ASTM D4107-20

Standard Test Method for Tritium in Drinking Water

SIGNIFICANCE AND USE
5.1 This test method was developed for measuring tritium in water to determine if the concentration exceeds the regulatory statutes of drinking water. This test method also is applicable for the determination of tritium concentration in water as required by technical specifications governing the operations of nuclear power facilities. With suitable counting technique, sample size, and counting time a detection limit of less than 37 Bq/L (1000 pCi/L) is attainable by liquid scintillation.
SCOPE
1.1 This test method covers the determination of tritium in drinking water by liquid scintillation counting of the tritium beta particle activity.  
1.2 This test method is used successfully with drinking water. It is the user’s responsibility to ensure the validity of this test method for untested water matrices.  
1.3 The tritium concentrations, which can be measured by this test method utilizing currently available liquid scintillation instruments, range from less than 0.037 Bq/mL (1 pCi/mL) to 555 Bq/mL (15 000 pCi/mL) for a 10-mL sample aliquot. Higher tritium concentrations can be measured by diluting or using smaller sample aliquots, or both.  
1.4 The maximum contaminant level for tritium in drinking water as given by the United States Environmental Protection Agency (U.S. EPA) National Primary Drinking Water Regulations (NPDWR) is 0.740 Bq/mL (20 pCi/mL). The NPDWR lists a required detection limit for tritium in drinking water of 0.037 Bq/mL (1 pCi/mL), meaning that drinking water supplies, where required, should be monitored for tritium at a sensitivity of 0.037 Bq/mL (1 pCi/mL). In Appendix X1, Eq X1.3 is given for determining the necessary counting time to meet the required sensitivity for drinking water monitoring.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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.  
1.7 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: 30-Jun-2020
• ICS: 13.060.50 - Examination of water for chemical substances
• Technical Committee: D19 - Water
• Drafting Committee: D19.04 - Methods of Radiochemical Analysis

Relations

• Refers: ASTM D1129-13(2020)e2 - Standard Terminology Relating to Water
• Effective Date: 01-May-2020
• Refers: ASTM D7902-20 - Standard Terminology for Radiochemical Analyses
• Effective Date: 01-May-2020
• Refers: ASTM D7902-18 - Standard Terminology for Radiochemical Analyses
• Effective Date: 01-Feb-2018
• Refers: ASTM D7902-16 - Standard Terminology for Radiochemical Analyses
• Effective Date: 01-Feb-2016
• Refers: ASTM D7902-14e1 - Standard Terminology for Radiochemical Analyses
• Effective Date: 15-Jan-2014
• Refers: ASTM D7902-14 - Standard Terminology for Radiochemical Analyses
• Effective Date: 15-Jan-2014
• Refers: ASTM D2777-12 - Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
• Effective Date: 15-Jun-2012
• Refers: ASTM D3648-04(2011) - Standard Practices for the Measurement of Radioactivity
• Effective Date: 01-Jan-2011
• Refers: ASTM D3370-10 - Standard Practices for Sampling Water from Closed Conduits
• Effective Date: 01-Dec-2010
• Refers: ASTM D1129-10 - Standard Terminology Relating to Water
• Effective Date: 01-Mar-2010
• Refers: ASTM D3370-08 - Standard Practices for Sampling Water from Closed Conduits
• Effective Date: 01-Oct-2008
• Refers: ASTM D2777-08 - Standard Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
• Effective Date: 15-Jan-2008
• Refers: ASTM D3370-07 - Standard Practices for Sampling Water from Closed Conduits
• Effective Date: 01-Dec-2007
• Refers: ASTM D1129-06a - Standard Terminology Relating to Water
• Effective Date: 01-Sep-2006
• Refers: ASTM D1129-06ae1 - Standard Terminology Relating to Water
• Effective Date: 01-Sep-2006

Overview

ASTM D4107-20 – Standard Test Method for Tritium in Drinking Water provides a robust methodology for detecting and quantifying tritium (³H) in drinking water. Developed by ASTM International, this standard outlines protocols for measuring tritium concentrations to evaluate compliance with regulatory limits and technical specifications, particularly in contexts such as public water supplies and nuclear facility operations. The test employs liquid scintillation counting to achieve sensitive detection of tritium beta particle activity in water samples.

Key reasons for monitoring tritium include safeguarding public health, meeting environmental regulatory requirements, and supporting the safe operation of nuclear power facilities. Public water systems must monitor tritium at levels as specified by regulatory bodies, such as the U.S. Environmental Protection Agency (EPA).

