IPC-TM-650 Test Methods Manual: Association Connecting Electronics Industries

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Number

2.3.25.1
ASSOCIATION CONNECTING Subject
ELECTRONICS INDUSTRIES ®
Ionic Cleanliness Testing of Bare PWBs
2215 Sanders Road
Northbrook, IL 60062-6135 Date Revision
October 2000
Originating Task Group
IPC-TM-650 Bare Board Cleanliness Assessment Task Group

TEST METHODS MANUAL 5-32c

1 Scope This test is used to determine the total ionic con- • Sodium chloride - reagent grade
tent extractable from on, and absorbed within, the surface of
• Analytical balance accurate to 0.0001 grams
printed wiring boards (PWBs), for the purposes of process
control. The conductivity of the extract solution is measured
WARNING: 2-propanol is a flammable material. The 2-propanol /
and the results are expressed as sodium chloride equivalence
water mixture is also flammable. Exercise caution when using this
per unit area.
solution.

2 Applicable Documents 5 Procedure


IPC-TM-650 Test Method 2.3.25, Detection and Measure-
5.1 Extraction
ment of Ionizable Surface Contaminants by Resistivity of Sol-
vent Extract (ROSE) NOTE: Throughout this procedure, do not touch the sample
boards with bare hands. Use the clean room gloves specified
3 Test Specimens or use clean forceps.

The test specimen may be any unpopulated PWB. The num-


5.1.1 Calculate the surface area of the PWB using:
ber of specimens depends on the process control plan or
Area (in cm2) = Length x Width x 2
product drawings/prints.

5.1.2 Prepare a volume of extract solution specified in 4.


4 Apparatus or Material

• An automated Resistivity of Solvent Extract (ROSE) tester 5.1.3 Using clean room gloves or clean forceps, place the
PWB into virgin KAPAK™ bags. Choose the bag size to give
• Conductivity dip probe with appropriate meter with tem-
at least an additional 2.5 cm [1.0 in] on each side of the board
perature compensation
to minimize the amount of extract solution used. Allow at least
• Hydrometer (0.800 - 0.900) for ROSE tester calibration an additional 5 cm [2.0 in] above the board top.

• Thermometer for ROSE tester calibration


5.1.4 Using a pipette or graduated cylinder, add a volume of
• Clean room (non-ionic) gloves or forceps the extract solution into the bag. The amount will depend on
the area of the board surface. This usually varies from 0.8
• KAPAK™ plastic bags or equivalents (see 6.9)
mL/cm2 [5.2 mL/in2] up to about 3 mL/cm2 [19 mL/in2]. For
• Bag sealing equipment example, a 10 cm x 11.5 cm [3.94 in x 4.53 in] board would
require about 100 mL of solution. The amount of solution
• Water bath, capable of sustaining an 80°C ± 2°C [176°F ±
should just cover the board completely when most of the air
3.6°F] temperature
is forced out of the bag.
• Second water bath capable of sustaining a 25°C ± 1°C
[77°F ± 1.8°F] temperature 5.1.5 Force most of the air from the bag and heat seal the
bag. This involves contact with a hot metal bar. Take reason-
• Precision solvent measurement equipment, such as class A
able precautions to keep extract solution from contacting the
pipettes
hot bar. Alternatively, the top of the bag may be folded over
• Volumetric glassware and clipped shut.
• Plastic ware - high density polyethylene, polymethylpentene
5.1.6 Place the bag(s) vertically in a water bath which has
(polypentene) or equivalent.
stabilized at 80°C [176°F]. Make sure that the boards do not
• Extract solution: 25% v/v deionized water (18 MΩ-cm nomi- float above the water line. Do not allow the water from the
nal resistivity), 75% v/v 2-propanol (electronic or HPLC bath to enter the bag or for extract solution to leak out of the
grade). No alternative solution or composition is allowed. bag.

Material in this Test Methods Manual was voluntarily established by Technical Committees of IPC. This material is advisory only
and its use or adaptation is entirely voluntary. IPC disclaims all liability of any kind as to the use, application, or adaptation of this Page 1 of 4
material. Users are also wholly responsible for protecting themselves against all claims or liabilities for patent infringement.
Equipment referenced is for the convenience of the user and does not imply endorsement by IPC.
IPC-TM-650
Number Subject Date
2.3.25.1 Ionic Cleanliness Testing of Bare PWBs October 2000

Revision

5.1.7 Allow the boards to extract in this manner for a period


of time of 60 ± 5 minutes.

5.1.8 Following the extraction of 5.1.7, remove the bags


from the water bath and allow the extract solution to cool for

Conductivity
at least 30 minutes, with the specimen still in the bag.

5.1.9 Using clean tongs or forceps, remove the PWB from


the bag.

