Designation: D 6414 99

AMERICAN SOCIETY FOR TESTING AND MATERIALS

100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

Standard Test Methods for

Total Mercury in Coal and Coal Combustion Residues by

Acid Extraction or Wet Oxidation/Cold Vapor Atomic
Absorption1
This standard is issued under the fixed designation D 6414; 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 (e) indicates an editorial change since the last revision or reapproval.

mercury is reduced to elemental mercury. The mercury vapor is

determined by flameless cold-vapor atomic absorption spectroscopy.
4.2 Test Method BMercury in the analysis sample is
solubilized by heating the test sample in a mixture of nitric and
sulfuric acids with vanadium pentoxide.5 The acid solutions
produced are transferred into a vessel in which the mercury is
reduced to elemental mercury. The mercury vapor is determined by flameless cold-vapor atomic absorption spectroscopy.

1. Scope
1.1 These test methods cover procedures to determine the
total mercury content in a sample of coal or coal combustion
residue.
1.2 The values stated in SI units are regarded as the
standard.
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.

5. Significance and Use

5.1 The emission of mercury during coal combustion can be
an environmental concern.
5.2 When representative test portions are analyzed according to one of these procedures, the total mercury is representative of concentrations in the sample.

2. Referenced Documents
2.1 ASTM Standards:
D 121 Terminology of Coal and Coke2
D 1193 Specification for Reagent Water3
D 2013 Method of Preparing Coal Samples for Analyses2
D 3173 Test Method for Moisture in the Analysis Sample of
Coal and Coke2
D 5142 Test Methods for the Proximate Analysis of the
Analysis Sample of Coal and Coke by Instrumental
Procedures2
D 3180 Practice for Calculating Coal and Coke Analyses
from As-Determined to Different Bases2
IEEE/ASTM SI 10 Standard for Use of the International
System of Units (SI): The Modern Metric System4

6. Apparatus
6.1 Apparatus for Test Method A:
6.1.1 Analytical Balance, with a sensitivity of 0.1 mg.
6.1.2 Atomic Absorption Spectrophotometer, with a flameless cold-vapor mercury analysis system.
6.1.3 Digestion Vessels, 100- to 250-mL bottles with an
O-ring seal and screw cap. Bottle must be compatible for use
with aqua regia. Polycarbonate and HDPE are acceptable.
Bottles and cap assemblies shall be washed in 1-to-1 HCl then
dried before each use.

3. Terminology
3.1 For definitions of terms used in this standard, refer to
Terminology D 121.

NOTE 1Other bottle and cap assemblies may be used provided they
are compatible for use with aqua regia at a temperature of 80C.

6.1.4 Heat Source, a water bath capable of maintaining a

temperature of 80C.
6.1.5 Syringe and Filter, a 20-cm3 syringe and a 1-m PTFE
filter to fit syringe.
6.2 Apparatus for Test Method B:
6.2.1 Analytical Balance, with a sensitivity of 0.1 mg.
6.2.2 Atomic Absorption Spectrophotometer, with a flameless cold-vapor mercury analysis system.
6.2.3 Digestion Vessels, 16- by 150-mm disposable glass
test tubes.

4. Summary of Test Method

4.1 Test Method AMercury in the analysis sample is
solubilized by heating the test sample at a specified temperature in a mixture of nitric and hydrochloric acids. The acid
solutions produced are transferred into a vessel in which the
1
These Test Methods are under the jurisdiction of ASTM Committee D-5 on
Coal and Coke and are the direct responsibility of Subcommittee D05.29 on Major
Elements in Ash and Trace Elements of Coal.
Current edition approved April 10, 1999. Published May 1999.
2
Annual Book of ASTM Standards, Vol 05.05.
3
Annual Book of ASTM Standards, Vol 11.01.
4
Annual Book of ASTM Standards, Vol 14.04.

Crock, J.G., Open-File Report, U.S. Geological Survey, 8784, p.19.

D 6414
6.2.4 Heat Source, an aluminum block with 18-mm holes to
accommodate the disposable test tubes. The block shall be
capable of slowly reaching and maintaining a final temperature
of 150C. The block can be heated by placing it on a hot plate
or it can contain its own internal heating elements.

ues for which confidence limits are issued by a recognized

certifying agency such as the National Institute of Standards
and Technology (NIST). It is recommended that the user verify
the value with the certifying agency before using the CRM coal
for quality control purposes.

