Gravimetry (% Moisture)

Gliezl Allison G. Imperial Institute of Chemistry, University of the Philippines, Diliman, Quezon City Date Performed: June 19, 2013 Date Submitted: June , 2013

I.

Methodology

This experiment aims to determine the amount of moisture and phosphorus present in the fertilizer sample through gravimetric method by calculating the mass and its equivalent percentage amount in the sample. The experimental procedure of this experiment was divided into four parts. On the initial day, the crucible to be used for the entire experiment was prepared and labelled with a pencil. The crucible was then placed inside the oven at 110 C and was left until the next laboratory period. The crucible cover must always be left slightly ajar when inside the oven. For the second part, the crucible was removed using a pair of tongs from the oven and was placed inside the desiccator for drying. The crucible was left inside for 15 minutes. After cooling, the crucible was weighed using an analytical balance. The process done on the first day was repeated until a constant weight was achieved (a difference between 0.0002g - 0.0003g). Subsequently, the fertilizer sample was weighed by difference in the crucible. The weight was then recorded and the crucible containing the fertilizer sample is set inside the oven at 110 C for drying until the next laboratory meeting. For the third part of the experiment, the crucible with the fertilizer sample is removed from the oven and was transferred to the desiccator for 15 minutes of cooling. The initial weight of the crucible with fertilizer was recorded and the process of oven-drying was repeated for 30 minutes. This cycle continues until a constant weight is achieved with a waiting time interval of 30 minutes. While waiting for the crucible to settle at a constant weight, the following solutions were prepared: 500 mL solution of 10% MgSO47H20 and 500 mL 2M NH3.

After obtaining a constant weight, the fertilizer sample was then transferred to a 250-mL beaker and was dissolved with 40 mL of H2O. The fertilizer was filtered using a filter paper in order to obtain a clear filtrate. The clear filtrate was transported to a new 250-mL beaker and an addition of 45 mL of 10% MgSO47H20 was performed. Then, 150 mL of 2M NH3 was added drop by drop into the clear filtrate while vigorously stirring it. For the first 50 mL, a slow addition of the base was performed and a faster drop rate for the next 100 mL until a white precipitate forms. The mixture is left settled for 15 minutes before filtering. After the mixture has settled, the solution was poured into a preweighed filter paper. The beaker was washed with two 5 mL of distilled H20 in order to quantitatively transfer the remaining precipitate. Lastly, the precipitate is washed with two 10 mL of 95% ethanol and air-dried while the filter paper was spread open until the next laboratory period. For the final part of the experiment, the filter paper containing the precipitate is placed inside the oven at 110 C for an hour. After, the filter paper was then placed in a beaker and left to cool for 15 minutes inside the desiccator. The weight was recorded for both the filter paper and the fertilizer. II. Results and Discussion For the past centuries, less than 50% of the earths soil contains the essential organic nutrients needed to meet the current food production of the human race. Since some of the most vital nutrients are readily available from air and water, other macronutrients such as phosphorus, nitrogen, and potassium lack in sufficient amounts in the soil to support plant growth. Through the modern way of synthesizing new products, commercial fertilizers paved the way of replenishing the soil with its additional

nutrients to keep the plants healthy and increase its growth rate. In order to ensure the plants with adequate amount of these nutrients, it is important that the amounts of these nutrients are quantified with the help of gravimetric measures. The instrument used in this experiment is the electronic analytical balance. Compared to the mechanical balance, the analytical balance has a different principle of operation. When an object is placed on the pan of the analytical balance, the object pushes the pan down with a force given in this equation: F=mg where m is the mass and g is the acceleration of gravity. The null detector senses the displacement and sends an error signal to the circuit that generates a correction current. This current flows through the coil beneath the pan, thereby creating a magnetic field that is repelled by a permanent magnet under the pan. As the deflection decreases, the output of the null detector decreases. The current required to restore the pan to its initial position is proportional to the mass on the pan. (Harris, p23) On the other hand, the mechanical balance uses standard masses and a balance beam hanging on a sharp knife edge to measure the mass. The mass of the pan hanging from the balance point (another knife edge) at the left is balanced by a counterweight at the right. To remove weights from a bar that is above the pan and hidden inside the balance, the knobs are rotated. The balance beam is restored almost to its original position when the masses removed are nearly equal to the mass of the object on the pan. The slight difference from the original position is shown on an optical scale, whose reading is added to that of the knobs. (Harris, p23)
In the initial procedure, the weight of the crucible was taken until its value became constant. It is important to dry until constant weight because all solids tend to rapidly absorb moisture from the atmosphere. This kind of property can be seen in hygroscopic reagents. These kinds of substances will continually increase in weight the longer they are exposed to air. In order to avoid mechanical errors, this experiment required the crucible to be set at a

constant weight until the absorbed moisture is removed and set to a low standard level.

