Ion-Chromatographic Analysis of Anions in Grab Samples of Ultrapure Water (UPW) in The Semiconductor Industry

Designation: D7980 − 15
Standard Guide for

Ion-Chromatographic Analysis of Anions in Grab Samples
of Ultrapure Water (UPW) in the Semiconductor Industry1
This standard is issued under the fixed designation D7980; 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 3.2.1 HDPE, n—high-density polyethylene

1.1 This guide applies to ultrapure water that is thought to 3.2.2 IC, n—ion chromatograph
contain low ppt (parts-per-trillion, weight/weight) levels of
3.2.3 PEEK, n—polyether ether ketone
anionic contaminants (for example, bromide, chloride, fluoride,
nitrate, nitrite, phosphate, and sulfate). To minimize carry-over 3.2.4 ppb, n—parts-per-billion (weight/weight)
problems between analyses, it is best to limit the concentration 3.2.5 ppt, n—parts-per-trillion (weight/weight)
of any one contaminant to approximately 200 ppt (although
this limit is only an approximation and may vary, depending on 3.2.6 UPW, n—ultrapure water
the user’s application).
4. Significance and Use
1.2 This guide is intended to help analysts avoid contami-
nation of ultrapure-water samples, since contamination control 4.1 This guide is intended to help analysts in the semicon-
is the primary challenge when quantifying ppt-level anions in ductor industry. Examples of the usefulness of anion monitor-
grab samples. ing include: (1) determining when ion-exchange resin beds (in
water-purification systems) need to be regenerated, and (2)
1.3 This guide does not include recommendations for col-
ensuring that anion levels are low enough to allow the water to
lecting samples from the water source.
be used for the manufacture of semiconductor devices.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 4.2 To ensure that the anions are indeed at low-ppt levels, it
responsibility of the user of this standard to establish appro- is recommended to check the conductivity of a subsample
priate safety and health practices and determine the applica- before proceeding with Section 5 of this guide. This check does
bility of regulatory limitations prior to use. not need to be exact; its purpose is simply to let the analyst
know if the conductivity is higher than that of the highest-level
2. Referenced Documents standard solution being tested. Any high reading signifies that
the sample, if analyzed, might contaminate the instrument.
2.1 ASTM Standards:2
D1129 Terminology Relating to Water
D5127 Guide for Ultra-Pure Water Used in the Electronics 5. Guidelines
and Semiconductor Industries 5.1 General Considerations:
5.1.1 In working with grab samples of ultrapure water,
3. Terminology concentrate on controlling contamination, which is the over-
3.1 Definitions: riding challenge when analyzing for anions in UPW. Precau-
3.1.1 For definitions of terms used in this standard, refer to tions must be taken, including the following. Wear gloves (for
Terminology D1129. example, nitrile) that do not shed anions. Do not touch
3.2 Acronyms: anything that might contact the samples. Minimize anionic
contamination in the laboratory air; for example, do not work
in the same lab where concentrated mineral acids are being
1
This guide is under the jurisdiction of ASTM Committee D19 on Water and is used or where acid fumes might be brought in by means of the
the direct responsibility of Subcommittee D19.05 on Inorganic Constituents in ventilation system.
Water.
Current edition approved Feb. 15, 2015. Published March 2015. DOI: 10.1520/ 5.1.2 Use only fresh, running-from-the-tap UPW whenever
D7980-15.
2
water is needed. For guidelines regarding maximum contami-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
nation levels allowed in this water, consult Guide D5127;
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on recommendations are based on the type of semiconductor
the ASTM website. device that ultimately is involved. To ensure highest purity and
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
D7980 − 15
minimize the build-up of contamination, keep the water stream UPW and cap for storage. Rinse the cap, too; while rinsing the
flowing at all times (a slow rate is acceptable when the water bottle, leave the cap filled with UPW. Before capping the bottle
stream is not in use). for storage, rinse the cap once more with UPW. In all of these
5.2 Ion Chromatograph (IC): rinsing procedures, use only UPW that has been obtained fresh
5.2.1 Use caution in selecting the IC that will be used for and running from the tap.
these analyses. While an entirely new instrument is not NOTE 1—Early-eluting organic acids (for example, acetate, formate)
mandatory, a unit that has been used for, for example, parts- will be the most difficult species to eliminate from the background.