Key Topics

• Scope and Applicability:

  • Applicable to drinking water matrices
  • Defines the measurable tritium concentration range using current liquid scintillation instrumentation (less than 0.037 Bq/mL [1 pCi/mL] to 555 Bq/mL [15,000 pCi/mL])
  • Suitable for higher concentrations by adjusting sample preparation

• Regulatory Requirements:

  • Addresses U.S. EPA maximum contaminant level (MCL) for tritium: 0.740 Bq/mL (20 pCi/mL)
  • Required method detection limit: 0.037 Bq/mL (1 pCi/mL)

• Analytical Method:

  • Sample preparation includes alkaline permanganate distillation to remove interferences
  • Collection and preparation of the distillate for analysis
  • Mixing with scintillator solution and counting for beta activity measurement

• Quality Control:

  • Emphasizes laboratory quality assurance practices, including method blanks, matrix spikes, laboratory control samples, and independent reference material
  • Specifies performance checks for precision, bias, and recovery

• Precision and Uncertainty:

  • Collaborative data provides expected ranges for method precision and bias
  • Includes requirements for calculating counting time and detection limits

Applications

The practical value of ASTM D4107-20 lies in its widespread use across several key sectors:

• Public Drinking Water Utilities:
  • Routine tritium monitoring to comply with regulatory standards and ensure consumer safety
• Nuclear Power Industry:
  • Supports operational safety by monitoring and reporting tritium levels in facility effluents or nearby water bodies
• Environmental Testing Laboratories:
  • Offers standardized procedures for accurate radiochemical laboratory analysis and reporting
• Regulatory Compliance:
  • Ensures that analytical results are consistent, traceable, and defensible in regulatory or legal contexts
• Research:
  • Used in hydrology and environmental research to track tritium as a tracer in water movement and pollution studies

Related Standards

Monitoring tritium in drinking water may require reference to related methods and terminology to ensure comprehensive analysis:

• ASTM D1129: Terminology Relating to Water
• ASTM D1193: Specification for Reagent Water
• ASTM D3370: Practices for Sampling Water from Flowing Process Streams
• ASTM D2777: Practice for Determination of Precision and Bias of Applicable Test Methods
• ASTM D3648: Practices for the Measurement of Radioactivity
• ASTM D7902: Terminology for Radiochemical Analyses
• ANSI N42.22: Traceability of Radioactive Sources
• EPA National Primary Drinking Water Regulations (NPDWR): Regulatory framework for acceptable tritium levels
• BIPM-5 Decay Data Evaluation Project (DDEP): For decay data accuracy

---

Keywords: Tritium in drinking water, ASTM D4107, liquid scintillation counting, radioactivity in water, environmental compliance, nuclear facility monitoring, EPA drinking water standards, radiochemical analysis

