IPC-TM-650 TEST METHODS MANUAL

1 1 ScopeThis test procedure is designed to measure thelevel of anionic and cationic residues on the surface ofunpopulated (bare) printed boards by ion Applicable DocumentsIPC-WP-008 Setting Up Ion Chromatography Capability3 Test SpecimenAny printed board4 Apparatus and Chromatograph capable of accurately measuring ionconcentration down to parts per million (ppm). The equip-ment and chemistry should be set up and standardized perthe manufacturer s instructions. The separation column andeluent composition should be chosen to provide good sepa-ration of the ions of Water Bath capable of maintaining 80 2 C[176 F]. extraction gloves, , cleanroom vinyl gloves. (<3 ppm ofChloride). water with a starting resistivity of at least or ACS grade chemicals for eluent and regener-ant standard - traceable calibration standards ( ,NIST traceable).

2 Note:At the time of publication of this test method, a trace-able industry adipic acid standard does not exist. Future revi-sions to this test method will indicate such traceability (IPA), ACS grade or Flasks (Typically 25, 50, 100, and 1000 ml) Pipetting Equipment (such as Eppendorf) extract solution sample containers or auto-sampler vials if an auto-sampler is used with the syringes should be used for MANUAL Test Extraction ProcedureSelect a low-ion extraction bagsized to fit the board with approx. cm [ in] excess oneach side to minimize required extract solution, with severalinches at the top to allow for air expansion when the bag clean gloves when handling the samples to betested. Place each sample in an extraction a 10%/90% volume/volume 2-propanol /deionized water solution for the a known volume of the extraction solution tothe extraction bag covering the printed board (approx.)

3 Surface area). the same volume of extraction solution to anempty bag of the same lot for use as a the bags into the 80 2 C[176 F]water bath allowing the water to force most of the air from thebags. Do not allow any of the water from the water bath intothe extract solution in the bags. Fold the top of the bags overthe suspending bar and clip in place with binder clips. This willminimize solvent loss during the extraction, yet not create asealed bag. Alternatively, the bags may be heat sealed afterforcing most of the air from the the sample to soak for one hour (-0 min., +5min.). the bags from the water bath and allow thebags/solution to cool to room Lakeside Drive, Suite 309 SBannockburn, IL 60015-1249 IPC-TM-650 TEST METHODS Printed Board Cleanliness by IonChromatographyDate12/2009 RevisionOriginating Task GroupIon Chromatography/Ionic Conductivity Task Group(5-32a)Material in this Test METHODS MANUAL was voluntarily established by Technical Committees of IPC.

4 This material is advisory onlyand its use or adaptation is entirely voluntary. IPC disclaims all liability of any kind as to the use, application, or adaptation of thismaterial. Users are also wholly responsible for protecting themselves against all claims or liabilities for patent referenced is for the convenience of the user and does not imply endorsement by the bag to mix the contents. Transfer solutionto virgin sample vials for analysis or pull the sample solutiondirectly from the bag using a clean syringe for MANUAL the test board from the bag, using Calibration ions in the calibration procedure are a ions may be added to the determination if part per million (ppm) is 1 milligram of the ionic spe-cies (solute, , chloride ion) per 1000 grams of or purchase a combination stock anion stan-dard solution: 5 ppm fluoride, 25 ppm acetate, 50 ppm for-mate, 20 ppm methanesulfonic acid (MSA), 50 ppm chloride,50 ppm bromide, 20 ppm nitrate, 200 ppm adipate, 100 ppmsuccinate, 20 ppm sulfate, and 20 ppm standard stock can be prepared from 1000ppm stock solutions using the following formula:Combine ml fluoride; ml MSA, nitrate, phosphate,and sulfate; ml acetate.

5 Ml formate, chloride, andbromide; ml succinate; 5 ml adipate; in a 25 ml volumet-ric flask. Dilute to volume with 10% 2-propanol / 90% deion-ized water. The stock solution is stable for several weeks ifkept refrigerated. Warm to room temperature before or purchase a combination stock cation stan-dard solution: 5 ppm lithium, 50 ppm sodium, 50 ppm ammo-nium, 50 ppm potassium, 50 ppm magnesium, and 50 standard stock can be prepared from 1000ppm stock solutions using the following formula:Combine ml of the lithium standard and ml of thesodium, ammonium, potassium, magnesium, and calciumstandards in a 25 ml volumetric flask. Dilute to volume with10% 2-propanol / 90% deionized water. The stock solution isstable for several weeks if kept refrigerated. Warm to roomtemperature before volumes of anion calibration standard solutionfor a three point 1: ( ppm fluoride, ppm acetate, ppm formate, ppm methanesulfonic acid (MSA), chloride, ppm nitrite, ppm bromide, ppmnitrate, ppm adipate, ppm succinate, ppm sulfate,and ppm phosphate) Pipet 1 ml of the combination stockstandard solution to a 100 ml volumetric flask.

