Background Statement for SEMI Draft Document 5621B
NEW STANDARD: GUIDE FOR DETERMINING THE QUALITY OF ION
EXCHANGE RESIN USED IN POLISH APPLICATIONS OF ULTRAPURE
WATER SYSTEM
Notice: This background statement is not part of the balloted item. It is provided solely to assist the recipient in
reaching an informed decision based on the rationale of the activity that preceded the creation of this Document.
Notice: Recipients of this Document are invited to submit, with their comments, notification of any relevant
patented technology or copyrighted items of which they are aware and to provide supporting documentation. In this
context, “patented technology” is defined as technology for which a patent has issued or has been applied for. In the
latter case, only publicly available information on the contents of the patent application is to be provided.
Background Statement
NOTE: We are answering all the rejects received for Document 5621A. There were many rejects
and the majority of them are related, but none of them are technically persuasive. We are
changing this document subtype to a Guide and not a Test Method standard because the industry
is not familiar with the technique (LNS) that was used in the referenced method validation test
for particle analysis at 10 nm. The previously published SEMI C79 has data verifying the
accuracy of the LNS method.
Advanced semiconductor manufacturing is becoming more and more susceptible to particulate and organic
contamination. Ultrapure water (UPW) piping and piping components undergo rigorous cleanliness testing using the
SEMI F57 standard. While ion exchange (IX) resin has a similar surface area to that of the piping material, it is not
tested for its contribution to UPW contamination. Ion exchange resin used in UPW Polish loops represents a similar
source of contamination to piping materials due to its location in the water-purification process. Fresh ion exchange
resin is known to produce significant amounts of contamination when loaded in polishers. Different resin suppliers
provide different methods of resin preparation. Therefore, the absence of standardized testing and quality analyses
poses the risk of inadequate resin quality.
The value of the guide has become particularly important for the industry due to obvious limitations of the existing
particle metrology for both UPW quality and wafer defect monitoring. Laser Particle Counters (LPCs) used in high
volume semiconductor manufacturing have reached a practical measurement limit of 25 nm, with a counting
efficiency of only a few percent at this size. However, even at 25 nm, the size detection is above the half pitch of
current technology semiconductor devices, rendering the metrology unable to confirm the presence of potential
“killer particles” at the required sizes. The size of the particles to be controlled in UPW is also approaching the
capability of the filtration used. Lack of metrology capability, marginal filtration efficiency, and extremely high
concentration of the particles shedding from the virgin IX resin (see Appendix 2) substantially increase the risk to
the next generation of wafer manufacturing technology. UPW ITRS has suggested a risk-mitigation strategy based
on reduction of the particle challenge to the final filters.
This document describes a guide prepared to standardize the recommended conditions under which the ion exchange
resin quality can be evaluated.
It is important to emphasize that the methodology documented in the proposed guide has numerous limitations,
described below. However, the task force believes that this guide, even with its limitations, can mitigate the risk of
contamination from particle and other impurities. The purpose of this document is to standardize the resin test
conditions to compare the performance of different resins. Use of this guide should generate more data to allow for
revisions that will improve the method. Not having such a guide or having inadequate particle metrology poses
significant risk to advanced semiconductor manufacturing (based on the information from ITRS and SEMETECH)
It is also important to clarify that the type of the PSDS instrument (LNS) used in the guide validation testing is now
commercially available from Fluid Measurement Technologies, allowing wider accessibility to this technique.
References
ITRS documents:
http://www.itrs.net/Links/2013ITRS/2013Tables/Yield_2013Tables.xlsx
http://www.itrs.net/Links/2013ITRS/2013Chapters/2013Yield.pdf
Reference SEMATECH Report: Abbas Rastegar, Arun John Kadaksham, Matt House, Byunghoon Lee, Jae Choi,
Masahiro Kishimoto, Aron J. Cepler, Thomas Laursen, Takeya Shimomura: “EUV Mask and Blank Cleaning
Requirements for 16 nm HP node”. SEMATECH Albany September 2010
Review and Adjudication Information*
Task Force Review
IX Resin TF
Monday, March 30, 2015
2:00 PM to 3:00 PM (Pacific Time)
SEMI Headquarters in conjunction with the
NA Standards Spring 2015 Meetings
City, State/Country: San Jose, CA / USA
Slava Libman (Air Liquide)
Leader(s):
Group:
Date:
Time & Timezone:
Location:
Standards Staff:
Michael Tran (SEMI NA)
408.943.7019
mtran@semi.org
Committee Adjudication
NA Liquid Chemicals TC Chapter
Tuesday, March 31, 2015
2:00 PM to 5:00 PM (Pacific Time)
SEMI Headquarters in conjunction with the
NA Standards Spring 2015 Meetings
San Jose, CA / USA
Frank Parker / ICL
Frank Flowers / PeroxyChem
Michael Tran (SEMI NA)
408.943.7019
mtran@semi.org
*This meeting’s details are subject to change, and additional review sessions may be scheduled if necessary.
Contact the task force leaders or Standards staff for confirmation.
Telephone and web information will be distributed to interested parties as the meeting date approaches. If you will
not be able to attend these meetings in person but would like to participate by telephone/web, please contact
Standards staff.
Semiconductor Equipment and Materials International
3081 Zanker Road
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Phone: 408.943.6900, Fax: 408.943.7943
SEMI Draft Document 5621B
NEW STANDARD: GUIDE FOR DETERMINING THE QUALITY OF ION
EXCHANGE RESIN USED IN POLISH APPLICATIONS OF ULTRAPURE
WATER SYSTEM
1 Purpose
1.1 This document describes a guide for analysis of virgin high purity ion exchange (HPIX) resin suitable for use in
Ultrapure Water (UPW) polish applications. Further information regarding UPW systems can be found in SEMI F61.
1.2 The guide focuses on analysis of ion exchange resin used in UPW. This document defines parameters and test
conditions that will minimize the effect of contamination from the resin on the manufacturing process.
1.3 The purpose of the guide is to avoid prolonged rinse-up of the new resin when it is loaded into ion exchange
(polish) tanks. The guide results should be representative of full-scale applications.
2 Scope
2.1 This document includes instructions for virgin HPIX resin sample handling and test conditions.
2.2 The document provides an example of the performance of state-of-the-art resins; the data was obtained
following this guide. However the quality criteria are expected to be determined by the end user based on the userspecific needs.
2.3 It is the intent of this guide to focus on virgin HPIX resin. The quality parameters assessed by this method
