[Federal Register: March 26, 2008 (Volume 73, Number 59)]
[Notices]
[Page 16029]
[DOCID:fr26mr08-88]

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DEPARTMENT OF HOMELAND SECURITY

Coast Guard

[Docket No. USCG-2008-0187]

National Maritime Security Advisory Committee; Meeting

AGENCY: Coast Guard, DHS.

ACTION: Notice of meeting.

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SUMMARY: The National Maritime Security Advisory Committee (NMSAC) will
meet in Portsmouth, VA to discuss various issues relating to national
maritime security. This meeting will be open to the public.

DATES: The Committee will meet on Wednesday, April 16, 2008 from 9 a.m.
to 4 p.m. This meeting may close early if all business is finished.
Written material and requests to make oral presentations should reach
the Coast Guard on or before April 1, 2008. Requests to have a copy of
your material distributed to each member of the committee should reach
the Coast Guard on or before April 1, 2008.

ADDRESSES: The Committee will meet at the Renaissance Portsmouth Hotel
and Waterfront Conference Center, Portsmouth Ballroom 4, 425
Water Street, Portsmouth, VA. Send written material and requests to
make oral presentations to Captain Mark O'Malley, Commandant (CG-544),
Executive Director of NMSAC, U.S. Coast Guard Headquarters, Room 5302,
2100 2nd Street, SW., Washington, DC 20593-0001. This notice may be
viewed in our online docket, USCG-2008-0187 at http://
www.regulations.gov.

FOR FURTHER INFORMATION CONTACT: Mr. Ryan Owens, Assistant to DFO of
NMSAC, telephone<PHONE_NUMBER>.

SUPPLEMENTARY INFORMATION: Notice of this meeting is given under the
Federal Advisory Committee Act, 5 U.S.C. App. (Pub. L. 92-463).

Agenda of Meeting

    The agenda for the April 16, 2008 Committee meeting is as follows:
    (1) Presentation and Discussion of the Future Policy Issues Task
Statement.
    (2) Presentation and Discussion of the Maritime Transportation
Security User Fee Study Task Statement.
    (3) Report on the Status of the TWIC Program.
    (4) Briefing and Discussion on the Port Security Grant Program.
    (5) Briefing and Discussion on the National Strategy for Small
Vessel Security.
    (6) Briefing and Discussion on the National Concept of Operations
for Maritime Domain Awareness (Tentative).
    (7) Briefing and Discussion of the Long Range Identification and
Tracking (LRIT) system.

Procedural

    This meeting is open to the public. Please note that the meeting
may close early if all business is finished. At the Chair's discretion,
members of the public may make oral presentations during the meeting.
If you would like to make an oral presentation at a meeting, please
notify the DFO no later than April 1, 2008. Written material for
distribution at a meeting should reach the Coast Guard no later than
April 1, 2008. If you would like a copy of your material distributed to
each member of the committee in advance of a meeting, please submit 25
copies to the DFO no later than April 1, 2008.

Information on Services for Individuals With Disabilities

    For information on facilities or services for individuals with
disabilities or to request special assistance at the meeting, contact
the DFO as soon as possible.

    Dated: March 13, 2008.
M.P. O'Malley,
Captain, U.S. Coast Guard, Chief, Office of Port and Facility
Activities, Designated Federal Official, NMSAC.
 [FR Doc. E8-6145 Filed 3-25-08; 8:45 am]

BILLING CODE 4910-15-P


[Federal Register Volume 80, Number 1 (Friday, January 2, 2015)]
[Notices]
[Pages 105-106]
[FR Doc No: 2014-30557]

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DEPARTMENT OF TRANSPORTATION

Pipeline and Hazardous Materials Safety Administration

Delayed Applications

AGENCY: Office of Hazardous Materials Safety, Pipeline and Hazardous
Materials Safety Administration (PHMSA), DOT.

ACTION: List of application delayed more than 180 days.

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SUMMARY: In accordance with the requirements of 49 U.S.C. 5117(c),
PHMSA is publishing the following list of special permit applications
that have been in process for 180 days or more. The reason(s) for delay
and the expected completion date for action on each application is
provided in association with each identified application.

FOR FURTHER INFORMATION CONTACT: Ryan Paquet, Director, Office of
Hazardous Materials Special Permits and Approvals, Pipeline and
Hazardous Materials Safety Administration, U.S. Department of
Transportation, East Building, PHH-30, 1200 New Jersey Avenue
Southeast, Washington, DC 20590-0001,<PHONE_NUMBER>

Key to ``Reason for Delay''

1. Awaiting additional information from applicant
2. Extensive public comment under review
3. Application is technically complex and is of significant impact or
precedent-setting and requires extensive analysis
4. Staff review delayed by other priority issues or volume of special
permit applications

Meaning of Application Number Suffixes

N--New application
M--Modification request
R--Renewal Request
P--Party To Exemption Request

     Issued in Washington, DC, on December 8, 2014.
Donald Burger,
Chief, General Approvals and Permits.

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                                                                                Reason for    Estimated date
            Application No.                             Applicant                      delay       of completion
----------------------------------------------------------------------------------------------------------------
                                         Modification to Special Permits
----------------------------------------------------------------------------------------------------------------
9847-M.................................  FIBA Technologies, Inc. (FIBA),                       4      12-31-2014
                                          Millbury, MA.
14617-M................................  Western International Gas & Cylinders,                4      01-31-2015
                                          Inc., Bellville, TX.
13359-M................................  BASF Corporation, Florham Park, NJ.....               4      01-31-2015
11903-M................................  Comptank Corporation Bothwell, ON......               4      01-31-2015
15832-M................................  Baker Petrolite Corporation (BPC),                    4      12-31-2014
                                          Sugar Land, TX.
----------------------------------------------------------------------------------------------------------------
                                         New Special Permit Applications
----------------------------------------------------------------------------------------------------------------
15767-N................................  Union Pacific Railroad Company,Omaha,                 1      12-31-2014
                                          NE.
16001-N................................  VELTEK, Malvern, PA....................               4      12-31-2014
16039-N................................  UTLX Manufacturing LLC, Alexandria, LA.               4      12-31-2014
16061-N................................  Battery Solutions, LLC, Howell, MI.....               4      12-31-2014
16137-N................................  Diversified Laboratory Repair,                        4      12-31-2014
                                          Gaithersburg, MD.
16118-N................................  Toyota Motor Sales, U.S.A., Inc.,                     4      01-31-2015
                                          Torrance, CA.
16155-N................................  B.J. Alan Company dba Phantom                         4      12-31-2014
                                          Fireworks, Canfield, OH.
16121-N................................  U.S. Department of Defense (DOD), Scott               4      01-31-2015
                                          AFB, IL.
16154-N................................  Patriot Fireworks, LLC, Ann Arbor, MI..               4      12-31-2014
16181-N................................  Arc Process, Inc., Pflugerville, TX....               4      01-31-2015

