1、 FORD LABORATORY TEST METHOD AD 002-01 Date Action Revisions 2000 08 07 Editorial no technical change A. Cockman 2000 03 09 Editorial no technical change A. Cockman 1992 05 11 Printed copies are uncontrolled Page 1 of 4 Cop yright 2000, Ford Global Technologies, Inc. ANALYSIS OF LIMESTONE, RAW DOMOM
2、ITE AND SINTERED DOLOMITE Solutions Required Oxalic Acid - 10 % Dissolve 100 G of H 2 C 2 O 4 H 2 O in distilled water and dilute to 1000 mL. Dibasic Ammonium Phosphate - 10 % Dissolve 100 g of (NH 4 ) 2 HPO 4 in distilled water and dilute to 1000 mL. Brom Cresol Purple Indicator Dissolve 0.5 g in 1
3、00 mL of distilled water and filter. Barium Chloride - 10 % Dissolve 100 g of Ba Cl 2 2H 2 O in distilled water and dilute to 1000 mL. Standard Potassium Permanganate - Approximately 0.2 N Weigh 19.2 g of C.P. KmnO 4 and dissolve in 3000 mL of distilled water. Let age for one week. Filter through a
4、fritted glass crucible. Store in a dark glass stoppered bottle. Standardize as follows : Weigh 0.6 g of Bureau of Standards #40 C sodium oxalat e and transfer to a 400 mL beaker. Dissolve in 200 mL of hot distilled water (85 C) and add 15 mL of H 2 SO 4 (1:1). Titrate with 0.2 N KmnO 4, allowing the
5、 first few drops to decolorize before adding more, then add at the rate of about 15 mL per minute. A s the end point is approached, add the KmnO 4 drop by drop until a permanent pink color persists. weight of Na 2 C 2 O 4 = weight of oxalate equivalent to 1 mL of KmnO 4 mL of KMnO 4 Na 2 C 2 O 4 - 1
6、 mL = normality factor 0.067 The permanganate may also be stand ardized against Bureau of Standards Dolomite #88 following all the steps of the procedure. Conditioning and Test Conditions All test values indicated herein are based on material conditioned in a controlled atmosphere of 23 +/ - 2 C and
7、 50 +/ - 5 % relat ive humidity for not less than 24 h prior to testing and tested under the same conditions unless otherwise specified. FORD LABORATORY TEST METHOD AD 002-01 Page 2 of 4 Copyright 2000, Ford Global Technologies, Inc. Procedure Ignition Loss (On Sintered Dolomite Only) The ignition l
8、oss is determined on the whole grain sample as follows: Weigh 20 g of the whole grain sample into a tared platinum dish. Ignite for 2 h in a muffle furnace at 1000 C. Cool in a desiccator and reweigh. loss in weight x 100 = % ignition loss weight of sample Note: When the whole grain sample is crushe
9、d, it should be t ransferred immediately to a clean, tightly capped bottle as the material absorbs CO 2 and H 2O rapidly from the atmosphere. Silica Weigh 0.5 of the dry sample (dried at 125 +/ - 5 C) and transfer to a 250 mL beaker. Add 10 mL of water, 10 mL of HCl, cove r and heat to dissolve the
10、sample. Add 20 mL of HclO 4 (60 %) and take to fumes on the hot plate. Heat for 15 minutes while HclO 4 is refluxing in the beaker. Remove from the plate, cool, rinse the cover and sides of beaker with distilled water and dilute to 50 mL. Add 10 mL of HCl (conc.) and filter through Whatman #42 paper
11、 into a 400 mL beaker. Wash silica alternately with hot water and hot HCl (5 %) till free of iron salts and finally with hot water till free of acid. Save filtrate for R 2 O 3 determin ation. Transfer the paper and silica to a platinum crucible and ignite at 50 +/ - 5 C until carbon is destroyed and
12、 finally at 1000 C. Cool and weigh. weight of SiO 2 x 100 = % SiO 2 weight of sample Combined Oxides To the filtrate from the silica d etermination add 3 drops of Brom Cresol Purple indicator and enough NH 4OH (conc.) to turn the solution blue. Heat to boiling and boil for 3 minutes. Filter through
13、Swedish paper into a 400 mL beaker and wash well with hot dilute NH 4Cl (2 %). Save the fi ltrate for Ca determination. Ignite the paper and residue in a platinum crucible at 665 C until carbon is destroyed and finally at 1000 C for 15 minutes. Cool in a desiccator and weigh as combined oxides (R 2
14、O 3 ). weight of oxides x 100 = % R 2 O 3 weight of sample FORD LABORATORY TEST METHOD AD 002-01 Page 3 of 4 Copyright 2000, Ford Global Technologies, Inc. Calcium Place the filtrate from the R 2 O 3 determination on a pad on the hot plate, insert a stirring rod to prevent subsequent bumping, and br
15、ing solution to a boil. Add 20 mL of oxalic acid (10 %) and again bring to a boil. While the solutio n is boiling add NH 4 OH (conc.) from a drop bottle until the solution is blue, then 10 drops in excess, and continue boiling for one minute. Remove the beaker from the plate and set in a warm place
16、for hour. Filter through Swedish paper into a 600 mL be aker and wash with cold water. Save filtrate for magnesium. Ignite the precipitate of calcium oxalate in a platinum or porcelain crucible until carbon is destroyed and finally at 1000 C for five minutes. Cool, brush the CaO into the beaker in w
