CHEMICAL TEST

 Lost on Ignition
o Procedure:
1. Weight 1g cement sample into pre-ignited and pre-weighed platinum/porcelain crucible
2. Ignite at 950 +/- 50°C for 15 mins.
3. Cool, place the crucible inside the desiccator
4. Weigh
o Formula:
Wt of sample before ignition−Wt of sample after ignition
1. % LOI = ×100
Wt of sample
 Insoluble Residue
o Reagents:
1. Sodium Hydroxide solution,
2. Hydrochloric Acid
3. Methyl red indicator.
4. Hot water is needed for washing.
o Procedure:
1. Start the test by weighing one gram of sample. Place the sample in the evaporating dish.
2. Add 25 ml. of water and 5 ml. hydrochloric acid.
3. Grind the material with the flattened end of the glass rod and stir until decomposition is complete.
4. Then dilute the solution to 50 ml.
5. Place it in a stove and digest the solution until it boils.
6. Filter the solution through a Medium textured paper,
7. And wash the residue with hot water.
8. Set aside 225 to 260 ml. of the filtrate for use in Sulfur tri-oxide determination.
9. Then put the residue back into the dish.
10. Add 100 ml. NaOH solution and 1 to 2 drops methyl red indicator.
11. Put the dish back in the stove and digest until it boils.
12. Acidify the solution with hydrochloric acid.
13. Filter or wash the residue with hot water, then discard the filtrate.
14. Place the residue in the crucible and ignite it in a at furnace at 900°to 1000°C.
15. Cool the ignited residue in a dessicator.
16. Then weigh the ignited residue, represent the weight by a. Then weigh the empty crucible, represent the
weight by b.
o Formula:
a−b
1. % I . R .= ×100
c
 MgO
o Reagents:
1. Ammonium Phosphate Dibasic
2. Hydrochloric Acid
3. Ammonium Hydroxide
4. Ammonium Oxalate
5. Methyl Red Indicator
o Procedure:
1. Start the test by weighing 0.5 gram of sample and place it in an evaporating dish
2. Add 10 ml. water and 10 ml. hydrochloric acid and stir.
3. Grind the materials until decomposition is complete.
4. Place the solution in the stove or hot plate and evaporate to dryness at low temperature.
5. Add 10 ml. water and 10 ml. hydrochloric acid and digest until it boils.
6. Filter and wash the residue with hot water. Discard the residue.
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 7. Add 1-2 drops methyl red indicator to the filtrate, then heat to boiling.
8. Treat the solution with ammonium hydroxide until brown precipitate occurs.
9. Heat the solution to boiling.
10. Filter and wash the residue with hot water. Discard the residue.
11. Acidify the filtrate with hydrochloric acid then add 30 ml. of ammonium oxalate solution.
12. Add ammonium hydroxide until the color turns yellow and white precipitate appears
13. Let the solution stand for one hour, then filter and wash with hot water. Discard
14. the residue.
15. Again, acidify the resulting filtrate with Hydrochloric acid until it turns pink.
16. Add 10 ml. Ammonium Phosphate dibasic.
17. Then add 30 ml. ammonium hydroxide until the solution becomes yellow.
18. Stir the solution vigorously until a precipitate is formed.
19. Let the solution stand overnight. Filter and wash with Ammoniacal solution. Discard the filtrate.
20. Place the residue in a crucible and ignite at 11000 C, Cool, and weigh as Magnesium Pyrophosphate
Mg2 P2 O2
21. Add 10 ml. Ammonium Phosphate dibasic.
22. Then add 30 ml. ammonium hydroxide until the solution becomes yellow.
23. Stir the solution vigorously until a precipitate is formed.
24. Let the solution stand overnight. Filter and wash with Ammoniacal solution. Discard the filtrate.
25. Place the residue in a crucible and ignite at 11000 C, Cool, and weigh as Magnesium Pyrophosphate
Mg2 P2 O2
o Formula:
 % MgO=W ×72.4
 Where: W=grams of Magnesium; 72.4= molecular ratio of 2 MgO to Mg2P2O7 (0.362) divided by the
weight of sample used and multiplied by 100.
 SO3
o Reagents:
1. Barium Chloride
o Procedure:
1. First, add 10 ml. of barium chloride Solution to the filtrate reserve from the preceding test.
2. Place it on the stove and digest the solution until a white precipitate appears, and let it stand overnight.
3. After this, filter and wash the residue with hot water.
4. Place the residue in the porcelain or platinum crucible and ignite at 800° to 900°C.
5. Cool and then weigh
o Formula:
W × 34.3
1. SO 3=
Wt . of sample
where: W=grams of Barium Sulfate; 34.3= molecular ratio of SO3 to BaSO4 (0.343) multiplied by 100.

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