ASTM D1886-94(1998)
(Test Method)Standard Test Methods for Nickel in Water
Standard Test Methods for Nickel in Water
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 to 15 Test Method B-Atomic Absorption, Chelation-Extraction 10 to 1000 [mu]g/L 16 to 24 Test Method C-Atomic Absorption, Graphite Furnace 5 to 100 [mu]g/L 25 to 33
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 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 hazards statements, see Notes 4, 6, 9, and 14.
1.4 Two former colorimetric test methods were discontinued. Refer to Appendix X1 for historical information.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn
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Designation:D 1886–94 (Reapproved 1998)
Standard Test Methods for
Nickel in Water
This standard is issued under the fixed designation D 1886; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope D1129 Terminology Relating to Water
, ,
2 3 4
D1192 Specification for Equipment for Sampling Water
1.1 These test methods cover the atomic absorption
and Steam in Closed Conduits
determination of nickel in water and wastewaters. Three test
D1193 Specification for Reagent Water
methods are given as follows:
D1687 Test Methods for Chromium in Water
D1688 Test Methods for Copper in Water
Concentration
D1691 Test Methods for Zinc in Water
Range Sections
Test Method A—Atomic Absorption,
D2777 Practice for Determination of Precision and Bias of
Direct 0.1 to 10 mg/L 7-15
Applicable Methods of Committee D-19 on Water
Test Method B—Atomic Absorption,
D3370 Practices for Sampling Water from Closed Con-
Chelation-Extraction 10 to 1000 µg/L 16-24
Test Method C—Atomic Absorption,
duits
Graphite Furnace 5 to 100 µg/L 25-33
D3557 Test Methods for Cadmium in Water
1.2 Test Methods A, B, and C have been used successfully
D3558 Test Methods for Cobalt in Water
withreagentgradewaterandnaturalwaters.EvaluationofTest
D3559 Test Methods for Lead in Water
Method C was also made in condensate from a medium Btu
D3919 Practice for Measuring Trace Elements in Water by
coal gasification process. It is the user’s responsibility to
Graphite FurnaceAtomicAbsorption Spectrophotometry
ensure the validity of these test methods for other matrices.
D4841 Practice for Estimation of Holding Time for Water
1.3 This standard does not purport to address all of the
Samples Containing Organic and Inorganic Constituents
safety concerns, if any, associated with its use. It is the
3. Terminology
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica- 3.1 Definitions:
bilityofregulatorylimitationspriortouse.Forspecifichazards
3.1.1 For definitions of terms used in these test methods,
statements, see Note 4, Note 6, Note 9, and Note 14. refer to Terminology D1129.
1.4 Two former colorimetric test methods were discontin-
3.2 Definitions of Terms Specific to This Standard:
ued. Refer to Appendix X1 for historical information. 3.2.1 total recoverable nickel—an arbitrary analytical term
relating to the recoverable forms of nickel that are determin-
2. Referenced Documents
able by the digestion method that is included in these test
2.1 ASTM Standards:
methods.
D858 Test Methods for Manganese in Water
4. Significance and Use
D1066 Practice for Sampling Steam
D1068 Test Methods for Iron in Water 4.1 Elementalconstituentsinpotablewater,receivingwater,
and wastewater need to be identified for support of effective
pollution control programs. Test MethodsA, B, and C provide
These test methods are under the jurisdiction of ASTM Committee D-19 on
the techniques necessary to make such measurements.
Water and are the direct responsibility of Subcommittee D19.05 on Inorganic
4.2 Nickel is considered to be relatively nontoxic to man
Constituents in Water.
Current edition approved Sept. 15, 1994. Published November 1994. Originally and a limit for nickel is not included in the EPA National
published as D1886–61T. Last previous edition D1886–90.
Interim Primary Drinking Water Regulations. The toxicity of
Chilton, J. M., “Simultaneous Colorimetric Determination of Copper, Cobalt,
nickel to aquatic life indicates tolerances that vary widely and
and Nickel as Diethyldithiocarbamates,”Analytical Chemistry, Vol 25, 1953, pp.
thatareinfluencedbyspecies,pH,synergisticeffects,andother
1274–1275.
Platte,J.A.,andMarcy,V.M.,“ANewToolfortheWaterChemist,”Industrial
factors.
Water Engineering, May 1965.
Brown,E.,Skougstad,M.W.,andFishman,M.J.,“MethodsforCollectionand
Analysis of Water Samples for Dissolved Minerals and Gases,” Techniques of
Water-Resources Investigations of the U.S. Geological Survey, Book 5, Chapter , EPAPublication No. EPA-570/9-76-003 was originally published in 1976, and
1970, p. 115. amended in 1980. Contact the Environmental Protection Agency, 401“ M” ST.,
Annual Book of ASTM Standards, Vol 11.01. S.W., Washington, DC 20406 for availability.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
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D 1886
4.3 Nickel is a silver-white metallic element seldom occur- D3557),chromium(TestMethodsD1687),cobalt(TestMeth-
ring in nature in the elemental form. Nickel salts are soluble ods D3558), copper (Test Methods D1688), iron (Test Meth-
and can occur as a leachate from nickel-bearing ores. Nickel ods D1068), lead (Test Methods D3559), manganese (Test
salts are used in metal-plating and may be discharged to Methods D858), and zinc (Test Methods D1691).
surface or ground waters.
