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SEMI F40-0699 © SEMI 1999 3 b) C o mponents that require a contain er (see Section 9.6). 10.3 Each group is dis cussed indiv i d u al ly. Use Table 1 to determine the appropriate g roup for each com pone nt. 10.4 G enera…
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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).
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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.
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10.6.3 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).
10.6.4 Gaskets and O-rings: A minimum of two grams
of component per 100 mL of test fluid is required to
perform any of the tests. To concentrate a sample and
lower the detection limit of the test method, increase the
amount of component per 100 mL of fluid.
10.6.5 Example of procedure for components that
require a container
10.6.5.1 Clean and prepare 8 covered containers per
Section 10.4.1 and 7.1.1.
10.6.5.2 Place the component into 3 containers per
Section 10.6.
10.6.5.3 Flush all containers (3 with co mponents and 5
as blanks) according to Section 10.4.2 (rinse 10 times
for 2 minutes per Table 1).
10.6.5.4 Fill all containers with the test media of
choice (see Section 2.3 for definition of test media).
10.6.5.5 Soak according to Section 10.4.3 (soak one
week per table 1), agitate all containers once a day for
one minute per Section 10.4.4.
10.6.5.6 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.
11 Procedure for Preparing Components for
Bulk Polymer Analysis
11.1 Table 2 lists the amount of material required to
achieve the indicated level of detection. Obtaining the
amount may require using 1) an entire component, 2) a
segment of a large component (such as piece of piping
or valve), or 3) an appropriate quantity of smaller
components (such as O-rings).
11.2 No further pretreatment is req uired except for
inorganic analysis. See Section 11.3.
11.3 Additional Pretreatment for Inorganic Bulk
Analysis
11.3.1 If the intent of the inorganic analysis is to
examine the as-received material from a supplier, no
further pretreatment is required.
11.3.2 After the proper amount of the material is
obtained, place it in a clean container and clean it using
the procedure outlined below.
NOTE: This procedure may also be used to pre-clean
containers and caps to meet the criteria specified in
Section 7.1.1. If pre-cleaning performance criteria is
not achieved with this procedure another procedure
should be used or the concentrations, times, and
temperatures noted in this procedure could be varied to
achieve required result.
11.3.3 Agitate the material in ultrapure IPA for 2
minutes. Drain the IPA from the material and replenish
with ultrapure IPA. Allow the material to soak for 30
minutes.
11.3.4 Drain the IPA from the material and replace
with UPW. Agitate the material for 2 minutes.
11.3.5 Soak the material in 1:1 ultrapure nitric acid :
UPW for 2–4 hours.
11.3.6 Drain the nitric acid from the material and
replace with UPW. Agitate the material for 2 minutes.
11.3.7 Soak the material in 1:1 ultrapure HCl : UPW
for 2–4 hours.
11.3.8 Drain the HCl from the material and replace
with the test fluid. Agitate the material for 2 minutes.
Drain the material and replenish with test fluid and
agitate for an additional two minutes.
12 Data Presentation
12.1 See Table 3 for a list of the units to report for
individual component types. Record the following:
a) Report the test fluid used and test temperature.
b) Report if the components were prepared for
testing as received or after the rinse
pretreatment.
c) Report the volume of test fluid used.
d) Report the soak time
e) Report the wetted surface area of the
component. If the precise wetted surface area
is not known please record the assumed or
estimated wetted surface area and note it is
estimated.
f) If multiple components (such as gaskets, or O-
rings) were used, report the total wetted
surface area of the components.
g) Report the manufacturer, model number, and
lot number (if known) for each component
tested.
13 Related Documents
13.1 ASTM Standards
1
1
American Society for Testing and Materials (ASTM). 1916 Race St.
Philadelphia, PA 19103.