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Standard Test Procedure for Measuring the Dissolution of Aluminum Hardeners TP-2 S tand ard Test P ro ced ure fo r M easuring the D isso lutio n o f A lum inum H ard eners Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS --``,``,,,,`,,,,`,`,`,,-`-`,,`,,`,`,,`--- No warranty or guarantee of any kind, expressed or implied, by the Aluminum Association or its member companies accompanies this information. Accordingly, the Aluminum Association and its member companies assume no responsibility or liability for their use whether based on warranty, contract, negligence, strict liability product liability, or otherwise. The use by any member or nonmember of this test procedure is purely voluntary. The Association’s publication of this test procedure does not in any respect prevent or restrict any member or nonmember from manufacturing or supplying products tested under this or any other test procedure. All Aluminum Association published standards, data, specifications and other material are reviewed at least every five years and revised, reaffirmed or withdrawn. Users are ad vised to contact the Aluminum Association to ascertain whether the information in this publication has been superseded in the interim between publication and proposed use. Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS - - ` ` , ` ` , , , , ` , , , , ` , ` , ` , , - ` - ` , , ` , , ` , ` , , ` - - - Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS - - ` ` , ` ` , , , , ` , , , , ` , ` , ` , , - ` - ` , , ` , , ` , ` , , ` - - - Standard Test Procedure for Measuring The Dissolution of Aluminum Hardeners 1. Scope The Aluminum Association dissolution test procedure can be used to determine the suitability of an aluminum hardener product for alloying purposes. The test procedure describes a method for measuring dissolution time and recovery of the hardener element under standardized conditions. This method is not intended to predict dissolution rate or recovery under production conditions in commercial opera- tions. 2. Applicable Specifications and Registration Records — The following specifica- tions or registration records (the issue in effect on date of material purchase) form a part of the test procedure: 2.1 The Aluminum Association Registration Record, “International Designations and Chemical Composition Limits for Aluminum Hardeners” (Gray Sheets). 2.2 OSHA - 1910.1200 Hazard Communication Standard. 2.3 ASTM Standard E34, Test Methods for Chemical Analysis of Aluminum and Aluminum-Base Alloys, and ASTM E88, Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical Composition. 2.4 ASM Handbook, Volume 9, Metallography and Microstructures, 2004, p. 771. 2.5 ASTM B215, Standard Methods for Sampling Finished Lots of Metal Powders. 2.6 ASTM E716, Standard Practice for Sampling Aluminum and Aluminum Alloys for Spectrochemical Analyses. 3. Sample Location, Sample Frequency and Lot Definition 3.1 Ingot - Each heat of material shall be considered a lot. An ingot, selected randomly from a heat, may be considered representative of the lot. 3.2 Briquet - A lot is defined as a finite quantity produced under uniform condi- tions and should be clearly identified on material packaging. A shipment may contain more than one lot. Sample selection for chemical analysis shall be on a one lot basis and shall consist of one briquet pulled from each of three and not more than five randomly-selected shipping containers. Combined, these briquets are termed a “gross lot sample” and will be the basis for a discreet analytical determination. Multiple “gross lot samples” shall be pulled if multiple chemical determinations are required. Sample selection for dissolu- tion rate testing shall be completed in a similar manner, however, the total number of briquets required is to be based on addition level, and test bath weight. This sample should be held separate from analytical sample(s). Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS - - ` ` , ` ` , , , , ` , , , , ` , ` , ` , , - ` - ` , , ` , , ` , ` , , ` - - - 3.3 Canned Hardeners - A lot is defined as a finite quantity, all of which is produced under the same conditions. A single can shall be pulled from a randomly-selected product container. 3.4 Powder - A lot is defined as a finite quantity, all of which is produced under the same conditions. A powder sample of the required weight shall be taken from a randomly-selected product container using approved sample cutting techniques. 4. Sample Preparation 4.1 Chemical Analysis - The randomly-selected samples shall be prepared as follows: 4.1.1 Ingot - The sample for chemical analysis shall be comprised of dry drillings. The drillings shall be obtained from five (5) positions of the ingot, diagonally located (Figure 1), and shall include approximate equal weight of drill chips from top, middle and bottom for each sample point of the ingot. The drillings shall be mixed to form the sample 4.1.2 Briquet - The chemical analysis sample(s) for briquetted hardeners shall consist of ground material taken from the “gross lot sample” described in Section 3.2. The entire “gross lot sample” must be crushed with a mortar and pestle or mechanical pulverizer, taking care to minimize contamina- tion or carryover. The resulting powder must freely pass through an 8 mesh (2.36mm) screen. The entire sample is then blended in a suitably-sized blender. It is recommended that a suitably-volatile-blending-aid addition be made during the blending step. The blended gross sample is then passed through a sample splitter to obtain four subsamples, 25 to 50 grams weight each. If a blending aid was added, it should be dried from the final subsamples before analysis. Three subsamples are analyzed. The final lot composition estimate is the average of the three separate analytical values. 4.1.3 Powder - The required amount of powder shall be obtained from the sample using approved sample cutting techniques, per ASTM B215. 4.2 Dissolution Rate - For determination of dissolution rate and recovery and metal- lographic examination, samples shall be prepared as follows: 4.2.1 Ingot - The randomly-selected ingot shall represent the heat. The sample for the dissolution test shall consist of one piece of the required weight, including top and bottom surface from the center position of the ingot. 4.2.2 Briquet - The “dissolution sample” collected as per Section 3.2 shall represent the production lot. It should consist of the required total briquet weight to meet addition level requirements for the involved test bath weight. Use of partial briquets should be avoided. 4.2.3 Powder and Cans - A randomly-selected powder sample or split sample, from the can, shall represent the batch or lot. 5.Chemical Composition 5.1 Procedure - The sample prepared in accordance with Section 4.1 shall be analyzed in accordance with ASTM Standard E34, Test Methods for Chemical Analysis of Aluminum and Aluminum-Base Alloys, and ASTM E88, Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical Composition. Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS - - ` ` , ` ` , , , , ` , , , , ` , ` , ` , , - ` - ` , , ` , , ` , ` , , ` - - - 5.2 Requirements - The hardeners, if registered, shall conform to the chemical composition limits shown in The Aluminum Association’s Registration Record “International Designations and Chemical Composition Limits for Aluminum Hardeners” or, if not registered, the hardener composition shall be as agreed by the supplier and purchaser. 6. Dissolution Test Procedure Description - This standard test procedure is applicable for determining the dissolution rate of aluminum master alloys, or additives, in 99.7% aluminum and the recovery of the alloying element. 