For general methods, see the publication " Recommended Methods of Manure Analysis A3769 ".

Agricultural Service Laboratory
Animal Waste Procedures (listed below)

September 14, 2006

TABLE OF CONTENTS

Sample Preparation
Ammonium Nitrogen
Total Nitrogen
Mineral Analysis
pH
Nitrate Nitrogen
Calcium Carbonate Equivalency
Soluble Phosphorus
Arsenic

Sample Preparation

1. All solid waste samples must be submitted to the lab in the lab sample bags

2.  Bottles are available for lagoon samples.

3. Laboratory numbers are assigned to the sample submission form and the data sheet.
The lab numbers are written on the sample bags and bottles with a sharpie. The first
digit of the lab number is 3. The next two digits are the month. The last four digits
are the sample number for the year.

4. Since animal waste has an odor and is a bio-safety hazard it must be handled
either in a bio-safety cabinet or under a hood. Special training is required for the
handling of animal waste samples.

5. For solid waste samples, check analyses desired on data sheet.  Record tare weight
of paper bag.  Add 100 - 200 g sample, weigh, and record wet weight.  Place in the oven
to dry at 80oC overnight. Place remainder of sample in the refrigerator for ammonium-
nitrogen.  Record dry weight in morning. Grind for other analyses.

6. For lagoon samples, record tare weight of 150 mL beaker. Mix sample in container
then pour appropriate amount into the beaker and record wet weight. Dry in oven at
80oC. Record dry weight. Place fresh unused portion of lagoon sample into refrigerator
for analyses. Check analyses desired on data sheet. An "A" must be written on the form
next to the lab number since the sample is analyzed "as-is". (The "A" must be entered
in DEMENU.)

Analyses

Ammonium-Nitrogen determination - liquids and solids (report to 3 decimal places for
liquids. Report 2 decimal places for solids).

Weigh about 2 grams of a representative sample into a tared Erlenmeyer flask.
Record weight on flask to 2 decimal places. Add 20 mL 2 M KCl. Shake for
30 min. Filter sample into digestion tube. Transfer weight to tube. Enter weight
into distillation unit. Distill Sample. Titrate with H2SO4 solution using the boric
acid indicator.

To make 2 M KCl, weigh 298.24 g KCl into a 2 L volumetric flask. Dilute to
volume with deionized H20.

Ref: Delaware.

Total Nitrogen - Liquids (report to 3 decimal places)

Mix sample in container and place representative sample in tared Kjeldahl
digestion tube. Weigh 5 g of sample. Use 5.000 in the calculation on the control
unit. Follow procedure for nitrogen determination for feed samples.

Total Nitrogen - Solids

Run nitrogen according to feeds procedure.

Calculation for ammonia determination and total nitrogen.

Mineral Analysis - Liquids

Weigh 5 g into 100 mL digestion tube. From ICP printout move decimal 3
places to the left for P, K, Ca, Mg, and S. Move decimal 1 place to the left for
Zn, Cu, Mn, and Na. Record P, K, Ca, Mg, and S in % with 4
decimal places. Record Zn, Cu, Mn, and As in ppm with 2 decimal places. (If
As is not detectable record a 1 on the data sheet.)

Mineral Analysis - Solids

Ash according to wet ashing procedure. Record results according to feed procedure.
If As is required, see below.

pH

Scoop about 10 g of solid sample into paper cup. Add 20 mL deionized water. Let sample
stand for 30 minutes then read pH. Record results with one decimal place. For liquids,
measure pH directly.

NO3-N

Follow plant procedure for analyzing NO3-N on solids and also add 0.17 g Ag2SO4 to each sample to remove
chloride interference. Use paper cup. Record results with no decimal places for solids.
Follow water procedure for analyzing NO3-N on liquids.  Record results with two decimal places for liquids.

Calcium Carbonate Equivalency - (CCE)

Standards:

Potassium Biphthalate Solution (0.6476N): Prepare by dissolving 33.0648 g of pure,
dry KHP in about 450 mL of deionized water in a 500 mL volumetric flask. Dilute to
volume and mix well.

Standard NaOH solution (0.6476N): Prepare 2.5 L quantity by diluting 113 mL of 40%
NaOH w/w into 2387 mL deionized H2O. Standardize by titrating against KHP solution
prepared above. Pipet 50 mL of KHP solution into a 150 mL beaker, add a few drops of
phenolphthalein indicator and titrate the NaOH into the KHP solution to a permanent
light pink endpoint. If exactly 25.00 mL of NaOH is not titrated, adjust NaOH
solution and repeat. Protect from exposure to air by a soda-lime tube or other
suitable means.

Standard HCl solution (0.9714N): Dilute 200 mL conc. HCl into 2300 mL of deionized
water. Standardize against 0.6476N NaOH by dispensing 25 mL of HCl from a buret into
a 150 mL beaker. Add a few drops of phenolphthalein indicator and titrate HCl against
NaOH to a permanent light pink endpoint. If exactly 37.50 mL of NaOH are not titrated,
adjust HCl solution and repeat.

Reagents:

Phenolphthalein indicator: Dissolve 1.0 g phenolphthalein powder in 70 mL of ethanol,
add 30 mL of deionized water and mix well.

Sample Preparation:

Weigh exactly 1.0 g of sample and transfer quantitatively into a 250 mL conical beaker.
Add 25.00 mL of 0.9714N HCl, add about 50 mL of deionized water, cover with a watch
glass and bring to boiling on a hot plate for 5 minutes. Remove from heat, cool and
rinse condensate from watch glass back into beaker. Also, rinse walls of beaker with
minimal amount of deionized water.

Procedure:

Add a few drops of phenolphthalein indicator to sample and titrate with 0.6476N NaOH
with continuous stirring. Titrate to same light pink endpoint used to standardize
solutions. Record mL of NaOH titrated.

Calculations:

CaCO3 Equivalent = (75 - 2(mL NaOH titrated)) x 1.629

Reference:

Adapted from Method 955.01, 16th edition of the Official Methods of Analysis,
Association of Official Agricultural Chemists.

Soluble Phosphorus