9. Interferences
9.1 Sodium, potassium, sulfate, and chloride (9000 mg/L
5. Purity of Reagents
each), calcium, magnesium and iron (4000 mg/Leach), nitrate
5.1 Reagent grade chemicals shall be used in all tests.
(2000 mg/L), and cadmium, lead, copper, zinc, cobalt, and
Unlessotherwiseindicated,itisintendedthatallreagentsshall
chromium (10 mg/L each) do not interfere.
conform to the specifications of the Committee on Analytical
Reagents of the American Chemical Society where such NOTE 1—Background correction by techniques such as a continuum
source, nonabsorbing lines, or chelation-extraction, may be necessary for
specifications are available. Other grades may be used,
low levels of nickel for some types of water. Instrument manufacturer’s
provided it is first ascertained that the reagent is of sufficiently
instructions for use of the specific correction technique should be
high purity to permit its use without lessening the accuracy of
followed.
the determination.
5.2 PurityofWater—Unlessotherwiseindicated,references 10. Apparatus
towatershallbeunderstoodtomeanreagentwaterconforming
10.1 AtomicAbsorptionSpectrophotometer,foruseat232.0
toSpecificationD1193,TypeI.Otherreagentwatertypesmay
nm.
be used, provided it is first ascertained that the water is of
NOTE 2—The manufacturer’s instructions should be followed for all
sufficiently high purity to permit its use without lessening the
instrumentalparameters.Wavelengthsotherthan232.0nmmaybeusedif
bias and precision of the determination. Type II water was
they have been determined to be equally suitable.
specified at the time of the round-robin testing of this test
10.2 Nickel Hollow-Cathode Lamp—Multielement hollow-
method.
cathode lamps are available and also have been found satis-
factory.
6. Sampling
10.3 Pressure-Reducing Valves—The supplies of fuel and
6.1 Collect the sample in accordance with Practice D1066,
oxidant shall be maintained at pressures somewhat higher than
Specification D1192, or Practices D3370, as applicable.
the controlled operating pressure of the instrument by suitable
6.2 Samples shall be preserved with HNO (sp gr 1.42) to a
valves.
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 11. Reagents and Materials
sample shall be filtered through a 0.45-µm membrane filter
11.1 Hydrochloric Acid (sp gr 1.19)—Concentrated hydro-
before acidification. The holding time for samples may be
chloric acid (HCl).
calculated in accordance with Practice D4841.
NOTE 3—If a high reagent blank is obtained, distill the HCl or use a
spectrograde acid.
TEST METHODA—ATOMICABSORPTION, DIRECT
NOTE 4—Caution:When HCl is distilled, an azeotropic mixture is
formed(;6NHCl).Therefore,wheneverconcentratedHClisusedinthe
7. Scope
preparation of reagents or in the procedure, use twice the volume of the
7.1 This test method covers the determination of dissolved
distilled HCl.
and total recoverable nickel and has been used successfully
11.2 Nitric Acid (sp gr 1.42)—Concentrated nitric acid
with reagent water, tap water, river water, lake water, ground
(HNO ).
water, a refinery effluent, and a wastewater.
NOTE 5—If a high reagent blank is obtained, distill the HNO or use a
7.2 This test method is applicable in the range from 0.1 to 3
spectrograde acid.
10 mg/L of nickel. The range may be extended upward by
11.3 Nitric Acid (1+499)—Add 1 volume HNO (sp gr
dilution of the sample.
1.42) to 499 volumes of water.
8. Summary of Test Method
11.4 Nickel Solution, Stock (1.0 mL5 1.0 mg Ni)—
Dissolve 4.953 g of nickelous nitrate [Ni(NO ) ·6H O] in a
8.1 Nickel is determined by atomic absorption spectropho-
3 2 2
mixture of 10 mL of HNO (sp gr 1.42) and 100 mL of water.
tometry. Dissolved nickel is determined by aspirating the
Dilute to 1 L with water.
filteredsampledirectlywithnopretreatment.Totalrecoverable
11.5 NickelSolution,Standard(1mL50.1mgNi)—Dilute
nickel is determined by aspirating the sample following
100.0 mLof the stock nickel solution and 1 mLof HNO to 1
hydrochloric-nitric acid digestion and filtration. The same
L with water.
digestion procedure is used for cadmium (Test Methods
11.6 Oxidant:
11.6.1 Air,whichhasbeenpassedthroughasuitablefilterto
remove oil, water, and other foreign substances is the usual
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
oxidant.
listed by the American Chemical Society, see Analar Standards for Laboratory
11.7 Fuel:
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
11.7.1 Acetylene—Standard, commercially available acety-
andNationalFormulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD. lene is the usual fuel. Acetone, always present in acetylene
D 1886
TABLE 1 Precision and Concentration, Direct Aspiration
cylinders, can affect analytical results. The cylinder should be
(Test Method A)
replaced at 50 psig (345 kPa).
