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Diana Sadowski CH-234L Analytical Chemistry May 5, 2011

THE DETERMINATION OF NITROGEN IN SOIL

PURPOSE: The purpose of this lab is to determine and compare the amount of nitrogen in four samples of soil by using the Kjeldahl method for nitrogen determination. BACKGROUND: The Kjeldahl method for nitrogen determination was introduced by Johan Kjeldahl in 1883 at a meeting of the Danish Chemical Society. Originally used to determine the amount of nitrogen in malt, the Kjeldahl method has been modified and refined and now used for testing a wide variety of samples including but not limited to soil, animal and human food, and beverages. The Kjeldahl method is broken down into three steps; digestion, distillation, and titration. As stated in A Guide to Kjeldahl Nitrogen Determination digestion is, the decomposition of nitrogen in organic samples utilizing a concentrated acid solution. This is accomplished by boiling a homogeneous sample in concentrated sulfuric acid. The end result is an ammonium sulfate solution (Labconco).

Distillation as stated in in A Guide to Kjeldahl Nitrogen Determination is, adding excess base to the acid digestion mixture to convert NH4+ to NH3, followed by boiling and condensation of the NH3 gas in a receiving solution (Labconco).

Diana Sadowski CH-234L Analytical Chemistry May 5, 2011

THE DETERMINATION OF NITROGEN IN SOIL

Titration as stated in in A Guide to Kjeldahl Nitrogen Determination is, to quantify the amount of ammonia in the receiving solution. (Labconco).

The samples that I decided to analyze were soil samples. I took four different soil samples; one soil sample was Miracle-Grow, another sample was from my back yard in south central Wisconsin, the third was from out in a cow pasture at a farm in south central Wisconsin and the last sample was from the same farm from but out in their corn field. The reason I decided to do this experiment is because back home life is centered around soil. Soil is the basis of many peoples income, from the small time gardeners to the large farms. Nitrogen is essential to the growth of plants, which is the reason I decided to determine the amount of nitrogen in soil. Where I took the samples from was important. Potting soil has a controlled amount of nitrogen in it for optimal growing, the soil from my back yard is mainly sand which has limited amount of nitrogen. The last two samples were from a local farm one from out in the cow pasture, cows excrement puts a lot of nitrogen into the soil but sometimes can put way to much in. and the last sample was from the corn field. Corn is one of those plants that uptakes nitrogen and dont replace it back into the soil so it if the farmer doesnt rotate what they grow in that field every couple of years, it could lead to soil that doesnt have enough nitrogen in it anymore to grow what the farmer wants efficiently. I want to determine which type of soil has the highest concentration. My hypothesis is that the pasture soil will have the most, then potting soil after that corn field soil and finally lastly the sandy soil from the back yard.

Diana Sadowski CH-234L Analytical Chemistry May 5, 2011 Procedure: -

THE DETERMINATION OF NITROGEN IN SOIL

In a 500mL digestion flask weigh out one gram of soil as exactly as possible. Add 15 mL of concentrated (18M) sulfuric acid, 7 grams of potassium sulfate, and .04g of copper as a catalyst. Bring to a rolling boil using a sand bath, heat until a white fume can be seen in the flask then continue heating for 60 to 90 minutes. Cool flask Cautiously add 250mL of water to the flask. Set up a distillation apparatus.

Add 45% NaOH 20mL for every 5mL of sulfuric acid (60mL for one sample). Raise temperature to boiling and trap distilled vapors in a solution of 15 mL of 2M HCL mixed with 70mL of water. Titrate with .1 M standardized NaOH.

Observations: When boiled for an hour the mixture of sulfuric acid, soil, copper and potassium sulfate turned from a dark brown to a luminescent green to a pure white color. When adding NaOH the solution turned a blue color During the digestion process of the potting soil some of the soil splattered on the side of the flask. Also the potting soil did not change color as the other did. During the distillation process, the tube draining the water out of the condenser popped off the condenser resulting in the cold water running through the condenser to splash into the hot sand bath which resulted in a explosion of sand all throughout the vent hood. Luckily everything was sealed off or covered so the results shouldnt be affected by the incident. Just a lot of cleaning up was needed.

Diana Sadowski CH-234L Analytical Chemistry May 5, 2011 Data: Standardizing NaOH Titration initial final total Corn Field (1.0001g) Titration initial final total

THE DETERMINATION OF NITROGEN IN SOIL

grams KHP 1 0.01 28.69 28.68 2 1 28.6 27.6 3 0.29 28.65 28.36 Pasture (1.0000g) Titration initial final total

1 0.4997

2 0.4999

3 0.5003

1 0.11 57.5 57.39

2 0 57.1 57.1

3 0.15 56.9 56.75

1 0.02 47.59 47.57

2 0.02 46.99 46.97

3 0 47 47

Backyard (1.0000g) Titration initial final total

1 0.01 93.9 93.89

2 0.49 93.57 93.08

3 0 93.56 93.56

Potting Soil (1.0000g) Titration initial final total

1 0.01 91.59 91.58

2 0.01 89.9 89.89

3 0 90.95 90.95

Calculations:

Diana Sadowski CH-234L Analytical Chemistry May 5, 2011 Standardized NaOH molarity: moles KHP moles NaOH M NaOH

THE DETERMINATION OF NITROGEN IN SOIL

0.002446751 0.002448

0.00245

0.002446751 0.002448 0.00245 0.085312106 0.088686 0.086378

average M

0.086792

Concentration of Nitrogen: (.086792 moles NaOH/1L NaOH) X ( 1 mole NH4/1 mole NaOH) = mole NH4

Mole NH4/L titrated= M NH4

M of NH4 corn M of NH4 pature M of NH4 backyard M of NH4 potting soil

1.512319 1.52 1.529374 1.824511 1.847818 1.846638 0.924401 0.932445 0.927661 0.947718 0.965536 0.954283

average M average M average M average M

1.520564556 1.839655767 0.928169166 0.955845357

What this means: The soil that had the highest concentration of nitrogen was the pasture soil with an average of 1.840 M. The second highest concentration was the corn field soil with an average of 1.521 M, the next concentration was the potting soil with an average of 0.956 and the lowest concentration was the backyard with 0.928M. I was correct with the hypothesis about the highest and the lowest soil concentrations. But I was surprised that the soil in the corn field had a higher concentration than the potting soil.

Labconco. (N/A). A guide to Kjeldahl nitrogen determination. Retrieved on May 5, 2011 from http://www.expotechusa.com/catalogs/labconco/pdf/KJELDAHLguide.PDF

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