6 Add 20 micro-liters of 1000 ppm nitrite purchased stock solution and diluteto volume with 10% 2-propanol / 90% deionized water. Mixwell. Prepare fresh daily. (Nitrite is not stable over long periodsof time) 2: ( ppm fluoride, ppm acetate, formate, ppm methanesulfonic acid (MSA), ppmchloride, ppm nitrite, ppm bromide, ppm nitrate, ppm adipate, ppm succinate, ppm sulfate, ppm phosphate) Pipet 1 ml of the combination stock stan-dard solution to a 50 ml volumetric flask. Add 40 microliters of1000 ppm nitrite purchased stock solution and dilute to vol-ume with 10% 2-propanol / 90% deionized water. Mix fresh daily. (Nitrite is not stable over long periods oftime). 3: ( ppm fluoride, ppm acetate, formate, ppm methanesulfonic acid (MSA), ppmchloride, ppm nitrite, ppm bromide, ppm nitrate, ppm adipate, ppm succinate, ppm sulfate, ppm phosphate) Pipet 1 ml of the combination stock stan-dard solution to a 25 ml volumetric flask.

7 Add 80 microliters of1000 ppm nitrite purchased stock solution and dilute to vol-ume with 10% 2-propanol / 90% deionized water. Mix fresh daily. (Nitrite is not stable over long periods oftime). volumes of cation calibration standard solu-tion for a three point 1: ( ppm lithium, ppm sodium,ammonium, potassium, magnesium, and calcium) Pipet 1 mlof the combination stock cation standard solution to a 100 mlvolumetric flask and dilute to volume with 10% 2-propanol /90% deionized water and mix well. Prepare fresh 2: ( ppm lithium, ppm sodium,ammonium, potassium, magnesium, and calcium) Pipet 1 mlof the combination stock standard solution to a 50 ml volu-metric flask and dilute to volume with 10% 2-propanol / 90%deionized water and mix well. Prepare fresh Printed Board Cleanliness by Ion ChromatographyDate12 3: ( ppm lithium, ppm sodium,ammonium, potassium, magnesium, and calcium) Pipet 1 mlof the combination stock standard solution to a 25 ml volu-metric flask and dilute to volume with 10% 2-propanol / 90%deionized water and mix well.

8 Prepare fresh a minimum 3 point calibration per the chromato-graph manufacturer s recommended METHODS for both anionsand cations, verifying correct standard concentrations havebeen entered into the the baselines and update the calibration asrequired to obtain a good calibration curve. The correlationfactor (R2) for the curves should be a minimum of , withhigher values desirable. Any point on the calibration curveshould not deviate from the expected value by more than 10%.Note:The organic acids standards will typically not form a lin-ear calibration and a quadratic curve may be Analytical analysis of the extract solution should be done assoon as possible after extraction, butshallbe no longer thanfour days from the extraction the chromatograph per the manufacturers rec-ommended method and allow it to come to a stable sample solutions for anion and cation content,utilizing best analytical technique and laboratory Calculation of from the chromatograms are typically reportedin parts per million (ppm).

9 Surface Area CalculationRecord the surface areaof printed board (length x width x 2), , a rectangularprinted board with no cutouts. Alternatively, the surface areaof the printed board can be determined from CAD software orother machine vision recognition system. Surface area shouldbe known to three significant are to be expressed as micrograms ( g) of ionper square centimeter based on the extraction volume and thecalculated sample surface area. g/cm2=(SC BL)x VolAreawhere:SC = ppm from IC ( g/mL)BL = PPM from the bag blankVol = final volume (ml)Area = surface area (cm2)Note: ppm value is actually specimen value minus all ions NotesA repeatable and reproducible ionic cleanliness evaluationmethod requires some level of skill in accurately running an ionchromatography unit. The reader may find IPC-WP-008 to beof Printed Board Cleanliness by Ion ChromatographyDate12/2009 RevisionPage3of3