Reagent Water:
NOTE 6—Warning:“Purified” grade acetylene containing a special
¯
Concentration (X), mg/L 7.74 0.84 3.93
proprietarysolventratherthanacetoneshouldnotbeusedwithpoly(vinyl
S 0.502 0.102 0.383
T
S 0.261 0.045 0.324
chloride) tubing as weakening of the walls can cause a potentially
O
Natural Water:
hazardous situation.
¯
Concentration (X), mg/L 7.74 0.84 3.87
S 0.629 0.108 0.401
T
12. Standardization
S 0.420 0.067 0.192
O
12.1 Prepare a blank and at least four standard solutions to
bracket the expected nickel concentration range of the samples
TABLE 2 Determination of Bias, Direct Aspiration
to be analyzed by diluting the standard nickel solution with
(Test Method A)
HNO (1+499) as described in 11.5. Prepare the standards
Statistically
(100 mL) each time the test is to be performed.
Amount Amount Significant
12.2 Fortotalrecoverablenickeladd0.5mLofHNO (spgr
Added, Found, Bias, mg/L Bias, % (95 %
1.42) and proceed as directed in 13.2 through 13.4. For mg/L\ mg/L Confidence
Level)
dissolved nickel proceed with 13.5.
Reagent Water:
12.3 Atomize the blank and standards and record the instru-
8.0 7.74 −0.26 −3 yes
ment readings. Atomize HNO (1+499) between each stan-
0.8 0.84 +0.04 +5 yes
dard.
4.0 3.93 −0.07 −2 no
Natural Water:
12.4 Prepare an analytical curve by plotting the absorbance
8.0 7.74 −0.26 −3 yes
versus the concentration for each standard on linear graph
0.8 0.84 +0.04 +5 yes
paper. Alternatively, read directly in concentration if this
4.0 3.87 −0.13 −3 yes
capability is provided with the instrument.
TEST METHOD B—ATOMICABSORPTION,
13. Procedure
CHELATION-EXTRACTION
13.1 Measure 100.0 mL of a well-mixed acidified sample
into a 125-mL beaker or flask.
16. Scope
16.1 This test method covers the determination of dissolved
NOTE 7—If only dissolved nickel is to be determined, start with 13.5.
and total recoverable nickel and has been used successfully
13.2 Add 5 mL of HCl (sp gr 1.19) to each sample.
with reagent water, tap water, river water, artificial seawater
13.3 Heat the samples on a steam bath or hotplate in a
and a synthetic (NaCl) brine.
well-ventilated fume hood until the volume has been reduced
16.2 This test method is applicable in the range from 10 to
to 15 to 20 mL, making certain that the samples do not boil.
1000µ g/L of nickel. The range may be extended upward by
NOTE 8—Forsampleswithhighlevelsofsuspendedmatterordissolved
dilution of the sample.
solids, the amount of reduction in volume is left to the discretion of the
17. Summary of Test Method
analyst.
17.1 Nickelisdeterminedbyatomicabsorptionspectropho-
13.4 Cool and filter the samples through a suitable filter,
tometry. The element, either dissolved or total recoverable, is
such as fine-textured, acid-washed, ashless paper, into 100-mL
chelated with pyrrolidine dithiocarbamic acid and extracted
volumetricflasks.Washthefilterpapertwoorthreetimeswith
with chloroform. The extract is evaporated to dryness, treated
water and bring filtrate to volume.
with hot nitric acid to destroy organic matter, dissolved in
13.5 Atomize each filtered and acidified sample and deter-
hydrochloricacid,anddilutedtoaspecifiedvolumewithwater.
mine its absorbance or concentration.Atomize HNO (1+499)
The resulting solution is then aspirated into the air-acetylene
between samples.
flame of the spectrophotometer. The digestion procedure sum-
14. Calculation
marized in 8.1 is used for total recoverable nickel. The same
chelation-extraction procedure is used for cadmium (Test
14.1 Calculatetheconcentrationofnickelineachsample,in
milligrams per litre, using 12.4. Methods D3557), cobalt (Test Methods D3558), copper (Test
Methods D1688), iron (Test Methods D1068), lead (Test
15. Precision and Bias
Methods D3559), and zinc (Test Methods D1691).
15.1 The precision of this test method was tested by eleven
18. Interferences
laboratories in reagent water, natural waters, a refinery effluent
18.1 See 9.1.
and in a wastewater. Five laboratories reported data for two
operators. The precision of this test method is shown in Table
19. Apparatus
1; the bias is shown in Table 2.
19.1 All apparatus described in Section 10 are required.
15.2 It is the user’s responsibility to ensure the validity of
20. Reagents and Materials
this test method for waters of untested matrices.
20.1 BromphenolBlueIndicatorSolution(1g/L)—Dissolve
0.1 g of bromphenol blue in 100 mL of 50% ethanol or
Supporting data are available from ASTM Headquarters. Request RR:
D19–1038. isopropanol.
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