Difference between revisions of "106.3.2.46 TM-46, Analysis of Cements and Fly Ashes"

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m (Per CM, article moved to conform with Sec 106. Old EPG 106.7.46 had no appreciable history and 1018 hits)
 
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This method analyzes cement, ground granulated blast furnace slag and fly ash by Atomic Absorption Spectrophotometry for the following elements:
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<div style="float: right; margin-left: 30px; margin-bottom: 30px;">__TOC__</div>
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This method analyzes cements and fly ashes by Inductively Coupled Plasma (ICP) Emission Spectroscopy.
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:Calcium (CaO)
 
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:Silicon (SiO<sub>2</sub>)
 
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:Aluminum (Al<sub>2</sub>O<sub>3</sub>)
 
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:Iron (Fe<sub>2</sub>O<sub>3</sub>)
 
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:Magnesium (MgO)
 
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:Potassium (K<sub>2</sub>O)
 
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:Sodium (Na<sub>2</sub>O)
 
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Titanium Dioxide(TiO<sub>2</sub>) and Phosphorus Pentoxide(P<sub>2</sub>O<sub>5</sub>) are analyzed using Inductively Couple Plasma Spectrophotometry.
 
  
 
==106.3.2.46.1 Reagents and Apparatus==
 
==106.3.2.46.1 Reagents and Apparatus==
  
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1) Atomic Absorption Spectrophotometer conforming to the specifications set forth in ASTM C 114.
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1) Inductively Coupled Plasma Emission Spectroscopy conforming to the specifications set forth in ASTM C 114.
  
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2) Graphite crucibles, 7.88 ml capacity, made from purified graphite. These should be preignited in a muffle furnace for 20 minutes at 950°C prior to use.
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2) Graphite crucibles, 7.88 ml capacity, made from purified graphite.
  
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3) Clear plastic beakers (Polypropylene), 400 ml capacity.
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3) Clear plastic beakers (Polypropylene), 250 ml capacity.
  
 
4) Magnetic stirring bars. The length of the bars used should be approximately 1/2 in. less than the inside diameter of the plastic beakers.
 
4) Magnetic stirring bars. The length of the bars used should be approximately 1/2 in. less than the inside diameter of the plastic beakers.
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6) Nitric Acid (HNO<sub>3</sub>). Sp. Gr. 1.42
 
6) Nitric Acid (HNO<sub>3</sub>). Sp. Gr. 1.42
  
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7) Hydrochloric Acid (HCl), Sp. Gr. 1.19
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7) NIST Standard and CCRL Samples. A supply of NIST cement and past CCRL proficiency samples stored in a desiccator.
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8) Lanthanum Oxide (La<sub>2</sub>O3), 99.99 percent pure, low calcium.
 
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9) Lanthanum Solution - 10 percent. Add 200 ml of distilled water to 117.28 g of lanthanum oxide (La<sub>2</sub>O<sub>3</sub>) in a 2000 ml beaker. While stirring, carefully add 500 ml of hydrochloric acid. When solution is complete, cool to room temperature, transfer to a 1000 ml volumetric flask and dilute to volume with distilled water.
 
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10) Standard Samples. A supply of National Bureau of Standards cement samples.
 
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11) 1000 ppm Calcium Stock Solution. This solution can be purchased from a number of sources or it can be prepared in the laboratory from a suitably pure calcium compound.
 
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12) 1000 ppm Silicon Stock Solution. This solution can be purchased from a number of
 
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sources or it can be prepared in the laboratory from a suitably pure silicon compound.
 
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13) 1000 ppm Aluminum Stock Solution. This solution can be purchased from a number of sources or it can be prepared in the laboratory from a suitably pure aluminum metal.
 
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14) 1000 ppm Iron Stock Solution. This solution can be purchased from a number of sources or it can be prepared in the laboratory from a suitably pure iron compound.
 
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15) 1000 ppm Magnesium Stock Solution. This solution can be purchased from a number of sources or it can be prepared in the laboratory from a suitably pure magnesium compound.
 
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16) 1000 ppm Potassium Stock Solution. This solution can be purchased from a number of sources or it can be prepared in the laboratory from a suitably pure potassium compound.
 
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17) 1000 ppm Sodium Stock Solution. This solution can be purchased from a number of sources or it can be prepared in the laboratory from a suitably pure sodium compound.
 
  
 
==106.3.2.46.2 Procedure==
 
==106.3.2.46.2 Procedure==
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===106.3.2.46.2.1 Selection of Standards===
 
===106.3.2.46.2.1 Selection of Standards===
  
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Select a series of national Bureau of Standards cement samples to bracket the expected concentration of the elements in the cement or fly ash samples. In those cases where standards are unavailable in the correct concentration range, the standard solutions may be adjusted to higher levels of the element of interest by addition of the proper amount of the stock solutions listed in items 11 –17 of EPG 106.3.2.46.1 Reagents and Apparatus.
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Select a series of NIST and past CCRL proficiency cement samples to bracket the expected concentration of the elements in the cement and/or fly ash samples.
  