include quantitative measures of particle contribution, metallic contribution, organics contribution, residue after
evaporation (non-volatile residue), and broken beads content.
2.4 The guide takes the wetted-stream performance of virgin HPIX resin into consideration and reflects the current
manufacturing processes of the resin manufacturers.
2.5 Leach-out test methods are referenced within this document provide values for both static and dynamic
conditions. Although the static leach-out test method is sufficient to determine resin quality, the end user will decide
whether to use a dynamic leach-out test method; dynamic test methods provide conditions closer to mimicking the
actual mixed bed operation. Choosing either a dynamic leach test or a static leach test is determined by the end user
needs. Dynamic leach tests will be used to estimate the rinse-up flush volume. Static leach tests will be used for
quality assurance when baseline virgin resin quality has already been established (otherwise use the dynamic leach
test to estimate the rinse-up time).
2.6 Only mixed virgin HPIX resin is used for the test within this document. When the resin is supplied in nonmixed form (anionic and cationic), a mixed sample is used for analysis.
2.7 The guide assumes that the virgin ion exchange resin tested is representative of the virgin HPIX resin to be
loaded in the mixed beds tanks. The resin shelf life, storage, and delivery conditions should be taken into account
when planning the testing.
2.8 This guide applies to virgin HPIX resin as well as Point-of-Use (POU) ion exchange modules intended for use
in semiconductor manufacturing tools and ancillary equipment.
2.9 This guide includes recommended analytical testing that the end user can perform; the end user should
determine which analyses are required and whether to conduct optional testing.
NOTICE: SEMI Standards and Safety Guidelines do not purport to address all safety issues associated with their
use. It is the responsibility of the users of the Documents to establish appropriate safety and health practices, and
determine the applicability of regulatory or other limitations prior to use.
3 Limitations
3.1 This guide applies solely to virgin HPIX resin testing. Quality and performance of the associated equipment
(ion exchange beds, piping and piping components) are not included in the guide.
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
development) activity. All other reproduction and/or distribution without the prior written consent of SEMI is prohibited.
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3.2 Virgin HPIX resin tested by following the guide is intended for use in the Polishing system of ultrapure water
(UPW) systems only (located downstream the UPW tank). The specified test method conditions may exceed the
needs of resin used in primary mixed beds and other less critical applications.
3.3 The guide is designed to assess contamination from the resin in an “as received” state; onsite resin handling
may add contaminants. The effects of the onsite handling are beyond the scope of this document, but should be
considered by the supplier or user.
3.4 Performance of pre-mixed resin vs. mixed in the lab is expected to be different. The sample should be prepared
(mixed) in the same way it is done for the actual application (pre-mixed by manufacturer vs. mixed on site).
3.5 This guide is not intended to supersede customer specifications.
3.6 Virgin HPIX resin samples tested under the conditions specified by this guide may vary in their performance
from the resin used in the actual UPW system. Resin inconsistency should be addressed with the resin supplier or by
conducting a statistical analysis of the resin quality data.
3.7 The accuracy of the data generated by this guide is limited to the accuracy of the analytical techniques used to
measure resin quality.
3.8 Tolerances in the figures used in the guide (such as flow rate, concentration, etc.) are +/-10% unless otherwise
stated.
3.9 This guide application is limited to the ambient temperature UPW system. Other applications, such as Hot UPW
system or different treatment solvent have not been considered in this document.
3.10 The reference data provided in Appendix 2 is representative for 2014 state-of-the-art resin quality and may not
be fully representative for future state-of-the-art resin.
3.11 Limited experience and data are currently available in application of this guide. Additional reproducibility
studies may need to be conducted by the end user when defining performance criteria for the resin tested.
3.12 This guide recommends a simplified option of the static leach test versus dynamic leach test, mimicking actual
Polish mixed operation. Although data in Appendix 2 suggested that static leach test may be representative for the
analysis of the resin performance under dynamic conditions, the choice of the method should take into account the
fact of the limited amount of data collected by the date of publication of this document.
4 Referenced Documents
4.1 SEMI Standards
SEMI E49 — Guide for High Purity and Ultrahigh Purity Piping Performance, Subassemblies, and Final Assemblies
SEMI F40 — Practice For Preparing Liquid Chemical Distribution Components for Chemical Testing
SEMI F104 — Particle Test Method Guide for Evaluation of Components Used in Ultrapure Water and Liquid
Chemical Distribution Systems
SEMI F57 — Specification for Polymer Materials and Components Used in Ultrapure Water and Liquid Chemical
Distribution Systems
SEMI F61 — Guide for Ultrapure Water Systems used in Semiconductor Processing
SEMI F63 — Guide for Ultrapure Water Used in Semiconductor Processing
SEMI S2 — Safety Guideline for Semiconductor Manufacturing Equipment
4.2 ASTM Standards1
ASTM D4779 — Total, Organic, and Inorganic Carbon in High Purity Water by Ultraviolet (UV) or Persulfate
1
ASTM International, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, USA; Telephone: 610.832.9585, Fax: 610.832.9555,
http://www.astm.org
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
development) activity. All other reproduction and/or distribution without the prior written consent of SEMI is prohibited.
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Oxidation, or Both, and Infrared Detection
ASTM D5544 — Standard Test Method for On-line Measurement of Residue After Evaporation of High-Purity
Water
ASTM D5904 — Standard Test Method of Total Carbon, Inorganic Carbon, and Organic Carbon in Water by UV,
Persulfate Oxidation and Membrane Conductivity Detection
4.3 Other Documents
International Technology Roadmap for Semiconductors (ITRS) 2
NOTICE: Unless otherwise indicated, all documents cited shall be the latest published versions.
5 Units
5.1 Parts per million (ppm) is equivalent to μg/mL or mg/L, where 1 L approximately equals 1 kg.
5.2 Parts per billion (ppb) is equivalent to ng/mL or μg/L, where 1 L approximately equals 1 kg.
5.3 Parts per trillion (ppt) is equivalent to pg/mL or ng/L, where 1 L approximately equals 1 kg.
5.4 Micrometer is a unit of length equal to one millionth of a meter, or one thousandth of a millimeter.
6 Terminology