15991-N................................  Dockweiler, Neustadt-Glewe, Germany....               4      12-31-2014
----------------------------------------------------------------------------------------------------------------
                                      Renewal Special Permits Applications
----------------------------------------------------------------------------------------------------------------
11602-R................................  East Tennessee Iron & Metal, Inc.,                    4      12-31-2014
                                          Rogersville, TN.
11860-R................................  GATX Corporation, Chicago, IL..........               4      12-31-2014
15580-R................................  Wisconsin Central Ltd., Homewood, IL...               4      12-31-2014
15458-R................................  Southern States LLC, Hampton, GA.......               4      01-31-2015
----------------------------------------------------------------------------------------------------------------

[FR Doc. 2014-30557 Filed 12-31-14; 8:45 am]
BILLING CODE 4910-60-M


EVALUATION OF VALUATION TREATMENT OF REATMENT BULK ULK ELEMENTAL LEMENTAL MERCURY ERCURY D 1 APPENDIX D. ANALYTICAL PROTOCOLS, TECHNICAL BACKGROUND DOCUMENT: MERCURY WASTES, EVALUATION OF TREATMENT OF BULK ELEMENTAL MERCURY, FINAL REPORT FEBRUARY 8, 2002 SUBMITTED FOR: U. S. ENVIRONMENTAL PROTECTION AGENCY ARIEL RIOS BUILDING OFFICE OF SOLID WASTE 1200 PENNSYLVANIA AVENUE, N. W. WASHINGTON, D. C. 20460 SUBMITTED BY: SCIENCE APPLICATIONS INTERNATIONAL CORPORATION ENGINEERING AND ENVIRONMENTAL MANAGEMENT CORP. 11251 ROGER BACON DRIVE RESTON, VIRGINIA 20190 EPA CONTRACT NO. 68 W 98 025 WORK ASSIGNMENT NO. 3 8 SAIC PROJECT NO. 06 0758 08 1373 000 ANALYTICAL NALYTICAL PROTOCOLS ROTOCOLS D 2 APPENDIX D. ANALYTICAL PROTOCOLS SOP Titles Procedure for the Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium and Potassium in SoilD 3 Undisturbed Bulk Density Analytical ProcedureD 10 Determining the Cation Exchange Capacity ( CEC) of SoilD 12 pH Analytical ProcedureD 14 Determining the Acidity of SoilD 17 Hydraulic Conductivity   Constant Head MethodD 20 Texture Procedure   Pipette MethodD 23 Redox Potential of a Soil SampleD 28 Cation Exchange Capacity by Sodium Saturation in Calcareous SoilsD 31 Determination of Total Organic Carbon in Soil by CombustionD 35 1/ 3 Bar   German MethodD 38 ChloridesD 39 EVALUATION OF VALUATION TREATMENT OF REATMENT BULK ULK ELEMENTAL LEMENTAL MERCURY ERCURY D 3 This page intentionally left blank. D 4 AGVISE Laboratories, Inc. NORTHWOOD, ND STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.12.13 SOP TITLE: Procedure for the Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium and Potassium in Soil REVISED BY: Larry Wikoff TITLE: Nutrient Laboratory Manager REPLACES SOP NUMBER: NUT. 02.12.12 REASON FOR REVISION: Add use of ICP to method.

APPROVALS:

Larry Wikoff Date Julie M. Johnson Date Nutrient Laboratory Manager Quality Assurance Manager Robert Deutsch Date Robert Wallace Date President CEO Effective Date PURPOSE: To define the analytical method used to determine soil cation exchange capacity. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.12.13 SOP TITLE: Procedure for the Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium and Potassium in Soil D 5 PROCEDURE: 1. To extract the samples, use a 1.0 gm soil scoop to transfer the sample to 50 ml Erlenmeyer flasks in Potassium extraction tray, according to SOP NUT. 06.02   " Soil Scoop Procedure." Scoop a check sample after the last sample in each tray.

2. Use an appropriate dispenser or a dispenser pump to add 10.0 ml of Potassium Extracting Solution to each sample. For each batch of samples, check one aliquot with a graduated cylinder to determine the actual volume dispensed and record the volume on the raw data lab sheet. This volume is to be at 10.0 ml or reject and recalibrate and check volume again.

3. Shake for 5 minutes at 200 ( ± 10%) epm on a mechanical shaker.

4. Filter through sodium free 9 cm filter paper into an ICP filtering tray or into plastic cups in Potassium filter trays, labeled the same as the extracting tray.

5. Remove the filter papers and read the extract on the ICP according to SOP NUT. 01.25   " Optima 3000 & 3100 Operating, Calibration and Maintenance Procedure" and SOP NUT. 02.93   " Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium, and Potassium for Cation Exchange Capacity using ICP". Record the results on the raw data lab sheet or capture electronically. For all samples: Read the standards after every tray. If the read standard is more than ± 10% of the known standard, the run must be retested Record the standard readings on the raw data lab sheet. The check sample must fall within the limits set in SOP NUT. 04.03   " The Use and Ranges of Check Soil".

6. Samples may also be analyzed using the Atomic Absorption Spectrophotometer. Use Steps 6 through 10 when using the Atomic Absorption Spectrophotometers. Read the extracts for Potassium and Sodium on the Atomic Absorption Spectrophotometer, according to SOP NUT. 01.21   " Atomic Absorption Spectrophotometer Operating Procedure   Buck Scientific Models" & NUT. 01.23   " Atomic Absorption Spectrophotometer Operating Procedure   Perkin Elmer 100".

