
• ASTM D1688 - Test Methods for Copper in Water
• ASTM D1691 - Test Methods for Zinc in Water
• ASTM D3557, D3558, D3559 - Test Methods for Cadmium, Cobalt, and Lead in Water
• ASTM D3919 - Practice for Measuring Trace Elements in Water by Graphite Furnace Atomic Absorption Spectrophotometry
• ASTM D5673 - Inductively Coupled Plasma-Mass Spectrometry
• ASTM D3370, D1066 - Practices for Sampling Water from Flowing Process Streams and Steam
• ASTM D1193 - Specification for Reagent Water

ASTM D1886-14(2021)e1 stands as a comprehensive and reliable reference for laboratories and environmental managers tasked with monitoring nickel concentrations in water, ensuring the continued protection of ecosystems and compliance with international water quality assessment standards.

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.
´1
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 [e-mail]. 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
´1
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.
´1
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 Fortotalrecoverablenickeladd0.5mLofHNO (spgr 15.1 The precision of this test method was tested by eleven
1.42) and proceed as directed in 13.2 through 13.4. For
laboratories in reagent water, natural waters, a refinery effluent
dissolved nickel proceed with 13.5. and in a wastewater. Five laboratories reported data for two
operators. The precision of this test method is shown in Table
12.3 Analyze at least four working standards containing
1; the bias is shown in Table 2.
concentrations of nickel that bracket the expected sample
concentration, prior to analysis of samples, to calibrate the
instrument. Atomize the blank and standards and record the
Supporting data have been filed at ASTM International Headquarters and may
instrument readings. Atomize HNO (1 + 499) between each
3 beobtainedbyrequestingResearchReportRR:D19-1038.ContactASTMCustomer
standard. Service at [e-mail].
´1
D1886 − 14 (2021)
TABLE 2 Determination of Bias, Direct Aspiration
complete analytical test method including any sample preser-
(Test Method A)
vation and pretreatment steps.
Statistically
16.3.3 Calculate the mean and standard deviation of the
Amount Amount Significant
seven values and compare to the acceptable ranges of bias in
Added, Found, Bias, mg/L Bias, % (95 %
mg/L mg/L Confidence
Table 2. This study should be repeated until the recoveries are
Level)
within the limits given in Table 1. If a concentration other than
Reagent Water:
the recommended concentration is used, refer to Practice
8.0 7.74 −0.26 −3 yes
D5847 for information on applying the F test and t test in
0.8 0.84 +0.04 +5 yes
4.0 3.93 −0.07 −2 no
evaluating the acceptability of the mean and standard devia-
Natural Water:
tion.
8.0 7.74 −0.26 −3 yes
0.8 0.84 +0.04 +5 yes
16.4 Laboratory Control Sample (LCS):
4.0 3.87 −0.13 −3 yes
16.4.1 To ensure that the test method is in control, prepare
and analyze a LCS containing a known concentration of nickel
with each batch (laboratory-defined or twenty samples). The
15.2 It is the user’s responsibility to ensure the validity of
laboratory control samples for a large batch should cover the
this test method for waters of untested matrices.
analytical range when possible. The LCS must be taken
through all of the steps of the analytical method including
15.3 ThissectiononprecisionandbiasconformstoPractice
sample preservation and pretreatment. The result obtained for
D2777 – 77 which was in place at the time of collaborative
a mid-range LCS shall fall within 615 % of the known
testing. Under the allowances made in 1.4 of Practice
concentration.
D2777 – 13, these precision and bias data do meet existing
16.4.2 If the result is not within these limits, analysis of
requirements of interlaboratory studies of Committee D19 test
samples is halted until the problem is corrected, and either all
methods.
thesamplesinthebatchmustbereanalyzed,ortheresultsmust
16. Quality Control
be qualified with an indication that they do not fall within the
performance criteria of the test method.
16.1 In order to be certain that analytical values obtained
using these test methods are valid and accurate within the
16.5 Method Blank:
confidencelimitsofthetest,thefollowingQCproceduresmust
16.5.1 Analyze a reagent water test blank with each
be followed when analyzing nickel.
laboratory-defined batch. The concentration of nickel found in
16.2 Calibration and Calibration Verification:
the blank should be less than 0.5 times the lowest calibration
16.2.1 Analyze at least four working standards containing
standard. If the concentration of nickel is found above this
concentrations of nickel that bracket the expected sample level, analysis of samples is halted until the contamination is
concentration, prior to analysis of samples, to calibrate the
eliminated, and a blank shows no contamination at or above
instrument (see 12.3). The calibration correlation coefficient this level, or the results must be qualified with an indication
shall be equal to or greater than 0.990.
that they do not fall within the performance criteria of the test
16.2.2 Verify instrument calibration after standardization by method.
analyzing a standard at the concentration of one of the
16.6 Matrix Spike (MS):
calibration standards. The concentration of a mid-range stan-
16.6.1 To check for interferences in the specific matrix
dard should fall within 615 % of the known concentration.
being tested, perform a MS on at least one sample from each
Analyze a calibration blank to verify system cleanliness.
laboratory-defined batch by spiking an aliquot of the sample
16.2.3 If calibration cannot be verified, recalibrate the
with a known concentration of nickel and taking it through the
instrument.
analytical method.