NOTE 1: General terms for UPW systems can be found in SEMI F61.
6.1 Abbreviations and Acronyms — General terms and acronyms used in this standard are listed below and may be
defined in SEMI F61.
6.1.1 DMA — Differential Mobility Analyzer
6.1.2 HPIX — High Purity Ion Exchange Resin used in Polish or POU
6.1.3 HPW — High Purity Water
6.1.4 HVM — High Volume Manufacturing
6.1.5 ICP-MS — Inductively Coupled Plasma Mass Spectrometry
6.1.6 ITRS — International Technology Roadmap For Semiconductors
6.1.7 LC-OCD — Liquid Chromatography With Organic Carbon Detector
6.1.8 LNS — Liquid Nano-Particle Sizing System (example of PSDA used for the Validation Testing – see results
in Appendix)
6.1.9 LPC — Laser Particle Counter
6.1.10 NRM — Nonvolatile Residue Monitor
6.1.11 NVR — Nonvolatile Residue (also called Residue After Evaporation or RAE)
6.1.12 PFA — Perfluoroalkoxy
6.1.13 POU – Point of Use
6.1.14 PSDA — Particle Size Distribution Analyzer
6.1.15 PVDF — Polyvinylidene Fluoride
6.1.16 SEM — Scanning Electron Microscope
6.1.17 TOC — Total Organic Carbon
6.1.18 UPW — Ultra Pure Water
6.2 Definition
2
http://www.itrs.net/
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
development) activity. All other reproduction and/or distribution without the prior written consent of SEMI is prohibited.
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6.2.1 Background — the contaminant concentrations in the test system reported by analyzers such as PSDA, NRM,
TOC, and others. Background is measured in the static leach test containers or when UPW flows through the
dynamic leach test skid (after rinsed and cleaned components have reached a steady-state of background
contamination). Background includes contributions from the UPW and the test equipment components.
6.2.2 Delta Measurement — the UPW contaminant analyte concentration difference between the inlet of the resin
column and the outlet of the resin column. Useful when the inlet analyte concentration is too unstable during the test
period to allow the proper use of an average background measurement. Delta Measurement can be achieved by
using two calibrated analyzers that have had their responses matched on the same water sample.
6.2.3 Dynamic Leach Test Skid (see Figure 1) — the system providing resin-evaluation test analysis. The test skid
includes piping, resin column, flow meters, pressure gauges, valves, regulators, sample ports, etc.
6.2.4 Virgin HPIX Resin — an unused high quality ion exchange resin that has not been regenerated.
UPW return or drain
Vent to
drain
P2
P1
UPW
UPW
Particle
Sizing/Counting
Monitor
UPW return or drain
48" Long
1" I.D.
Non-volatile
Residue Monitor
UPW return or drain
Total Organic
Carbon Monitor
UPW return or drain
Total effluent
flow rate - 420 _
+ 20 mL/min
Temp
UPW return or drain
Vent to
drain
Figure 1
General Test Schematic Diagram for Dynamic Leach Test
7 Dynamic Leach Test Skid Configuration
7.1 The dynamic leach test skid should be made of high purity components, meeting SEMI F57 quality
requirements. Figure 1 presents the required configuration of the skid. The ion exchange column is made of PVDF
with PFA tubing connecting the column to the UPW system and analytical equipment.
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
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7.2 Minimum operating pressure should be sufficient to feed the instruments downstream of the ion exchange
column, typically 25 psig (172 kPa). Install the pressure gauges and flow meters downstream or sidestream to avoid
contamination. Pressure on the feed side to the column should be 207-310 kPa (30 – 45 psig) to reduce potential
micro-bubble formation. The high pressure limit depends upon the materials of construction (for safety and leak
prevention).
7.3 Use ultrapure, low-particle, low-TOC, low-shedding piping systems in all wetted flow paths from the UPW
source to the dynamic leach test skid to ensure that adequate water quality is maintained. Consider the
recommendations within SEMI E49 when designing and assembling the system.
7.4 Protect the test system from excessive vibration which could lead to high particle-background counts.
7.5 Minimum operating pressure downstream of the dynamic leach test skid should be 138 kPa (20 psig) during
testing to avoid gas bubbles.
7.6 The UPW should be in compliance with the following minimum requirements:
7.6.1 Temperature: 23 5C (77  9F).
7.6.2 Resistivity: 18 MΩ•cm at 25°C (77°F).
7.6.3 TOC: < 2 ppb.
7.6.4 NVR: < 0.2 ppb.
7.6.5 Maximum recommended particle-concentration background level: <1 particle/ml (> 0.05 m). Background
particle levels measured by PSDA are dictated by the resin performance expectations (see Figure A2-2, Appendix
2)
7.6.6 To ensure a stable background level, before beginning the test install and rinse the ion exchange column in an
enclosed ISO Class 7 (per current revision of ISO 14644, roughly equivalent to FED STD 209E Class 10,000), or
better, environment. Follow procedures necessary to maintain ISO Class 7, or better, when handling any part of the
test system, or during the testing. Deviation from these conditions may be approved by the end user, while
maintaining the intent of the clean environment. End users requiring more exacting testing should follow more
stringent testing requirements.
7.6.7 Instrumentation, including flow meters, pressure gauges/transducers and temperature sensors, are calibrated in
accordance with the manufacturers’ procedures and frequency.
7.6.8 Bubbles cause metrology errors; orient the test column and the plumbing between the components under test
to limit bubble entrapment. Position the ion exchange column vertically and vent the test skid to prevent gas
accumulation and bubble formation. Exception: UPW flow through the ion exchange column must be from the top
to the bottom to prevent resin separation. Provisions must be included in the test stand to capture and divert bubbles
before they enter the instrumentation supply lines.
8 Sample Recommendations
8.1 Test a representative ion exchange virgin resin sample from the batch under consideration.
8.2 To take a virgin resin sample from the drums at the end user location, follow this procedure:
8.2.1 Avoid construction and other maintenance activities in the area where the sample is taken.
8.2.2 Rinse the outside of the drums with high purity water before opening to remove contamination collected
during transport and storage. Allow the water to drip off the drums.
8.2.3 Don clean room suit and low-zinc gloves.
8.2.4 Prepare clean bags for the resin sampling and shipping. Use double-bagged packaging (the inner bags should
be qualified for lower particulates, while the outer bags should have low gas permeability).
8.2.5 Take resin from a previously unopened drum.
8.2.6 Open a representative drum and open the protective bags inside the drum.
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
Permission is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
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8.2.6.1 If resin prepared for testing is supplied from different batches or was stored under different conditions, you
may need to test more than one sample.