6.1 Dissolution Test Supplies and Equipment 6.1.1 Supply of 99.7% (P1020A) pure virgin aluminum with the following limits on impurities. Silicon 0.10 max Iron 0.20 max Others, each 0.03 Total 0.10 Aluminum BALANCE Other aluminum purity levels, mutually acceptable to the supplier and purchaser, may be used. 6.1.2 Electric resistance furnace capable of maintaining 1382°F ±10°F (750°C ±5°C), and large enough to contain the required size crucible (Section 6.1.3). 6.1.3 A crucible of material, inert to liquid aluminum or one with a suitable coating to render it inert, such as silicon carbide, clay-bonded graphite with Terrepain 55M coating or cast iron with Dykote (a Foseco product) coating. Alternative coatings, found to be equivalent, may be used. The size of the crucible shall be adequate to hold a heat large enough to provide the required number and size of samples. 6.1.4 Calibrated and certified thermocouple and controller indicator capable of controlling and measuring temperature up to 1392°F (755°C). 6.1.5 One appropriately-sized sampling ladle. 6.1.6 Graphite melt skimmer with flat paddle surface. 6.1.7 Clean aluminum plate. 6.1.8 One standard, Type B, ASTM, E716, center-pour mushroom sample mold. 6.1.9 Sixty-minute timer. 6.1.10 Graphite stirring rod, 1-inch diameter x 24” long (25.4 mm diameter x 609 mm long). 6.1.11 Argon supply and appropriate tubes for fluxing. 6.1.12 Spectrochemical analysis equipment. 6.1.13 Lathe and tools for machining spectrochemical disc sample. 6.1.14 Magnaflux Digital Conductivity Meter, Model FM140, or equivalent. 6.1.15 Notebook. 6.1.16 Personal protective clothing and face shield. Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS --``,``,,,,`,,,,`,`,`,,-`-`,,`,,`,`,,`--- 6.2 Procedure for Dissolution Test 6.2.1 Weigh aluminum (Section 6.1.1) to provide the desired heat size, place in appropriately-sized, clean, skull-free crucible (Section 6.1.3), and record weight of aluminum in notebook. 6.2.2 Heat the aluminum to an appropriate temperature and stabilize so that after addition of hardener, aluminum temperature shall be: 6.2.2.1 1337°F ±10°F (725° ±5°C) for products to be used in a remelt facility. 6.2.2.2 1382°F ±10°F (750° ±5°C) for products to be used in a smelter facility. 6.2.2.3 Other test temperatures may be used, subject to mutual agreement by the supplier and the purchaser. 6.2.3 Flux melt with dry Argon flow rate of 4 cubic feet per hour for 10 minutes. 6.2.4 Skim the dross from the aluminum surface, deposit skim on clean aluminum plate or cast into suitable mold. When cooled to ambient tem- perature, weigh dross and record weight. 6.2.5 Take an initial blank sample for chemical analysis. 6.2.5.1 Float the sample ladle on surface of the metal until it reaches temperature of the melt. If this chills the melt below the desired temperature, then heat ladle in a furnace. 6.2.5.2 Tilt the sample ladle and fill with molten metal. 6.2.5.3 Remove sample ladle and pour contents into the preheated (350°F [177°C]) mushroom sample mold, return excess metal to crucible. 6.2.5.4 After sample has solidified, remove from mold and number sample “0”. 6.3 Nominal target composition for elements that are found in commercial alloys: Bismuth 0.10% or 0.50% Boron 0.02% Chromium 0.25% Copper 0.05% or 5.0% Iron 0.50% or 1.0% Lead 0.50% Magnesium 0.50% or 5.0% Manganese 1.2% Nickel 0.7% Silicon 1.0% or 12.0% Strontium 0.02% Titanium 0.05% or 0.20% Vanadium 0.08% Zirconium 0.12% NOTE: Refer to OSHA-1910.1200 Hazard Communications Standard Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS - - ` ` , ` ` , , , , ` , , , , ` , ` , ` , , - ` - ` , , ` , , ` , ` , , ` - - - 6.4 Based upon the remaining heat size, calculate the quantity of hardener product required (equation below). Weigh hardener to be added, record calculation and weights in notebook. W E W EH D A H = × where: WH = Weight of hardener alloy to be added, lbs (kg) ED = Element content desired in melt, percent EH = Element content of hardener, percent (actual content reported by supplier or as determined by the user) WA = Weight of aluminum melt, lbs (kg) 6.5 Add the weighed hardener to the molten aluminum. Materials less dense than the aluminum should be held below the aluminum surface using coated steel or graphite tools. 