Procedures

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.)

Liquids and Solids

1. Weigh about 2 grams of a representative sample into a tared Erlenmeyer flask.
2. 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.
3. To make 2 M KCl, weigh 298.24 g KCl into a 2 L volumetric flask. Dilute to volume with deionized H20.
4. Report to 3 decimal places for liquids. Report 2 decimal places for solids.

Liquids 

1. 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.
2. Report to 3 decimal places.

Solids

1. Run nitrogen according to feeds procedure.
2. Calculation for ammonia determination and total nitrogen.
3. %NH₄-N or %Total N = 1.401 x N H₂SO₄ x (mL acid)/sample wt (g)

Liquids

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

Solids

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

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

1. Follow soil Cd reduction procedure for analyzing NO_3-N on solids. Dilute as necessary. Record results with no decimal places for solids.
2. Follow water Cd reduction procedure for analyzing NO_3-N on liquids. Dilute as necessary. Record results with two decimal places for liquids.

Standards

1. 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.
2. 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.
3. 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

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

Sample Preparation

1. Weigh exactly 1.0 g of sample and transfer quantitatively into a 250 mL conical beaker.
2. 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.
3. Remove from heat, cool and rinse condensate from watch glass back into beaker.
4. Also, rinse walls of beaker with minimal amount of deionized water.

Procedure

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

Calculations

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

Reference:

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

Reagents

1. Deionized water
2. ICP standard for phosphorus

Apparatus

1. Shaker
2. 250 mL Erlenmeyer Flasks with stoppers
3. Balance
4. Whatman No. 40 filter paper and filter funnels
5. Disposable pipets
6. ICP test tubes

Procedure

1. Determine dry matter of sample.
2. Weigh amount of fresh sample necessary to come up with the equivalent of 1.0 grams dry sample (use computer program to determine weight to use). Weigh into tared 250 mL Erlenmeyer flask. (Do samples in duplicate).
3. Bring weight to 100 g with water. Note: For liquid samples if dry matter < 0.5 %, the liquid can be filtered directly without adding more water.
4. Stopper and shake for 60 minutes.
5. Filter sample through No. 40 Whatman or equivalent filter paper into an ICP test tube.
6. Analyze filtrate for P on the ICP. Analyze samples same day as preparation.

Calculations

1. The ICP values will be on a dry weight basis. Exception: If DM < 0.5% and, therefore, if liquid sample is filtered directly, there is no dilution factor, therefore, the direct reading from the ICP is ppm on an as-samples "A" basis, so the ICP reading should be final value on report. To get that value, take (ICP reading) / ((100)(dry matter)). For example, if ICP value = 30 and DM = 0.23, report 30 /((100)(0.23)) = 1.3043.
2. For other samples, dilution is 1 to 100 (1.0 g dry weight to 100 g). Record with 2 decimals for liquids and 0 decimals for solids. Examples: If ICP value = 42.33 record 42 for solids and 42.33 for liquids.

Reference

1. Sharpley, Andrew and Barton Moyer, 2000. Phosphorus Forms in Manure and Compost and Their Release during Simulated Rainfall. J. Environ. Qual. 29:1462 - 1469.

Procedure

1. Use wet ash HNO3/H2O2 digest chemicals and apparatus.
2. Weigh 1 gram solid or liquid sample into digestion tube calibrated to 20 mL.
3. Add about 7 mL HNO3 and let sit overnight with funnel in top under hood.
4. Digest with HNO3 according to procedures.
5. Instead of adding the third aliquot of H2O2, remove sample from digestion block.
6. Add 10 mL 1:10 HNO3.
7. Let cool for 15 minutes.
8. Dilute with deionized water to the 20 mL mark.
9. Pour into ICP test tube for analysis.

ICP Information

1. Make 2 ppm standard from 1000 ppm stock (1:500).
2. Make 2 ppm (50:100) and 0.5 (25:100) ppm solutions from 2 ppm standard.
3. Set 2 ppm to 40, 1 ppm to 20, and 0.5 ppm to 10 on the ICP to account for the dilution factor.
4. As wavelength - 189.042.