Standards Content (Sample)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4107 − 20
Standard Test Method for
Tritium in Drinking Water
This standard is issued under the fixed designation D4107; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.1 This test method covers the determination of tritium in
drinking water by liquid scintillation counting of the tritium
2. Referenced Documents
beta particle activity.
2.1 ASTM Standards:
1.2 This test method is used successfully with drinking
D1129Terminology Relating to Water
water.Itistheuser’sresponsibilitytoensurethevalidityofthis
D1193Specification for Reagent Water
test method for untested water matrices.
D2777Practice for Determination of Precision and Bias of
1.3 The tritium concentrations, which can be measured by
Applicable Test Methods of Committee D19 on Water
thistestmethodutilizingcurrentlyavailableliquidscintillation
D3370Practices for Sampling Water from Flowing Process
instruments, range from less than 0.037 Bq/mL (1 pCi/mL) to
Streams
555 Bq/mL (15000 pCi/mL) for a 10-mL sample aliquot.
D3648Practices for the Measurement of Radioactivity
Higher tritium concentrations can be measured by diluting or
D7902Terminology for Radiochemical Analyses
using smaller sample aliquots, or both.
2.2 Other Documents:
ANSI N42.22Traceability of Radioactive Sources to the
1.4 The maximum contaminant level for tritium in drinking
National Institute of Standards and Technology (NIST)
water as given by the United States Environmental Protection
and Associated Instrument Quality Control
Agency (U.S. EPA) National Primary Drinking Water Regula-
BIPM-5Decay Data Evaluation Project (DDEP)
tions (NPDWR) is 0.740 Bq/mL (20 pCi/mL). The NPDWR
NUDAT2
lists a required detection limit for tritium in drinking water of
0.037 Bq/mL (1 pCi/mL), meaning that drinking water
3. Terminology
supplies, where required, should be monitored for tritium at a
3.1 Definitions:
sensitivity of 0.037 Bq/mL (1 pCi/mL). In Appendix X1, Eq
3.1.1 For definitions of terms used in this standard, refer to
X1.3 is given for determining the necessary counting time to
meet the required sensitivity for drinking water monitoring. Terminology D1129.
3.1.2 For definitions of terms used in this standard relating
1.5 The values stated in SI units are to be regarded as
to radiochemical analysis, refer to Terminology D7902.
standard. No other units of measurement are included in this
standard.
4. Summary of Test Method
1.6 This standard does not purport to address all of the
4.1 A100-mLdrinking water sample aliquot is treated with
safety concerns, if any, associated with its use. It is the
a small amount of sodium hydroxide and potassium
responsibility of the user of this standard to establish appro-
permanganate,distilled,andaspecifiedfractionofthedistillate
priate safety, health, and environmental practices and deter-
is collected for tritium analysis. The alkaline treatment pre-
mine the applicability of regulatory limitations prior to use.
vents other radionuclides, such as radioiodine and radiocarbon
1.7 This international standard was developed in accor-
from distilling over with the tritium. Some drinking water
dance with internationally recognized principles on standard-
supplies will contain trace quantities of organic compounds,
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
This test method is under the jurisdiction ofASTM Committee D19 on Water the ASTM website.
andisthedirectresponsibilityofSubcommitteeD19.04onMethodsofRadiochemi- Available from Institute of Electrical and Electronics Engineers, Inc. (IEEE),
cal Analysis. 445 Hoes Ln., Piscataway, NJ 08854-4141, http://www.ieee.org.
CurrenteditionapprovedJuly1,2020.PublishedJuly2020.Originallyapproved Available from BIPM, Sèvres Cedex, France, https://www.bipm.org.
in 1991. Last previous edition approved in 2013 as D4107–08 (2013). DOI: Available from National Nuclear Data Center at Brookhaven National
10.1520/D4107-20. Laboratory, W Princeton Ave, Yaphank, NY 11980, http://www.nndc.bnl.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4107 − 20
especiallysurfacewatersourcesthatcontainfishandotherlife. 7.3 Distillation Apparatus—For aqueous distillation,
The permanganate treatment oxidizes trace organics in the 250-mL and 1000-mL round bottom borosilicate flasks, con-
sample aliquots which could distill over and cause quenching necting side arm adapter, condenser, graduated cylinder,
interferences.Amiddlefractionofthedistillateiscollectedfor boiling chips, and heating mantle.
tritium analysis because the early and late fractions are more
8. Reagents and Materials
apt to contain interfering materials for the liquid scintillation
counting process.
8.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
4.2 As the sample distills, there is a gradient in the tritium
all reagents shall conform to the specifications of the Commit-
concentration in the accumulating distillate due to isotope
tee onAnalytical Reagents of theAmerican Chemical Society,
effects; therefore, it is important to collect the same fraction of