In order to obtain the weight of the crucible and also the fertilizer, an alternate procedure of weighing by difference is taken into account to protect the analytical balance from corrosion. This is one of the advantages of weighing by difference compared to placing the chemical directly on the weighing pan. Also, weighing by difference negates all possible errors therefore a more accurate value of the substance is obtained since only the weight of that specific substance is weighed regardless of the other instruments present. In the experiment, the constant weight remained the same even though a systematic error was made by accidentally touching the crucible. But as far as the results have shown, the weight is still at its constant weight of 42.157 g. Then, 3 g of ground fertilizer was measured into the crucible to be weighed by difference. This procedure is important before drying so that the laboratory sample has the same composition as the bulk sample. The smaller the sample size, the greater is the need for fine grinding and high sample homogeneity. After the acquiring 3.0747 g of fertilizer, the sample was then placed inside the oven at 110 C and cooled before weighed. This procedure is essential before weighing the sample because the balance is calibrated to work at a specific temperature. Any change in air pressure or temperature may produce various weights. If the object transfers heat to the balance pan, the metal will expand and contract that will yield errors. Also, since the analytical balance is in use, the enclosures should function as it should be, which is to remove any variations in the air current. If the heat in the crucible transfer to the air inside the balance, the pressure inside the container will increase; thus pushing the balance pan and increasing the reading. Subsequently, the process of oven-drying and cooling in the desiccator is repeated until constant weight is achieved. For the third part of the experiment, the crucible undergone two cycles of oven drying and cooling because the initial weight of

the crucible with the fertilizer amounted to 45.0530 g and after 30 minutes of oven-drying, the resultant weight of the crucible with fertilizer lowered to 45.0511 g which yields to a difference of 0.0019 g. This value cannot be accepted since a reading can only be considered as a constant weight if the difference is between 0.0002-0.0003 g. This is because of the consideration for the homogeneity and quantitative measurement of the sample. By subtracting the constant weight of the crucible from the weight of the crucible with the fertilizer, the obtained weight of the mass fertilizerdry is 2.9013 g. Then, by subtracting the dry mass of the fertilizer from the wet mass, a value of 0.1734 g was obtained. This means that 0.1734 g of H20 is present in the fertilizer sample. By the equation 1 as shown below, the percent moisture that is present in the fertilizer sample equates to 5.64% of the total mass fertilizeras-received

In the next part of the experiment, the phosphorus of the fertilizer sample was precipitated as magnesium ammonium phosphate hexahydrate. Following the equation, 5 H2O(l) + HPO42-(aq) + NH4+(aq) + Mg2+(aq) + OH-(aq) MgNH4PO46H2O(s) NH3 is used as the precipitating reagent instead of NH4Cl because NH4Cl produces Cl- ions that may react with Mg2+ found in the solution which may form as MgCl2(s). The formation of this compound might cause an interference in the desired precipitate. The requirements for precipitation states that the precipitation must be complete and the final form of the substance must be known. Also, the precipitate should react only with the analyte, should be stable, and must be filterable. Moreover, the particle size of the precipitate should also be considered. Based on the experiment, the particle size is affected by experimental variables such as reactant concentrations in the precipitating solution, precipitate solubility, rate of addition and mixing of reactants, and temperature. This can be proven using the Von Weimarn equation which states that, (Equation 2)

(Equation 1)
% H 2O =

Weight Sample (Weight Sample with Crucible - Weight Crucible ) 100

Weight of Sample

Determining the amount of moisture present in fertilizer is essential because this represents the bulk sample; representing a part of a whole. Thus determining the moisture content of fertilizers benefit the customers, scientists, manufacturers and farmers for different reasons. First, there is a limit as to how much water should be present in certain types of fertilizer. Second, the grade of fertilizers depend on the amount of water they contain. And lastly, the quality of the fertilizer will be questioned if the moisture levels in the fertilizers exceed the manufacturers recommended levels. Other methods used in determining moisture content includes: convection and forced draft ovens, vacuum oven, microwave oven, and infrared lamp drying. In the next part of the experiment, a clear filtrate is obtained by filtering the incompletely dissolved sample. Then, 45 mL of 10% MgSO47H20 and 50 mL of 2M NH3 was added. The slow drop rate of the base is significant because it builds up the formation of the precipitate and the fast drop rate aids in making the formation proceed in the precipitate formation.

R=

(Q-S) S

Where Q is the concentration of the solute and S is the solubility equilibrium. This equation explains the slow drop rate of the NH3 so that the average Q is low thus yielding to a low supersaturation. Acquiring a low supersaturation will promote particle growth which will lead to larger precipitates.