5.2 Measurement – DIP Probe Method

5.2.1 Calibration of Bridge This is essential in this method


Solution Concentration
because there can be no correlation between resistivity/ in micrograms NaCl/Liter
conductivity readings and NaCl equivalents without calibra- IPC-2325-1
tion.
Figure 1 Nomogram of Conductivity vs. Solution
Concentration
5.2.1.1 Prepare a standard NaCl solution from a weight of
dry reagent grade NaCl salt dissolved in deionized water to
5.2.2 Test Procedure - DIP Probe
produce a final diluted concentration of 0.06 g/liter NaCl (5 mL
equals 300 µg NaCl). NOTE: If desired, this test can be run at other temperatures;
however, the calibration process must be repeated for the
5.2.1.2 Place 1 liter of the 2-propanol water solution (at the alternative temperature. This calibration process need only be
calibration temperature of the bridge in use) in a plastic bea- done once, providing the conductivity cell has not been
ker. exposed to harsh chemicals which would alter the cell con-
stants. If the conductivity cell is routinely used on harsh
NOTE: The 75 % v/v 2-propanol solution must be used in this
chemical solutions (e.g., plating baths), then the calibration
calibration. Water cannot be used since it is not the test solu-
tion used in the procedure. The test solution used in this cali- should be repeated before every test run.
bration can be recleaned by passing through the DI column
until the required resistivity/conductivity is obtained. 5.2.2.1 Place the Kapak™ bags containing the extract solu-
tions into the 25°C [77°F] water bath and allow the extract
5.2.1.3 From a 50 mL burette, add to the liter of test solu- solutions to reach 25°C [77°F].
tion, 5 mL of the standard 0.06 g/liter NaCl solution. Stir and
measure resistivity/conductivity. 5.2.2.2 Insert the conductivity probe into the Kapak™ bag
containing the room-temperature extract solution. It is impor-
5.2.1.4 From a 50 mL burette, add to the liter of test solu- tant that the extract solution be measured at the same tem-
tion, 20 additional mL of the standard 0.06 g/liter NaCl solu- perature used for the calibration solutions. Immerse the probe
tion, for a total of 25 mL. Stir and measure resistivity/ to a suitable depth.
conductivity.
NOTE: A ‘‘suitable depth’’ is one which covers the cell elec-
trodes, but not an immersion which covers the wiring. Many
5.2.1.5 From a 50 mL burette, add to the liter of test solu-
cells are marked with a scribed line which indicates the proper
tion, 25 additional mL of the standard 0.06 g/liter NaCl solu-
tion, for a total of 50 mL. Stir and measure resistivity/ immersion depth.
conductivity.
5.2.2.3 Gently agitate the solution. Read the conductivity of
5.2.1.6 Plot a three point nomogram of Conductivity vs. the solution. The time between immersion of the cell and tak-
Solution Concentration (in µg/liter NaCl). See Figure 1 for ing the reading should be the same as used for the calibration
example. You should get a linear relationship. Use a best fit curve. Sufficient time should be allowed for the reading to
line obtained with a piecewise linear method. come to equilibrium (no change for two minutes).

Page 2 of 4
IPC-TM-650
Number Subject Date
2.3.25.1 Ionic Cleanliness Testing of Bare PWBs October 2000

Revision

NOTE: Between measurements, rinse the cell with deionized 5.3.5 Carefully open the test bag and quickly pour the
water and leave the cell soaking in virgin extract solution. extract solution into the test cell. To minimize CO2 absorption,
Never use a dry cell as this is bad technique. the addition should be made as quickly as possible and the
cell cover quickly replaced.
5.2.2.4 Using the linear relationship formed in 5.2.1.6,
determine the concentration of sodium chloride correspond- 5.3.6 The instrument should very quickly reach equilibrium
ing to the conductivity reading. Use the equation given below (10 - 15 seconds) and then should remain essentially
to determine the total micrograms of sodium chloride equiva- unchanged for the remainder of the two minute run.
lence per square centimeter (µg NaCl Eq. /cm2)
5.3.7 Log the reading in total µg of sodium chloride equiva-
Using the nomogram:
lence per cm2.
Conductivity of Unknown →
Concentration of Unknown
5.3.8 Static ROSE Calculation Example:
Testing a bare board, 10 cm x 20 cm [3.9 in x 7.9 in]
Concentration Volume of Extract Solution
(µg/liter) x (liter) Surface area is 10 cm x 20 cm x 2 = 400 cm2 [62 in2]
Extracted Surface Area (cm ) 2 Bag size should be about 15 cm x 30 cm [5.9 in x 12 in] or
larger
= µg NaCl Eq./cm2 Extract solution would be about 620 mL
ROSE volume input to 4620 mL (4000 mL to cover sprays
5.2.2.5 If the conductivity of the unknown solution is outside and 620 mL from extraction)
of the bounds represented on the existing nomogram, then ROSE tester cell volume set to 4000 mL.
continue the technique used to generate the nomogram (see Run time - 2 minutes
5.2.1) until the bounds contain the conductivity of the
unknown solution. 5.4 Measurement – Dynamic ROSE Tester Method

5.3 Measurement – Static ROSE Tester Method 5.4.1 Perform a system verification check.
NOTE: This section was developed using an Omegameter
600SMD with a 10,000 mL cell. Make appropriate changes to 5.4.2 Program the instrument with the appropriate surface
the procedure to accommodate other static ROSE testers. area of the board.

