Background Statement for SEMI Draft Document 5421A
New Standard: TEST METHOD FOR PARTICLE REMOVAL
PERFORMANCE OF LIQUID FILTER RATED BELOW 30 nm WITH ICPMS
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
This document is an extension of Doc. 5297 (published as SEMI C82) which describes the test method for particle
removal performance of liquid filter rated 20-50 nm with optical particle counter.
The test particle as tracer material is gold nanoparticle (GNP) certified as National Institute of Science and
Technology (NIST) -Reference Material, as similarly used at SEMI C82 standard.
This document describes the test method for below 30 nm-rated filter mainly used for chemical filtration by using
GNP and ICP-MS as particle concentration detector.
If you have any questions on this ballot, please contact the following Task Force leaders or SEMI Staff:
Liquid Filter Task Force co-leaders:
Takuya Nagafuchi (Nihon Entegris) at takuya_nagafuchi@entegris.com
Takehito Mizuno (Nihon Pall) at takehito_mizuno@ap.pall.com
SEMI Staff :
Chie Yanagisawa (SEMI Japan) at cyanagisawa@semi.org
The ballot results will be reviewed and adjudicated at the meetings indicated in the table below. Check
www.semi.org/standards under Calendar of Events for the latest update.
Review and Adjudication Information
Task Force Review
Committee Adjudication
Group:
Liquid Filter TF
Japan Liquid Chemicals Committee
Date:
Friday, Apr 11, 2014
Friday, Apr 11, 2014
Time & Timezone:
14:00-15:00, Japan Time
15:00-17:00, Japan Time
Location:
SEMI Japan Office
SEMI Japan Office
City, State/Country:
Tokyo, Japan
Tokyo, Japan
Leader(s):
Takuya Nagafuchi (Nihon Entegris)
Takehito Mizuno (Nihon Pall)
Hiroshi Tomita (Toshiba)
Hiroyuki Araki (Dainippon Screen Mfg.)
Standards Staff:
Chie Yanagisawa (SEMI Japan)
+81.3.3222.5863 / cyanagisawa@semi.org
Chie Yanagisawa (SEMI Japan)
+81.3.3222.5863 / cyanagisawa@semi.org
The task force review meeting’s details are subject to change, and additional review sessions may be scheduled if
necessary. Contact 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.
If you need a copy of the documents in order to cast a vote, please contact the following person within SEMI.
Chie Yanagisawa
SEMI Standards, SEMI Japan
Tel: 81.3.3222.5863
Email: cyanagisawa@semi.org
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DRAFT
SEMI Draft Document 5421A
New Standard: TEST METHOD FOR PARTICLE REMOVAL
PERFORMANCE OF LIQUID FILTER RATED BELOW 30 nm WITH ICPMS
1 Purpose
1.1 This document is to provide a standard of mono-dispersed gold nanoparticle (GNP) challenge test for liquid
filter rated below 30 nm using ICP-MS.
2 Scope
2.1 This document covers a mono-dispersed GNP challenge test method for below 30 nm rated liquid filter.
2.2 This document defines a test condition for mono-dispersed GNP challenge test.
2.3 The following areas are to be addressed in this document:
 The test condition such as fluid, flow rate, pressure, GNP concentration, ligand concentration, membrane
treatment etc.
 The type of filter evaluated.
 The type of gold nanoparticle (GNP)
 The method of membrane treatment prior to the test for decreasing the adsorbing effect.
 The description of the test result.
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 The test procedure is destructive; the filter cannot be returned into operation.
3.2 Fresh filter shall be used for this test procedure.
3.3 Material purity and potential leaching of dissolved contaminants are not addressed by this standard. SEMI F57
does not address this issue for final filters therefore the end user may decide to consider such testing when selecting
different types of filters.
3.4 Test parameters affect the outcome of the test described in this standard, therefore test results are a qualitative
rather than a quantitative of filter performance. This standard recommends testing filters under the conditions
optimized in this standard and describe the conditions in test report.