7. For Calcium and Magnesium: A) To prepare samples, use either step a), b), or c). a) Use a 1000 µ l auto pipet to take a 1.00 ml aliquot of each sample, transferring them to cups in a CEC tray, numbered the same as the Potassium tray. Use a pipet or dispenser to add 1.00 ml of 2% Lanthanum Chloride Solution. Use a dispenser to add 8.00 ml of deionized water. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.12.13 SOP TITLE: Procedure for the Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium and Potassium in Soil D 6 b) Use the Hamilton Microlab Dilutor to dispense 1000 µ l of sample and 9000 µ l of the 1: 9 Dilution of 2% Lanthanum Chloride Solution. c) Use a 1000 µ l auto pipet to take a 1.00 ml aliquot of each sample, transferring them to cups in a CEC tray, numbered the same as the Potassium tray. Use a dispenser to add 9.00 ml of the 1: 9 Dilution of 2% Lanthanum Chloride Solution.

B) Read on the Atomic Absorption Spectrophotometer, according to SOP NUT. 01.21   " Atomic Absorption Spectrophotometer Operating Procedure   Buck Scientific Models" & NUT. 01.23   " Atomic Absorption Spectrophotometer Operating Procedure   Perkin Elmer 100".

C) Record the results on the raw data lab sheet or capture electronically. a) If the samples are low in calcium and/ or magnesium and levels can not be detected, the following procedure may be used: 1) Use a 1 gm soil scoop and transfer soil two times for a total of 2 gm of soil to an Erlenmeyer flask in a potassium extraction tray. Use an appropriate dispenser and add 20 ml of Potassium Extracting Solution to each sample. Shake for 5 minutes on a mechanical shaker. Filter through 11 cm filter paper into plastic cups. This extracting method is needed in order to have at least 10 ml of extract. 2) Use a pipet to transfer 9 ml of each sample to a plastic cup. Use a pipet or dispenser to add 1.0 ml of 2% Lanthanum Chloride to each sample. 3) Read on the AA and calculate by: Sample ( ppm) = AA Reading/ 9 Record the calculated reading on the raw data lab sheet.

D) Check all pipets and dispensers with a graduated cylinder to determine actual volume dispensed and record the volume on the raw data lab sheet. This should be at exact volumes, dispensed or reject and calibrate pipets and check volumes again.

8. For all samples: Read the standards after every tray. If the read standard is more than ± 10% of the known standard, the run must be re tested. Record the standard readings on the raw data lab sheet.

9. If the sample exceeds the highest standard by more than 10%, an appropriate dilution is made. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.12.13 SOP TITLE: Procedure for the Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium and Potassium in Soil D 7 10. The check sample must fall within the limits set in SOP NUT. 04.03   " The Use and Ranges of Check Soil". If the check soil does not fall within these limits, the lab manager or technician III may approve the check soil( s) or may have the samples re tested.

REAGENTS: · POTASSIUM EXTRACTING SOLUTION ( 1N Ammonium Acetate): 10 L 50 L Ammonium Hydroxide 690 ml 3450 ml Acetic Acid 600 ml 3000 ml 1. Rinse out the carboy with deionized water then fill about 3/ 4 full. 2. IN ( OR IN FRONT OF) THE FUME HOOD use a graduated cylinder to add the Ammonium Hydroxide. Rinse the cylinder with Deionized Water into the carboy. 3. Use the graduated cylinder to add the Acetic Acid. Rinse the cylinder with Deionized Water into the carboy.

DANGER: Ammonium Hydroxide and Acetic Acid both are corrosive and produce corrosive fumes. Use gloves and face protection when handling. Work in ( or in front of) the fume hood to avoid inhaling the fumes.

4. Mix the solution by shaking with the lid on, with an electric mixer, or a magnetic stir plate and bar. 5. Fill the carboy to volume with deionized water and mix again. 6. Check the pH and adjust to 8.5. If the pH is over 8.5, add Acetic Acid. If under 8.5, add Ammonium Hydroxide.

( 1.0 N Ammonium Acetate Concentrate): 1. Add 400 ml of concentrate to a 2000 ml volumetric flask. 2. Dilute to volume. Mix the solution thoroughly. 3. Adjust the pH of this solution to 8.5. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.12.13 SOP TITLE: Procedure for the Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium and Potassium in Soil D 8 · 2% LANTHANUM CHLORIDE SOLUTION: 2000 ml Lanthanum Oxide 47.00 g Cesium Chloride 12.60 g Hydrochloric Acid 72.0 ml 1. Weigh the Lanthanum Oxide and transfer it to a flask. 2. Weigh the Cesium Chloride and add it to the flask. 3. Fill about 2/ 3 full with Deionized Water and swirl to mix. 4. Use a graduated cylinder to measure the Hydrochloric Acid and add it to the flask. 5. Swirl until dissolved. 6. Bring to volume with deionized water and mix thoroughly.

· 1: 9 DILUTION OF 2 % LANTHANUM CHLORIDE SOLUTION: Dilute 250 ml of 2 % Lanthanum Chloride solution to 2000 ml with deionized water in a volumetric flask.

STANDARDS: FOR THE ICP: · ICP High CEC Std.   ( Calcium 1500 ppm, Magnesium 300 ppm, Sodium 40 ppm, and Potassium 72 ppm in solution) ( Calcium 15,000 ppm, Magnesium 3000 ppm, Sodium 400 ppm, and Potassium 720 ppm in soil) 1. 80 mls of 1000 ppm Sodium Standard. 2. 144 mls of 1000 ppm Potassium Standard. 3. 7.492gms of oven dried Calcium Carbonate. 4. 0.995 gms of oven dried Magnesium Oxide. 5. 20 mls of concentrated Hydrochloric Acid. 6. Dilute to 2000 mls with Potassium Extraction Solution.

· ICP Medium CEC Std.   ( Calcium 1000 ppm, Magnesium 200 ppm, Sodium 20 ppm, and Potassium 36 ppm in solution) ( Calcium 10,000 ppm, Magnesium 2000 ppm, Sodium 200 ppm, and Potassium 360 ppm in soil) 1. 40 mls of 1000 ppm Sodium Standard. 2. 72 mls of 1000 ppm Potassium Standard. 3. 4.995gms of oven dried Calcium Carbonate. 4. 0.663 gms of oven dried Magnesium Oxide. 5. 20 mls of concentrated Hydrochloric Acid. 6. Dilute to 2000 mls with Potassium Extraction Solution. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.12.13 SOP TITLE: Procedure for the Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium and Potassium in Soil D 9 · ICP Low CEC Std.   ( Calcium 500 ppm, Magnesium 100 ppm, Sodium 10 ppm, and Potassium 16 ppm in solution) ( Calcium 5000 ppm, Magnesium 1000 ppm, Sodium 100 ppm, and Potassium 160 ppm in soil) 1. 20 mls of 1000 ppm Sodium Standard. 2. 32 mls of 1000 ppm Potassium Standard. 3. 2.497gms of oven dried Calcium Carbonate. 4. 0.332 gms of oven dried Magnesium Oxide. 5. 20 mls of concentrated Hydrochloric Acid. 6. Dilute to 2000 mls with Potassium Extraction Solution.

