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SEMI F40-0699 © SEMI 1999 2 6 Summa ry of Pra ctice 6.1 Thi s docum ent describes two d i f ferent co mpon e nt preparation procedu res (see Figure 1): a) procedure for preparin g co m ponents and collecting a sample for…

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SEMI F40-0699 © SEMI 19991
SEMI F40-0699
PRACTICE FOR PREPARING LIQUID CHEMICAL DISTRIBUTION
COMPONENTS FOR CHEMICAL TESTING
This practice was technically approved by the Global Facilities Committee and is the direct responsibility of
the North American Facilities Committee. Current edition approved by the North American Regional
Standards Committee on December 18, 1998. Initially available on www.semi.org January 1999; to be
published June 1999.
1 Purpose
1.1 This document defines component preparation and
pretreatment procedures for chemical test methods used
to evaluate liquid chemical distribution system
components.
2 Scope
2.1 This document includes preparation procedures
that can be applied to components such as tubing,
piping, valves, regulators, fittings, gaskets, O-rings, and
filter housings.
2.2 This document defines and specifies all of the
component pretreatment and analyze preparation
procedures for liquid chemical distribution system
components common to the test methods listed (see
Table 3). Each type of component should be pretreated
and prepared according to the procedures of this
document before it can be tested using the identified
chemical test methods.
2.3 This document defines preparation and
pretreatment procedures used for the evaluation of
liquid chemical distribution system components in test
fluids. This practice is intended for use with 49% HF,
30% H
2
O
2
, 29% NH
4
OH, IPA and ultrapure water. The
document defines the purity of chemicals that can be
used for leaching and rinsing liquid chemical
distribution system components.
3 Limitations
3.1 Although ozonated water is commonly used in
ultrapure water systems, no provisions are made in this
document for evaluations using ozonated water.
Therefore, some of the procedures may not be directly
applicable to ozonated water.
3.2 The preparation procedures described in this
practice primarily involve static testing including
agitation. Dynamic testing, i.e., continuous flow, may
alter the chemical test results. Static component
preparation procedures are not directly applicable to
dynamic testing.
3.3 This preparation procedure applies to ambient
temperature only with the exception of ultrapure water
which may be tested at ambient temperature and up to
85°C.
3.4 Filter cartridges are not covered in this document
due to the requirement for dynamic testing.
4 Referenced Documents
4.1 None.
5 Terminology
5.1 Acronyms and Abbreviations
5.1.1 DSC differential scanning calorimetry
5.1.2 FEP fluorinated ethylene-propylene
5.1.3 FTIR — Fourier transform infrared spectroscopy
5.1.4 H
2
O
2
— hydrogen peroxide
5.1.5 HF — hydrofluoric acid
5.1.6 IPA — Isopropyl alcohol
5.1.7 NH
4
OH — ammmonium hydroxide
5.1.8 NVR — nonvolatile residue
5.1.9 PE — polyethylene
5.1.10 PFA — perfluoroalkoxy
5.1.11 PP — polypropylene
5.1.12 PVDF — polyvinylidene fluoride
5.1.13 TGA thermal gravimetric analysis
5.1.14 TOC — total organic carbon
5.1.15 UPW — ultrapure water
5.2 Definitions
5.2.1 blank extraction A container of test fluid
which does not see the component under test. It follows
the entire procedure and is handled in the same manner
in order to show the background of the lab or test area.
SEMI F40-0699 © SEMI 1999 2
6 Summary of Practice
6.1 This document describes two different component
preparation procedures (see Figure 1):
a) procedure for preparing components and
collecting a sample for extraction analyses
b) procedure for pretreating or preparing
components for bulk polymer analysis.
6.2 Table 1 specifies the flush time, soak time, and
container material for extracting leachable
contaminants. Sample size requirements for bulk
analyses are listed in Table 2.
6.3 This practice should be performed before analysis
by industry standard extraction and bulk test methods
used to evaluate liquid chemical distribution
component. Available industry standard test methods
are listed in Table 3 and the Related Documents
section.
7 Apparatus and Materials
7.1 Containers, as defined in Table 1.
7.1.1 All containers and caps used in component and
blank extraction should be thoroughly cleaned. A
typical recommended cleaning procedure is outlined in
Section 11.3. However, any cleaning procedure is
acceptable as long as the subsequent blank extraction
yields impurity concentrations that do not exceed 10%
of the specification for the material being tested. For
example, if a given impurity is specified for a
maximum of 1.0 µg/cm
2
, the blank extraction
concentration should not exceed 0.1 µg/cm
2
.
NOTE: In situations where the detection limit is greater
than 10% of the specification for the polymer material,
the detection limit of the instrument converted into
µg/cm
2
will suffice, provided it does not exceed the
specification for the material being tested.
7.2 Test Fluids
7.2.1 For purposes of this practice , references to water
shall be understood to mean ultrapure water as defined
by maximum individual metal and anion impurity levels
of 0.1 parts per billion by weight 1 × 10
-9
(ppbw) or
less, total organic carbon (TOC) levels of 10 ppbw or
less, nonvolatile residue levels of 0.1 parts per million
by weight 1 × 10
-6
(ppmw) or less, resistivity of 18
megohm-cm or greater, and reactive silica impurity of
less than 1.0 ppb.
7.2.2 References to HF, NH
4
OH and H
2
O
2
shall be
understood to refer to chemicals with a minimum of a
semiconductor grade purity and meet the criteria in
section 7.1.1. The impurity concentrations of the
chemical must not exceed 10% of the lowest anticipated
concentration for the analyte(s) of interest.
7.2.3 Ultrapure Nitric Acid, less than 1 ppb for each
trace metal.