3.5 Test shall be conducted as side by side comparison using more than one filter. Accordingly, the variability of
the challenged particle in size is allowed in this test.
4 Referenced Standards and Documents
4.1 SEMI Standards and Safety Guidelines
SEMI F110 — Test Method for Mono-dispersed Polystyrene Latex (PSL) Challenge of Liquid Filters
SEMI C79 — Guide to Evaluate the Efficacy of Sub-15 nm Filters Used in Ultrapure Water (UPW) Distributions
Systems
SEMI C82 — Test Method for Particle Removal Performance of Liquid Filter Rated 20 – 50 nm with Liquid-Borne
Particle Counter.
NOTICE: Unless otherwise indicated, all documents cited shall be the latest published versions.
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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LETTER (YELLOW) BALLOT
Document Number: 5421A
Date: 2/9/2016
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Phone: 408.943.6900, Fax: 408.943.7943
DRAFT
Document Number: 5421A
Date: 2/9/2016
LETTER (YELLOW) BALLOT
5 Terminology
5.1 Abbreviations and Acronyms
5.1.1 APD— 2-amino-2-hydroxymethyl-1,3-propanediol
5.1.2 DLS — dynamic light scattering
5.1.3 FM — flow meter
5.1.4 GNP — gold nanoparticle
5.1.5 ICP-MS — inductively coupled plasma – mass spectroscopy
5.1.6 LPM — liter per minute (L/min)
5.1.7 LRV — log reduction value
5.1.8 MSA — Mercaptosuccinic acid
5.1.9 NIST — National Institute of Standards and Technology
5.1.10 OPC — optical particle counter
5.1.11 P — pressure gauge
5.1.12 PSL — polystyrene latex
5.1.13 SAXS — small angle X-ray scattering
5.1.14 T — thermometer
5.1.15 UPW — ultrapure water
5.2 Definitions
5.2.1 background — the gold concentration when feeding the water without GNP.
5.2.2 challenge — the feed the water including GNP and ligand to test filter.
5.2.3 efficiency — particle removal efficiency of filter measured by this test method. It is the effectiveness of the
filter in removing the particles, and is measured as (Upstream – Downstream)/Upstream × 100.
5.2.4 ligand — ion or molecule (chemicals) that could bind with the surface of gold nanoparticle.
5.2.5 log reduction value (LRV) — log reduction value of filter measured by test method. This is measured as
logarithmic value of ratio of upstream to downstream particle counts.
6 Summary of Test Method
6.1 This test method describes that test equipment and procedures for determining the particle removal efficiency of
liquid filter (below 30 nm) with the water including ligand and GNP by calculating the difference of the number of
challenged particle between upstream and downstream. The concentration of challenged GNP is measured with ICPMS.
7 Apparatus
7.1 Test Device
7.1.1 For this test method, use the schematic shown in Figure 1.
7.1.2 The standard test device shall consist of a pre-filter, flow meters, a particle and ligand injection device, static
mixer, pressure gauges, a test filter, a particle counter, flow control valves, a resistivity sensor, a thermometer, and
tubing connecting them.
7.1.3 The pore size of a pre-filter shall be equal to or smaller than the pore size of a test filter.
7.1.4 Use a flow meter with an allowable error to less than 5% full scale and of appropriate range.
7.1.5 Use a pressure gauge with an allowable error to less than 1% full scale and of appropriate range.
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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DRAFT
7.1.6 Use a thermometer with an allowable error to less than 1% full scale and of appropriate range.
7.1.7 Use a tubing with an inner diameter that does not lead to significant pressure loss for the fluid medium used in
the test.