FOR THE ATOMIC ABSORPTION SPECTROPHOTOMETER: · Potassium and Sodium: 1. Pipet 1000 ppm Potassium and Sodium Standards into 500 ml volumetric flasks, according to the chart below. 2. Dilute to volume with Potassium Extracting Solution, and mix thoroughly.

STANDARD # 1 STANDARD # 2 ml ppm ppm in soil ml ppm ppm in soil Potassium 8 16 160 18 36 360 Sodium 5 10 100 10 20 200 STANDARD # 3 ml ppm ppm in soil Potassium 36 72 720 Sodium 20 40 400 · Calcium and Magnesium: 1. Pipet 1000 ppm Calcium and Magnesium Standards into 500 ml volumetric flasks, according to the chart below. 2. Add 50 ml Lanthanum Chloride Solution. 3. Add 50 ml Extracting Solution. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.12.13 SOP TITLE: Procedure for the Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium and Potassium in Soil D 10 4. Dilute to volume with Deionized Water and mix thoroughly.

STANDARD # 1 STANDARD # 2 ml ppm ppm in soil ml ppm ppm in soil Calcium 25 50 50 50 100 100 Magnesium 5 10 100 10 20 200 STANDARD # 3 ml ppm ppm in soil Calcium 75 150 150 Magnesium 15 30 300 REFERENCES: Brown, J. R., and Darryl Warncke. 1988. Recommended Cation Tests and Measures of Cation Exchange Capacity. In W. C. Dahnke, ( ed.). Recommended Chemical Soil Test Procedures for the North Central Region. North Central Region Publication No. 221 ( Revised). North Dakota Agricultural Experiment Station Bulletin 499 ( Revised). D 11 AGVISE Laboratories, Inc. NORTHWOOD, ND STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.02.05 SOP TITLE: Undisturbed Bulk Density Analytical Procedure REVISED BY: Lucinda S. Moen TITLE: Laboratory Technician III REPLACES SOP NUMBER: NUT. 02.02.04 REASON FOR REVISION: Update Cover Page.

APPROVALS:

Robert Deutsch Date Julie M. Johnson Date President/ Nutrient Laboratory Manager Quality Assurance Manager Robert Wallace Date CEO Effective Date STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.02.05 SOP TITLE: Undisturbed Bulk Density Analytical Procedure D 12 PURPOSE: To define the analytical method for determining the bulk density of undisturbed soil samples received in sampling tubes.

PROCEDURE: 1. Determine the diameter of the soil tube. Use the inside diameter of the soil probe used to take the sample if it is known. Otherwise use a ruler or caliper to measure the inside diameter of the soil tube itself. Record the value to the nearest 0.1cm.

2. Measure the length of the soil core and record the total length to the nearest 0.1cm. If multiple cores represent the sample, sum the lengths of the individual cores that make up the sample.

3. Calibrate the balance following SOP NUT. 01.01   " Use and Maintenance of Laboratory Balances."

4. Weigh a tray ( or several trays) suitable to hold all the soil from the core, and record the weight( s) to at least the nearest 0.1g.

5. Place all the soil on the tray( s) and dry in restricted access soil dryer at 105 ± 5 ° C for at least 12 hours.

6. Weigh the tray( s) containing the dry soil and record the weight( s) to at least the nearest 0.1g.

7. Calculate the bulk density:

Bulk Density = Dry Soil Weight Pi * ( Core Radius) 2 * ( Core Length)

REFERENCE: Blake, G. R. 1965. Bulk Density. In Methods of Soil Analysis, Part 1. American Society of Agronomy. Madison, WI. D 13 AGVISE Laboratories, Inc. NORTHWOOD, ND STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.03.03 SOP TITLE: Determining the Cation Exchange Capacity ( CEC) of Soil REVISED BY: Julie M. Johnson TITLE: Quality Assurance Manager REPLACES SOP NUMBER: NUT. 02.03.02 REASON FOR REVISION: Update Cover Page and Minor Revisions.

APPROVALS:

Robert Deutsch Date Julie M. Johnson Date President/ Nutrient Laboratory Manager Quality Assurance Manager Robert Wallace Date CEO Effective Date STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.02.03 SOP TITLE: Determining the Cation Exchange Capacity ( CEC) of Soil D 14 PURPOSE: Determining the Cation Exchange Capacity ( CEC) of a soil sample.

PROCEDURE: 1. Determine the calcium, magnesium, sodium and potassium of the soil sample by following the procedures described in SOP NUT. 02.12   " Procedures for the Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium and Potassium in Soil".

2. Determine the acidity of the soil sample by following the procedures described in SOP NUT. 02.11   " Determining the Acidity of Soil".

3. Calculate the CEC using one of the following methods:

Method 1: lbs per acre Ca / 400 = Meq per 100 gm Ca lbs per acre Mg / 240 = Meq per 100 gm Mg lbs per acre K / 780 = Meq per 100 gm K lbs per acre Na / 460 = Meq per 100 gm Na 8 × ( 8.00   buffer pH) = Meq per 100 gm H CEC = sum of the Meq per 100 gm ( Ca + Mg + K + Na + H)

Method 2: ppm Ca / 200 = Meq per 100 gm Ca ppm Mg / 120 = Meq per 100 gm Mg ppm K / 390 = Meq per 100 gm K ppm Na / 230 = Meq per 100 gm Na 8 × ( 8.00   buffer pH) = Meq per 100 gm H CEC = sum of the Meq per 100 gm ( Ca + Mg + K + Na + H) D 15 AGVISE Laboratories, Inc. NORTHWOOD, ND STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.05.08 SOP TITLE: pH Analytical Procedure REVISED BY: Linda M. Anderson TITLE: Laboratory Technician III REPLACES SOP NUMBER: NUT. 02.05.07 REASON FOR REVISION: Update Title Page and Minor Revisions.