7.2.4 Ultrapure Hydrochloric Acid, less than 1 ppb for
each trace metal.
7.2.5 Ultrapure Isopropyl Alcohol, less than 1 ppb for
each trace metal.
8 Precautions
8.1 Safety Precautions
8.1.1 This practice may involve hazardous materials,
operations, and equipment. This practice does not
purport to address the safety considerations associated
with its use. It is the responsibility of the user to
establish appropriate safety and health practices and to
determine the applicability of regulatory limitations
before using this practice.
8.2 Technical Precautions
8.2.1 The component preparations must be conducted
in clean environments that prevent contamination of the
components and containers at the parts per trillion level
for the analyte(s) of interest. A clean environment may
require the use of a cleanroom (for those procedures
which can be performed in a cleanroom).
8.2.2 For all testing other than differential scanning
calorimetry (DSC), thermal gravimetric analysis
(TGA), and Fourier transform infrared spectroscopy
(FTIR), the component preparation should take place in
a controlled environment to minimize contamination.
9 Sampling and Test Specim ens
9.1 The components selected for testing should reflect
the current manufacturing capabilities of the supplier.
10 Procedure for Preparing C omponents and
Collecting an Extraction Sample for Analysis
10.1 Component preparation for contaminants that can
be leached from liquid chemical distribution
components is different from component preparation
for bulk polymer analysis. Components are flushed and
then soaked to extract surface contamination. Refer to
Table 1 for procedures for handling specific
components.
10.2 The liquid chemical distribution system
components described in this section are divided into
two groups:
a) Components that require capping (see
Section 9.5).
SEMI F40-0699 © SEMI 19993
b) Components that require a container (see
Section 9.6).
10.3 Each group is discussed individually. Use Table 1
to determine the appropriate group for each component.
10.4 General Procedure
10.4.1 The blank extraction is a container of test fluid
without a component which follows the entire
procedure and is handled in the same manner. Please
consult the specific test method for the number of test
fluid samples to be prepared and the statistical
treatment. This would include a number of containers
for both component and blank extractant. Use cleaned
containers that meet the criteria specified in Section
7.1.1. An example of a cleaning procedure is outlined in
Section 11.3.
10.4.2 Use UPW to fill and then drain the component
or container 10 times. After each fill, leave the water in
the component or container for two minutes before
draining.
10.4.3 Fill an 11th time with the appropriate test fluid
(see Section 2.3); use this fill for the test. Refer to
Table 1 to determine the soak time for each component
or container.
10.4.4 Agitate once a day for one minute. Orbital
shakers or manual agitation can be used, but no foreign
materials may contact the test fluid; therefore, stir bars
cannot be used. Components and/or containers are to
remain sealed during agitation to prevent splashing or
spilling. Components in containers (such as gaskets)
should remain completely submerged throughout the
extraction.
10.5 Components that Require Capping (Tubing,
Piping, Valves, Regulators, and Filter Housings)
10.5.1 This practice is appropriate for static samples
with one end permanently sealed and one end loosely
capped. Since the sealing process may contaminate the
sample, one end should be sealed prior to precleaning.
Use cleaned caps meeting the criteria specified in
Section 7.6.1. The cap must be manufactured from the
same material as the component or from a compatible
material that will not contaminate the sample.
10.5.2 As surfactants and solvents may leave a residue
that could alter the test results, do not use them for
precleaning.
10.5.3 During sample collection for metal analysis, the
components must be acid stabilized to a pH of 2
(approximately 3 drops of concentrated nitric acid per
250 mL of UPW) to stabilize for certain trace metals
(i.e., iron and chromium).
10.5.4 Tubing and piping: Fill the component with test
fluid to within one inch of the top of the component to
allow free space for agitation. In the case of tubing or
pipes, to maximize the exposed surface area of the pipe
to the volume of fluid and to minimize the surface area
of the end cap, it is recommended that the ratio of the
surface area of the pipe to the surface area of the end
cap be 10 or greater. The equation to determine the
ratio is 4L/D, where L is the length of the pipe or tubing
and D is the diameter.
10.5.5 Valves, regulators, and fittings: To allow for
maximum fluid volume, fill valves, regulators, and
fittings with the appropriate test fluid to within five mL
of the top to allow for agitation. Multiple components
may be required to obtain the necessary volume for the
test. Valves, regulators, and fittings must be capped at
both ends. In the case of valves, this practice assumes
that normally opened valves will be used.
10.5.6 Filter housings: Fill the component with the
appropriate test fluid to within one inch of the top of the
housing to allow free space for agitation. The inlet and
outlet of the housing must be capped.
10.5.7 Example of procedure for components that
require capping
10.5.7.1 Clean and prepare 8 covered containers per
Sections 10.4.1 and 7.1.1.
10.5.7.2 Flush component and blank extraction
containers (3 components and 5 blank extraction
containers) according to Section 10.4.2 (rinse 10 times
for 2 minutes per Table 1).
10.5.7.3 Fill all components and blank extraction
containers with the test media of choice (see Section 2.3
for definition of test media).
10.5.7.4 Soak according to Section 10.4.3 (soak one
week per table 1), agitate all components and blank
extraction containers once a day for one minute per
Section 10.4.4.
10.5.7.5 Decant the contents of the component into 3
remaining empty containers.
10.5.7.6 At completion of this practice analytical tests
should be performed on test fluid from each container
see test methods noted in Table 3 and related
documents section.
10.6 Components that Require a Container (Gaskets,
and O-Rings)
10.6.1 Containers must have sufficient internal volume
to perform the required test. Often, 100 mL of
extracted test fluid will be required per test.
10.6.2 Surfactants and solvents may leave a residue
that could alter the test results; do not use them for pre-
cleaning.