8.2.6.2 If the amount of resin in a single drum is < 10% of the total amount of the resin to be used, you may need to
sample more than one drum in order to obtain representative results.
8.2.7 Sample resin immediately after you open the drum.
8.2.7.1 Take the sample from the top of the drum to prevent excess liquid from being taken with the sample.
8.2.7.2 Remove approximately 5 cm (2”) of the upper resin layer.
8.2.7.3 Take 1L of the resin sample for a static leach test and 1L for a dynamic leach test.
8.2.7.4 Minimize exposure of the resin sample to ambient contamination.
8.2.7.5 Use gentle motion to avoid damaging the resin beads.
8.3 Place the resin in a prepared clean bag and seal the bag.
8.4 Wrap the resin sample in bubble wrap to protect it during shipping.
8.5 Place the resin sample in a cooler and ship to the lab using fast direct delivery (do not exceed one week in
shipment). Add “FRAGILE” sticker.
NOTE 1: Resin sample handling and packaging may impact the test results. Samples submitted for testing should reflect standard
practices of handling and packaging by the resin manufacturer in accordance with the typical manufacturing processes.
9 Test Methodology
9.1 Leach-Out Parameters
9.1.1 This document does not provide specific quality requirements for leachable parameters. The end user must
define quality requirements based upon the process-specific sensitivity to contamination, the ion exchange polish
system design, and the data provided in Appendix 2. The results in Appendix 2 are based on the benchmarking study
and indicate the actual range of performance of typical resins used in ion exchange polish applications.
9.1.2 Success criteria considerations for TOC and particle release. Contamination by organic compounds causes
silicon oxidation, affects etching uniformity, wafer and mask cleaning, adhesion of the resist, gate oxide breakdown
voltage, epitaxial growth, atomic layer deposition (ALD), chemical vapor deposition (CVD) of silicon nitride or
other thin film deposition.
9.1.2.1 Loading virgin HPIX resin for applications with tight target levels for TOC and particles poses risk to the
final UPW quality.
9.1.2.1.1 In HVM facility where a number of parallel polish mixed beds are used, TOC contribution of less than 0.3
ppb is considered insignificant if the resin is replaced in only one of the parallel polish tanks. The UPW from
additional tanks dilutes the TOC from the tank with new virgin resin.
9.1.3 Critical particle size is specific to the end user’s manufacturing process and technology. Particles released by
the virgin HPIX resin can contaminate devices and critical surfaces as well as disrupt the photolithography process,
thereby decreasing yields.
9.1.4 Based upon the UPW particle concentration target (in particles per liter) and the assumption that the final
filter will provide some particle retention, the end user can estimate the acceptable particle concentration for the
polish tank effluent. If the resin change-out is spread over a year particle leach out from additional tanks dilutes the
particle concentration from the tank being measured.
9.1.5 Metal leach consideration also depends upon the end user metal specifications. Metallic contamination can
alter the electrical properties of microelectronic devices and corrode or etch microelectronic devices and critical
surfaces during fabrication, causing immediate or future device failure.
9.1.6 For high purity applications susceptible to metals contamination, the end user should conduct an HCl leach
using quality criteria based on Appendix 2 “best in class” performance. For less critical applications, it is
recommended that UPW extraction is used with all metals to be below the detection limits, as indicated in Appendix
2.
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
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9.1.7 One week rinse time is considered the maximum acceptable time period based on the common industry
practice.
NOTE 2: Using the performance quality criteria, “best in class” HPIX resin is recommended where tightest quality is required
(per Appendix 2). Application of stringent requirements may affect schedule and cost.
9.2 Other Parameters
9.2.1 The following recommendations are provided for estimating the whole-bead content.
NOTE 2: If the virgin HPIX resin does not meet end user quality requirements, the end user should consult the resin supplier.
9.2.1.1 Whole bead content: the virgin ion exchange resin is considered acceptable for use in polish tanks if the
resin contains > 90% of whole and non-cracked beads and > 95% of unbroken beads.
9.3 Particle Contribution Test
9.3.1.1 UPW is used for the particle contribution testing. The following instruments are employed:
9.3.1.2 In-situ PSDA
9.3.1.3 In-situ NRM (if most of the NVR = particles)
9.3.1.4 Grab sample LPC
9.3.1.5 Grab Sample PSDA
9.3.1.6 Grab Sample SEM
9.3.2 The Dynamic Leach Test evaluates particle contribution performance of the virgin ion exchange resin in a
continuous flushing mode and provides an indication of the volume of UPW required to bring particle levels to meet
the end user’s requirements.
9.4
Organic Contamination
9.4.1 The measurement of TOC is a common water quality screening method for organic materials; maximum TOC
levels should be < 0.5ppb but the actual effects of the individual compounds can depend on the structure of the
molecules, and the semiconductor manufacturing processes. Any organic compound in ultrapure water is a potential
nutrient to increase bacterial growth. Methods other than measuring TOC, such as LC-OCD, may be required to
assess the identification of individual organic contaminants.
9.4.1.1 The TOC analyzer must correctly measure the organic Carbon contained in organic compounds that also
include Nitrogen, Sulfur, Phosphorus, and Chlorine in their structures.
9.4.1.2 Use LC-OCD to identify either unusual organic compounds or those compounds that are present in
unusually high concentrations. Refer to the example of an LC-OCD chromatogram shown in Appendix 2.
9.4.1.3 Use the static leach test to evaluate virgin ion exchange resin quality, using Appendix 2 data for reference.
9.4.1.4 Use the dynamic leach test to evaluate the TOC rinse-up volume, this is effective when done in conjunction
with particle testing. If the source UPW TOC level fluctuates during the test period, a delta measurement between
the column inlet and outlet for the TOC may be required.
9.4.2 The temperature of virgin ion exchange resin during a static leach test should be 40 ± 3°C. A temperature
specification is used to achieve comparable data for ion exchange resin and components and is not indicative of
service temperatures.
9.4.3 Report measured values of TOC in micrograms of contamination per liter of resin tested (g/L). Detection
limits (also defined in g/L) should be reported for all measured values of TOC.
NOTE 3: The static leach test using UPW, even one of a15-hour duration, has limitations. The values measured using a static
leach test do not directly relate to the trace contaminant values which could be present in a flowing stream of liquid. Virgin ion
exchange resin quality can be defined using the correlation studies for dynamic and static leach tests shown in Appendix 2.