where such specifications are available. Other grades may be
the distillate for all samples and standards for tritium analysis.
used, provided it is first ascertained that the reagent is of
4.3 Thecollecteddistillatefractionisthoroughlymixedand
sufficiently high purity to permit its use without lessening the
a portion (up to 10 mL) is mixed with liquid scintillator
accuracy of the determination. Some reagents, even those of
solution, and after dark adapting, is counted in the liquid
highpurity,maycontainnaturally-occurringradioactivity,such
scintillation counting system for tritium beta particle activity.
as isotopes of uranium, radium, actinium, thorium, rare earths,
potassium compounds, or artificially produced radionuclides,
5. Significance and Use
orcombinationsthereof.Consequently,whensuchreagentsare
5.1 Thistestmethodwasdevelopedformeasuringtritiumin
used in the analysis of low-radioactivity samples, the activity
water to determine if the concentration exceeds the regulatory
of the reagents should be determined under analytical condi-
statutes of drinking water. This test method also is applicable
tions that are as close as practicable to those used for the test
for the determination of tritium concentration in water as
sample. The activity contributed by the reagents should be
requiredbytechnicalspecificationsgoverningtheoperationsof
accounted for and applied as a correction when calculating the
nuclear power facilities. With suitable counting technique,
test sample result.
samplesize,andcountingtimeadetectionlimitoflessthan37
8.2 Purity of Water—Unless otherwise indicated, references
Bq/L (1000 pCi/L) is attainable by liquid scintillation.
towatershallbeunderstoodtomeanreagentwaterconforming
to Specification D1193, Type III.
6. Interferences
8.3 Reagents of Distillation Treatment:
6.1 Reduceddetectionefficiencymayresultfromquenching
8.3.1 Sodium Hydroxide Pellets.
in the sample scintillator mixture. Quenching is caused by
8.3.2 Potassium Permanganate.
impurities in the sample, which can inhibit the transfer of
8.4 Background Water, with tritium activity below the
energy,orbycoloredmaterials,whichmayabsorbsomeofthe
emitted light. Corrections for quenching can be made by the minimumdetectableactivity(mostdeepwellwatersarelowin
tritium content).
useofstandardadditionsorbytheratiomethod. Theapproach
describedinthistestmethod,distillationafteralkalineperman-
8.5 Scintillator Solutions:
ganate treatment, eliminates quenching substances, as well as
8.5.1 Dioxane Liquid Scintillator Solution—Dissolve4gof
radionuclides which might be present in a volatile chemical
scintillation-grade PPO (2,5-diphenyloxazole), 0.05 g of
form such as radioiodine and radiocarbon.Aboiling chip must
scintillation-grade POPOP [1,4-bis (5-phenyloxazolyl-2-yl)-
be used with each distillation to avoid bumping, which can
benzene], and 120 g of naphthalene in 1 L of spectroquality,
amount to a carry-over excursion.
1,4-dioxane. Store the solution in a dark (amber) bottle. This
6.2 Scintillator stock solution or samples exposed to day- solution can be used with glass or polyethylene vials.
8.5.2 Solution G Scintillator Solution—Dissolve 18 g of
light must be dark-adapted. Also, toluene- or xylene-base
scintillators exposed to fluorescent lighting should be dark- scintillation-grade PPO (2,5-diphenyloxazole) and 3.6 g of
scintillation-grade BIS-MSB [p-bis (o-methylstyryl) benzene]
adapted for a minimum of 6 h and dioxane base scintillators
exposed to fluorescent lighting for 24 h. All fluors should be in 2 L of spectroquality p-xylene. Add 1 L of Triton N-101
detergent to the p-xylene scintillator solution. Dissolve 50 g of
checked for excitation under lighting conditions being used,
SXS (sodium xylene sulfonate) in 100 mL of water and add
and if possible, they should be exposed only to red light.
7. Apparatus
Corning Part No. 9060 has been found satisfactory for this purpose.
7.1 Liquid Scintillation Spectrometer, coincidence-type.
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington,
7.2 Liquid Scintillation Vials, of low-potassium glass are
DC. For suggestions on the testing of reagents not listed by theAmerican Chemical
recommended. Polyethylene vials may be used when other
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
than dioxane scintillator solution is used.
copeial Convention, Inc. (USPC), Rockville, MD.
The sole source of supply of the apparatus known to the committee at this time
is Rohm and Haas Company, Independence Mall West, Philadelphia, PA 19105. If
Bush,E.T.,“GeneralApplicabilityoftheChannelsRatioMethodofMeasuring you are aware of alternative suppliers, please provide this information to ASTM
LiquidScintillationCountingEfficiencies,” Analytical Chemistry,Vol35,No.1024, International Headquarters. Your comments will receive careful consideration at a
1963. meeting of the responsible technical committee, which you may attend.
D4107 − 20
this solution to the p-xylene scintillator-Triton solution. Mix 11. Procedure
thoroughly. Store the solution in a dark (amber) bottle. This
11.1 Add 0.5 g of sodium hydroxide and 0.1 g of potassium