Test filter
Prefilter
UPW
Static Mixer
T1
P1
P2
FM
Ligand
GNP
Figure 1
Schematic of Typical Test Setup (Example)
7.2 Particle Injection Device
7.2.1 Use a particle injection device that can inject a particle at a constant flow rate without a pulsation.
7.3 Ligand Injection Device
7.3.1 Use a ligand injection device that can inject a ligand at a constant flow rate without a pulsation.
7.4 ICP-MS
7.4.1 Use an ICP-MS capable of detecting more than 0.1 ppb quantitative limit of gold.
7.4.2 Sample solution containing GNP shall be dissolved with aqua regia prior to injecting into ICP-MS.
8 Reagents and Materials
8.1 Ultrapure Water (UPW)
8.1.1 Use the supply UPW with the resistivity more than 17MΩ･cm.
8.1.2 Temperature of the UPW shall be adjusted to 25±5℃.
NOTE 1: As some ligands or other surfactants are added to actual challenge solution, there is no need to adhere to the resistivity
described in 8.1.1 at challenge test.
8.2 Gold nanoparticle (GNP)
8.2.1 Use the mono-dispersed GNP certified by NIST or the mono-dispersed NIST-traceable GNP.
8.2.2 The mono-dispersed GNP with below 30 nm of particle size is used.
NOTE 2: In Appendix 2, the average particle size of NIST reference materials (RM) is described
8.3 Ligand
8.3.1 Use a ligand to make colloidal GNP stably disperse and decrease the interaction between GNP and filter
media. (please see the Appendix 1)
9 Test Specimens
9.1 Use a virgin liquid filter from rating below 30 nm.
9.2 Any size and type of filter, such as disk, capsule or cartridge, can be used in the test.
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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Document Number: 5421A
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DRAFT
10 Procedure
10.1 General Procedures
10.1.1 The filter is evaluated by the following procedures:
 Testline background
 Filter pretreatment and filter flushing
 Background
 Challenge
10.2 Testline background
10.2.1 Background testing is required for every test before installing the test filter into the test line (see Figure 1 or
Figure 2).
10.2.2 Set the test condition (flow rate and pressure)
 UPW (Resistivity: ≥17MΩ･cm, temperature: 25±5℃)
 FM
Choose either standard below:
1.
Filter size standard: n L/min at 25.4*n mm-sized (n inch-sized) filter, (n=1,2,3,4,5….)
2.
Filter media surface area standard: the flow rate to achieve the flux of >0.1 ml/min/cm2.
 P2: ≥100 kPa
NOTE 3: A downstream pressure of at least 100 kPa has to be maintained in order to eliminate air in the system.
10.2.3 Collect the test line water and measure gold concentration with ICP-MS.
10.2.4 Confirm the concentration becomes below detection limit, and record.
10.3 Filter Pretreatment
10.3.1 Pre-wetting is needed if the test filter is hydrophobic (Follow filter manufacturer's instructions).
10.3.2 Pretreatment fluid is aqueous solution of a ligand used at the challenge test. The concentration shall be same
with the concentration at the challenge test.
NOTE 4: The condition of ligand concentration to achieve the lowest adsorbing effect depends on membrane type. Accordingly,
it is necessary to optimize it in advance. Please see Appendix 1 in terms of how to set the ligand condition.
10.3.3 Fill the membrane pore with the pretreatment fluid by flowing after installing into the test line.
10.3.3.1 After ¶10.3.3, soak filters in the pretreatment fluid for a minimum of 30 min.
10.4 Background
10.4.1 Start UPW flow and ligand injection.
10.4.2 Close the air-vent valve after venting air from the filter upstream.
10.4.3 Set the test condition (flow rate and pressure).
 UPW (Resistivity: ≥17MΩ･cm, temperature: 25±5℃)
 FM
Choose either standard below:
1.
Filter size standard: n L/min at 25.4*n mm-sized (n inch-sized) filter, (n=1,2,3,4,5….)
2.
Filter media surface area standard: the flow rate to achieve the flux of >0.1 ml/min/cm2.
 P2: ≥100 kPa
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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Document Number: 5421A
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DRAFT
NOTE 5: A downstream pressure of at least 100 kPa has to be maintained in order to eliminate air in the system.
10.4.4 Collect the downstream of the filter and measure gold concentration with ICP-MS
10.4.4.1 Record the concentration.
NOTE 6: If the gold concentration does not become below detection limit, terminate the challenge test and re-check test line and
other apparatuses. Then, restart the challenge test from 10.4.