16.2.4 It is recommended to analyze a continuing calibra-
16.6.2 Thespikeconcentrationplusthebackgroundconcen-
tion blank (CCB) and continuing calibration verification
tration of nickel must not exceed the high calibration standard.
(CCV) at a 10 % frequency. The results should fall within the
The spike must produce a concentration in the spiked sample
expected precision of the method or 615 % of the known
that is 2 to 5 times the analyte concentration in the unspiked
concentration.
sample,or10to50timesthedetectionlimitofthetestmethod,
16.3 Initial Demonstration of Laboratory Capability:
whichever is greater.
16.3.1 Ifalaboratoryhasnotperformedthetestbefore, or if
16.6.3 Calculate the percent recovery of the spike (P) using
there has been a major change in the measurement system, for
the following formula:
example,newanalyst,newinstrument,andsoforth,aprecision
and bias study must be performed to demonstrate laboratory P 5 100@A V 1V 2 BV #/CV
~ !
s s
capability.
where:
16.3.2 Analyze seven replicates of a standard solution
A = analyte known concentration (mg/L) in spiked sample,
prepared from an Independent Reference Material containing a
midrange concentration of nickel. The matrix and chemistry of
B = analyte known concentration (mg/L) in unspiked
the solution should be equivalent to the solution used in the
sample,
collaborative study. Each replicate must be taken through the
´1
D1886 − 14 (2021)
with hot nitric acid to destroy organic matter, dissolved in
C = known concentration (mg/L) of analyte in spiking
hydrochloricacid,anddilutedtoaspecifiedvolumewithwater.
solution,
The resulting solution is then aspirated into the air-acetylene
V = volume (mL) of sample used, and
s
V = volume (mL) of spiking solution added. flame of the spectrophotometer. The digestion procedure sum-
marized in 8.1 is used for total recoverable nickel. The same
16.6.4 Thepercentrecoveryofthespikeshallfallwithinthe
chelation-extraction procedure is used for cadmium (Test
limits, based on the analyte concentration, listed in Test
Methods D3557), cobalt (Test Methods D3558), copper (Test
Method D5810, Table 1. If the percent recovery is not within
Methods D1688), iron (Test Methods D1068), lead (Test
these limits, a matrix interference may be present in the sample
Methods D3559), and zinc (Test Methods D1691).
selected for spiking. Under these circumstances, one of the
following remedies must be employed: the matrix interference
19. Interferences
must be removed, all samples in the batch must be analyzed by
19.1 See 9.1.
a test method not affected by the matrix interference, or the
results must be qualified with an indication that they do not fall
20. Apparatus
within the performance criteria of the test method.
20.1 All apparatus described in Section 10 are required.
NOTE 10—Acceptable spike recoveries are dependent on the concen-
trationofthecomponentofinterest.SeeTestMethodD5810foradditional
21. Reagents and Materials
information.
21.1 Bromphenol Blue Indicator Solution (1 g/L)—Dissolve
16.7 Duplicate:
0.1 g of bromphenol blue in 100 mL of 50 % ethanol or
16.7.1 To check the precision of sample analyses, analyze a
isopropanol.
sample in duplicate with each laboratory-defined batch. If the
21.2 Carbon Disulfide (CS ).
concentrationoftheanalyteislessthanfivetimesthedetection
limit for the analyte, a matrix spike duplicate (MSD) should be
21.3 Chloroform (CHCl ).
used.
21.4 Filter Paper—See 11.1.
16.7.2 Calculate the standard deviation of the duplicate
values and compare to the precision in the collaborative study 21.5 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
chloric acid (HCl) (see Note 4 and Note 5).
using an F test. Refer to 6.4.4 of Practice D5847 for informa-
tion on applying the F test.
21.6 Hydrochloric Acid(1+2)—Add 1 volume of hydro-
16.7.3 If the result exceeds the precision limit, the batch
chloric acid (HCl), sp gr 1.19, to 2 volumes of water.
must be reanalyzed or the results must be qualified with an
21.7 Hydrochloric Acid (1 + 49)—Add 1 volume of hydro-
indication that they do not fall within the performance criteria
chloric acid (HCl), sp gr 1.19, to 49 volumes of water.
of the test method.