5.3.1 Perform a system verification check. 5.4.3 Cycle the instrument to the beginning cleanliness
point.
5.3.2 Set the instrument to an appropriate amount of sol-
vent volume. A target solution level should be 1.5 mL for one 5.4.4 Carefully open the test bag and quickly pour the
cm2 of board surface. It is not necessary to cover the spray extract solution into the test cell. To minimize CO2 absorption,
jets (if applicable). If the lid is on the test cell, the CO2 mixing the addition should be made as quickly as possible and the
is minimized. cell cover quickly replaced.

5.3.3 Enter the appropriate surface area into the instrument. 5.4.5 When the instrument completes the test, log the read-
ing in total µg of sodium chloride equivalence per cm2.
5.3.4 To allow for the volume of solvent that is to be added,
the instrument setup volume will be set at the minimum vol- 6 Notes
ume (e.g., 2300 mL) plus the volume of solution in the extrac-
tion bag (e.g., 100 mL). 6.1 The background for this test method may be found in
technical papers:
Dwell time or run time: 2 minutes
Pass / Fail Value: None ‘‘Rationale and Methodology for a Modified Resistivity of Sol-
Begin the test and follow the test prompts. vent Extract Test Method,’’ Philip W. Wittmer, IPC 1995 Fall
Remove the cell cover. Meeting Proceedings, S13-4.

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IPC-TM-650
Number Subject Date
2.3.25.1 Ionic Cleanliness Testing of Bare PWBs October 2000

Revision

‘‘Ionic Cleanliness of LPISM Circuit Boards,’’ Hank Sanftle- 6.8 This method is best suited for monitoring and control of
ben, IPC 1995 Fall Meeting Proceedings, S13-3. a previously optimized process and should not be used to
generate acceptance data unless part of a larger correlation
6.2 IPC-HDBK-001 ‘‘Handbook and Guide to the Require- study. Values generated with this method should be corre-
ments for Soldered Electrical and Electronic Assemblies to lated to acceptable electrical performance if used for accep-
Supplement ANSI/J-STD-001’’ is another source for under- tance.
standing ROSE testing in general.
6.9 Kapak™ 500 Series Bags can be obtained from:
6.3 This method may also be known as the modified-ROSE Kapak Corporation
test. This test, due to its longer extraction time and higher 5305 Parkdale Drive
extraction temperature, has demonstrated better correlation Minneapolis, MN 55416
with the total ion determination by ion chromatography than 800-527-2557
IPC-TM-650, Test Method 2.3.25, Detection and Measure- www.kapak.com
ment of Ionizable Surface Contaminants by Resistivity of Sol- A secondary source of Kapak™ or Scotchpak™ polyester
vent Extract (ROSE) Method. However, as a bulk contamina- bags or pouches can be obtained from:
tion measurement method, it cannot distinguish individual ion VWR International
species. 1310 Goshen Parkway
West Chester, PA 19380
6.4 From an analytical standpoint, the dip probe method is Orders: 1-800-932-5000
preferred as more repeatable than the automated ROSE Web Orders: www.vwrsp.com
testers and avoids many of the test inaccuracies (e.g., CO2
absorption from spray agitation) inherent in those instruments. If an alternative to the Kapak™ bag or Scotchpak™ is
It should be stressed that the dip probe method is an electro- desired, the bag must have the following characteristics:
lytic conductivity measurement and must be temperature- • No extractable ionic material in 75% 2-propanol / 25% DI
compensated. water at 80°C [176°F] for 60 minutes

6.5 The dip probe calibrations can be run at multiple tem- • 0.01 cm [0.0039 in] wall thickness minimum
peratures and a family of curves generated, widening the test • Heat sealable or mechanical seal
window for use with this method. Higher temperatures, how-
ever, will lead to a faster 2-propanol evaporation rate. The test 6.10 There is some concern regarding ROSE tester cell size.
can also be run with more dilute concentrations, prepared by Testing a 2 cm x 2 cm [0.79 in x 0.79 in] board in a 20,000
series dilution. mL cell causes such a severe dilution as to cause the signal
to be lost in the noise. A recommended cell size is 5000 mL
6.6 Conductivity cells have a ‘‘constant’’ value. Measured or less. Smaller cell volumes will allow for a more measurable
readings must be multiplied by this constant. Exposure to result. If a smaller cell, or running with a smaller test volume,
harsh chemicals may alter the constant, making a are not an option, then the number of bare boards can be
re-calibration necessary. Do not allow the probe used for this increased, all extracted separately, and the extract solutions
procedure to contact sticky, oily, or resinous liquids (e.g., flux). all tested at once.

6.7 This procedure is intended to be a process control aid 6.11 When testing hybrids or microelectronics, be aware
and as such, no pass-fail criteria is stated. It is expected that that 2-propanol stored in glass containers can leach out
the fabricator/assembler will determine, with their customer, materials such as sodium, borates, and silica. 2-propanol
the necessary pass-fail criteria for their product by this stored in plastic containers does not have such a leaching
method. problem.

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