ASTM D4453-91(1997)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D 4453 – 91 (Reapproved 1997)
Standard Practice for
Handling of Ultra-Pure Water Samples
This standard is issued under the fixed designation D 4453; 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.
1. Scope etc., and during the actual analysis by contaminated reagents
and sample cells and loop systems. It is also possible that trace
1.1 This practice covers concepts for handling ultra-pure
contaminants can be lost from samples by volatilization or
water samples needed for the measurement of ever-decreasing
precipitation, by diffusion into the matrix of the container
levels of specified impurities that are encountered in the
material,andby“platingout”onthewallsofsamplinglinesby
operation of modern high-pressure boilers and turbines. The
flow phenomena.
handling of blanks associated with the analysis of ultra-pure
3.2 Strict adherence to a given procedure is necessary to
water samples is also covered by this practice. The techniques
achieve good results at trace levels of analysis because very
presented can help the investigator increase the accuracy of
small differences in procedure execution will affect precision
analyses performed.
and the addition or loss of nanogram amounts of analyte may
1.2 This practice is applicable to water and steam samples
affect the accuracy of a determination.
from “zero solids treated” once-through or drum-type boilers,
reactor coolant water, electronic grade water, or any other
4. Reagents and Materials
processwaterwhereanalyteconcentrationsareinthelowparts
4.1 Purity of Reagents—Reagent grade chemicals shall be
per billion (micrograms per litre) range.
usedinalltests.Itisintendedthatallreagentsshallconformto
1.3 This standard does not purport to address all of the
the specifications of the Committee onAnalytical Reagents of
safety problems, if any, associated with its use. It is the
theAmerican Chemical Society, where such specifications are
responsibility of the user of this standard to establish appro-
available. Other grades may be used, provided it is first
priate safety and health practices and determine the applica-
ascertained that the reagent is of sufficiently high purity to
bility of regulatory limitations prior to use. Specific hazards
permit its use without lessening the accuracy of the determi-
statements are given in Note 1, Note 3, and Note 4.
nation.
2. Referenced Documents 4.2 Purity of Water— Reference to high-purity water shall
be understood to mean water conforming to Specification
2.1 ASTM Standards:
3 D1193, Type I reagent water, or demineralized water which
D 1066 Practice for Sampling Steam
has additionally been polished using a cartridge water purifi-
D 1193 Specification for Reagent Water
cation system with an organic removal cartridge and 0.2-µm
3. Significance and Use
final filter.
4.3 Hydrochloric Acid (1+1)—Dilute concentrated hydro-
3.1 The determination of trace impurities (on the order of
chloric acid with an equal quantity of Type II reagent water.
parts per billion) in ultra-pure water places extreme require-
4.4 NitricAcid(1+1)—Diluteconcentratednitricacidwith
ments on all aspects of the analytical system. This is particu-
an equal quantity of Type II reagent water.
larlytruewhenubiquitousspeciessuchassodiumandchloride
4.5 Nitric Acid, ultra-pure.
are of interest because they can potentially be introduced as
4.6 Methanol.
contaminants at almost every step of an analytical procedure.
4.7 Methylene Chloride, pesticide grade.
Contamination can occur during sample collection, during
4.8 Nitrogen, organic-free.
sample storage by leaching of improperly cleaned containers,
during sample transfer, and by handling with pipets, syringes,
5. Procedure
5.1 Environmental Conditions—Under no circumstances
are experiments using any substance containing sodium or
This practice is under the jurisdiction ofASTM Committee D-19 onWater and
is the direct responsibility of Subcommittee D19.11 onWater for Power Generation
and Process Use.
Current edition approved Oct. 15, 1991. Published January 1992. Originally
published as D4453–85. Last previous edition D4453–85. “Reagent Chemicals,American Chemical Society Specifications,”Am. Chemi-
This practice suggests the use of specific techniques. As new techniques are cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
developedorrequiredbylowerlimits,revisionofthispracticewilllikelybeneeded. theAmerican Chemical Society, see “Analar Standards for Laboratory Chemicals,”
Annual Book of ASTM Standards, Vol 11.01. 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.
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.
D 4453 – 91 (1997)
chloride ions to be conducted or smoking allowed within the 5.2.3.4 Bottles must be either heated at 400°C in a muffle
area where any phase of trace sodium or chloride work is furnace (or dry heat sterilizer) for 30 min or solvent rinsed as
conducted. in 5.2.3.5 if adequate equipment is not available.
5.2.3.5 Rinse with solvents in the following order: metha-
NOTE 1—Precaution:When performing trace organic analyses, do not
nol, methylene chloride. If gloves are worn, there may be
allowtheuseofvolatileorganicsolventsorsmokingatthesametimeand
contamination from plasticizers.
within the area.
NOTE 2—To check for plasticizers (phthalates), soak 0.5 g of the
5.2 Sample Containers and Their Treatment:
material cut into small pieces in 50 mLof methylene chloride. Decant the
5.2.1 Analysis of Trace Metals:
methylene chloride and inject 2 µLinto a GC/MS. Check for the presence
5.2.1.1 Bottles of the following materials should be ad-
of phthalate peaks and if they are present, use another brand of gloves.
equate: TFE-fluorocarbon FEP, linear polyethylene, conven-
NOTE 3—Precaution:When rinsing with methylene chloride, use a
tional polyethylene, and polycarbonate. Caps should be made
fume hood with proper exhaust flow.
of the same material or, if not available, the caps should be
5.2.3.6 Dry with organic-free nitrogen to drive off the
lined with one of the suggested materials.
volatile methylene chloride.
5.2.1.2 FillthebottlewithHCl(1+1)andallowtostandfor
5.2.3.7 Immediately cap the bottle with a TFE-
48 h at room temperature (80°C for TFE-fluorocarbon), then
fluorocarbon-lined or aluminum-lined cap which has been
empty and rinse with Type II water.
previously cleaned using the same method.
5.2.1.3 FillthebottlewithHNO (1+1)andallowtostand
5.2.4 Analysis of Trace Volatile Organics:
for 48 h at room temperature (80°C for TFE-fluorocarbon),
5.2.4.1 The sample container must be glass with a TFE-
then empty and rinse with
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