1、This document is restricted and may not be sent outside Navistar, Inc. or reproduced without permission from Corporate Technical Standards. Suppliers are required to assume all patent liability. 2009 Navistar, Inc. AUGUST 2009 Page 1 of 4 NAVISTAR, INC. CEMS (CORPORATE ENGINEERING MATERIAL SPECIFICA
2、TION) NUMBER: CEMS BT-43 TITLE: Barium, Calcium, Magnesium and Zinc In Oil CURRENT ISSUE DATE: August 2009 WRITTEN/REVIEWED BY: Materials Engineering APPROVED BY: Materials Engineering SUPERSEDES ISSUE OF: October 2001 This specification may involve hazardous materials, equipment, and procedures. Th
3、is specification does not purport to address all of the safety issues associated with its use. The user is responsible to consult appropriate safety and health practices and to determine the applicability of regulatory limits prior to use. Change Notice: Replaced “International Truck and Engine Corp
4、oration” with “Navistar, Inc.” per corporate directive. 1.0 SCOPE This method covers a rapid and accurate procedure for determining the amounts of barium, calcium, magnesium and zinc in unused lubricating oils. 2.0 APPARATUS 2.1 Magnetic stirrer. 2.2 100 ml porcelain evaporating dish. 2.3 Hot plate
5、or bath capable of maintaining solutions 70 to 80C. 2.4 Muffle furnace capable of maintaining 700 + 25C. 2.5 250 ml beaker. 2.6 Funnel. 2.7 Titration burette. 2.8 Analytical balance. 2.9 Desiccator. 3.0 MATERIAL 3.1 Sulfuric Acid solution, 1:1 (H2SO4) 3.2 Disodium Ethylenediaminetetra-acetate, dihyd
6、rate, reagent grade. 3.3 Magnesium Sulfate (MgSO47H2O), reagent grade. 3.4 Eriochrome Black T, reagent grade. 3.5 Triethanolamine, reagent grade. 3.6 Ethyl alcohol. 3.7 Ammonium Chloride (NH4Cl), reagent grade. 3.8 Ammonium Hydroxide (NH4OH), reagent grade. 3.9 Methyl Red, reagent grade. 3.10 Ammoni
7、um Chloride, 20% solution (NH4Cl). 3.11 Ammonium Hydroxide solution, 5:95 (NH4OH). 3.12 Ammonium Oxalate, reagent grade (NH4)2C2O4. 3.13 Ammonium Phosphate, Dibasic, 20% solution (NH4)2HPO4 3.14 Potassium Cyanide, 20% solution (KCN) 3.15 Formaldehyde, 4% solution (HCHO). 3.16 Hydrochloric Acid solut
8、ion, 1:50 (HCl). 3.17 Hydrochloric Acid solution, 1:1 (HCl). NUMBER: CEMS BT-43 TITLE Barium, Calcium, Magnesium And Zinc In Oil CURRENT ISSUE DATE: August 2009 This document is restricted and may not be sent outside Navistar, Inc. or reproduced without permission from Corporate Technical Standards.
9、 Suppliers are required to assume all patent liability. 2009 Navistar, Inc. AUGUST 2009 Page 2 of 4 3.18 Sodium Hydroxide, 30% (NaOH). 3.19 Distilled water. 3.20 ph papers, ranges 1 to 6 and 6 to 12. 3.21 Filter paper, medium porosity, ashless. 4.0 SOLUTION PREPARATION 4.1 EDTA - 0.01 Molar Dissolve
10、 3.723 g of disodium ethylenediaminetetra-acetate, dihydrate, in distilled water and dilute to 1 liter. 4.2 Magnesium Sulfate - 0.01 Molar Dissolve 2.465 g MgSO47H2O in distilled water and dilute to 1 liter. Standardize against EDTA solution. 4.3 Eriochrome Black T Indicator Dissolve 0.2 g Eriochrom
11、e Black T in 5 ml of ethyl alcohol and mix with 15 ml of triethanolamine. 4.4 Methyl Red Indicator Dissolve 0.25 g Methyl Red in 15 ml of ethyl alcohol. Dilute to 250 ml with distilled water. 4.5 Buffer Solution - pH 10 Dissolve 35 g NH4Cl in 150 ml distilled water. Add 285 ml concentrated NH4OH and
12、 dilute to 500 ml with distilled water. 5.0 PROCEDURE BARIUM 5.1 Approximately 10 g of sample, weighed to the nearest mg, is placed in a 100 ml porcelain evaporating dish. 5.1.1 Burn off organic matter on a hot plate and then in a muffle furnace at 600C for approximately 10 minutes. 5.1.2 After it h
13、as cooled, wet it completely with H2SO4 1:1 and heat on hot plate until all the H2SO4 fumes are expelled. 5.1.3 Place in muffle furnace maintained at 700C for a period required to burn off all the carbon. 5.1.4 Cool, add 20 ml HCl 1:1 and evaporate to moist dryness-avoid spattering. 5.1.5 Transfer r
14、esidue to 250 ml beaker using hot HCl 1:50. Final volume of solution should not exceed 100 ml. 5.1.6 If a precipitate forms in this dilute HCl solution, add 2 ml of H2SO4 1:1 and boil for a few minutes. Let stand on hot plate (70 to 80C) until completely settled out. If no precipitate forms, barium
15、is not present. Proceed directly to Step 5.2. 5.1.7 To separate the barium sulfate precipitate, filter through a medium porosity, ashless filter paper and wash with hot water adding the wash water to the filtrate. Final volume of the solution should not exceed 150 ml. 5.1.8 Place the filter paper co