7. Sample
7.1 Prepare the analysis sample in accordance with Method
D 2013 by pulverizing the material to pass a 250-m (No. 60)
sieve.
7.2 Analyze separate test portions for moisture content in
accordance with Test Method D 3173 or Test Methods D 5142.

9. Procedure
9.1 Preparation of Test Solution A (Extraction Step):
9.1.1 Weigh a test portion of approximately 1 g of the
sample into a digestion bottle. Record the weight (Ws) to the
nearest 0.0001 g.
9.1.2 Quantitatively add 2 mL of concentrated nitric acid
and 6 mL of concentrated hydrochloric acid to the digestion
bottle and secure the cap.
9.1.3 Transfer the digestion bottle and contents to a water
bath that has been heated to 80C and heat for 1 h. Secure the
digestion bottle in such a way as to keep the contents below the
surface of the water.
9.1.4 After 1 h, remove the digestion bottle and allow to
cool to room temperature.

Test Method A for the Analysis of Mercury by Using Acid

Extraction
8. Reagents
8.1 Purity of ReagentsReagent grade chemicals shall be
used. 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.6 Other grades can 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 AcidsUse trace metal purity grade acids or
equivalent. Redistilled acids are acceptable.
8.3 Purity of WaterUse water equivalent to ASTM Type II
reagent water of Specification D 1193.
8.4 Mercury Standard Stock Solution [1000 ppm (1000
g/mL)]Dissolve 1.0800 g of mercury (II) oxide (HgO) in a
minimum volume of HCl (1+1) and dilute to 1 L with water.
Alternatively, use a commercially available stock solution
specifically prepared for atomic absorption spectrometry.
8.5 Mercury Standard Solution (100 ng/mL)Prepare the
mercury standard solution fresh daily. Dilute 5 mL of the
mercury standard stock solution to 500 mL with deionized
water. Further dilute 10 mL of this intermediate solution to 1 L
with deionized water.
8.6 Nitric AcidConcentrated (HNO3, sp. gr. 1.42).
8.7 Hydrochloric AcidConcentrated (HCl, sp. gr. 1.19).
8.8 Sodium Chloride/Hydroxylamine Sulfate Solution
Dissolve 12 g 6 0.01 g of sodium chloride and 12 g 6 0.01 g
of hydroxylamine sulfate in water and dilute to 100 mL.
8.9 Potassium Permanganate Solution (5 g/100 mL)
Dissolve 5 g of potassium permanganate (KMnO4) in water
and dilute to 100 mL.
8.10 Stannous Chloride Solution (100 g/L)Dissolve 100 g
of stannous chloride dihydrate (SnCl22 H2O) in 300 mL of
concentrated hydrochloric acid (HCl, sp. gr. 1.19) and CAUTIOUSLY dilute to 1 L with water. This solution is stable for
approximately one week if refrigerated.
8.11 Certified Reference Material (CRM)Use Certified
Reference Material (CRM) coals with dry-basis mercury val-

NOTE 2Caution: Carefully relieve the pressure by slowly removing

the cap.

9.1.5 Add 36.5 mL of water and mix the contents.

9.1.6 Add 5 mL of 5 % potassium permanganate solution.
Allow the mixture to stand for 10 min.
9.1.7 Add 0.5 mL of the hydroxylamine sodium chloride
solution and mix. If a pink color persists for more than 1 min,
add an additional 0.5 mL of the hydroxylamine sodium
chloride solution and mix. Note the total volume and record
this volume (V) for use in the final calculations.
9.2 Preparation of Reagent BlankPrepare a reagent blank
by repeating the procedure in 9.1 but without the test portion of
the sample.
9.3 Preparation of Control Sample:
9.3.1 Prepare a test portion of a CRM coal for analysis using
the procedure described in 9.1. Record the expected value of
mercury, the certified value in the coal, as CRME.
9.3.2 Alternatively, weigh a test portion of 1 g of a CRM.
After the addition of the nitric and hydrochloric acids to the
digestion bottle, add mercury standard solution (8.5). The
volume of mercury standard solution to be added should yield
an amount of mercury approximately equivalent to that in the
CRM coal (Note 3).
9.3.3 Calculate the expected value of mercury CRME as
follows
CRME 5 ~Wcrm*CRM 1 Vstandard*0.1!/Wcrm

(1)

where:
Wcrm

5 dry weight of the CRM coal used for preparation of the quality control sample, g;
CRM
5 certified value of mercury in the quality control sample;
Vstandard 5 volume of mercury standard solution added to
the digestion bottle, mL; and
0.1
5 the concentration of the mercury standard
solution, g/mL.