APPROVALS:

Robert Deutsch Date Julie M. Johnson Date President/ Nutrient Laboratory Manager Quality Assurance Manager Robert Wallace Date CEO Effective Date STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.05.08 SOP TITLE: pH Analytical Procedure D 16 PURPOSE: To define the analytical method used to determine soil pH.

EQUIPMENT: ° pH Meter ° Soil Scoop PROCEDURE: 1. Set up pH/ Salt trays, putting small plastic cups in each space.

2. Mark each cup with its appropriate sample number.

3. Using a 5 gm soil scoop, scoop the soil samples into the cups, according to SOP NUT. 06.02   " Soil Scoop Procedure." Scoop at least one check sample per 10 samples.

4. Use a dispenser to add 5 ml of deionized water to each sample. For each batch of samples, check one aliquots of water with a graduated cylinder to determine the actual volume dispensed, and record the volume on the raw data lab sheet.

5. Stir the samples, and then wait 10 minutes before reading them.

6. Calibrate the pH meter before reading each batch: a. Use the appropriate instruction manual for the pH meter being used and follow the instructions for calibrating the meter. b. Use pH buffers 4.00, 7.00 and 10.00 to calibrate the pH meter. c. Enter the buffers at the end of the run on the raw data lab sheet to see if the meter held the calibration. Acceptable Ranges are as follows:

4.00 7.00 10.00 Min 3.94 6.94 9.94 Max 4.06 7.06 10.06 7. Fill an adequately large enough beaker with deionized water for rinsing the electrode. Put clean water in the beaker for each run.

8. RINSE THE ELECTRODE IN THE DEIONIZED WATER BEAKER BEFORE EACH SAMPLE. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.05.08 SOP TITLE: pH Analytical Procedure D 17 9. Read each sample by stirring it with the electrode until a fairly steady reading is obtained. THE READING SHOULD BE TAKEN WHILE THE SAMPLE IS BEING STIRRED.

10. Record the reading for each sample on the raw data lab sheet.

11. Turn off the pH meter after all the samples are read and store the electrodes in pH 7 or pH 4 buffer.

REAGENTS: pH ELECTRODE FILLING SOLUTION ( 4M KCl): 500 ml Potassium Chloride 150 g 1. Weigh the Potassium Chloride into a beaker. 2. Add about 400 ml deionized water and stir on a magnetic stirrer until dissolved. Warm slightly if necessary. 3. Dilute to volume with deionized water and stir until mixed.

REFERENCES: Ecken, D. J. 1988. Recommended pH and Lime Requirement Tests. W. C. Dahnke, ( ed.). Recommended Chemical Soil Test Procedures for the North Central Region. North Central Region Publication No. 221 ( Revised). North Dakota Agricultural Experiment Station Bulletin 499 ( Revised).

Peck, T. R. 1988. Standard Soil Scoop. W. C. Dahnke, ( ed.). Recommended Chemical Soil Test Procedures for the North Central Region. North Central Region Publication No. 221 ( Revised). North Dakota Agricultural Experiment Station Bulletin 499 ( Revised). D 18 AGVISE Laboratories, Inc. NORTHWOOD, ND STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.11.09 SOP TITLE: Determining the Acidity of Soil REVISED BY: Linda Anderson TITLE: Laboratory Technician III REPLACES SOP NUMBER: NUT. 02.11.08 REASON FOR REVISION: Update Cover Page and Method APPROVALS:

Julie Johnson Date Mary Thingelstad Date Nutrient Laboratory Manager Quality Assurance Manager Robert Deutsch Date Robert Wallace Date President CEO Effective Date STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.11.09 SOP TITLE: Determining the Acidity of Soil D 19 PURPOSE: To determine the acidity of a soil sample for use in calculating the CEC of the soil.

SCOPE: Using the Adam Evans method to determine the Acidity of a soil sample. Ref.: Soil Testing and Plant Analysis Laboratory Manual, 1989, J. Benton Jones, Jr.

EQUIPMENT REQUIRED: 1. pH meter BUFFER SOLUTION: 1. Using a one Liter flask with a magnetic stirrer, dissolve 74 g of potassium chloride in approximately 500 ml of water.

2. Add 10.5 g of potassium hydroxide, stir and dissolve.

3. Add 20 g of p nitrophenol, stir and dissolve.

4. Add 15 g of boric acid.

5. Dilute to 1 L with water and stir. You may need to heat to dissolve.

METHOD: 1. To the 5 grams of soil and 5 ml of deionized water used for pH of soil ( Refer to SOP NUT. 02.05   pH Analytical Procedure), add 5 ml of Adams Evans buffer. Scoop a check sample after the last sample in each tray. Check the dispenser with a graduated cylinder and record this amount on the raw data lab sheet.

2. Shake or stir for 10 minutes.

3. Let stand for 30 minutes.

4. Prepare a standard by mixing 5 ml of deionized water with 5 ml of Adams Evans buffer solution. Use this solution to calibrate the pH meter to 8.00. The Acceptable Range is as follows: Min   7.92 Max   8.08 5. Read samples and record pH to nearest 0.01 on the raw data lab sheet for Acidity. This reading is the buffer pH. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.11.09 SOP TITLE: Determining the Acidity of Soil D 20 CALCULATIONS: meq acidity ( H+) / 100 g = 8 × ( 8.00 buffer pH) D 21 AGVISE Laboratories, Inc. NORTHWOOD, ND STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.34.03 SOP TITLE: Hydraulic Conductivity   Constant Head Method REVISED BY: Garis Pollert TITLE: Nutrient Laboratory Analyst REPLACES SOP NUMBER: NUT. 02.34.02 REASON FOR REVISION: Update Cover Page, Procedures and Minor Revisions APPROVALS:

Robert Deutsch Date Julie M. Johnson Date President/ Nutrient Laboratory Manager Quality Assurance Manager Robert Wallace Date CEO Effective Date STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.34.03 SOP TITLE: Hydraulic Conductivity   Constant Head Method D 22 PURPOSE: To define the analytical method for determining the hydraulic conductivity of a saturated soil.

EQUIPMENT: ° Constant Head Hydraulic Conductivity Apparatus ( See Figure 1). ° Container to hold water.