solution should be used with glass vials since the p-xylene
permanganate to a 100-mL aliquot of the sample in a 250-mL
solvent evaporates slowly through the wall of the polyethylene
distillation flask. Add a boiling chip to the flask. Connect a
vials.
side-arm adapter and a condenser to the outlet of the flask.
8.5.3 Other commercially available scintillators can be
Place a graduated cylinder at the outlet of the condenser. Heat
used, such as the environmentally safe di-isopropyl napthalene
the sample to boiling to distill, collect the first 10 mL of
based scintillators. It is the responsibility of the user to verify
distillate as a separate fraction and discard it.
the acceptability of a substitute scintillator.
11.2 Collectthenext50mLofdistillatefortritiumanalysis.
8.6 Tritium standard solution as tritiated water traceable to
Thoroughly mix the 50-mL distillate fraction.
the SI through a national metrology institute (NMI) such as
NOTE 1—It is important that only the first 10-mLfraction be discarded
NIST, or an ANSI N42.22 reference material provider with a
or the same fraction for samples and standards alike since there is a
concentration of approximately 17 kBq/mL.
gradient in the tritium concentration of the distillate.
11.3 Thoroughly mix 4 mL of the distillate with 16 mL of
9. Sampling
the dioxane scintillator or 10 mL of distillate with 12 mL of
9.1 Collect the sample in accordance with Practices D3370.
Solution G scintillator in a liquid scintillation vial. Three
aliquots of each sample distillate should be analyzed for
9.2 Sincetritiumindrinkingwaterislikelytobeintheform
tritium.
of T O or HTO, there is no need for special handling or
preservation.
11.4 Prepare background standard tritium-water solutions
for counting, using the same amount of water and the same
10. Calibration
scintillator as used in the preparation of samples. Use low
tritium background distilled water for these preparations (dis-
10.1 Determination of Recovery and Detection Effıciency
tillate of most deep well water sources is acceptable, but each
Factors:
source should be checked for tritium activity before using).
10.1.1 Prepare in a 1-L volumetric flask, a tritium standard
11.5 Dark-adaptallsampletestsources(STS),backgrounds,
solution containing approximately 17 Bq/mL using low level
tritiumbackgroundrawwater,RWS(undistilled),andstandard and standards. Count the STS, background subtraction counts,
and standards at least long enough to meet the required
tritium activity. Label this solution as raw water tritium
standard solution, RWTS. detection limit (0.037 Bq/mL) for the sample (see Appendix
X1 for calculating counting time for required detection limit).
10.1.1.1 Distill approximately 600 mL of water obtained
TheDRWSdistillateSTSshouldbecountedforsufficienttime
from the same raw water source (RWS) as above (without
to accumulate at least 50 000 net counts.
tritium activity added). Use this distillate for background
tritiumdeterminations.Usingthedistillateandstandardtritium
12. Calculation
activity, prepare a tritium standard solution in a 500-mL
volumetricflasktocontainthesamespecificactivityastheraw
12.1 Calculate the detection effıciency, ε, and its associated
water tritium standard solution. Label this solution as distilled
uncertainty, u(ε), as follows:
water tritium standard solution, DWTS.
R 2 R
DWTS b
10.1.2 Aqueous Alkaline Permanganate Distillation—Place ε 5 (1)
A
DWTS
a 100-mL aliquot of the RWTS solution in a 250-mL distilla-
tion flask.Add 0.5 g of sodium hydroxide, 0.1 g of potassium R R
DWTS b
S D
permanganate, and a boiling chip. Proceed with the distillate t t u~A !
DWTS b DWTS
ε 5 1ε (2)
u~ !
! 2 S D
according to the procedure described in 11.1, discard 10 mL, A A
DWTS DWTS
and collect 50 mL of distillate for analysis. Mix the 50-mL
where:
distillate fraction. Repeat the distillation with two more
A = activity of distilled water tritium standard, in
DWTS
100-mLaliquotsfortriplicateanalyses.Thisisthedistilledraw
becquerels (Bq),
water tritium standard (DRWTS).
R = background subtraction count count rate, in
b
10.1.3 Prepare for counting three aliquots of the DRWTS
−1
counts per second (s ),
distillate tritium standard solution (from 10.1.2), three aliquots −1
R = distilled water tritium standard count rate (s ),
DWTS
of the DWTS, and three aliquots of the distilled raw water (for
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D4107 − 08 (Reapproved 2013) D4107 − 20
Standard Test Method for
Tritium in Drinking Water
This standard is issued under the fixed designation D4107; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This test method covers the determination of tritium in drinking water by liquid scintillation counting of the tritium beta
particle activity.
1.2 This test method is used successfully with drinking water. It is the user’suser’s responsibility to ensure the validity of this
test method for untested water matrices.
1.3 The tritium concentrations, which can be measured by this test method utilizing currently available liquid scintillation
