1、 FORD LABORATORY TEST METHOD BI 020-12 Date Action Revisions 2001 03 13 Revised Editorial no technical change A. Cockman 1992 06 29 Printed copies are uncontrolled Page 1 of 6 Copyright 2001, Ford Global Technologies, Inc. DETERMINATION OF COMBUSTIBLE ORGANIC PIGMENTS (CARBON BLACK) IN PRESENCE OF I
2、NORGANIC PIGMENTS (ASH) Application The procedure describes the approved filtration method of essentially water borne electrocoating material for the determination of the combined weight of organic and inorganic pigments (Part 1), the determination of ash (Part 2) and the determination, in electrode
3、posited uncured paint films, of organic and inorganic pigments (Part 3). Apparatus Required Vacuum Variable from 760 mm Hg to 20 mm Hg. Oven 210 F Low Conversion (Cenco Central Scientific Co.) Catalog No. 95105 A. Laboratory Balance Analytical +/- 0.1 mg (or equivalent). Desiccator Calcium chloride,
4、 Will Scientific, Catalog No. D-10821 or equivalent. Pipettes Volumetric 1 mL, 2 mL, 3 mL, 4 mL, 5 mL, 10 mL, 25 mL, Will Scientific Catalog No. J-21751 or equivalent. Filtering Flask 1,000 mL, Millipore Corp. Catalog No. XX1004705 or equivalent. Pyrex Filter Holder Millipore Corp. Catalog No. XXX10
5、0470 or equivalent. Filter Funnel 300 mL, Millipore Corp. Catalog No. XX1004704. Vacuum Hose 4 ft. gum rubber 5/8“ O.D., 1/4“ I.D., Millipore Corp. Catalog No. XX7100004. FORD LABORATORY TEST METHOD BI 020-12 Page 2 of 6 Copyright 2001, Ford Global Technologies, Inc. Spring Action Clamp Millipore Co
6、rp. Catalog No. XX1004703. Watch Glasses 90 mm, Will Scientific Catalog No. D-28146 or equivalent. Tweezers 3 1/2“ length, blunt edge, Will Scientific Catalog No. 11301 or equivalent. Filter Discs UR 1.5 micron, UH 0.5 micron, UG 0.25 micron Tan; solvent resistant, Millipore Corp. Policeman Wide tip
7、ped, Will Scientific Catalog No. 23371 or equivalent. Crucibles, Porcelain 30 mL or 40 mL, Will Scientific Catalog No. M-10106 or equivalent. Furnace Muffle Will Scientific Catalog No. 14691 or equivalent. Bunsen Burner Will Scientific Catalog No. 7206 or equivalent. Triangle Will Scientific Catalog
8、 No. 27521 or equivalent. Combustion Capsule 1 3/4“ diameter, Will Scientific Catalog No. 10226 or equivalent. Magnetic Stirrer Will Scientific Catalog No. L-25216 or equivalent. Beakers 100 mL, 1,500 mL, Pyrex, Will Scientific Catalog No. D-4191 or equivalent. Glass Funnel 75 mm diameter, Will Scie
9、ntific Catalog No. D-14158 or equivalent. Volumetric Flask 250 mL, Will Scientific Catalog No. J-13951 or equivalent. Aluminum Dishes 50 mL, Will Scientific Catalog No. 11146 or equivalent. FORD LABORATORY TEST METHOD BI 020-12 Page 3 of 6 Copyright 2001, Ford Global Technologies, Inc. Chemicals Req
10、uired Ethyl Cellosolve Reagent Grade, Gage Products Co., 625 Wanda, Ferndale, MI. Toluene Reagent Grade, E.H. Sargent Catalog No. BX9460. Diethyl Amine Reagent Grade, E.H. Sargent Catalog No. EK92. Ammonium Bicarbonate Reagent Grade, E.H. Sargent Catalog No. BK0610. Methyl Alcohol Reagent Grade, E.H
11、. Sargent, Catalog No. BK9069. Pentoxone Reagent Grade, Gage Products Co., 625 Wanda, Ferndale, MI. Preparation of Solvent Mixture 20 mL - Ethyl Cellosolve 10 mL - Toluene 3 mL - Diethyl Amine For a total of - 33 mL Preparation of Flocculating Agent Mix 7 grams ammonium bicarbonate in 100 mL deioniz
12、ed water. Store in refrigerator. Preparation of Stripping Solution Mix 133 mL ethyl cellosolve with 67 mL toluene. Test Procedure 1. Determination of combined weight of organic and inorganic pigment. (a) Filter Selection 1.1 Using a volumetric pipet, place a sample of paint, containing approximately