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 Analar 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.

NOTE 3A test portion of 0.9-g dry weight of a CRM coal with 0.11
g/g (110 ng/g) of mercury is weighed out as a quality control sample. To

D 6414
10.2 Purity of AcidsUse trace metal purity grade acids or
equivalent. Redistilled acids are acceptable.
10.3 Purity of WaterUse water equivalent to ASTM Type
II reagent water of Specification D 1193.
10.4 Mercury Standard Stock Solution [1000 ppm (1000
g/mL)]Dissolve 1.0800 g of mercury (II) oxide (HgO) in a
minimum volume of HCl (1+1) and dilute to 1 L with water.
Alternatively, use a commercially available stock solution
specifically prepared for atomic absorption spectrometry.
10.5 Mercury Standard Solution (100 ng/mL)Prepare the
mercury standard solution fresh daily. Dilute 5 mL of the
mercury standard stock solution to 500 mL with deionized
water. Further dilute 10 mL of this intermediate solution to 1 L
with deionized water.
10.6 Nitric AcidConcentrated (HNO3, sp. gr. 1.42).
10.7 Hydrochloric AcidConcentrated (HCl, sp. gr. 1.19).
10.8 Sulfuric AcidH2SO4, sp. gr. 1.83).
10.9 Vanadium Pentoxide, V2O5Remove traces of mercury by roasting the V2O5 in a fume hood at a temperature
below 690C, the melting point of V2O5, in a porcelain dish
using a muffle furnace or a Fisher burner.

yield an amount approximately equivalent to that present in the CRM coal,

0.9 mL of the mercury standard solution is added to the digestion bottle
after the addition of the nitric and hydrochloric acids. CRME calculates to
0.21 g/g.

9.4 Atomic Absorption Analyses:

9.4.1 Instrument ConditionsFollow the instrument manufacturers recommended procedure to align the optical cell in
the beam path of the atomic absorption spectrophotometer and
optimize the performance of the instrument and the flameless
cold-vapor apparatus.
9.4.2 Instrument Calibration:
9.4.2.1 Prepare 50 mL of 0.5, 1, 3, 5, and 10 ng/mL (ppb) of
mercury calibration standards in a solution of 10 % HCl by
serial dilution of the mercury standard solution.
9.4.2.2 Add a specified volume (Vcal) of a calibration
solution to the reduction flask or reduction system.
NOTE 4If an autosampler equipped with a peristaltic pump is used for
delivery of both calibration and analyses sample solutions to the reduction
system, a specific volume is not required.

9.4.2.3 Either manually or by means of an autosampling

device begin the analyses of the calibration solution by adding
enough stannous chloride solution so as to ensure complete
reduction of the mercury in the calibration solution.
9.4.2.4 Record the absorbance of the calibration standard.
Repeat for each calibration standard.
9.4.3 Analysis of Test Solution A:
9.4.3.1 Using the 20-cm3 syringe, draw Test Solution A into
the syringe.
9.4.3.2 Fit the syringe with a 1-m filter.
9.4.3.3 Filter a volume equivalent to Vcal of Test Solution A
into the reduction flask or reduction system.

NOTE 6Warning: V2O5 is highly toxic, an irritant, and a possible

mutagen.