instruments, range from less than 0.037 Bq/mL (1 pCi/mL) to 555 Bq/mL (15 000 pCi/mL) for a 10-mL sample aliquot. Higher
tritium concentrations can be measured by diluting or using smaller sample aliquots, or both.
1.4 The maximum contaminant level for tritium in drinking water as given by the United States Environmental Protection
Agency (U.S. EPA) National Interim Primary Drinking Water Regulations (NIPDWR)(NPDWR) is 0.740 Bq/mL (20 pCi/mL). The
NIPDWRNPDWR lists a required detection limit for tritium in drinking water of 0.037 Bq/mL (1 pCi/mL), meaning that drinking
water supplies, where required, should be monitored for tritium at a sensitivity of 0.037 Bq/mL (1 pCi/mL). In Appendix X1, Eq
X1.3 is given for determining the necessary counting time to meet the required sensitivity for drinking water monitoring.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D2777 Practice for Determination of Precision and Bias of Applicable Test Methods of Committee D19 on Water
D3370 Practices for Sampling Water from Flowing Process Streams
D3648 Practices for the Measurement of Radioactivity
D7902 Terminology for Radiochemical Analyses
2.2 Other Documents:
ANSI N42.22 Traceability of Radioactive Sources to the National Institute of Standards and Technology (NIST) and Associated
Instrument Quality Control
BIPM-5 Decay Data Evaluation Project (DDEP)
This test method is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.04 on Methods of Radiochemical
Analysis.
Current edition approved June 15, 2013July 1, 2020. Published July 2013July 2020. Originally approved in 1991. Last previous edition approved in 20082013 as
D4107 – 08.D4107 – 08 (2013). DOI: 10.1520/D4107-08R13.10.1520/D4107-20.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’sstandard’s Document Summary page on the ASTM website.
American National Glossary of Terms in Nuclear Science and Technology, available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New
York, NY 10036, www.ansi.org.Available from Institute of Electrical and Electronics Engineers, Inc. (IEEE), 445 Hoes Ln., Piscataway, NJ 08854-4141, http://www.ieee.org.
Available from BIPM, Sèvres Cedex, France, https://www.bipm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4107 − 20
NUDAT2
3. Terminology
3.1 Definitions—Definitions: For definitions of terms used in this test method, refer to Terminology D1129. For terms not
defined in this test method or in Terminology D1129, reference may be made to other published glossaries.
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
3.1.2 For definitions of terms used in this standard relating to radiochemical analysis, refer to Terminology D7902.
4. Summary of Test Method
4.1 In this test method, a A 100-mL drinking water sample aliquot is treated with a small amount of sodium hydroxide and
potassium permanganate, distilled, and a specified fraction of the distillate is collected for tritium analysis. The alkaline treatment
is to prevent prevents other radionuclides, such as radioiodine and radiocarbon from distilling over with the tritium. Some drinking
water supplies will contain trace quantities of organic compounds, especially surface water sources that contain fish and other life.
The permanganate treatment is to oxidize oxidizes trace organics in the sample aliquots which could distill over and cause
quenching interferences. A middle fraction of the distillate is collected for tritium analysis because the early and late fractions are
more apt to contain interfering materials for the liquid scintillation counting process.
4.2 As the sample distills, there is a gradient in the tritium concentration in the accumulating distillate due to isotope effects;
therefore, it is important to collect the same fraction of the distillate for all samples and standards for tritium analysis.
4.3 The collected distillate fraction is thoroughly mixed and a portion (up to 10 mL) is mixed with liquid scintillator solution,
and after dark adapting, is counted in the liquid scintillation counting system for tritium beta particle activity.
5. Significance and Use
5.1 This test method was developed for measuring tritium in water to determine if the concentration exceeds the regulatory
statutes of drinking water. This test method also is applicable for the determination of tritium concentration in water as required
by technical specifications governing the operations of nuclear power facilities. With suitable counting technique, sample size, and
counting time a detection limit of less than 37 Bq/L (1000 pCi/L) is attainable by liquid scintillation.
6. Interferences
6.1 A reduced Reduced detection efficiency may result from quenching in the sample scintillator mixture. Quenching is caused
by impurities in the sample, which can inhibit the transfer of energy, or by colored materials, which may absorb some of the emitted
light. Corrections for quenching can be made by the use of internal standardsstandard additions or by the ratio method. The
approach described in this test method, distillation after alkaline permanganate treatment, eliminates quenching substances, as well