10.5 Challenge
10.5.1 Prepare the challenge mono-dispersed GNP. When the challenge solution is diluted, it is necessary to use
UPW characterized at 8.1 and agitate sufficiently. The prepared challenge solution shall be used in the test within
24h. Preferably, the particle size in the solution also should be evaluated with the instrument such as DLS, and
SAXS in case the particle aggregation might occur. The purpose of this measurement is to confirm that no existence
of large aggregated particle in the challenge solution. Large particles may affect removal efficiency of the tested
filter, which may cause overestimate the removal capability of the filter. If obviously larger particles than estimated
challenge particle size are observed, the challenge test shall be terminated.
10.5.2 Set the test condition (flow rate and pressure).
 FM
Choose either standard below:
1.
Filter size standard: n L/min at 25.4*n mm-sized (n inch-sized) filter, (n=1,2,3,4,5….)
2.
Filter media surface area standard: the flow rate to achieve the flux of >0.1 ml/min/cm 2.
 P2: ≥100kPa
NOTE 7: A downstream pressure of at least 100 kPa has to be maintained in order to eliminate air in the system.
10.5.3 Turn on the injection pump which delivers the challenge solution prepared at 10.5.1.
10.5.4 Begin injection at rate to achieve <100 ppb (calculated actual number diluted from the original GNP
concentration).
NOTE 8: The challenge level shall be defined in terms of the concentration at the filter after diluting in the main flow. Record
downstream pressure reading.
10.5.5 Run test for achieving below the order of 1010 pcs/cm2 of the number of total challenged particle by tuning
challenged GNP concentration and time. Table 1 summarizes examples of the testing condition.
Table 1 Examples of the test condition in terms of concentration filter surface area, and challenging time.
GNP
size
(nm)
GNP
concentration
(ppb)
GNP
particles
(pcs/ml)
Flow rate
(L/min)
Filter
Surface
area (cm2)
Time
(min)
Accumulated
challenge
level
(pcs/cm2)
Membrane
coverage
area (cm2)
Membrane
Coverage
rate
(%)
20
10
7.0E+7
10
20,000
60
2.1E+9
131.9
0.7
10
5
2.9E+8
10
20,000
60
4.3E+9
67.2
0.3
10.5.5.1 Record particle levels in upstream and downstream each.
10.5.5.2 Monitor particle levels downstream of the filter.
10.5.6 Turn off injection pump.
10.5.7 Turn flow off at inlet valve.
10.5.8 Open drain and vent valves.
10.5.9 Remove test filter.
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Document Number: 5421A
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DRAFT
11 Calculations
11.1 Particle removal efficiency (%) and LRV are calculated using the average of the data points from last half for
downstream levels and the measured upstream value.
% Efficiency = (Upstream – Downstream)/Upstream × 100%
LRV = Log(Upstream/Downstream)
(1)
(2)
12 Report
12.1 Include the system setup, which includes the particle data system settings.
12.2 Include calculated efficiencies and LRV, shown in Table 1 (sample data).
12.3 Report resistivity, temperature and flux.
Table 2 Sample Data Format (Example)
Filter / Filter size/ Lot number
A
Average GNP size (nm) and Coefficient variation (-)
30, < 20%
GNP manufacturer/ Lot number
A
GNP concentration (N/ml)
1E+8
Water resistivity (MΩ)
18.2
Water temperature (℃)
23
Challenging time (min)
60
Ligand / Ligand concentration (mmol/L)
MSA / 0.3
Main flow rate (L/min)
10
Side flow rate (L/min)
0.1
Flux (ml/min/cm2)
0.5
ICP-MS manufacturer/ Model number
A
Background Average (ppb)
< DL
Upstream Average (ppb)
50
Downstream Average (ppb)
0.05
Efficiency (%)
99.9
LRV (-)
3
#1 Downstream values were calculated by averaging last half data recorded.
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APPENDIX 1
Ligand addition
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].