9.4.4 Metallic Contamination Test
9.4.4.1 Metallic contamination specifications and testing may be needed for ion exchange virgin resin samples
tested. It is particularly important for UPW applications where sensitivity to trace metals is high.
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
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9.4.4.2 Virgin HPIX resin should conform to the end user’s specifications. In a UPW the static leach test, no metals
should be detected in the leach solution. Refer to Appendix 2 for information on the metal extractable.
9.4.5 Use either UPW or acid for the static leach tests.
9.4.5.1 Use a static leach test with UPW for all semiconductor applications.
9.4.5.2 Use a static leach test with HCl for processes susceptible to metal contamination.
9.4.6 The temperature of virgin of ion exchange resin during a static leach test should be 40 ± 3°C for UPW and the
ambient temperature (23± 2°C) for HCl. A temperature specification is used to achieve representative data for ion
exchange resin and is not indicative of service temperatures.
9.4.7 Report measured values of metallic contamination in micrograms of contamination per liter of resin tested
(g/L). Detection limits (also defined in ug/L) should be reported for all measured values.
NOTE 4: The static leach test using UPW or HCl, even one of a 15-hour duration, has limitations. The values measured using a
static leach test do not directly relate to the trace contaminant values which could be present in a flowing stream of liquid.
9.5 Broken Beads
9.5.1 Broken Beads may indicate a problem in the resin manufacturing or handling process and cause clogging in
the resin beds. Virgin HPIX resin with many broken beads may also produce high particle content. Check the resin
for broken or cracked beads before conducting any other tests.
9.5.2 Using deionized water and a representative sample of the virgin HPIX resin, prepare four microscope slides.
Do not allow the slides to dry out. Count the number of each bead classification as described below:
9.5.2.1 Count the number of whole perfect beads, cracked but whole beads, and broken fragments (equal to or
larger than half a bead) in the samples on the slides. Record the numbers until the total number of beads counted is
> 100.
9.5.2.2 The total number of beads counted is defined as:
Total Beads = Number of Whole Perfect Beads + Number of Cracked but Whole Beads +
Number of Broken Beads / 2
(1)
NOTE 6: Division of broken beads by a factor of 2 implies that the bead is split into two pieces and both are counted. Although
the reality may be different, this approach provides a normalized estimate taking into account various possibilities.
9.5.2.3 Calculation and Results:
(A) % Whole = Number of Whole Perfect Beads × 100 / Total Beads
(2)
(B) % Cracked = Number of Cracked But Whole Beads × 100 / Total Beads
(3)
(C) % Broken = Number of Broken Beads × 100 / Total Beads
(4)
Verify that: (A) % + (B) % + (C) % = 100%
(5)
9.5.3 Repeat the bead count on the other three slides and calculate the average result.
9.5.4 Success Criteria: If B<10% and C<5%, the resin is acceptable for the use in polish tank.
NOTE 7: Follow the sample handling recommendations in § 8 of this document.
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
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10 Leach Test Procedures
10.1 General Procedures
10.1.1 The preferred order of test method steps is shown below. The shaded cell indicates pre-screening steps.
Reject any virgin HPIX resin samples that do not meet any of the pre-screening criteria.
Broken Bead Content — establishes basic integrity of the resin beads
↓
Make Go/No Go Decision
↓
Particle test — assesses the leach-out potential of particles from the virgin ion exchange resin beds using a static
leach test
↓
Optional particle test — assesses the time to rinse particles from the resin using a dynamic
leach test.
↓
Optional particle test — assesses the elemental composition and particles dimensional
characteristics using SEM
↓
Organics test — assesses the leach-out potential of organic compounds from the virgin ion exchange resin beds
using a static leach test.
↓
Optional organics test – assesses the time to rinse particles from the resin using a dynamic
leach test.
↓
Optional organics speciation test – speciates organics using LC-OCD (static leach test sample)
↓
Metal test — assesses the leach-out potential of metals from the virgin ion exchange resin beds using a UPW
static leach test.
↓
Optional metal test— assesses the leach-out potential of metals from the virgin ion exchange
resin beds using an HCl static leach test.
↓
Create Final Report
Figure 2
The Test Method Process Flow
11 Test Procedure
11.1 Dynamic Leach
11.1.1 The dynamic leach test determines the projected UPW volume and time required to rinse the virgin HPIX
resin (see Appendix 2 for an example of test data).
11.1.1.1 Preparations/Equipment:
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11.1.1.2 Column dimensions represent a full-scale polish tank 2.54 cm (1inch) diameter by 121.92 cm (4ft) bed
depth. See § 7 for column details.
11.1.1.3 Column Material: refer to § 7.1.
11.1.1.4 Hydraulic conditions: Representative of full-scale polish tanks 0.049 m/s (20 gpm/ft2).
NOTE 7: If the polish tank is rinsed under lower flow than the normal operation flow, the particle level may increase once the
bed put on-line.
11.1.1.5 Metrology: PSDA, NRM, TOC.
11.1.1.6 Establish a test baseline by running UPW through the empty column until all the required parameters are
met. TOC = test skid background level. Particles non-detect, (at the noise level) for PSDA and NVR = test skid
background level.
11.1.1.7 Pack column in an ISO Class 7 or better, environment (per current revision of ISO 14644, roughly
equivalent to FED STD 209E Class 10,000).
11.1.1.8 To avoid separation, do not make slurry of the resin. Do not agitate the column (pack as you load by
tapping on the walls).
11.1.1.9 Column pre-flush: Install the test column in the test apparatus (see Figure 1). Direct effluent to a drain or
reclaim it; to prevent bubbles from being introduced, do not allow effluent to enter the on-line metrology. To avoid
hydraulic shock, slowly open the UPW valves. Slowly fill the column from the top while venting excess air from the
top and bottom of the column.
11.1.1.10 When the column is full of water, increase the UPW flow rate to 1 LPM and flush for three minutes.
11.1.1.11 Reduce the flow to 0.42 LPM and start measuring effluent.
11.1.1.12 Data Collection: Run UPW through the column for three days and collect data from PSDA, NRM, TOC.
11.1.1.13 Subtract background TOC values from the test data provided a stable background is maintained
throughout the test (incoming TOC does not vary by more than ± 0.1 ppb). If incoming TOC varies by more than ±
0.1 ppb, subtract the actual incoming TOC (instantaneous) from the downstream TOC data.
11.1.1.14 Prepare Report: Plot a log/log linear regression and extrapolate the time taken to achieve the success
criteria.
11.1.1.15 The linear log-log slope may change as the surface rinse mechanism can be replaced with diffusion out of