21.8 Nickel Solution, Stock (1.0 mL = 200 µg Ni)—
16.8 Independent Reference Material (IRM):
Commercially purchase or dissolve 0.9906 g of nickelous
16.8.1 In order to verify the quantitative value produced by
nitrate (Ni(NO ) ·6H O) in water containing 1 mL of HNO
3 2 2 3
the test method, analyze an Independent Reference Material
(sp gr 1.42) and dilute to 1 L with water. A purchased nickel
(IRM) submitted as a regular sample (if practical) to the
stock solution of appropriate known purity is also acceptable.
laboratory at least once per quarter. The concentration of the
IRM should be in the concentration mid-range for the method 21.9 Nickel Solution, Standard (1.0 mL = 2.0 µg Ni)—
chosen. The value obtained must fall within the control limits Dilute10.0mLofnickelsolution,stockand1mLofHNO (sp
established by the laboratory. gr 1.42) to 1 L with water. This standard is used to prepare
working standards at the time of analysis.
TEST METHOD B—ATOMIC ABSORPTION,
21.10 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
CHELATION-EXTRACTION
(HNO ) (see Note 6).
17. Scope 21.11 Pyrrolidine Dithiocarbamic Acid-Chloroform
Reagent—Add 36 mLof pyrrolidine to 1 Lof CHCl . Cool the
17.1 This test method covers the determination of dissolved
solution and add 30 mL of CS (21.2) in small portions,
and total recoverable nickel and has been used successfully
swirling between additions. Dilute to 2 L with CHCl . The
with reagent water, tap water, river water, artificial seawater
reagent can be used for several months if stored in a cool, dark
and a synthetic (NaCl) brine.
place. (Warning—All components of this reagent are highly
17.2 This test method is applicable in the range from 10 to
toxic. Carbon disulfide is also highly flammable. Prepare and
1000µ g/L of nickel. The range may be extended upward by
use in a well-ventilated hood. Avoid inhalation and direct
dilution of the sample.
contact.)
21.12 Sodium Hydroxide Solution (100 g/L)—Dissolve 100
18. Summary of Test Method
g of sodium hydroxide (NaOH) in water and dilute to 1 L.
18.1 Nickel is determined by atomic absorption spectropho-
(Warning—This is a very exothermic reaction.)
tometry. The element, either dissolved or total recoverable, is
21.13 Oxidant—See 11.7.
chelated with pyrrolidine dithiocarbamic acid and extracted
with chloroform. The extract is evaporated to dryness, treated 21.14 Fuel—See 11.8.
´1
D1886 − 14 (2021)
TABLE 3 Precision and Concentration, Chelation–Extraction
22. Standardization
(Test Method B)
22.1 Prepare a blank and sufficient standards containing
Reagent Water:
from 0.0 to 100 µg of nickel by diluting 0.0 to 50.0-mL
Concentration (X), µg/L 784.2 56.8 398.5
S 146.4 15.2 35.1
portions of nickel standard solution to 100 mL with water
T
S 41.02 9.18 22.97
O
(21.9). Analyze at least three working standards containing
Natural Water:
concentrations of nickel that bracket the expected sample
Concentration (X), µg/L 794.4 53.6 399.4
S 133.9 11.2 37.7
concentration, prior to analysis of samples, to calibrate the T
S 70.9 12.6 11.1
O
instrument.
22.2 For total recoverable nickel use 125-mL beakers or
flasks, add 0.5 mL of HNO (sp gr 1.42) (21.10) and proceed
3 23.9 Repeat the extraction with 10 mLof CHCl (21.3) and
as directed in 23.2 through 23.15. For dissolved nickel use
drain the CHCl layer into the same beaker.
250-mL separatory funnels and proceed as directed in 23.5
NOTE 14—If color still remains in the CHCl extract, reextract the
through 23.15.All samples and standards should be treated the
aqueous phase until the CHCl layer is colorless.
same.
23.10 Place the beaker on a hotplate set at low heat or on a
22.3 Read directly in concentration if this capability is
steam bath, and evaporate to near dryness. Remove beaker
provided with the instrument or construct an analytical curve
from heat and allow residual solvent to evaporate without
by plotting the absorbances of standards versus micrograms of
further heating. (Warning—Perform in a well-ventilated
nickel or prepare a linear plot.
hood.) See Note 9.
23.11 Hold the beaker at a 45° angle and slowly add
23. Procedure
dropwise 2 mL of HNO (sp gr 1.42) (21.10), rotating the
23.1 Measure
...