17、hich the first precipitation of calcium was made, rinse the crucible with a little water and 10 mL of HCl (conc.) and transfer to the beaker. Warm to dissolve the calcium oxide and dilute to 200 mL with hot water. Add indicator, NH 4 OH and precipitate the calcium a second time. Filter, wash the pap
18、er and precipitate with cold water six times and finally with hot water three times. Combine the filtrates for magnesium. Place the beaker in which the calcium precipitation was made under the funnel and pierce the pa per. Rinse the calcium oxalate into the 400 mL beaker and wash the paper well with
19、 hot water. Dilute to 200 mL with hot water, add 15 mL of H 2 SO 4 (1:1) and stir to dissolve calcium oxalate. Titrate with standard approximately 0.2 N KmnO 4. Add the perma nganate a few drops at a time allowing the solution to decolorize before adding more. When the first few drops have been cons
20、umed add KmnO 4 at a more rapid rate (10 - 15 mL per minute) making sure it is decolorized as fast as it is added. When the end po int is almost reached, stop the titration and add the filter paper to the beaker. Break it up with stirring and continue the titration to a permanent pink color. mL of K
21、MnO x normality factor x 0.0020 = g Ca 4 weight of sample g Ca x 1.399 x 100 = % Ca O g Ca x 2.497 x 100 = % CaCO 3 Magnesium Acidify the combined filtrates from the calcium determination with HCl (conc.) and evaporate to 300 mL. Cool in ice water and add 25 mL of diammonium phosphate solution (10 %
22、). Make alkaline with NH 4 OH (conc.) a nd add 5 mL in excess for each 100 mL of solution. Stir to precipitate the magnesium. Let stand for 4 - 6 hours or overnight if magnesium is low (under 2 %). FORD LABORATORY TEST METHOD AD 002-01 Page 4 of 4 Copyright 2000, Ford Global Technologies, Inc. Filte
23、r through a close paper and wash with dilute NH 4 OH (5:95). Place a clean beaker under th e funnel and dissolve the precipitate in 40 mL of hot dilute HCL (10 %). Add 1.5 mL of diammonium phosphate, dilute to 150 mL and cool in ice water. Add NH 4OH until alkaline and 5 mL in excess. Let stand for
24、4 hours or overnight. Filter through a close paper and wash with cold, dilute NH 4 OH (5 %). Place the paper and precipitate in a tared platinum crucible and dry on the hot plate. Ignite at 720 C until carbon is destroyed and finally at 1000 C to constant weight. weight of Mg 2 P 2 O 7 x 0.3623 x 10
25、0 = % MgO weight of sample weight of Mg 2 P 2 O 7 x 0.7577 x 100 = % MgCO 3 weight of sample Total Sulphur Weigh 5 g of sample and transfer to a 600 mL beaker. Cover the sample with bromine water. Add 50 mL of HNO (conc.), cover and digest for 5 minutes. Add 50 mL of HclO 4 (60 %) and evaporate almo
26、st to dryness. Cool, dilute to 50 mL and warm to dissolve salts. Filter through a close paper into a 400 mL beaker and wash with hot distilled water. Add 2 mL of HCl (conc.), dilute to 100 mL and heat to boiling. Add 10 mL of BaCL 2 (10 %), stir and digest at near the boiling point for 1 hour. Set a
27、side and allow to cool. Filter through #42 Whatman paper and wash with dilute HCl (1 %) and finally with hot water. Ignite at a low temperature (720 C) in a porcelai n crucible. Cool, transfer the precipitate to a 250 mL beaker. Add 4 mL of HCl and digest for a few minutes on the hot plate. Dilute t
28、o 200 mL, heat to boiling, add 5 mL of BaCl 2 and allow to settle in a warm place. Cool, filter wash and ignite as befor e to constant weight. Run a blank on all reagents, following all the steps of the procedure. (weight of BaSO 4 - blank) x 0.1373 x 100 = % S 4 weight of sample Phosphorus Weigh 2
29、g of the sample and dissolve in 20 mL of HCl (1:1) in a 250 mL beaker. A dd 5 mL of HNO 3 (conc.) and 20 mL of HclO 4 (60 %) and take to fumes of HCO 4 Cool, dilute with 50 mL of warm water and filter into a 250 mL Erlenmeyer flask. (If the amount of silica is large or in an umpire analysis, ignite
30、the silica, volatilize with H 2 S O 4 and HF dilute and filter and add the filtrate to the main solution.) To the solution in the flask add 10 mL of HNO 3 (conc.) and enough NH 4 OH (conc.) to neutralize the solution (use litmus). Add HNO 3 (conc.) until acid and 2 mL in excess. Dilute to 10 0 mL an
31、d add 40 mL of molybdate solution and shake for 5 minutes. Finish as in Procedure AA 3 - 1, Phosphorus in Iron and Steel. Chemicals, materials, parts, and equipment referenced in this document must be used and handled properly. Each party is respo nsible for determining proper use and handling in its facilities.