13、 0.2 - 0.4 gm non-volatiles into a 100 mL beaker (non-volatiles determined according to FLTM BI 120-08). FORD LABORATORY TEST METHOD BI 020-12 Page 4 of 6 Copyright 2001, Ford Global Technologies, Inc. 1.2 Insert filter holder into vacuum flask and connect to vacuum line. Using a blunt edge tweezers
14、, remove one 0.5 micron filter disc from filter package, center on filter holder and wet with ethyl cellosolve. Clamp filter funnel onto filter holder. Add 33 mL of the “solvent mixture“ and 3 mL “flocculating agent“ to the beaker. Stir for 10 minutes using a magnetic stirrer. 1.3 Pour contents into
15、 filtration funnel and apply vacuum, to filter approximately 6 mL/minute. If pigment passes through the filter (discolored filtrate) repeat steps 1 - 2 using a smaller pore size filter disc. In case of slow filtration, use a larger pore size. (b) Micro-Filtration Procedure (Quantitative) 1.4 Transfe
16、r a paint sample containing about 75 mg total pigment (for instance 3 mL) into a 100 mL beaker by use of a volumetric pipette*. Record volume as (A) grams. Add 33 mL “solvent mixture“ and 3 mL “flocculating agent“ to the beaker. Stir mixture for 10 minutes using the magnetic stirrer. 1.5 Remove filt
17、er disc, selected according to Section 1.3, from filter pack and place on watch glass. Place filter and watch glass into a 210 F oven for 15 minutes. This removes residual moisture from filter. Remove watch glass from oven and immediately cover with a second watch glass. Without delay, weigh filter
18、disc to +/- 0.1 mg and record weight as (B). Return filter to its watch glass and cover as above. 1.6 Using a wash bottle, wet the top of the filter holder with ethyl cellosolve. Place filter disc on filter holder and center. Place filter funnel on filter holder and gently clamp in place. Remove mag
19、netic bar from sample beaker and stir contents of beaker for 1 minute using a rubber policeman. Carefully pour contents of beaker (part 1.4) into filter funnel. Rinse beaker 3 times with 1 - 2 mL portions of ethyl cellosolve. Use rubber policeman in the quantitative transfer of sample to funnel. App
20、ly the proper amount of vacuum and increase in small increments to visually maintain a steady rate of filtration (approximately 6 mL/minute). After the solvent has passed through the filter, wash the inside of the funnel with 5 mL toluene. Next wash the pigment with 5 mL of pentoxone, followed by 5
21、mL of toluene. *The density of materials which contain about 10 % non-volatiles by weight is sufficiently close to 1 gm/mL to allow pipetting. 1.7 Break the vacuum by detaching rubber hose from flask. Detach clamp from funnel and remove funnel with a slow tilting motion. Remove filter disc from filt
22、er holder, using tweezers and place onto a watch glass. If small amounts of pigment remain on the funnel, dry funnel in a 210 F oven for 1 minute. Gently brush pigment onto filter using a 1/4“ fine bristled artist brush. 1.8 Place watch glass with filter disc into a 210 F oven for 20 minutes. FORD L
23、ABORATORY TEST METHOD BI 020-12 Page 5 of 6 Copyright 2001, Ford Global Technologies, Inc. 1.9 Weigh filter disc with pigment to +/- 0.1 mg and record as (C). Calculations: Weight of Total Pigment: D = C - B or total pigment per 100 gs paint: E = D x 100 = % total pigment in paint A If the grams non