PROCEDURE: 1. Set up an apparatus similar to Figure 1.

2. Scoop each sample into a plastic cylinder that has a cover of cloth on one end. Cover the cloth end with a cover or cap and tap on the counter 10 times to settle the disturbed sample, remove cover. If the sample arrives in an acetate or metal tube, the hydraulic conductivity is performed on the sample undisturbed. Cut the tubes into appropriate lengths using a saw. Place a cylinder extension on top of the soil tube and seal. Make sure that the seal is watertight. Place a cloth on the bottom of the soil tube.

3. Place samples, cloth covered end, down into water. Allow the samples to soak at least 16 hours until they are saturated.

4. Turn on the water supply for the upper trough.

5. Transfer the samples to the rack and start the siphons to maintain a constant head of water on each of the samples.

6. After the water level on top of a sample becomes stabilized, collect the percolate in a suitable container for a known amount of time.

7. Record the time and the amount of water in the container. Measure and record the hydraulic head difference ( DH). Record the temperature of the water. Measure the length of the soil column and the diameter of the cylinder used.

CALCULATIONS: Hydraulic conductivity = ( Q/ A* t) × ( L/ D H) Q = Water that passes through the sample at a known time t = Known time A = Cross sectional area of the sample L = Length of the sample D = Hydraulic head difference across sample ( See Figure 1) * Figure 1: STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.34.03 SOP TITLE: Hydraulic Conductivity   Constant Head Method D 23 * Drawing taken from reference listed below REFERENCES:

Black, C. A. ( ed). 1965. Methods of Soil Analysis, Part 1, American Society of Agronomy, Inc., Madison, Wisconsin. D 24 AGVISE Laboratories, Inc. NORTHWOOD, ND STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.56.04 SOP TITLE: Texture Procedure   Pipette Method REVISED BY: Garis Pollert TITLE: Laboratory Nutrient Analyst REPLACES SOP NUMBER: NUT. 02.56.03 REASON FOR REVISION: Update Cover Page, Clarify Procedure Order & Minor Revisions APPROVALS:

Robert Deutsch Date Julie M. Johnson Date President/ Nutrient Laboratory Manager Quality Assurance Manager Robert Wallace Date CEO Effective Date STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.56.04 SOP TITLE: Texture Procedure   Pipette Method D 25 PURPOSE: To define the analytical procedure used to determine soil texture (% sand, silt, and clay) using a pipette method.

EQUIPMENT: ° Pipettes ° Thermometer ° Stop watch or clock with second's hand ° Balance ° Shaker REAGENTS: ° 10% Sodium hexametaphosphate Solution: Dissolve 100 GM of sodium hexametaphosphate in 1 L H 2 0.

Determine a correction factor by pipetting or dispensing 10 ml of the solution into a preweighed container. Place the container in an oven at 105 ± 5oC until dry. Weigh the container on a balance to at least three decimal places. Calculate the correction factor and write it on the container.

( Container + Residue   Container Empty) Blank Factor = ( 20 )

° 30% Hydrogen Peroxide ( H 2 O 2) ° Acetic Acid PROCEDURE: 1. Weigh out approximately 10 g of soil. Record the weight on the raw data lab sheet. Weigh in or transfer to a container, such as a fleaker, that has been weighed to at least three decimal places. Follow SOP NUT. 01.01   " Use and Maintenance of Laboratory Balances" to calibrate the balance.

2. If the % Organic Matter is 1.0 %, Step 2 and 3 are not necessary, skip to step 4. To the samples that are > 1.0%, add 10 ml of deionized water, 10 ml of 30% Hydrogen Peroxide, and 1 drop of Acetic Acid. Swirl the mixture; cover with a watch glass and heat at approximately 60 ° C. When the temperature is reached, add Hydrogen Peroxide in 5 ml increments approximately every 15 minutes until the organic matter is oxidized. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.56.04 SOP TITLE: Texture Procedure   Pipette Method D 26 3. After the organic matter is removed, the containers are oven dried at 105 ± 5 ° C, and then weighed to at least three decimal places.

4. Add 10 ml of the 10% Sodium Hexametaphosphate to each container and bring the volume up to approximately 150 ml with deionized water.

5. Cap and shake the containers on a horizontal shaker overnight ( 12 hours minimum).

6. Add 10 ml of the 10% Sodium Hexametaphosphate solution to a container and bring the volume up to approximately 150 ml. This sample is referred to as a BLANK.

7. The stoppers are then removed and the volume of each container is brought up to 400 ml with deionized water.

8. The temperature of the BLANK is taken and recorded on the raw data lab sheet.

9. Cap the container and shake vigorously for 10 seconds to ensure that no soil adheres to the bottom of the container.

10. Shake the container vigorously for 15 seconds, end over end. Note the time and allow the container to stand for the desired settling time based on the temperature of the BLANK ( See Table 1).

11. Run the pipette calibration by pipetting DI water into a tarred container and recording the weigh in the appropriate spaces provided on the form. Do this for three consecutive readings. The average is taken for the calibration figure.

12. Pipette 20 ml of the samples, at a depth of 3 cm, at the time corresponding with the temperature of the BLANK ( See Table 1). Rinse the pipette by sampling 20 mls of DI water.

13. Each aliquot is discharged into a tarred weighing dish, along with the deionized water used to rinse the pipette.

14. Place the weighing dishes in an oven at 105 ± 5 ° C. When the samples are dry, weigh on a balance to at least three decimal places and record the weight under the " Can Dry Wt." on the raw data lab sheet. These containers can be dried with the sand containers.

15. Using deionized water, wash the remaining sample through a 45 m m sieve. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.56.04 SOP TITLE: Texture Procedure   Pipette Method D 27 16. Transfer the soil from the sieve to a tarred container. Place the sample in a drying oven at 105 ± 5 ° C until dry. Weigh the container with the sample on a balance to at least three decimal places and record the weight under the " Sand Dry Wt." on the raw data lab sheet.

Table 1. Settling times at corresponding temperatures for pipetting < 2 µ m fraction at 3 cm depth.