10.10 Stannous Chloride Solution (100 g/L)Dissolve 100

g of stannous chloride dihydrate (SnCl22H2O) in 300 mL of
concentrated hydrochloric acid (HCl, sp. gr. 1.19) and CAUTIOUSLY dilute to 1 L with water. This solution is stable for
approximately one week if refrigerated.
10.11 Sodium Dichromate, 25 % (w/v) SolutionDissolve
25 g of Na2Cr2O72H2O in water and dilute to 100 mL.
10.12 Complex Reducing SolutionDissolve 30 g of hydroxylamine hydrochloride and 30 g of sodium chloride (NaCl)
in approximately 500 mL of water. Slowly add 100 mL of
concentrated sulfuric acid. Allow the solution to cool, then
dilute to 1 L with water.
10.13 Certified Reference Material (CRM)Use Certified
Reference Material (CRM) coals with dry-basis mercury values for which confidence limits issued by a recognized
certifying agency such as NIST. It is recommended that the
user verify the value with the certifying agency before using
the CRM coal for quality control purposes

NOTE 5A laboratory centrifuge may also be used to separate the

solids from the test solution.

9.4.3.4 Determine the absorbance (As) of the Test Solution

A using the procedure described in 9.4.2.
9.4.3.5 Using 10 % HCl, dilute test solutions with mercury
absorbances greater than the highest calibration standard to
give an estimated absorbance equivalent to the 3-ng/mL
calibration standard and reanalyze.
9.4.3.6 Record the dilution factor as DF.
9.4.4 Analysis of the Reagent BlankDetermine the absorbance (Ab) of the reagent blank using the procedure described
in 9.4.3.
9.4.5 Analysis of the Quality Control SampleDetermine
the absorbance (Aqs) of the quality control sample using the
procedure described in 9.4.3.

11. Procedure
11.1 Preparation of Test Solution B:
11.1.1 Weigh a test portion of 0.15 g of the test sample into
a 16- by 150-mm disposable test tube. Record the weight (Ws)
to the nearest 0.0001 g.
11.1.2 Add approximately 0.1 g of V2O5, 3.5 mL of concentrated HNO3, and 1.5 mL of concentrated H2SO4. Swirl to
mix the contents. Place the test tube in the aluminum heating
block and cover with a watch glass.
11.1.3 Adjust the temperature of the heating block so that it
gradually reaches a temperature of 150C in 4 h. Maintain
heating at this temperature for 16 h.
11.1.4 After heating, carefully remove the test tube from the
aluminum heating block, allow to cool, and dilute the solution
to a final volume of 15 mL (V) with water. Securely cap the test
tube and mix the contents. Centrifuge the test tube and its

Test Method B for the Analysis of Mercury by Using Wet

Oxidation Extraction
10. Reagents
10.1 Purity of ReagentsReagent grade chemicals shall be
used. 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.6 Other grades can 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.
3

D 6414
contents for 5 min at 1000 rpm.
11.2 Reagent BlankPrepare a reagent blank by repeating
the procedure in 11.1 but without the test portion of the sample.
11.3 Quality Control Sample:
11.3.1 Prepare a CRM coal for analysis using the procedure
described in 11.1. Record the certified value as CRM.
11.3.2 Alternatively, weigh a test portion of 0.15 g of a
CRM. After the addition of the nitric acid, add mercury
standard solution (10.5) to the test tube. The volume of the
mercury standard solution to be added should yield an amount
of mercury approximately equivalent to that in the CRM coal
(Note 7). Calculate the expected value CRME of mercury
using Eq 1.

11.4.3 Analysis of Test Solution B:

11.4.3.1 Add a volume equivalent to Vcal of Test Solution B
into the reduction flask or reduction system.
11.4.3.2 Determine the absorbance (As) of the Test Solution
B using the procedure described in 11.4.2.
11.4.3.3 Using 3N H2SO4, dilute test solutions with mercury
absorbances greater than the highest calibration standard to
give an estimated absorbance equivalent to the 3-ng/mL
calibration standard and reanalyze. Record the dilution factor
as DF.
11.4.3.4 Analysis of the reagent blankDetermine the absorbance (Ab) of the reagent blank using the procedure
described in 11.4.2.
11.4.3.5 Analysis of the quality control sampleDetermine
the absorbance (Aqs) of the quality control sample using the
procedure described in 11.4.2.

NOTE 7A test portion of 0.15 g of a CRM coal with 0.11 g/g (110
ng/g) of mercury is weighed out as a quality control sample. To yield an
amount approximately equivalent to that present in the CRM coal, 0.15
mL of the mercury standard solution is added to the test tube after the
addition of the nitric acid. CRME calculates to 0.21 g/g.