the resin beads.
11.2 Static Leach
11.2.1 Preparations/Equipment:
11.2.1.1 Container Material: High purity PFA to minimize background contamination. The container must be precleaned and qualified for the tests to be conducted.
11.2.1.2 The criteria for the qualification imply that all the parameters tested in the container filled with UPW
should be either less than detection limits or significantly lower than the values of the test results. Background
values higher than detection limits should be included in the report.
11.2.1.3 Container made from the same materials as in ¶ 10.2.1.1 filled with UPW (used for background subtraction
in the report).
11.2.1.4 Container volume must be sufficient for the analyses (at least 500 mL). If optional PSDA grab sample test
is chosen additional 200-250 ml volume is required for the analysis.
11.2.1.4.1 Mark the working level of the container.
11.2.1.5 Measure working volume of the container by filling it with UPW to the level to be used in the test.
11.2.1.6 Volume ratio: 2:1 of UPW to resin ratio.
NOTE 8: Resin shrinks as it is mixed with UPW.
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
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11.2.1.7 UPW quality: Minimum background contribution 18+ MΩ∙cm, < 10 ppb TOC, minimum 0.1μm final filter
pore size.
11.2.2 Metrology
11.2.2.1 Particles: LPC (0.3-1µm), PSDA (optional for critical applications, 10nm - 0.5 µm), SEM (optional for
troubleshooting)
11.2.2.2 Organics: Analyze with a TOC meter or LC-OCD for speciation (optional).
11.2.2.3 Metals: Analyze with ICP-MS.
11.2.3 UPW Static Leach Test Procedure:
11.2.3.1 Add ~200 mL of resin to the pre-cleaned 500 mL PFA container.
11.2.3.2 Fill container with UPW. Measure the total volume of the container and the volume of UPW added to the
resin. Calculate the resin volume by subtracting the UPW volumes from the total container volume.
11.2.3.3 Pre-rinse the resin: Manually shake the container; pour off as much water as possible, while being careful
not to lose any of the resin.
NOTE 9: Shake the container gently.
11.2.3.4 Repeat step in ¶ 11.2.3.3 ten times.
11.2.3.5 Conduct UPW static leach test: fill the container with UPW and place in an oven at 40± 3C for 15 hrs.
11.2.3.6 Remove container from oven.
11.2.3.7 Shake (using orbital shaker) at 75 rpm for one hour.
11.2.3.8 Pour off the UPW and collect samples for measuring particles by LPC, SEM (optional) and PSDA
(optional), as well as metals, TOC, and organic speciation (optional).
11.2.4 Conduct HCl static leach test (optional):
11.2.4.1 Place 10g of resin in a 125mL PFA bottle with 50 ml 1:3HCl (35%) solution at ambient temperature.
11.2.4.2 Manually shake the resin/HCl solution for 10 seconds.
11.2.4.3 Leach for one hour.
11.2.4.4 Manually shake the leach solution for 10 seconds and then allow the resin to settle for 30min.
11.2.4.5 Pour off acid solution for metals analysis.
11.2.4.6 Blank solution should be prepared following the same steps of the resin extraction. The blank values
should be included in the report.
NOTE 10: Acid purity should be high to allow for detection of the metals at the required level of the specification.
12 Resin Quality Validation
12.1 The virgin HPIX resin supplier should define, establish, and execute a testing program for the resin based
upon the definitions outlined in this document. The testing program should specify the frequency of resin testing and
identify any necessary corrective action plan if the resin does not meet the quality needs of the end user.
12.2 The resin is considered to be representative of the entire batch. Samples should be randomly selected from a
batch manufactured under current production processes.
13 Related Standards and Other Documents
S. Huber, A. Balz, M. Abert, W. Pronk (2011). Characterization of aquatic humic and non-humic matter with sizeexclusion chromatography e organic carbon detection e organic nitrogen detection (LC-OCD-OND). Water
Research, volume 45, issue 2, January 2011
This is a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
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14 Summary Report Form
Material Description
Material Manufacturer:
Material Part #:
Material Serial #:
Section
______________________________
______________________________
______________________________
______________________________
Description of Test
Lab(s) Used: ________________________________________
Dates of Analysis ____________________________________
Leaching Volume (ml)_________________________________
Leaching Surface Area (m2)_____________________________
Specification Value
(See #1)
11.1
11.2
11.2
11.2
11.1
11.2
9.5
Measured
Value
Conforms? √
(See #2)
Particle Contribution Rinse Test
(indicate particle target size used
for PSDA)
PSDA results for static leach
(indicate particle target size used
for PSDA)
Particles Leach, #/ml resin
>0.3u
>0.5u
>1 u
Metallic Contamination
(indicate type of the Leach
procedure)
Aluminum
Arsenic
Barium
Boron
Calcium
Chromium
Copper
Iron
Lead
Lithium
Magnesium
Manganese
Nickel
Potassium
Sodium
Strontium
Zinc
Cobalt
Tin
Total Organic Carbon (TOC)
Contamination from Rinse Test
Total Organic Carbon (TOC)
Contamination from Static Test
Broken Beads, %
#1 Fill in the appropriate specification.
#2 If a specific test is not required, write “N/A.”
By my signature, I hereby sign that the above
information is correct.
Signature:
Detection
Limits
-
UPW or HCl Leach
-
Comments:______________________________
_______________________________________
_______________________________________
_______________________________________
_______________________________________
_______________________________________
_______________________________________
_______________________________________
___
_______________________________
____________
Print
Name:_________________________________
_________
Date:
_______________________________
This is ____________
a Draft Document of the SEMI International Standards program. No material on this page is to be construed as an official or adopted Standard or Safety Guideline.
Permission
is granted to reproduce and/or distribute this document, in whole or in part, only within the scope of SEMI International Standards committee (document
Company
development) activity. All other reproduction and/or distribution without the prior written consent of SEMI is prohibited.
Name:_________________________________
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APPENDIX 1
ILLUSTRATION OF PERFECT WHOLE AND CRACKED BEADS
NOTICE: The material in this Appendix is an official part of SEMI [designation number] and was approved by full
letter ballot procedures on [A&R approval date].
Figure A1-1
Perfect Beads
Figure A1-2
Cracked Beads
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APPENDIX 2
VALIDATION TESTING OF THE RESIN QUALITY ASSESSMENT
PROCEDURE
NOTICE: The material in this Appendix is an official part of SEMI [designation number] and was approved by full
letter ballot procedures on [A&R approval date].
A2-1 Validation Testing for the Resin Quality Assessment Procedure
A2-1.1 Prepared by Balazs and CT Associates, Inc. of the SEMI IX Task Force.
A2-2 Dynamic Rinse Testing
A2-2.1 Test Parameters:

Particles by LNS

Organics by TOC

Non-volatile residue by NRM

Performed by CT Associates, Inc.

1” PVDF columns

Samples provided by Siemens, Lanxess, Purolite, Itochu (Mitsubishi), and Kurita

The data is presented anonymous with random order of samples used the same letter assignments to
suppliers were used in the dynamic and static tests
UPW return or drain
Vent to
drain
P2
P1
UPW
UPW
Particle
Sizing/Counting
Monitor
UPW return or drain
48" Long
1" I.D.
Non-volatile
Residue Monitor
UPW return or drain
Total Organic
Carbon Monitor
UPW return or drain
Total effluent
rate rate - 420 mL/min
UPW return or drain
Vent to
drain
Figure A2-1
Test Apparatus
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Table A2-1 Background Levels
Resin Sample
TOC (ppb)
NVR (ppt)
Particles ≥ 10 nm (#/ml)
A
0.69
220
1.29E+07
B
0.65
209
1.20E+07
C
0.79
262
1.22E+07
D
0.71
241
1.40E+07
E
0.68
226
1.40E+07
F
0.49
197
1.14E+07
Spool
0.66
238
1.51E+07
Average
0.67
228
1.31E+07
Standard Deviation
0.09
22
1.33E+00
Cv (%)
13.6%
9.5%
10.1%
1.9
0.18
42
2.60E+00
NOTE 11: “Spool” represents the test resin column with no resin.
Cumulative Particle Concentration Added
(#/mL > 10 nm)
1e+9
Resin A
Resin B
Resin C
Resin D
Resin E
Resin F
Spool
1e+8
1e+7
1e+6
1e+5
1
10
100
1000
Flush Volume (liters UPW)
Figure A2-2
Cumulative Particle Concentration Measured in Dynamic Leach Test
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1e+10
Cumulative Particle Concentration
(#/mL > 10 nm)
Resin A
Resin B
Resin C
Resin D
Resin E
Resin F
Spool
Ave Background
1e+9
1e+8
1e+7
1e+6
0
500
1000
1500
2000
Flush Volume (liters UPW)
Figure A2-3
Cumulative Particle Concentration Measured in Dynamic Leach Test (linear coordinates)
5000
Resin A
Resin B
Resin C
Resin D
Resin E
Resin F
Spool
Ave. Background
Non-volatile residue (ppt)
4000
3000
2000
1000
0
500
1000
1500
2000
Flush Volume (liters)
Figure A2-4
Non-volatile Residue Measured in Dynamic Leach Test (linear coordinates)
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Non-volatile residue added (ppt)
10000
Resin A
Resin B
Resin C
Resin D
Resin E
Resin F
Spool
1000
100
10
1
10
100
1000
Flush Volume (liters)
Figure A2-5
Non-volatile Residue Measured in Dynamic Leach Test (log-log coordinates)
14
Resin A
Resin B
Resin C
Resin D
Resin E
Resin F
Spool
Ave. Background
12
TOC (ppb)
10
8
6
4
2
0
1
10
100
1000
Flush Volume (Liters)
Figure A2-6
TOC Measured in Dynamic Leach Test (linear-log coordinates)
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100
Resin A
Resin B
Resin C
Resin D
Resin E
Resin F
Spool
TOC added (ppb)
10
1
0.1
0.01
1
10
100
1000
Flush Volume (Liters)
Figure A2-7
TOC Measured in Dynamic Leach Test (log-log coordinates)
NOTE 12: Unstable TOC values at the end of the experiments were due to the effect of the UPW temperature on the TOC
leachouts from the tested resin (TOC instrument provided temperature compensation).
Table A2-2 Dynamic Leach Summary
Particles ≥ 10nm
NVR
TOC
Sample ID
1E+7/ml
added (liters
UPW)
1E+6/ml
added (liters
UPW)
500 ppt
added (liters
UPW)
50 ppt
added (liters
UPW)
1 ppb added
(liters UPW)
0.2 ppb
added (liters
UPW
A
140
760
2
160
65
>1800
B
16
40
<1
<10
25
120
C
170
820
<1
<10
80
>1800
D
250
900
190
300
140
>1800
E
1020
>2000
240
>2000
215
>1800
F
190
1100
140
NA
205
1000
Spool
3
50
<1
<10
<1
<1
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A2-3 Static Leach Testing
A2-3.1 Test Parameters:

Metals by ICPMS

Particles by LPC, SEM, and LNS

Organics by TOC and LC-OCD

Performed by Air Liquide, Balazs

o
500 ml PFA container, Volume ratio 1:1 UPW to resin thorough pre-rinse 40°C leach (15 hrs.),
followed by 1hr. agitation
o
Samples provided by Siemens, Lanxess, Purolite, Itochu (Mitsubishi), and Kurita
o
The data is presented anonymous with random order of samples used
Numbering of the resin in both Dynamic and Static leach tests is consistent
Table A2-3 Total Organic Carbon and TOC Speciation of the Static Leach Samples
Organics, ppb
Resin
Sample
DOC
HOC
HMW
LMW
Acids
LM W
Neutral
X1
X2
X3
TOC
LC-OCD
ID
A
150
222
3
22
6
8
65
103
16
8
38
50
52
3
B
89
180
ND
37
C
220
295
ND
30
8
135
62
52
13
D
250
252
7
12
ND
68
30
101
39
E
190
261
12
52
5
30
35
107
26
F
250
336
ND
35
4
91
40
56
119
Baseline
ND
NA
NOTE:

HOC – hydrophobic

HMW – high molecular weight

LMW – low molecular weight

Synthetic Compounds:
o
X1 – matches retention time of ethanol
o
X2 – matches retention time of methanol
o
X3 – matches retention time of TMA
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X1
X2
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Ammonium
-- OCD
-- UVD
-- OND
LMW Acids
Project:
Balazs_130
Biopolymers
4
Building Blocks
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3
A
rel. Signal Response
2,5
Resin 14-00938
C
2
Resin 14-00943
B
Resin 14-00944
F
1,5
Resin 14-00958
E
1
Resin 14-00960
D
0,5
Resin Lot CHS
50007
0
0
50
100
150
200
Retention Time in Minutes
Figure A2-8
LC-OCD Chromatogram
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Figure A2-9
Particle Images by Scanning Electron Microscope (SEM)
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Cumulative Number Concentration (#/mL)
1e+9
Resin A
Resin B
Resin C
Resin D
Resin E
Resin F
Blank
1e+8
1e+7
1e+6
10
20
30
40
50
60
80
100
Particle Diameter (nm)
Figure A2-10
Grab Sample Particle Leach Analysis by LNS
Table A2-4 Grab Sample Particle Leach Analysis by LNS
Cumulative Concentration x 106 (#/mL)
Resin ID
≥ 10 nm
≥ 20 nm
≥ 30 nm
A
121
11.6
1.32
B
65
4.5
0.27
C
125
18.0
6.42
D
87
9.7
1.29
E
225
30.0
7.02
F
3052
92.6
26.8
31
2.7
0.51
Blank
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Table A2-5 Grab Sample Particle Leach Results of LPC and SEM Analyses
Resin
ID
LPC, particles per ml
SEM
>0.3
µm
>0.5
µm
>1
µm
>2
µm
0.1-0.2 µm
0.2-0.5 µm
0.5-1 µm
>1
µm
A
56,000
17,000
2,300
460
1500 ± 100
190 ± 20
97 ± 10
ND
B
290
84
7.5
0.7
97 ±10
<49
<49
<49
11,000
1,200
44000 ± 4000
3200 ± 300
630 ± 60
340 ± 30
C
930,000
140,000
D
45,000
12,000
880
97
1200 ± 100
150 ± 10
49 ± 5
49 ± 5
E
34,000
13,000
220
310
1300 ± 100
150 ± 10
49 ± 5
49 ± 5
F
41,000
6,400
550
91
1800 ± 200
290 ± 30
49 ± 5
49 ± 5
Blank
39
6.8
0.8
0.3
<49
<49
<49
<49
Table A2-6 Static Leach Metal Analysis by UPW Extraction
Metals
Resin Sample ID
Elements
Concentration, ng/ml (resin)
Detection Limits, ng/ml
(resin)
Detected
A
None
ND
0.002-0.08
B
None
ND
0.002-0.08
C
Fe
K
Na
0.04
0.06
0.07
0.02
0.02
0.01
D
None
ND
0.002-0.08
E
None
ND
0.002-0.08
F
None
ND
0.002-0.08
Blank
None
ND
0.002-0.08
NOTE:
30 elements were tested by high resolution ICPMS;
Only those above detection limits were reported;
Detection limits are 1-40 ppt in H2O for the metals tested (Ag, Al, As, Au, B, Ba, Be, Bi, Ca, Cd, Ce, Co, Cr, Cs, Cu, Fe, Ga,
Ge, Hg, K, Li, Mg, Mn, Mo, Na, Ni, Pb, Sn, Sr,Ti, W, Zr).
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Table A2-7 HCl Leach for Metals
IX Resin Sample ID
Elements
RL
Unit
A
B
C
D
E
F
Aluminum (Al)
0.1
ppb (ng/g)
0.5
1.7
5.6
6
0.2
2.6
Antimony (Sb)
0.1
ppb (ng/g)
*
*
*
*
*
*
Arsenic (As)
0.2
ppb (ng/g)
0.4
*
*
*
*
*
Barium (Ba)
0.05
ppb (ng/g)
0.08
*
0.11
0.09
*
*
Beryllium (Be)
0.1
ppb (ng/g)
*
*
*
*
*
*
1
ppb (ng/g)
5
*
22
*
*
2
0.1
ppb (ng/g)
*
*
*
*
*
*
1
ppb (ng/g)
12
2
85
8
2
19
Chromium (Cr)
0.1
ppb (ng/g)
7.1
1
3.6
4.9
7.9
10
Cobalt (Co)
0.05
ppb (ng/g)
0.19
*
0.09
*
0.05
0.23
Copper (Cu)
0.1
ppb (ng/g)
0.3
0.2
0.1
*
*
0.4
Gallium (Ga)
0.1
ppb (ng/g)
*
*
*
*
*
*
Germanium (Ge)
1
ppb (ng/g)
*
*
*
*
*
*
Gold (Au)
1
ppb (ng/g)
*
*
*
*
*
*
Iron (Fe)
1
ppb (ng/g)
330
2
21
4
4
110
Lead (Pb)
0.1
ppb (ng/g)
*
*
*
*
*
0.1
Lithium (Li)
0.05
ppb (ng/g)
*
*
*
*
0.16
*
Magnesium (Mg)
0.1
ppb (ng/g)
20
0.3
20
0.5
0.4
9
Manganese (Mn)
0.1
ppb (ng/g)
6.2
*
0.5
*
*
2.1
Molybdenum (Mo)
0.1
ppb (ng/g)
0.4
0.5
0.3
2.7
*
2.2
Nickel (Ni)
0.1
ppb (ng/g)
7.6
0.2
0.9
5.1
0.7
26
1
ppb (ng/g)
14
1
11
4
*
3
Silver (Ag)
0.5
ppb (ng/g)
*
*
*
*
*
*
Sodium (Na)
0.1
ppb (ng/g)
710
5
96
6.6
2.8
62
Strontium (Sr)
0.05
ppb (ng/g)
0.13
*
0.56
0.11
0.09
0.14
Tin (Sn)
0.1
ppb (ng/g)
*
*
*
*
*
*
Titanium (Ti)
1
ppb (ng/g)
*
*
*
*
*
*
Vanadium (V)
0.1
ppb (ng/g)
*
*
*
*
*
*
1
ppb (ng/g)
*
*
*
*
*
*
Zirconium (Zr)
0.1
ppb (ng/g)
0.2
0.7
0.2
0.2
*
*
Bismuth (Bi)
0.1
ppb (ng/g)
*
*
*
*
*
*
Mercury (Hg)
1
ppb (ng/g)
*
*
*
*
*
*
Tungsten (W)
1
ppb (ng/g)
*
*
*
*
*
Boron (B)
Cadmium (Cd)
Calcium (Ca)
Potassium (K)
Zinc (Zn)
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