A1-1 Purpose of ligand addition
A1-1.1 As the GNP used in this standard has very small size, some disturbance such as concentration change,
contamination of foreign object, and pH change could easily cause aggregation or sedimentation of GNP. Also, the
interaction between GNP and filter media is extremely high and GNP could be adsorbed on the surface of filter
media.
A1-1.2 In order to stabilize GNP colloidal system and prevent filter media from adsorbing GNP, it is preferable to
use ligand technique. Precious metal like gold and platinum can bind with sulfur element and the molecule including
amino group with a coordination bond 1) 2). Thus, the gold surface could be easily modified by molecules including
thiol or amino functional groups.
A1-2 Polyethylene filter
A1-2.1 For polyethylene filter, a branched or bulky ligand like Mercaptosuccinic acid (MSA) including carboxyl
group could reduce adsorbing effect 3). Figure A1-1 shows the schematic drawing of atomic configuration of MSA
molecule combing with GNP. GNP is entirely covered with MSA ligand by adding the ligand into GNP challenge
solution, and the GNP covered with MSA is difficult to approach to filter media surface by steric effect.
Furthermore, when the GNP challenge solution including MSA is injected into main line, it is expected that the
colloidal system might be instable because MSA concentration is rapidly decreased. Therefore, previously adding
MSA ligand into main line at upstream of GNP injection line.
A1-2.2 Also, p-mercaptobenzoic acid can be used as acting similar with MSA 3). Table A1-1 summarizes the
representative ligands which have an ability to reduce adsorptive interaction between GNP and PE membrane.
Figure A1-1
Schematic drawing of atomic configuration of MSA molecule combining with GNP. Sulfur element is
combined with gold element.
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Table A1-1 Representative ligands to have an ability to reduce adsorbing effect between GNP and
polyethylene media.
Ligand
Mercaptosuccinic acid (MSA)
Mercaptobenzoic acid
A1-3 Nylon filter
A1-3.1 As nylon molecular has an amide linkage with high positive polarity in the structure. It is well known that
nylon could adsorb various colloidal particles dispersing in liquid because those particles are almost negatively
charged in their surface. Studies show that the ligand with amino group, which directly combines with gold surface,
has a repulsive force against nylon molecular structure 3). Below table A1-2 shows the ligand examples for nylon
filter evaluation.
Table A1-2 Representative ligands to have an ability to reduce adsorbing effect between GNP and nylon
media.
Ligand
2-amino-2-hydroxymethyl-1,3-propanediol (APD)
2-amino-2-methyl-1,3-propanediol
2-amino-2-methyl-1-propanol
2-amino-1,3-propanediol
3-amino-1,2-propanediol
(R)-(-)02-amino-1-propanol
(S)-(+)-2-amino-1-propanol
A1-4 PTFE filter
A1-4.1 PTFE itself has lower surface tension and adsorbing capability; however, MSA ligand is suitable to reduce
the interaction between GNP and PTFE media.
A1-5 Investigation of proper ligand concentration
A1-5.1 As described in this document, the ligand condition to achieve the lowest adsorbing effect is varied with
membrane type. Though ligands probably some influence the membrane surface as well as challenge particle, it is
uncertain that which parameter or property of membrane has an impact in regard to particle removal efficiency.
However, it is supposed that pore size and surface etc. are key parameter in order to conduct at proper condition.
A1-5.2 Thus, it is necessary to examine proper condition in advance. Please refer to following example showing
particle penetration ratio is varied with ligand concentration.
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A1-5.2.1 (Example 1)
A1-5.2.1.1 Filter type: Polyethylene Membrane sheet, 47 mm in diameter
A1-5.2.1.2 Challenge GNP specification : 10 nm – 2.9E+10 pcs/mL
A1-5.2.1.3 Ligand – MSA 0 – 1.0 mmol/L, MSA solution was added to GNP solution.
A1-5.2.1.4 Filtration was performed by challenging with GNP solution containing MSA after prewetting the
membrane with Isopropyl alcohol at a flow rate of 5 mL/min. The schematic diagram of filtration equipment is
shown in Figure A1-2. Figure A1-3 shows that the penetration ratio of 10 nm GNP through polyethylene membrane.