6.6 For alloy hardeners, stir the melt vigorously for 30 seconds immediately before the first sample is taken and then for 10 seconds immediately before each additional sample. 6.6.1 Samples (Section 6.2.5) shall be taken as follows: (a) For first 10 minutes at 1-minute intervals. (b) For next 50 minutes at 10-minute intervals. (c) Skim dross from aluminum surface, cool, weigh, and record as in Section 6.2.4. 6.7 For briquets, do not stir for five minutes after addition. 6.7.1 Samples (Section 6.2.5) shall be taken as follows: (a) After addition, 2 minutes 20 minutes 5 minutes 30 minutes 10 minutes Final Sample (b) Ten-second stirring shall be performed after the 5-minute and 30- minute samples. The final sample shall be taken immediately after stirring for 10 seconds. (c) Skim dross from aluminum surface, cool, weigh and record as in Section 6.2.4. 6.8 For canned hardeners, stir for 60 seconds starting 30 seconds after addition. 6.8.1 Samples (Section 6.2.5) shall be taken as follows: (a) Every 5 minutes for 30 minutes. (b) After the 30-minute sample, stir for 10 seconds, then take final sample. Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS - - ` ` , ` ` , , , , ` , , , , ` , ` , ` , , - ` - ` , , ` , , ` , ` , , ` - - - (c) Skim dross from aluminum surface, cool, weigh and recordas in Section 6.2.4. 6.9 All samples shall be identified sequentially. 6.10 Observations for bubbles, fumes, flames or odors shall be made and recorded. 6.11 Record, in notebook, sample number, sampling time and temperature. 6.12 Analysis - Prepare the disk samples for spectrochemical analyses by removing the sprue and scalping 14-22% of the disk thickness off the as-cast disk face. Typical removal is 0.100 inch from the half-inch thick disk. Analyze (burn) the disk in at least two (2) locations (Figure 2). The spectrochemical analyses should be made within a 1/2-inch (12.7 mm) wide annular ring. The ring’s outer edge is 1/4 inch (6.33 mm) away from the outer edge of the disk (see Figure 3 in E716). The analyses is to be obtained using suitable reference materials (standards). Average the result of the two (2) burns and record the results. 6.13 Calculation of Element Recovery 6.13.1 Recovery is expressed as follows: R W W W E W E W E A H s n x n s A s H H n n x n = + − × − × × ×( ) = = ∑ = = 1 1 100 −− × −( )( ) = = = ∑ W E Es s s n x n n n n 1 2 Where: R = Recovery (%) Esn = Sample analysis, %, for hardener element in each respective sample taken: Esn=1 = Starting molten base metal analysis, %, for hardener element (formerly E2) Esn=x = Final sample’s analysis EH = Element content, %, of hardener charged - actual content reported by supplier, or as determined by purchaser. WA = Weight of starting aluminum melt, lbs. (g). WH = Weight of hardener added to melt, lbs. (g). Wsn = Weight of each respective sample taken, lbs. (g) n x n = = ∑ 1 = Sum of series of samples, first to last ⎛ ⎝⎜ ⎞ ⎠⎟ ⎡ ⎣ ⎢ ⎢ ⎤ ⎦ ⎥ ⎥ ⎡ ⎣ ⎢ ⎢ ⎤ ⎦ ⎥ ⎥ ⎛ ⎝⎜ ⎞ ⎠⎟ ⎡ ⎣ ⎢ ⎢ ⎤ ⎦ ⎥ ⎥ ⎡ ⎣ ⎢ ⎢ ⎤ ⎦ ⎥ ⎥ Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS --``,``,,,,`,,,,`,`,`,,-`-`,,`,,`,`,,`--- Example: WA = 9922g. WH = 147g. EH = 10.2% Ti (Supplier) Time (min) Wsn (g) Esn (%) Wsn × (Esn – Esn=1)___________ ___________ ___________ ________________ 0 (n=1) 1 (n=2) 2 3 5 10 15 (n=x) 119 131 145 129 127 101 142 0.005 0.128 0.142 0.145 0.152 0.153 0.153 — 16.113 19.865 18.060 18.669 14.948 21.016 Ws n x n n = = ∑ 1 = 894 W E Es s s n x n n n n× −( )= = = ∑ 1 2 = 108.671 Esn=1 = 0.005% Esn=x = 0.153% R = + −( )× − × × ×( ) − 9922 147 894 0 153 9922 0 005 100 147 10 2 108 67 . . . . 