12. Calculation
12.1 These calculations apply to both Test Method A and
Test Method B.
12.1.1 Calculate the dry weight of each test portion of
sample prepared for analysis as follows

11.4 Atomic Absorption Analyses:

11.4.1 Instrument ConditionsFollow the instrument
manufacturers recommended procedure to align the optical
cell in the beam path of the atomic absorption spectrophotometer and optimize the performance of the instrument and the
flameless cold vapor apparatus.
11.4.2 Instrument Calibration:
11.4.2.1 Prepare 500-mL calibration standards of 0.5, 1, 3,
5, and 10 ng/mL (ppb) of mercury by diluting in water aliquots
of the mercury standard solution (10.4) in 115 mL of concentrated HNO3, 50 mL of concentrated H2SO4, and 10 mL of the
25 % (w/v) sodium dichromate solution. Prepare fresh calibration standards every three months.
11.4.2.2 Prepare a 500-mL dilution solution by mixing 115
mL of concentrated HNO3, 50 mL of concentrated H2SO4, and
10 mL of the 25 % (w/v) sodium dichromate solution and
diluting to the mark with water. Prepare dilution solution every
three months.
11.4.2.3 Add a specified volume, Vcal, not to exceed 15 mL
of a calibration solution to the reduction flask or reduction
system.
11.4.2.4 Either manually or by means of an autosampling
device begin the analyses of the calibration solution by adding
enough complex reducing solution and stannous chloride
solution to ensure complete reduction of the mercury in the
calibration solution.
11.4.2.5 Record the absorbance of the calibration standard
(Note 8). Repeat for each calibration standard.

Wds 5 ~~100 Ma! * Ws!/100

(2)

where:
Wds 5 dry sample weight, g;
Ws 5 weight of test portion of sample; and
Ma 5 moisture in the analysis sample calculated according
to Test Method D 3173 or Test Methods D 5142.
12.2 Quality Control:
12.2.1 Calculation of Mercury Concentration of the Quality
Control Sample:
12.2.1.1 Absorbance matchingCalculate the concentration of mercury in ppm (g/g) in the quality control sample as
Mercury ppm ~g/g! dry basis 5 DF 3 ~V/Vds! 3 C
3 @~A Ab!/~Ac Ab!#

(3)

where:
A
5 absorbance of the quality control (Aqs) or analysis
sample (A);
Ac 5 absorbance of the calibration standard nearest A;
Ab 5 absorbance of the blank;
C
5 concentration of the calibration standard, ng/mL;
DF 5 dilution factor, if any;
V
5 volume of the analysis solution; and
Wds 5 dry sample weight, g.
12.2.1.2 Calibration curve:
12.2.1.2.1 Prepare a calibration curve by plotting absorbance of calibration standard minus blank response versus the
concentration of the calibration solution in ng/mL. For the
number of standards specified in this test method, it is
recommended that a linear fit of the form y 5 mx + b be used.
Other fits can be used but can require the preparation of
additional standards to ensure adequate degrees of freedom are
maintained (Note 9).

NOTE 8Automated flow injection systems may have to be modified to

include mixing loops when analyzing samples digested by Method B.
Typical over-the-counter mixing loops are made using 4-mm outer
diameter glass tubing wrapped around a 14-mm-diameter mandrel. Without the mixing loops, foaming in the gas-phase separator may occur. The
foaming interferes with the transfer of mercury vapor from the gas-phase
separator to the absorption cell of the cold-vapor atomic absorption
spectrophotometer. Descriptions and diagrams of a manifold used for the
automated generation of mercury vapor from samples digested according
to Method B are given by J.G. Crock and others.5 Automated flow
injection systems that have been modified to include mixing loops can also
be used to analyze samples digested by Test Method A.

NOTE 9It is recommended that a minimum five calibration standards

be used for a linear fit, six for a quadratic, seven for a cubic, and so forth.
This approach allows for the rejection of a particular calibration standard
for a curve while maintaining adequate degrees of freedom.