as radionuclides which might be present in a volatile chemical form such as radioiodine and radiocarbon. A boiling chip must be
used with each distillation to avoid bumping, which can amount to a carry over carry-over excursion.
6.2 Scintillator stock solution or samples exposed to daylight must be dark-adapted. Also, toluenetoluene- or xylene base
xylene-base scintillators exposed to fluorescent lighting should be dark-adapted for a minimum of 6 h and dioxane base scintillators
exposed to fluorescent lighting for 24 h. All fluors should be checked for excitation under lighting conditions being used, and if
possible, they should be exposed only to red light.
7. Apparatus
7.1 Liquid Scintillation Spectrometer, coincidence-type.
7.2 Liquid Scintillation Vials, of low-potassium glass are recommended. Polyethylene vials may be used when other than
dioxane scintillator solution is used.
7.3 Distillation Apparatus—For aqueous distillation, 250-mL and 1000-mL round bottom borosilicate flasks, connecting side
arm adapter, condenser, graduated cylinder, boiling chips, and heating mantle.
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where
Available from National Nuclear Data Center at Brookhaven National Laboratory, W Princeton Ave, Yaphank, NY 11980, http://www.nndc.bnl.gov.
Bush, E. T., “General Applicability of the Channels RadioRatio Method of Measuring Liquid Scintillation Counting Efficiencies,” Analytical Chemistry, Vol 35, No. 1024,
1963.
Corning Part No. 9060 has been found satisfactory for this purpose.
D4107 − 20
such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of sufficiently high
purity to permit its use without lessening the accuracy of the determination. Some reagents, even those of high purity, may contain
naturally-occurring radioactivity, such as isotopes of uranium, radium, actinium, thorium, rare earths, potassium compounds, or
artificially produced radionuclides, or combinations thereof. Consequently, when such reagents are used in the analysis of
low-radioactivity samples, the activity of the reagents should be determined under analytical conditions that are as close as
practicable to those used for the test sample. The activity contributed by the reagents should be accounted for and applied as a
correction when calculating the test sample result.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water conforming to
Specification D1193, Type III.
8.3 Reagents of Distillation Treatment:
8.3.1 Sodium Hydroxide Pellets.
8.3.2 Potassium Permanganate.
8.4 Background Water, with tritium activity below the minimum detectable activity (most deep well waters are low in tritium
content).
8.5 Scintillator Solutions:
8.5.1 Dioxane Liquid Scintillator Solution—Dissolve 4 g of scintillation-grade PPO (2,5-diphenyloxazole), 0.05 g of
scintillation-grade POPOP [1,4-bis (5-phenyloxazolyl-2-yl)-benzene], and 120 g of naphthalene in 1 L of spectroquality,
1,4-dioxane. Store the solution in a dark (amber) bottle. This solution can be used with glass or polyethylene vials.
8.5.2 Solution G Scintillator Solution—Dissolve 18 g of scintillation-grade PPO (2,5-diphenyloxazole) and 3.6 g of
scintillation-grade BIS-MSB [p-bis (o-methylstyryl) benzene] in 2 L of spectroquality p-xylene. Add 1 L of Triton N-101
detergent to the p-xylene scintillator solution. Dissolve 50 g of SXS (sodium xylene sulfonate) in 100 mL of water and add this
solution to the p-xylene scintillator-Triton solution. Mix thoroughly. Store the solution in a dark (amber) bottle. This solution
should be used with glass vials since the p-xylene solvent evaporates slowly through the wall of the polyethylene vials.
8.5.3 Other commercially available scintillators can be used, such as the environmentally safe di-isopropyl napthalene based
scintillators. It is the responsibility of the user to verify the acceptability of a substitute scintillator.
8.6 Tritium standard solution as tritiated water traceable to a National Standards Laboratory such as NIST or NPL, the SI
through a national metrology institute (NMI) such as NIST, or an ANSI N42.22 reference material provider with a concentration
of approximately 17 kBq/mL.
9. Sampling
9.1 Collect the sample in accordance with Practices D3370.
9.2 Since tritium in drinking water is likely to be in the form of T O or HTO, there is no need for special handling or
preservation.
10. Calibration
10.1 Determination of Recovery and Detection Effıciency Factors:
10.1.1 Prepare in a 1-L volumetric flask, a tritium standard solution containing approximately 17 Bq/mL using low level tritium
background raw water, RWS (undistilled), and standard tritium activity. Label this solution as raw water tritium standard solution,
RWTS.
10.1.1.1 Distill approximately 600 mL of water obtained from the same raw water source (RWS) as above (without tritium
activity added). Use this distillate for background tritium determinations. Using the distillate and standard tritium activity, prepare
a tritium standard solution in a 500-mL volumetric flask to contain the same specific activity as the raw water tritium standard