11 1403 775 49 61 100 1499 4 108 671 97 37 = −[ ]× −[ ] = . . . . . % 6.14 Dross Formation Measurement 6.14.1 Dross formation may be determined using the dross weight recorded from Sections 6.6.1 (c), 6.7.1 (c) or 6.8.1 (c). The percent of dross formed may be expressed as: D W W W D A H = × + 100 where: D = Dross formed, percent WD = Weight of dross WA = Net weight of aluminum melt WH = Weight of hardener added to melt 6.15 Metallographic Examination 6.15.1 When metallographic examination is required, the analytical samples shall be cut to obtain a section from the mid-radius (approximately the same distance from the center as the analytical “burn” locations) of the piece (Figure 2). The section removed shall be mounted and polished for metal- lographic examination of a surface perpendicular to the disc face. Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS --``,``,,,,`,,,,`,`,`,,-`-`,,`,,`,`,,`--- 6.15.2 The samples shall be mounted and polished in accordance with ASM Handbook, Volume 9, Metallography and Microstructures, 2004, p. 771. 6.16 Conductivity - Conductivity measurements made with a Magnaflux Digital Conductivity Meter or equivalent may be used to determine whether hardener is in solution, or dispersed in the aluminum. (Conductivity values for hardener concen- trations must be developed by the test user.) 6.17 Results 6.17.1 Element Recovery - Recovery is calculated for each sample taken. Recovery values are then plotted on graph paper to show relationship of recovery (ordinate) to elapsed time for the sample (absicca). Satisfactory hardener performance is indicated by rapid dissolution to a high recovery value. 6.17.2 Dross Formation - A hardener that produces a low percentage of dross and minimal bubbles, fumes, flames and odors is preferred. 6.17.3 Metallographic - The structure of the sample shall be examined for evidence of undissolved hardener element which may be unacceptable. Examples of undissolved hardener particles are shown in Figure 3. 6.17.4 Conductivity - Low conductivity indicates hardener is in solution. Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS - - ` ` , ` ` , , , , ` , , , , ` , ` , ` , , - ` - ` , , ` , , ` , ` , , ` - - - FIGURE 1: Typical location of drilling positions to obtain chip for wet chemical analysis of ingot. FIGURE 2: Disk sample preparation, typical mid-radius positions for spectrographic analysis and sample for metallographic examination. (See E716 for further details) + = Diagonal Sample + = Drill Positions Typical Scalp Depth Sample for metallographic examination, surface to be examined. + = Analytical Points (0.10″ (2.66 mm)) Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS --``,``,,,,`,,,,`,`,`,,-`-`,,`,,`,`,,`--- FIGURE 3: Photographs showing undissolved metal particles. (a) Undissolved Iron 250X (b) Undissolved Manganese 250X (c) Undissolved Titanium 250X Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS --``,``,,,,`,,,,`,`,`,,-`-`,,`,,`,`,,`--- Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS - - ` ` , ` ` , , , , ` , , , , ` , ` , ` , , - ` - ` , , ` , , ` , ` , , ` - - - Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/22 14:33:21 GMTNo reproduction or networking permitted without license from IHS --``,``,,,,`,,,,`,`,`,,-`-`,,`,,`,`,,`--- 1525 Wilson Boulevard, Suite 600, Arlington, VA 22209 www.aluminum.org Copyright The Aluminum Association Inc. Provided by IHS under license with AA Sold to:HYDRO ALUMINIUM DEUTSCHLAND GM, 01771604 Not for Resale,2009/10/2214:33:21 GMTNo reproduction or networking permitted without license from IHS - - ` ` , ` ` , , , , ` , , , , ` , ` , ` , , - ` - ` , , ` , , ` , ` , , ` - - -