D 6414
the limits of MLR and MLR+, prepare another portion of the
standard upon which the original mercury recovery was based.
Determine the absorbance of the new calibration standard.
If the mercury recovery calculated from the absorbance of
the new standard is within the MLR and MLR+ limits, then
proceed with calculation of the concentration of mercury in the
analysis samples.
12.2.2.4.2 If a calibration curve was used to calculate the
concentration of the quality control sample, examine the curve
for points that deviate significantly from the curve. Recalculate
the regression eliminating the suspect point(s) (Note 9). If the
value for the CRM falls within the MLR and MLR+ limits
based on the recalculated regression, then prepare another
portion of the standard(s) eliminated from the regression.
Determine the absorbance of the new standard(s). Recalculate
the regression incorporating the new standards. If the calculated mercury recovery of for CRME is within the MLR and
MLR+ limits, then proceed with calculation of the concentration of mercury in the analysis samples.
12.2.2.4.3 Verify the concentration of the mercury standard
solution from which the calibration standards have been
prepared. Prepare a new mercury standard solution from the
mercury standard stock solution. From the new mercury
standard solution, prepare a 2-ng/mL mercury solution and a
4-ng/mL mercury solution. Determine the absorbance of the
two solutions and of the quality control sample. Recalculate
the mercury recovery. If the recalculated values both fall within
the MLR and MLR+ limits, then the original mercury standard
solution is suspect. Prepare fresh calibration solutions from the
new mercury standard solution and reanalyze a separate aliquot
of the test solutions.
12.2.2.5 If it is not possible to reconcile the mercury
recovery within the limits of MLR and MLR+, then discard all
solutions and repeat the analysis of all samples.
12.3 Calculations for Test SamplesProvided the conditions in 12.2 are satisfied, calculate the mercury content of the
test samples using the same equation (Eq 3, or Eq 4, Eq 5) as
for the quality control sample.

12.2.1.2.2 Calculate the net absorbance for the quality

control sample as follows
Anet 5 A Ab

(4)

where:
A 5 absorbance of the quality control (Aqs) or analysis
sample (A) and
Ab 5 absorbance of the blank.
12.2.1.2.3 Read the concentration of the quality control
sample from the calibration curve as Cs.
12.2.1.2.4 Calculate the concentration of mercury in ppm
(g/g) in the quality control sample as follows
Mercury ppm ~g/g! dry basis 5 DF 3 ~V/Wds! 3 Cs

(5)

where:
Cs 5 concentration of the quality control sample read
from the calibration curve, ng/mL;
DF 5 is the dilution factor, if any;
V
5 volume of the analysis solution; and
Wds 5 dry sample weight, g.
12.2.2 Calculation of Mercury Recovery in the Quality
Control Sample:
12.2.2.1 Calculate the CRM confidence factor as follows
CRMF 5 100 * ~mercury limits/mercury value!

(6)

where:
mercury limits 5 the confidence limits from the certificate
issued by the certifying agency and
mercury value 5 the mercury value issued by the certifying
agency.
If CRMF is greater than 30 %, then the mercury recovery
limits (MLR) are:
MLR+ 5 100 + CRMF
MLR 5 100 CRMF.
If CRMF is less than or equal to 30 %, then the MLR are:
MLR+ 5 130
MLR 5 70.
12.2.2.2 Calculate the mercury recovery from the quality
control sample as follows
Mercury recovery 5 ~mercury ppm ~g/g!/CRME! 3 100

13. Report
13.1 Report the results of the mercury analysis on a dry
sample basis.
13.2 Procedures for converting the value obtained on the
analysis sample to other basis are described in Practice D 3180.
13.3 Report the recovery of mercury in the quality control
sample.
13.4 Report the digestion method used.

(7)

where:
mercury ppm (g/g) 5 the mercury value of sample calculated according to Eq 3 or Eq 5 in
g/g and
CRME
5 the expected value of mercury in the
quality control sample in g/g.
12.2.2.3 If the mercury recovery is between MLR and
MLR+, then proceed with calculation of the concentration of
mercury in the analysis samples.
12.2.2.4 If the mercury recovery is not between MLR and
MLR+, then check one or all of the following:
12.2.2.4.1 If absorbance matching was used to calculate the
concentration of the quality control sample, recalculate the
mercury recovery using two other calibration standards. If the
mercury recovery calculated using both standards falls within

14. Precision and Bias

14.1 The precision and bias of this test method for measuring mercury in coal is being determined and will be available
on or before March 2004.
15. Keywords
15.1 coal; coal combustion residues; cold-vapor atomic
absorption; mercury

D 6414
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.