Temperature Settling Times E C hr: min 17 2: 37 18 2: 33 19 2: 29 20 2: 26 21 2: 22 22 2: 18 23 2: 16 24 2: 13 25 2: 10 26 2: 7 27 2: 4 28 2: 1 29 1: 58 30 1: 56 STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.56.04 SOP TITLE: Texture Procedure   Pipette Method D 28 CALCULATIONS: % Sand = 100 ( Total Sand Weight / Total Soil Weight)

% Clay = ( Clay Weight) ( 400/ Pipet Volume) ( 100/ Total Soil Weight)

% Silt = 100   (% Sand + % Clay)

Where: Clay Weight = ( Can Dry Wt.   Can Tare Wt.)   ( Blank Factor)

Total Sand Weight = ( Sand Dry Wt.)   ( Sand Can Tare Wt.)

Soil Classification is determined from Textural Triangle REFERENCES: Indorante, S. J. March   April 1990. Particle Size Analysis is a Modified Pipette Procedure. Soil Science Society of America Journal. Volume 54.

Black, C. A. ( Ed). 1965. Methods of Soil Analysis, Part 1, American Society of Agronomy, Inc., Madison, Wisconsin.

Isaac, Robert. 1984. Methodology for the Analysis of Soil, Plant, Feed, Water and Fertilizer Samples. Georgia Soil Testing and Plant Analysis Laboratory.

Liegel, E. A., Simson and Schulte ( Ed). 1980. Wisconsin Procedures for Soil Testing, Plant Analysis, and Feed and Forage Analysis. Department of Soil Science, University of Wisconsin   Madison. D 29 AGVISE Laboratories, Inc. NORTHWOOD, N. D.

STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.58.02 SOP TITLE: Redox Potential of a Soil Sample REVISED BY: Garis Pollert TITLE: Nutrient Laboratory Analyst REPLACES SOP NUMBER: NUT. 02.58.01 REASON FOR REVISION: Update Title Page and Update Procedures.

APPROVALS:

Robert Deutsch Date Julie M. Johnson Date President/ Nutrient Laboratory Manager Quality Assurance Manager Robert Wallace Date CEO Effective Date STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.58.02 SOP TITLE: Redox Potential of a Soil Sample D 30 PURPOSE: To define the analytical method for determining the oxidation reduction potential of a soil sample.

EQUIPMENT: ° Redox Electrode ° Millivolt meter ° Thermometer CALIBRATION: 1. Prepare a Solution of: 105 ml Deionized Water + 3 ml H 2 SO 4 2.000 grams of Fe( NH 4) 2( SO 4) 2 * 6H 2 O 0.081 grams KMnO 4 Prepare in a beaker and stir with a magnetic stir bar.

Note: It is important that the solution is stirred slowly, to prevent air bubbles.

2. Take a millivolt reading of the above solution when all the solids have dissolved. The millivolt reading should be 474 ± 10 millivolts.

PROCEDURE: 1. Set up small plastic cups in trays.

2. Mark each sample with its appropriate sample number.

3. Scoop the soil samples into the cups using the 15 gram soil scoop, according to SOP NUT. 06.02, " Soil Scoop Procedure." Scoop a check sample after the last sample in each tray.

4. Add 15 ml of deionized water to each sample. For each batch of samples, check one aliquot of water with a graduated cylinder and record the volume on the lab sheet.

5. Slowly stir the samples with a glass stir rod.

6. Insert a stir bar into the beaker and record the stabilized millivolt reading while the sample is being stirred slowly. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.58.02 SOP TITLE: Redox Potential of a Soil Sample D 31 7. Record the temperature of the sample.

8. The pH may also be required. Follow the appropriate SOP and record the stabilized reading.

REFERENCE: Platinum Redox Electrode Instruction Manual. Model 96 78 00, 97 78 00. Orion Research Incorporated, 1991. D 32 AGVISE Laboratories, Inc. NORTHWOOD, ND STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.66.03 SOP TITLE: Cation Exchange Capacity by Sodium Saturation in Calcareous Soils REVISED BY: Gail Ducioame TITLE: Quality Control Specialist REPLACES SOP NUMBER: NUT. 02.66.02 REASON FOR REVISION: Update Title Page and Procedures APPROVALS:

Julie Johnson Date Mary Thingelstad Date Nutrient Laboratory Manager Quality Assurance Manager Robert Deutsch Date Robert Wallace Date President CEO Effective Date STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.66.03 SOP TITLE: Cation Exchange Capacity by Sodium Saturation in Calcareous Soils D 33 PURPOSE: To determine the cation exchange capacity of calcareous soil by sodium saturation.

EQUIPMENT: 1. Atomic Absorption Spectrophotometer 2. Vortex mixer 3. Centrifuge REAGENTS: SODIUM ACETATE, 1.0N 1. Dissolve 136 g of NaC2H3O2* 3H2O in water and dilute to 1000 ml. 2. Adjust the pH to 8.2 with acetic acid or sodium hydroxide solution.

ETHANOL, 95 percent AMMONIUM ACETATE, 1.0N ( 1.0 N Ammonium Acetate Concentrate)

1. Add 400 ml of concentrate to a 2000 ml volumetric flask. 2. Dilute to volume. Mix the solution thoroughly. 3. This makes a 1.0 N Ammonium Acetate solution with a working pH of 7.0. 1.0 N AMMONIUM ACETATE: 10 L 50 L Ammonium Hydroxide 690 ml 3450 ml Acetic Acid 600 ml 3000 ml 1. Rinse out the carboy with deionized water, then fill about 3/ 4 full. 2. IN ( OR IN FRONT OF) THE FUME HOOD use a graduated cylinder to add the Ammonium Hydroxide. Rinse the cylinder with Deionized Water into the carboy. 3. Use the graduated cylinder to add the Acetic Acid. Rinse the cylinder with Deionized Water into the carboy. DANGER: Ammonium Hydroxide and Acetic Acid both are corrosive and produce corrosive fumes. Use gloves and face protection when handling. Work in ( or in front of) the fume hood to avoid inhaling the fumes.

4. Mix the solution by shaking with the lid on or with an electric mixer or a magnetic stir plate and bar. 5. Fill the carboy to volume with deionized water and mix again. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.66.03 SOP TITLE: Cation Exchange Capacity by Sodium Saturation in Calcareous Soils D 34 6. Check the pH. If the pH is over 7.0, add Acetic Acid. If under 7.0, add Ammonium Hydroxide.

PROCEDURE: 1. Weigh out 4.0 g of soil into a 50 ml conical centrifuge tube.