The penetration ratio increased with an increase of MSA concentration. On the contrary, the gradual decrease of the
penetration ratio was observed at more than 0.3 mmol/L of MSA concentration. In this case, around 0.2 mmol/L of
MSA concentration is suitable to achieve the lowest adsorbing effect between GNP and membrane surface.
Figure A1-2
The schematic diagram of the filtration equipment installed with 47 mm in diameter disk membrane.
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Figure A1-3
The penetration ratio of 10 nm GNP through polyethylene membrane. At around 0.2 mmol/L of MSA
concentration, the highest penetration ratio could be observed.
A1-5.2.2 (Example 2)
A1-5.2.2.1 Filter type: Nylon6, 6 membrane sheet, 47 mm in diameter
A1-5.2.2.2 Challenge GNP specification : 5 nm – 2.5E+11 pcs/mL
A1-5.2.2.3 Ligand – APD 0 – 1.0 mmol/L, APD solution was added to GNP solution.
A1-5.2.2.4 Filtration was performed by challenging with GNP solution containing APD after prewetting the
membrane with Isopropyl alcohol at a flow rate of 5 mL/min. Figure A1-4 shows that the penetration ratio of 5 nm
GNP through nylon6,6 membrane. The penetration ratio was at constant at more than 0.05mmol/l of APD
concentration.
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Document Number: 5421A
Date: 2/9/2016
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LETTER (YELLOW) BALLOT
Document Number: 5421A
Date: 2/9/2016
Figure A1-4
The penetration ratio of 5 nm GNP through nylon6,6 membrane.
A1-5.2.3 (Example 3)
A1-5.2.3.1 Filter type: PTFE membrane sheet, 47 mm in diameter
A1-5.2.3.2 Challenge GNP specification : 10 nm – 2.9E+9 pcs/mL
A1-5.2.3.3 Ligand – MSA 0 – 1.0 mmol/L, MSA solution was added to GNP solution.
A1-5.2.3.4 Filtration was performed by challenging with GNP solution containing MSA after prewetting the
membrane with Isopropyl alcohol at a flow rate of 5 mL/min. Figure A1-5 shows that the penetration ratio of 5 nm
GNP through PTFE membrane.
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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Doc. 5421A  SEMI
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Phone: 408.943.6900, Fax: 408.943.7943
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LETTER (YELLOW) BALLOT
Document Number: 5421A
Date: 2/9/2016
Figure A1-5
The penetration ratio of 10 nm GNP through PTFE membrane.
A1-6 Filter pretreatment
A1-6.1 Ligands shall be injected into UPW main line. It is expected to have an effect of filter pretreatment
decreasing adsorbing effect before GNP challenge test. Also, stabilizing effect of GNP solution could be expected
when injecting GNP into main line. Please refer to SEMI C82 for more information.
A1-7 Hydrodynamic diameter of GNP dispersed in challenge solution
A1-7.1 Figure A1-6 and A1-7 shows the hydrodynamic diameter of 30nm-GNP dispersed in the solution containing
MSA and APD ligand, respectively. 1.0E+8 pcs/ml of GNP solution with a variety of MSA concentration were
prepared, and the hydrodynamic diameter was measured with DLS.
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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Doc. 5421A  SEMI
Semiconductor Equipment and Materials International
3081 Zanker Road
San Jose, CA 95134-2127
Phone: 408.943.6900, Fax: 408.943.7943
DRAFT
Figure A1-6
The hydrodynamic diameter of 30nm-GNP dispersed in MSA ligand solution with a variety of the ligand
concentration.
Figure A1-7
The hydrodynamic diameter of 30nm-GNP dispersed in APD ligand solution with a variety of the ligand
concentration.
A1-8 References
A1-8.1 G. Schmid, “Nanoparticles – From Theory to Application”, Wiley-Vch Verlag GmbH & Co. KgaA (2004).
A1-8.2 G. T. Hermanson, “Bioconjugate Techniques”, Elsevier (2008).