 
===106.3.2.46.2.2 Preparation of standard solutions and sample solutions===
 
===106.3.2.46.2.2 Preparation of standard solutions and sample solutions===
  
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Weigh 0.80 g of anhydrous LiBO<sub>2</sub> into a suitable mixing vessel, then add 0.5000 g of cement standard, cement sample, or fly ash sample. Mix thoroughly and transfer the mixture to a pre-ignited graphite crucible. Place the crucible in the mouth of a muffle furnace and heat at 950°C for five minutes (or until the mixture melts). Remove from the furnace and gently swirl to coagulate any particles of fusion mix remaining on the walls of the crucible. Place the crucible within the furnace and heat for 10 minutes. Remove from the furnace and immediately pour the molten melt into a clear polypropylene beaker containing 100 ml of 1:24 HNO<sub>3</sub> and a Tefloncoated magnetic stirring bar. Place the beaker on a magnetic stirring unit and stir for ten to fifteen minutes. Filter through Whatman No. 41 filter paper into a 500 ml volumetric flask.
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Place a ¼ teaspoon of anhydrous LiBO<sub>2</sub> into a graphite crucible. Using a test tube that just fits into the crucible, press down on the LiBO<sub>2</sub> to make a bed at the bottom of the crucible. Weigh 0.2500 +/- .0005 grams of sample into the bed of LiBO<sub>2</sub> and cover the sample with an additional ¼ teaspoon of LiBO<sub>2</sub>. Place the crucible in the mouth of a muffle furnace and heat at 1000°C for at least 30 minutes. Remove from the furnace and gently swirl to coagulate any particles of the fused mixture remaining on the walls of the crucible and immediately drop the fused bead into a clear polypropylene beaker containing 200 ml of 1:24 HNO<sub>3</sub> and a Teflon coated magnetic stirring bar. Place the beaker on a magnetic stirring unit and stir for ten to fifteen minutes. Filter through Whatman No. 41 filter paper into a 250 ml volumetric flask. Wash the beaker and filter paper thoroughly with 1:24 HNO<sub>3</sub>. Dilute to volume with 1:24 HNO<sub>3</sub> and mix well by inverting the volumetric flask multiple times. Prepare a fusion-blank solution in the same manner, omitting only the addition of sample.
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Wash the beaker and filter paper thoroughly with 1:24 HNO<sub>3</sub>. Dilute to volume with 1:24 HNO<sub>3</sub>, mix well, and transfer to a clean polyethylene bottle. Prepare a fusion-blank solution in the same manner, omitting only the addition of sample.
 
  
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Calibrate the instruments using the fusion-blank solution and the standard solutions, then, using the AA Spectrophotometer, determine percent SiO<sub>2</sub>, percent Al<sub>2</sub>O<sub>3</sub>, percent Fe<sub>2</sub>O<sub>3</sub>, percent K<sub>2</sub>O and percent Na<sub>2</sub>O on the sample solutions. Determine the percent TiO<sub>2</sub> and the percent P<sub>2</sub>O<sub>5</sub> using the ICP Spectrophotometer. Pipette 10 ml of 10% Lanthanum solution, 5 ml of HNO<sub>3</sub>, and a 2 ml aliquot of the solutions prepared in the above paragraph into a 100 ml volumetric flask and dilute to volume with distilled water. Determine percent CaO and percent MgO on this dilution.
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Calibrate the ICP using the fusion-blank and the fused NIST and CCRL proficiency cement samples of varying concentrations for each analyte. Determine percent CaO, MgO, Fe<sub>2</sub>O<sub>3</sub>, TiO<sub>2</sub> and SrO by pipetting 5 ml of the fused sample solution and create calibration lines using the same dilution with the NIST and CCRL proficiency cement stock solutions into a 100 ml volumetric flask and dilute to volume. The remaining analytes can be analyzed directly from the sample and stock solutions with no additional dilutions.
  