24、-volatile (F) per 100 grams paint has been determined according to FLTM BI 120-08 then: Grams Total Pigment per 100 grams N.V. = E x 100 F 2. Determination of Inorganic Pigments (c) Determination of Pigment Ash 2.1 Weigh crucible and record weight as “G“. Pipet a 10 mL bath sample into crucible. Pla
25、ce crucible into a 210 F oven until dry. Transfer crucible to triangle on ring stand and slowly burn off organics using a bunsen burner with hood. After charing, heat the crucible to a cherry red color. 2.2 Place crucible into a clean combustion capsule and heat in a 1400 F muffle furnace for 20 min
26、utes. Place crucible in desiccator for 25 minutes. Weigh to +/- 0.1 mg and record as (H). Calculations: Weight of Ash: I = H - G Grams of Ash per 100 grams of Paint J = I x 100 = 10 I 10 Grams of Ash per 100 grams N.V.: M = 10 I x 100 F (d) Determination of Factor for Conversion of Weight of Ash to
27、Weight of Inorganic Pigment (Optional). 2.3 Obtain a sample of paint of known inorganic and organic pigment composition. Determine weight of ash as in 2.1 - 2.2. Calculations: Factor for conversion of weight of ash to weight of inorganic pigment: O = M N 3. Determination of Organic Pigments in Uncur
28、ed Paint Films 3.1 Electrocoat two 4 x 12“ test panels (usually phosphated steel). Rinse coated panels with tap water to insure complete removal of unelectrocoated paint. FORD LABORATORY TEST METHOD BI 020-12 Page 6 of 6 Copyright 2001, Ford Global Technologies, Inc. 3.2 Place coated panel in a 1,50
29、0 mL beaker and rinse both sides with stripping solution by use of wash bottle. Approximately 90 mL will remove most of the paint film. Residual film is removed by wetting with stripping solution and wiping with a wide tipped spatula-type rubber policeman. Repeat for second panel. No more than 15 mi
30、nutes should be required to strip both panels. 3.3 Transfer material from 1,500 mL beaker to a 250 mL volumetric flask through a glass funnel. Rinse clean with stripping solution. Fill flask to volumetric mark using stripping solution. Mix thoroughly, place magnetic stirrer-bar into flask and agitat
31、e. (e) Determination of Weight of Stripped-Off Paint Solids 3.4 Place 50 mL aluminum dish into center of a second 50 mL aluminum dish, stretched by hand, and record weight of 2 dishes as (K). Pipette 25 mL from flask (under agitation) into inner dish. Slowly evaporate solvent, and bake in oven for r
32、equired time cycle (for instance 25 minutes at 360 F). Cool in desiccator and record weight as (L). Calculations: Weight of paint solids = (L - K) x 10 The factor of 10 gives the total solids weight in 250 mL of solvent (part 3.3). (f) Determination of Total Pigment and Inorganic Pigment in Film 3.5
33、 By use of pipetted 25 mL aliquots from agitated volumetric flask, follow Section 1.0 through Section 2.2. List of Symbols A = Weight of paint sample. B = Weight of filter disc. C = Weight of filter plus pigment. D = Weight of total pigment. E = Grams total pigment in 100 grams paint. F = Grams non-
34、volatiles per 100 grams paint. G = Weight of crucible. H = Weight of crucible plus ash. I = Weight of ash. J = Grams ash per 100 grams paint. K = Weight of aluminum dish. L = Weight of aluminum dish plus baked out paint. M = Grams ash per 100 grams non-volatiles. N = Grams of known inorganic pigment per 100 grams paint non-volatiles. O = Conversion factor for weight of ash to weight of inorganic pigment. Chemicals, materials, parts, and equipment referenced in this document must be used and handled properly. Each party is responsible for determining proper use and handling in its facilities.