per-million-level samples often needs extensive clean-up be- 5.4 Preparation of Standards:
fore the anion levels are acceptably low. When utilizing such 5.4.1 Follow the guidelines in 5.3 when selecting,
“used” chromatographs, replace all tubing with new lengths preparing, and storing containers for standards.
and clean the Load/Inject valve thoroughly with fresh, running- 5.4.2 Prepare all standards by weight, not by volume.
from-the-tap UPW; in some cases, the internal parts of this 5.4.3 Prepare all low-level standards [that is, approximately
valve will need to be replaced with new ones. 1 ppb (parts-per-billion, weight/weight) and lower] by pouring,
5.2.2 Use new PEEK (polyether ether ketone) tubing to since transfer pipets will contaminate.
plumb the instrument. 5.4.4 Remake low-level standards (that is, approximately 1
5.2.3 Use a low-back-pressure concentrator column for ppb and lower) daily.
sample loading; install the device such that the sample will be 5.4.5 Prepare and analyze the following types of blanks: (1)
loaded onto the bottom of the concentrator. a sample of the UPW that has been obtained fresh and running
5.2.4 Use columns with the smallest internal diameter from the tap (to test the purity of the UPW used for dilutions),
possible, thereby lowering the amount of sample that must be and (2) a standard-preparation blank. (The second type of
loaded to achieve a given level of sensitivity. Install new (from blank is a water sample that has been through all the prepara-
the manufacturer) columns to avoid carryover from previous tion steps needed to prepare any given working standard; the
applications. only difference is that an aliquot of UPW is added instead of
5.2.5 Keep tubing lengths at a minimum, to decrease dead- the usual stock standard.) When calibrating the IC, use the
volume. second type of blank to obtain data points for inclusion in the
5.2.6 Use columns that will give adequate separation of all calibration curve.
ions of interest and that will provide adequate sensitivity. 5.5 Loading the Concentrator Column:
5.3 Containers for Standards and Samples: 5.5.1 Use loading procedures that minimize contact with
5.3.1 Use new, UPW-soaked plastic [for example, potential sources of contamination. The best choices involve
polystyrene, high-density polyethylene (HDPE)] that will only a single piece of tubing that runs from the sample bottle
bleed down to acceptably low background levels. to the Load/Inject valve of the IC.
5.3.2 Use ONLY fresh, running-from-the-tap UPW for rins- 5.5.2 Do not “store” the aliquot (to be loaded) in a portion
ing and soaking; never use soap or acid to clean containers, as of tubing or other device at any time during the process.
they will introduce high levels of anionic contamination and 5.5.3 If the back pressure is low enough, pull the sample
make background reduction extremely difficult (if not impos- through the concentrator column; otherwise, push the aliquot
sible). through by means of a pressurizable container and inert,
5.3.3 Analyze the soaking water from UPW-soaked new ultrapure gas.
bottles to determine if the anion levels are acceptably low. (Not 5.5.4 Follow manufacturer’s instructions for determining
all brands and formulations of a given plastic type are equally the concentrator column’s break-through volume (that is, the
clean. For example, polystyrene tissue-culture flasks are typi- volume beyond which further concentrating will result in the
cally clean enough, but the background levels depend on the elution of some of the already trapped anions).
manufacturer. Other types of polystyrene containers, such as NOTE 2—Sensitivity of the analysis can be increased by concentrating
coffee cups, are not acceptable). a larger mass of water sample, as long as the break-through volume of the
5.3.4 Dedicate standards bottles to specific concentrations. concentrator column has not been exceeded.
NOTE 3—Automated liquid-handling devices for delivering precise
Also, dedicate a bottle to UPW, for use in making dilutions. volume for pre-concentration technique are acceptable, if such devices
5.3.5 When not in use, keep bottles filled (completely) with have been proven not to contaminate the sample.
UPW that has been obtained fresh and running from the tap.
5.3.6 After each use, immediately rinse bottles with UPW 6. Keywords
by emptying and then refilling at least 3–4 times. Once the 6.1 anions; contamination control; high purity; ion chroma-
cycles have been completed, fill the bottle to the brim with tography; trace analysis; ultrapure water
2
D7980 − 15
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Designation: D7980 − 15

Standard Guide for

1. Scope 3.2.1 HDPE, n—high-density polyethylene

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