16、ntaining the barium sulfate precipitate in a tared porcelain crucible, dry on a hot plate and burn off in a muffle furnace at 700C. 5.1.9 Cool the crucible in a desiccator and weigh to the nearest mg. 5.1.10 Calculation = g BaSO4 = weight of crucible and residue - weight of crucible (tare) g B aS O
17、4 x 0 .5 8 8 4 x 1 0 0 S a m p le w ei g h t % B a = NUMBER: CEMS BT-43 TITLE Barium, Calcium, Magnesium And Zinc In Oil CURRENT ISSUE DATE: August 2009 This document is restricted and may not be sent outside Navistar, Inc. or reproduced without permission from Corporate Technical Standards. Supplie
18、rs are required to assume all patent liability. 2009 Navistar, Inc. AUGUST 2009 Page 3 of 4 5.2 CALCIUM 5.2.1 With constant stirring of filtrate from Step 5.17, add NaOH (30% solution), drop by drop, to a pH of 6 using pH paper. 5.2.2 Add 2 ml of Buffer Solution. This will raise the solution to a pH
19、 of 10. A precipitate may form, however it will dissolve upon addition of EDTA, and it is of no concern. 5.2.3 Add 1 ml of KCN (20%) and warm gently. CAUTION: The solution must be alkaline before any addition of KCN, otherwise HCN gas will be liberated. 5.2.4 With constant stirring, add 3 drops of E
20、riochrome Black T indicator. Titrate with EDTA solution until the color changes from red to blue, and then add approximately 5 ml of EDTA in excess. Solution is stirred until any precipitate or cloudiness has disappeared and the solution is a clean, clear blue color. Ten (10) ml of MgSO4 solution ar
21、e added and the titration is completed with EDTA until all traces of red have disappeared. (In this step, a better end point is obtained if the solution contains 10 ml of MgSO4 solution. The MgSO4 solution is added as indicated and should not be added at the beginning of the titration.) Retain the s
22、olution in the beaker for the zinc determination. (Step 5.3.1). 5.2.5 Calculation (No Magnesium Present) mg Ca = (ml EDTA - ml MgSO4) x 0.4008 s a m p le w ei g h t i n g r a m s x 1 0 m g C a% C a = 5.2.6 (With Magnesium Present - Before this calculation can be made the Mg must be determined) mg Ca
23、 = (ml EDTA-Mg ml equivalent-ml MgSO4) x 0.4008 m g C as a m p le w ei g h t i n g r a m s x 1 0% C a = 5.3 ZINC 5.3.1 Add 5 ml of formaldehyde (4% solution) to the solution from Step (5.2.4). If zinc is present, the solution will turn red; titrate to blue color with EDTA. 5.3.2 Calculation mg Zn =
24、ml EDTA x 0.6358 m g Zns a m p le w ei g h t i n g r a m s x 1 0% Zn= 5.4 MAGNESIUM 5.4.1 If magnesium is suspected or present, proceed as follows: 5.4.2 Repeat Steps (5.1) thru (5.1.6) with another 10 g sample. 5.4.3 To separate the barium sulfate precipitate, filter through a medium porosity, ashl
25、ess filter paper and wash with hot water adding the wash water to the filtrate. Final volume of the solution should not exceed 150 ml. Discard filter paper and precipitate. 5.4.4 Boil the filtrate and add 10 to 15 ml of 20% NH4 Cl and 2 grams of Ammonium Oxalate, continue boiling until dissolved. 5.
26、4.5 Remove from hot plate, add a few drops of methyl red indicator and bring solution to neutral with concentrated NH4OH and add 3 ml in excess. (Ca will precipitate if present.) 5.4.6 Place a solution on hot plate to just below the boiling point until all precipitate settles out (approximately one-
27、half hour). NUMBER: CEMS BT-43 TITLE Barium, Calcium, Magnesium And Zinc In Oil CURRENT ISSUE DATE: August 2009 This document is restricted and may not be sent outside Navistar, Inc. or reproduced without permission from Corporate Technical Standards. Suppliers are required to assume all patent liab
28、ility. 2009 Navistar, Inc. AUGUST 2009 Page 4 of 4 5.4.7 Filter the precipitate through medium porosity filter paper, wash the precipitate with hot water combining the filtrate and washings. (The precipitate contains any Ca present in the sample and may be discarded at this point.) 5.4.8 Cool the fi
29、ltrate and add 1:1 HCl until the solution turns red. Add 15 ml of 20% (NH4)2HPO4 solution. 5.4.9 Add 5 ml of concentrated NH4H for every 100 ml of solution. Continue stirring for at least 10 to 15 minutes. Let sit until precipitate settles out. 5.4.10 Filter the precipitate into medium porosity filt
30、er paper and wash it with NH4OH (5:95). 5.4.11 Put the precipitate and filter paper into a tared porcelain crucible and burn off at 900 to 1000C. 5.4.12 Cool the crucible in a desiccator and weigh to + 1 mg. 5.4.13 Calculation w ei g h t of r es id u e w ei g h t of s a m p le % Mg = x 0 .2 1 8 5 x 1 0 0 Mg ml equivalent (to be used in calcium determination when Mg is present). % Mg x 1 0 0 0 .2 4 3 = m l e q u i v al e n t of EDT A s o l u ti o n 6.0 REPORT 6.1 Percent barium. 6.2 Percent calcium. 6.3 Percent magnesium. 6.4 Percent zinc.