 
==106.3.2.46.3 Calculation and Report==
 
==106.3.2.46.3 Calculation and Report==
  
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The method of calculation will vary with the make and model of instrument used. Report the elements determined as follows:
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Report the elements determined as follows:
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{| style="margin-left: 50px;"
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:% Silicon Dioxide (SiO<sub>2</sub>)
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|-
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:% Aluminum Oxide (Al<sub>2</sub>O<sub>3</sub>)
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| % Silicon Dioxide (SiO<sub>2</sub>) || % Chromium Oxide (Cr<sub>2</sub>O<sub>3</sub>)
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:% Iron Oxide (Fe<sub>2</sub>O<sub>3</sub>)
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|-
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:% Calcium Oxide (CaO)
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|% Aluminum Oxide (Al<sub>2</sub>O<sub>3</sub>) || % Zinc Oxide (ZnO)
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:% Magnesium Oxide (MgO)
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|-
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:% Potassium Oxide (K<sub>2</sub>O)
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| % Iron Oxide (Fe<sub>2</sub>O<sub>3</sub>) || % Manganic Oxide (Mn<sub>2</sub>O<sub>3</sub>)
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:% Sodium Oxide (Na<sub>2</sub>O)
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|-
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:% Titanium Dioxide (TiO<sub>2</sub>)
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| % Calcium Oxide (CaO) || % Strontium Oxide (SrO)  
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:% Phosphorus Pentoxide (P<sub>2</sub>O<sub>5</sub>)
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|-
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| % Magnesium Oxide (MgO) || % Barium Oxide (BaO)
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|-
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| % Potassium Oxide (K<sub>2</sub>O)
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|-
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| % Sodium Oxide (Na<sub>2</sub>O)
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|-
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| % Titanium Dioxide (TiO<sub>2</sub>)
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|-
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| % Phosphorus Pentoxide (P<sub>2</sub>O<sub>5</sub>)
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|}
 
[[Category:106.3.2 Material Inspection Test Methods]]
 
[[Category:106.3.2 Material Inspection Test Methods]]

Latest revision as of 10:43, 26 May 2023

This method analyzes cements and fly ashes by Inductively Coupled Plasma (ICP) Emission Spectroscopy.

106.3.2.46.1 Reagents and Apparatus

1) Inductively Coupled Plasma Emission Spectroscopy conforming to the specifications set forth in ASTM C 114.

2) Graphite crucibles, 7.88 ml capacity, made from purified graphite.

3) Clear plastic beakers (Polypropylene), 250 ml capacity.

4) Magnetic stirring bars. The length of the bars used should be approximately 1/2 in. less than the inside diameter of the plastic beakers.

5) Lithium Metaborate (LiBO2), Reagent Grade, anhydrous.

6) Nitric Acid (HNO3). Sp. Gr. 1.42

7) NIST Standard and CCRL Samples. A supply of NIST cement and past CCRL proficiency samples stored in a desiccator.

106.3.2.46.2 Procedure

106.3.2.46.2.1 Selection of Standards

Select a series of NIST and past CCRL proficiency cement samples to bracket the expected concentration of the elements in the cement and/or fly ash samples.

106.3.2.46.2.2 Preparation of standard solutions and sample solutions

Place a ¼ teaspoon of anhydrous LiBO2 into a graphite crucible. Using a test tube that just fits into the crucible, press down on the LiBO2 to make a bed at the bottom of the crucible. Weigh 0.2500 +/- .0005 grams of sample into the bed of LiBO2 and cover the sample with an additional ¼ teaspoon of LiBO2. Place the crucible in the mouth of a muffle furnace and heat at 1000°C for at least 30 minutes. Remove from the furnace and gently swirl to coagulate any particles of the fused mixture remaining on the walls of the crucible and immediately drop the fused bead into a clear polypropylene beaker containing 200 ml of 1:24 HNO3 and a Teflon coated magnetic stirring bar. Place the beaker on a magnetic stirring unit and stir for ten to fifteen minutes. Filter through Whatman No. 41 filter paper into a 250 ml volumetric flask. Wash the beaker and filter paper thoroughly with 1:24 HNO3. Dilute to volume with 1:24 HNO3 and mix well by inverting the volumetric flask multiple times. Prepare a fusion-blank solution in the same manner, omitting only the addition of sample.

Calibrate the ICP using the fusion-blank and the fused NIST and CCRL proficiency cement samples of varying concentrations for each analyte. Determine percent CaO, MgO, Fe2O3, TiO2 and SrO by pipetting 5 ml of the fused sample solution and create calibration lines using the same dilution with the NIST and CCRL proficiency cement stock solutions into a 100 ml volumetric flask and dilute to volume. The remaining analytes can be analyzed directly from the sample and stock solutions with no additional dilutions.

106.3.2.46.3 Calculation and Report

Report the elements determined as follows:

% Silicon Dioxide (SiO2) % Chromium Oxide (Cr2O3)
% Aluminum Oxide (Al2O3) % Zinc Oxide (ZnO)
% Iron Oxide (Fe2O3) % Manganic Oxide (Mn2O3)
% Calcium Oxide (CaO) % Strontium Oxide (SrO)
% Magnesium Oxide (MgO) % Barium Oxide (BaO)
% Potassium Oxide (K2O)
% Sodium Oxide (Na2O)
% Titanium Dioxide (TiO2)
% Phosphorus Pentoxide (P2O5)
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