A1-8.3 T. Mizuno et al., “A novel filter rating method using less than 30-nm gold nanoparticle and protective
ligand”, IEEE/TSM, vol. 22, No. 4, (2009) 452-461.
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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Doc. 5421A  SEMI
LETTER (YELLOW) BALLOT
Document Number: 5421A
Date: 2/9/2016
Semiconductor Equipment and Materials International
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San Jose, CA 95134-2127
Phone: 408.943.6900, Fax: 408.943.7943
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APPENDIX 2
Particle size of NIST Reference Material
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 Particle size of NIST Reference Material (RM)
A2-1.1 Table A2-1 and A2-2 summarize reference value mean size and expanded uncertainty of RM8011 and
RM8012.
Table A2-1 Reference value mean size and expanded uncertainty of RM8011 (10 nm)
Technique
Analyte Form
Mean Particle size
(nm)
Expanded
Uncertainty
Atomic Force Microscopy
Dry, deposited on substrate
8.5
±
0.3
Scanning Electron Microscopy
Dry, deposited on substrate
9.9
±
0.1
Transmission Electron Microscopy
Dry, deposited on substrate
8.9
±
0.1
Differential Mobility Analysis
Dry, aerosol
11.3
±
0.1
Dynamic Light Scattering
Liquid suspension
13.5
±
0.1
Small-Angle X-ray Scattering
Liquid suspension
9.1
±
1.8
Table A2-2 Reference value mean size and expanded uncertainty of RM8012 (30 nm)
Technique
Analyte Form
Mean Particle size
(nm)
Expanded
Uncertainty
Atomic Force Microscopy
Dry, deposited on substrate
24.9
±
1.1
Scanning Electron Microscopy
Dry, deposited on substrate
26.9
±
0.1
Transmission Electron Microscopy
Dry, deposited on substrate
27.6
±
2.1
Differential Mobility Analysis
Dry, aerosol
28.4
±
1.1
Dynamic Light Scattering
173º scattering angle (backscatter)
Liquid suspension
28.6
±
0.9
Dynamic Light Scattering
90º scattering angle
Liquid suspension
26.5
±
3.6
Small-Angle X-ray Scattering
Liquid suspension
24.9
±
1.2
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.
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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Doc. 5421A  SEMI
LETTER (YELLOW) BALLOT
Document Number: 5421A
Date: 2/9/2016
Semiconductor Equipment and Materials International
3081 Zanker Road
San Jose, CA 95134-2127
Phone: 408.943.6900, Fax: 408.943.7943
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APPENDIX 3
Actual filtration data
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].
A3-1 Actual filtration data
A3-1.1 Actual filtration results are summarized in Table A3-1.
Table A3-1 Actual filtration result (Examples)
Filter / Filter size/ Lot number
Polyethylene A / disk
Nylon B / disk
PTFE C / cartridge
Average GNP size (nm) and coefficient
variation (%)
10nm, < 10%
20nm, < 20%
20, < 20%
GNP manufacturer/ Lot number
A
A
A
GNP concentration (N/ml)
2.9E+9
3.5E+8
3.5E+7
Water resistivity (MΩ)
18.2
18.2
18.2
Water temperature (℃)
23
23
23
Challenging time (min)
4
4
60
Ligand / Ligand concentration (mmol/L)
MSA / 0.5
APD / 1.0
MSA / 6.7E-3
Main Flow rate
5 ml/min
5 ml/min
10 L/min
Side flow rate
-
-
0.1 L/min
Flux (ml/min/cm2)
0.5
0.5
0.5
ICP-MS manufacturer/ Model number
A
A
A
Background Average (ppb)
< DL
< DL
< DL
Upstream Average (ppb)
54.4
52.0
5.28
Downstream Average (ppb)
3.0
0.021
0.008
Efficiency (%)
94.5
> 99.9
99.8
LRV (-)
1.3
>3
2.3
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and the risk of infringement of such rights are entirely their own responsibility.
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Doc. 5421A  SEMI
LETTER (YELLOW) BALLOT
Document Number: 5421A
Date: 2/9/2016