ASTM D4453-02(2006)
(Practice)Standard Practice for Handling of Ultra-Pure Water Samples
Standard Practice for Handling of Ultra-Pure Water Samples
SIGNIFICANCE AND USE
The determination of trace impurities (on the order of parts per billion) in ultra-pure water places extreme requirements on all aspects of the analytical system. This is particularly true when ubiquitous species such as sodium and chloride are of interest because they can potentially be introduced as contaminants at almost every step of an analytical procedure. Contamination can occur during sample collection, during sample storage by leaching of improperly cleaned containers, during sample transfer, and by handling with pipets, syringes, etc., and during the actual analysis by contaminated reagents and sample cells and loop systems. It is also possible that trace contaminants can be lost from samples by volatilization or precipitation, by diffusion into the matrix of the container material, and by “plating out” on the walls of sampling lines by flow phenomena.
Strict adherence to a given procedure is necessary to achieve good results at trace levels of analysis because very small differences in procedure execution will affect precision and the addition or loss of nanogram amounts of analyte may affect the accuracy of a determination.
SCOPE
1.1 This practice covers concepts for handling ultra-pure water samples needed for the measurement of ever-decreasing levels of specified impurities that are encountered in the operation of modern high-pressure boilers and turbines. The handling of blanks associated with the analysis of ultra-pure water samples is also covered by this practice. The techniques presented can help the investigator increase the accuracy of analyses performed.
1.2 This practice is applicable to water and steam samples from "zero solids treated" once-through or drum-type boilers, reactor coolant water, electronic grade water, or any other process water where analyte concentrations are in the low parts per billion (micrograms per litre) range.
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. Specific hazards statements are given in 5.2.3.5, 5.1, and 5.3.7.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D4453–02 (Reapproved 2006)
Standard Practice for
Handling of Ultra-Pure Water Samples
This standard is issued under the fixed designation D4453; 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 contaminants at almost every step of an analytical procedure.
2 Contamination can occur during sample collection, during
1.1 This practice covers concepts for handling ultra-pure
sample storage by leaching of improperly cleaned containers,
water samples needed for the measurement of ever-decreasing
during sample transfer, and by handling with pipets, syringes,
levels of specified impurities that are encountered in the
etc., and during the actual analysis by contaminated reagents
operation of modern high-pressure boilers and turbines. The
and sample cells and loop systems. It is also possible that trace
handling of blanks associated with the analysis of ultra-pure
contaminants can be lost from samples by volatilization or
water samples is also covered by this practice. The techniques
precipitation, by diffusion into the matrix of the container
presented can help the investigator increase the accuracy of
material,andby“platingout”onthewallsofsamplinglinesby
analyses performed.
flow phenomena.
1.2 This practice is applicable to water and steam samples
3.2 Strict adherence to a given procedure is necessary to
from “zero solids treated” once-through or drum-type boilers,
achieve good results at trace levels of analysis because very
reactor coolant water, electronic grade water, or any other
small differences in procedure execution will affect precision
processwaterwhereanalyteconcentrationsareinthelowparts
and the addition or loss of nanogram amounts of analyte may
per billion (micrograms per litre) range.
affect the accuracy of a determination.
1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Reagents and Materials
responsibility of the user of this standard to establish appro-
4.1 Purity of Reagents—Reagent grade chemicals shall be
priate safety and health practices and determine the applica-
usedinalltests.Itisintendedthatallreagentsshallconformto
bility of regulatory limitations prior to use. Specific hazards
the specifications of the Committee onAnalytical Reagents of
statements are given in 5.2.3.5, 5.1, and 5.3.7.
theAmerican Chemical Society, where such specifications are
2. Referenced Documents available. Other grades may be used, provided it is first
ascertained that the reagent is of sufficiently high purity to
2.1 ASTM Standards:
permit its use without lessening the accuracy of the determi-
D1066 Practice for Sampling Steam
nation.