After precipitation, the digestion step follows where the precipitate stands in the presence of the hot mother liquor. This treatment promotes slow recrystallization of the precipitate. The particle size increases and impurities tend to be expelled from the crystal. (Harris, p.633) Also, the precipitate was rinsed with 95% ethanol in order to remove all of the precipitate The mass of the precipitate was obtained by subtracting the preweighed filter paper from the

mass of the filter paper with the fertilizer sample yielding to 1.0506 g. This value is then used using the equation,

(Equation 3) III. Conclusion

FW Phosphorus Mass Phosphorus=Weight Precipitate FW Precipitate

to obtain the mass of the phosphorus present. Substituting to the equation above, the mass of phosphorus is 0.1326 g with a percent composition of 4.313 % following the equation below
(Equation 4)
Weight Precipitate %Phosphorus= FW Phosphorus FW MgSO4o7H20 100 Weight Wet Sample

The percentage amount of phosphorusdry resulted to 4.57% and the mass of P2O5 amounted to 0.3038 g in the fertilizer sample. Also the percent composition of the P2O5as-received and P2O5 dry yielded to 9.881% and 10.47% which was obtained using these equations respectively, (Equation 5)

In conclusion, the amount of phosphorus present in the fertilizer is 10.47% which can be compared to the standard amount of phosphorus present in most fertilizers. Also, the resulting percent composition of water is 5.64%. This explains that the fertilizer does not only contain the macronutrients needed by the plants but it also contains other component. This experiment is highly successful since the results obtained where not invalid and all values were taken into account. The fertilizer was handled carefully, except for the accidental touch applied to the crucible. Other than that, the experiment was a success, obtaining credible results for the amount of moisture content and phosphorus present in the fertilizer sample.

% P2O5 as-received =
(Equation 6)

Mass of P2O5 Weight of fertilizer sample

% P2 O5 dry =

Mass of P2O5 Weight of mass fertilizer

dry

These results explains the minimum amount of phosphorus present in the fertilizer which should be enough to support the growth of plants by stimulating root growth, seed germination, and more efficient use of water. Moreover this guarantees the quality of the macronutrient present in the fertilizer.

IV. References

Harris , D. (2010). Quantitative Chemical Analysis 8th edition. Harris, D. C. (2006). Quantitative Chemical Analysis 7th edition. West, D., Skoog, D., Holler, J., & Crouch, S. (2004). Fundamentals of Analytical Chemistry.

V. Appendices Day 1 Day2 a. Initial weight of crucible b. Constant weight of crucible c. Weight of fertilizer sample d. Net mass of fertilizer e. Filter paper Day 3 f. Initial weight of crucible with fertilizer g. Weight after 30 minutes h. Weight after 30 minutes i. Constant weight Day 4 j. Filter paper with sample

42.1517 g 42.1517 g 3.0747 g 3.0747 g 1.3250 g 45.0530 g 45.0511 g 45.0532 g 45.0530 g 2.3756 g

Calculations a. Mass Fertilizer as-received = 3.0747 g (Weigh by difference) b. Mass Fertilizer dry = 45.0530 g 42.1517 g = 2.9013 g Constant weight of crucible = 42.1517 g Constant weight of crucible with fertilizer = 45.0530 g

c. Mass H20 = 3.0747 2.90139 = 0.17349 g Wet mass = 3.0747g Dry mass = 2.9013g d. % moisture

WeightSample(WeightSampleWithCrucible WeightCrucible) 100 WeightOfSample 0.1734 g (WeightH 2O) % H 2O 100 5.64% 3.0747 g (WeightOfSampleWithH 2O) % H 2O
e. Mass Precipitate = 2.3756g 1.3250g = 1.0506 g Mass of filter paper = 1.3250g Mass of filter paper with sample = 2.3756g f. Mass Phosphorus

MassPhosphorus WeightOf Pr ecipitate

1.0506 g 30.97 g Phosphorus 0.1326 g 245.42 g

FWphosphorus FWprecipitate

g. % Phosphorus as-received
Weight Pr ecipitate % Phosphorus FWphosphorus FWMgNH 4 PO4 6 H 2O 100 WeightNetSample

1.0506 g

30.97 g Phosphorus 0.1326 g 245.42 g 100 4.313% 3.0747 g 3.0747 g

h. % Phosphorus dry

% Phosphorusdry =
i. Mass of P2O5

0.1326 g 100 4.57% 2.9013g

P2O5 =WeightPrecipitate
j. % P2O5 as-received =

FW P2O5 141.94 g P2O5 1.0506 2 FWMg 2(245.42 g ) 0.3038g

%P2 05as received

k. % P2O5 dry

0.30389 g 100 9.881% 3.0747 g

%P2 05dry

0.30389 g 100 10.47% 2.9013g

Answers to Questions: (Refer to results and discussion)