ASTM D4453-17

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: D4453 − 16 D4453 − 17
Standard Practice for
Handling of High Purity 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. 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 practice covers concepts for handling high purity 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 high purity 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.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 6.2.3.5, 6.1, and 6.3.7.
2. Referenced Documents
2.1 ASTM Standards:
D1066 Practice for Sampling Steam
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
4. Significance and Use
4.1 The determination of trace impurities (on the order of parts per billion) in high purity 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.
4.2 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.
This practice is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.03 on Sampling Water and Water-Formed
Deposits, Analysis of Water for Power Generation and Process Use, On-Line Water Analysis, and Surveillance of Water.
Current edition approved Feb. 15, 2016Feb. 1, 2017. Published March 2016February 2017. Originally approved in 1985. Last previous edition approved in 20112016 as
D4453 – 11.D4453 – 16. DOI: 10.1520/D4453-16.10.1520/D4453-17.
This practice suggests the use of specific techniques. As new techniques are developed or required by lower limits, revision of this practice will likely be needed.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4453 − 17
5. Reagents and Materials
5.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. 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. 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.
5.2 Purity of Water—Reference to water that is used for reagent preparation, rinsing or dilution shall be understood to mean
water that conforms to the quantitative specifications of Type II reagent water of Specification D1193.
5.3 Hydrochloric Acid (1 + 1)—Dilute concentrated hydrochloric acid with an equal volume of water.
5.4 Nitric Acid (1 + 1)—Dilute concentrated nitric acid with an equal volume of water.
5.5 Nitric Acid, ultra-pure.
5.6 Methanol.
5.7 n-hexane.
5.8 Nitrogen, organic-free.
6. Procedure
6.1 Environmental Conditions—Any processes that might contaminate the analytes should be excluded from the sampling and
handling area, for example, smoke, volatile organic solvents, etc. (Warning—When performing trace organic analyses, do not
allow the use of volatile organic solvents or smoking at the same time and within the area.)
6.2 Sample Containers and Their Treatment:
6.2.1 Analysis of Trace Metals:
6.2.1.1 Bottles made from the following materials should be adequate: TFE-fluorocarbon FEP, HDPE, LDPE, Polypropylene,
and polycarbonate. Caps should be made of the same material or, if not available, the caps should be lined with one of the suggested
materials.
6.2.1.2 Fill the bottle with HCl (1 + 1) and allow to stand for 48 h at room temperature (80°C for TFE-fluorocarbon), then empty
and rinse with water.
6.2.1.3 Fill the bottle with HNO (1 + 1) and allow to stand for 48 h at room temperature (80°C for TFE-fluorocarbon), then
empty and rinse with water.
6.2.1.4 Fill the bottle about one third full with water, cap, shake, and empty. Wear disposable polyethylene gloves when
handling the bottles from this point onward. If a contaminated surface is touched, remove and replace the glove.
6.2.1.5 Repeat 6.2.1.4.
6.2.1.6 Completely fill the bottle with water, cap, and allow to soak for 48 h. After filling, place the bottle in a polyethylene bag
and seal the bag during the storage period. The water should be changed at weekly intervals during long storage periods.
6.2.2 Analysis of Other Trace Ions:
6.2.2.1 Containers made from the following materials should be adequate: HDPE, LDPE, polysulfone, polycarbonate,
polystyrene, polypropylene, and polymethyl pentene. The temperature of the samples should not be above 50°C when taken or
during the storage period to prevent leaching from the containers. (See 6.3.3.)
6.2.2.2 Fill the bottle one third full with water, cap, shake, and empty. Wear disposable polyethylene
...