solution. Label this solution as distilled water tritium standard solution, DWTS.
10.1.2 Aqueous Alkaline Permanganate Distillation—Place a 100-mL aliquot of the RWTS solution in a 250-mL distillation
flask. Add 0.5 g of sodium hydroxide, 0.1 g of potassium permanganate, and a boiling chip. Proceed with the distillate according
to the procedure described in 11.1, discard 10 mL, and collect 50 mL of distillate for analysis. Mix the 50-mL distillate fraction.
Repeat the distillation with two more 100-mL aliquots for triplicate analyses. This is the distilled raw water tritium standard
(DRWTS).
Reagent Chemicals, American Chemical Society Specifications,ACS Reagent Chemicals, Specifications and Procedures for Reagents and Standard-Grade Reference
Materials, American Chemical Society, Washington, DC. For Suggestionssuggestions on the testing of reagents not listed by the American Chemical Society, see
AnnualAnalar 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.
The sole source of supply of the apparatus known to the committee at this time is Rohm and Haas Company, Independence Mall West, Philadelphia, PA 19105. If you
are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of
the responsible technical committee, which you may attend.
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10.1.3 Prepare for counting three aliquots of the DRWTS distillate tritium standard solution (from 10.1.2), three aliquots of the
DWTS, and three aliquots of the distilled raw water (for background). Mix 4 mL of water with 16 mL of the dioxane scintillator
solution, or 10 mL of water with 12 mL of Solution G scintillator solution in a liquid scintillator vial (glass vials should be used
for detergent-type scintillator solutions). Shake well, dark-adapt the vials overnight, and count in a liquid scintillation counter.
Count each vial long enough to meet the required detection (0.037 Bq/mL) or longer (see Appendix X1 for calculating required
counting time).
11. Procedure
11.1 Add 0.5 g of sodium hydroxide and 0.1 g of potassium permanganate to a 100-mL aliquot of the sample in a 250-mL
distillation flask. Add a boiling chip to the flask. Connect a side-arm adapter and a condenser to the outlet of the flask. Place a
graduated cylinder at the outlet of the condenser. Heat the sample to boiling to distill, collect the first 10 mL of distillate as a
separate fraction and discard it.
11.2 Collect the next 50 mL of distillate for tritium analysis. Thoroughly mix the 50-mL distillate fraction.
NOTE 1—It is important that only the first 10-mL fraction be discarded or the same fraction for samples and standards alike since there is a gradient
in the tritium concentration of the distillate.
11.3 Thoroughly mix 4 mL of the distillate with 16 mL of the dioxane scintillator or 10 mL of distillate with 12 mL of Solution
G scintillator in a liquid scintillation vial. Three aliquots of each sample distillate should be analyzed for tritium.
11.4 Prepare background standard tritium-water solutions for counting, using the same amount of water and the same scintillator
as used in the preparation of samples. Use low tritium background distilled water for these preparations (distillate of most deep
well water sources is acceptable, but each source should be checked for tritium activity before using).
11.5 Dark-adapt all samples, sample test sources (STS), backgrounds, and standards. Count the samples, backgrounds, STS,
background subtraction counts, and standards at least long enough to meet the required detection limit (0.037 Bq/mL) for the
sample (see Appendix X1 for calculating counting time for required detection limit). The DRWS distillate STS should be counted
for sufficient time to accumulate at least 50 000 net counts.
12. Calculation
12.1 Detection Effıciency, ε: Calculate the detection effıciency, ε, and its associated uncertainty,u(ε), as follows:
R 2 R
DWTS b
ε 5 (1)
A
DWTS
R 2 R
DWTS b
ϵ5 (1)
A
DWTS
R R
DWTS b
t t u~A !
DWTS b DWTS
u ϵ 5 1ϵ (2)
~ ! ! S D
A A
DWTS DWTS
R R
DWTS b
S D
t t u~A !
DWTS b DWTS
u ε 5 1ε (2)
~ ! S D
! 2
A A
DWTS DWTS
where:
A = activity of distilled water tritium standard, in becquerels (Bq),
DWTS
−1
R = background aliquot count rate, in counts per second (s ),
b
−1
R = background subtraction count count rate, in counts per second (s ),
b
−1
R = distilled water tritium standard count rate (s ),
DWTS
u(A ) = standard uncertainty of the activity ADWTS (Bq),
DWTS
u(A ) = standard uncertainty of the activity A (Bq),
DWTS DWTS
t = count time for the distilled water tritium standard (seconds), and
DWTS
t = count time for the background sample (seconds).
b
12.2 Recovery Correction Factor, F:
R 2 R
DWTS b
F 5 (3)
ϵ3A
RWTS
R 2 R
DWTS b
F 5 (3)
ε 3A
RWTS
where:
−1
R = count rate of distilled raw water standard (s ), and
DRWTS
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A = activity of (undistilled) raw water tritium standard Bq.
RWTS
12.3 Sample Tritium Activity, AC, for each aliquot:Each Aliquot:
R 2 R
a b
AC 5 (4)
2λt
ϵ3F 3V 3e
R 2 R
a b
AC 5 (4)
2λt
ε 3F 3V 3e
where:
−1
R = sample aliquot gross count rate (s ),
a
−1
R = STS gross count ra
...