D1193 Specification for Reagent Water
4.2 Purity of Water— Reference to high-purity water shall
3. Significance and Use
be understood to mean water conforming to Specification
D1193, Type I reagent water, post treated with an organic
3.1 The determination of trace impurities (on the order of
removal cartridge or demineralized water which has addition-
parts per billion) in ultra-pure water places extreme require-
ally been polished using a cartridge water purification system
ments on all aspects of the analytical system. This is particu-
with an organic removal cartridge and 0.2-µm final filter.
larlytruewhenubiquitousspeciessuchassodiumandchloride
4.3 Hydrochloric Acid (1 + 1)—Dilute concentrated hydro-
are of interest because they can potentially be introduced as
chloric acid with an equal quantity of high purity water.
4.4 NitricAcid(1 + 1)—Diluteconcentratednitricacidwith
This practice is under the jurisdiction ofASTM Committee D19 on Water and
an equal quantity of high purity water.
is the direct responsibility of Subcommittee D19.03 on Sampling Water and
4.5 Nitric Acid, ultra-pure.
Water-Formed Deposits,Analysis of Water for Power Generation and Process Use,
4.6 Methanol.
On-Line Water Analysis, and Surveillance of Water.
CurrenteditionapprovedJuly1,2006.PublishedJuly2006.Originallyapproved
4.7 n-hexane.
in 1985. Last previous edition approved in 2002 as D4453–02. DOI: 10.1520/
D4453-02R06.
This practice suggests the use of specific techniques. As new techniques are
developedorrequiredbylowerlimits,revisionofthispracticewilllikelybeneeded.
3 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or “Reagent Chemicals,American Chemical Society Specifications,”Am. Chemi-
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
Standards volume information, refer to the standard’s Document Summary page on theAmerican Chemical Society, see “Analar Standards for Laboratory Chemicals,”
the ASTM website. BDH Ltd., Poole, Dorset, U.K., and the “United States Pharmacopeia.”
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4453–02 (2006)
4.8 Nitrogen, organic-free. 5.2.3.3 Rinse three times with high purity water.
5.2.3.4 Bottles must be either heated to a minimum of
5. Procedure
400°C in a muffle furnace (or dry heat sterilizer) for at least 30
5.1 Environmental Conditions—Any processes that might min or solvent rinsed as in 5.2.3.5.
contaminatetheanalytesshouldbeexcludedfromthesampling
5.2.3.5 Rinse with solvents in the following order: metha-
and handling area, e.g., smoke, volatile organic solvents, etc.
nol, n-hexane. Gloves worn during the solvent rinse may
(Warning—when performing trace organic analyses, do not
contain plasticizers (phthalates) that may cause contamination.
allow the use of volatile organic solvents or smoking at the
Polyurethane, polyethylene, or nitrile rubber gloves are not
same time and within the area.)
likelytohavephthalatesandshouldbeused.(Warning—when
5.2 Sample Containers and Their Treatment:
rinsing with solvents, use a fume hood with proper exhaust
5.2.1 Analysis of Trace Metals:
flow.)
5.2.1.1 Bottlesmadefromthefollowingmaterialsshouldbe
5.2.3.6 Dry with organic-free nitrogen to drive off the
adequate: TFE-fluorocarbon FEP, HDPE, LDPE, Polypropy-
volatile solvents.
lene, and polycarbonate. Caps should be made of the same
5.2.3.7 Immediately cap the bottle with a TFE-
material or, if not available, the caps should be lined with one
fluorocarbon-lined or aluminum-lined cap which has been
of the suggested materials.
previously cleaned using the same method.
5.2.1.2 FillthebottlewithHCl(1+1)andallowtostandfor
5.2.4 Analysis of Trace Volatile Organics:
48 h at room temperature (80°C for TFE-fluorocarbon), then
5.2.4.1 The sample container must be glass with a TFE-
empty and rinse with high purity water.
fluorocarbon-lined septum and screw cap properly tightene
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