2. Add 33 ml of sodium acetate solution.

3. Vortex the sample for approximately 10   30 seconds. Shake the sample for 5 minutes.

4. Centrifuge for 5 minutes or until the supernatant is clear.

5. Decant the liquid and discard.

6. Repeat this extraction ( Steps 2   4) three more times.

7. Add 33 ml of 95% Ethanol.

8. Vortex the sample for approximately 10   30 seconds. Shake the sample for 5 minutes.

9. Centrifuge for 5 minutes or until the supernatant is clear.

10. Decant the liquid and discard.

11. Repeat this extraction ( Steps 7   10) two more times.

12. Add 33 ml of ammonium acetate solution to the sample.

13. Vortex the sample for approximately 10   30 seconds. Shake the sample for 5 minutes.

14. Centrifuge for 5 minutes or until the supernatant is clear.

15. Decant the liquid into a 100 ml volumetric flask.

16. Repeat this extraction ( Steps 12   15) two more times. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.66.03 SOP TITLE: Cation Exchange Capacity by Sodium Saturation in Calcareous Soils D 35 17. Dilute the ammonium acetate extract to volume and mix.

18. Determine the sodium by using the method and standards in SOP NUT. 02.12.   " Procedures for the Determination of Ammonium Acetate Extractable Calcium, Magnesium, Sodium and Potassium in Soil."

19. If the samples exceed the highest standard by more than 10 %, an appropriate dilution is made and calculated.

CALCULATION: Cation Exchange Capacity by Sodium Saturation ( meq/ 100g) = Atomic Absorption Reading( ppm) * .01087 REFERENCES: Homer D. Chapman and Parker F. Pratt. 1978. Methods of Analysis for Soil, Plants, and Waters. Division of Agricultural Sciences. pp. 35   36. D 36 AGVISE Laboratories, Inc. NORTHWOOD, ND STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.92.00 SOP TITLE: Determination of Total Organic Carbon in Soil by Combustion SUBMITTED BY: Larry Wikoff TITLE: Nutrient Laboratory Manager REVISED BY:

TITLE:

REPLACES SOP NUMBER:

REASON FOR REVISION:

APPROVALS:

Larry Wikoff Date Julie M. Johnson Date Nutrient Laboratory Manager Quality Assurance Manager Robert Deutsch Date Robert Wallace Date President CEO Effective Date PURPOSE: To describe the procedure for determining total organic carbon in calcareous and noncalcareous soils using the LECO CR 412 Carbon Analyzer. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.92.00 SOP TITLE: Determination of Total Organic Carbon in Soil by Combustion D 37 EQUIPMENT: ° LECO CR 412 Carbon Analyzer ° Weigh Boats PROCEDURE: 1. Instrument Set Up: A. Check the O2 supply to furnace and set regulator to 40 psi as stated in the manual. B. Power up the furnace and allow it to come to temperature, about 1400oC. C. Check for proper gas flow as stated in the user manual for this system. D. Replace Anhydrone   if instrument indicates it is wet. E. Check the Ambient Monitor for proper instrument conditions. Print table and place it in the appropriate calibration logbook. All data must be signed and dated by the individual generating the data.

2. Calibration: A. Calibration data is stored in the calibration logbook. B. Check current calibration curve by combusting three replicates ( approximately 0.2g of a known low standard) as detailed in the system calibration logbook. Document information on the standard such as supplier, lot number, and ppm concentration in the calibration logbook. 3. System should be recalibrated if: 1. The value of standard varies more than 5% relative to the expected value. 2. Carbon content of unknown samples is expected to be above the current calibration curve. 3. The oxygen tank is changed. 4. The CR 412 Carbon Analyzer has sat idle for four weeks or more. D. Calibrate by combusting at least 7 replicates of the known low and high ppm standard, 0.2g within 5% and 0.09g within 5%, respectively. E. Record calibration data in the appropriate calibration logbook. All data must be signed and dated by the individual generating the data.

3. Sample Analysis: A. All samples tested for organic carbon content must be checked for inorganic carbon by placing several drops of 2M HCl on a small amount of soil ( approximately 0.2g) to check for carbonates. If no carbonates are present ( no effervescence observed), place approximately 0.25g into a weighing dish and heat at 104oC ( 2 to16 hours) to allow carbon to be determined on an oven dry weight basis. Store samples in a desiccator until ready to weigh. STANDARD OPERATING PROCEDURE SOP NUMBER: NUT. 02.92.00 SOP TITLE: Determination of Total Organic Carbon in Soil by Combustion D 38 B. Follow this procedure if carbonates are present as indicated by effervescence. Place enough soil in a weighing dish for the desired reps allowing 0.25g/ rep. Next, add 2M HCl until effervescence stops. Oven dry the samples as in Step A for noncalcareous soils. C. Weigh about 0.200g of the oven dried soil into a combustion crucible and record the weight. Manually enter the recorded weight in the instruments analysis screen menu. D. Percent carbon is calculated by the instrument and printed. Record this value on the appropriate lab sheet.

4. System Shutdown: A. Shutdown the system by choosing " LOG OFF" on the screen. The furnace temperature will be reduced and oxygen flow through the instrument will be stopped.

REFERENCES: LECO CR 412 Instrument manual, revised 1995. STANDARD OPERATING PROCEDURE SOP TITLE: 1/ 3 Bar   German Method 1 The MWC is frequently described in American literature as FC ( field capacity, pF # 0.3)

2 The FC is frequently described in American literature as 1/ 3 bar FMC ( field moisture capacity, pF # 2.5)

D 39 Subsequently, the following operations are carried out:

1) Taring of Buchner funnels with premoistened filter ( A, A', A")

MWC1 determination:

2) One aliquotes of approx. 100 g each ( filled to the rim) are divided into tared Buchner funnels. Soil allowed again to drip off. Soil is saturated and allowed to stand overnight. Funnels to be covered with a reversed watch glass in order to prevent drying out of the soil.

FC2 determination: 1/ 3 Bar 4) Covering/ sealing of Buchner funnels with 1   2 layers of parafilm and slight pressing down of film on soil. Tightness of parafilm at the Buchner funnel to be checked so that no air current can go through the soil. This step serves to prepare for the FC determination.

5) Application of a saturation potential of 1/ 3 bar to the suction bottles ( vacuum regulator setting:   0.33 bar, manometer setting: 666 mbar), ° 0.33 bar should not fall below otherwise high pressure is exerted on the soil via the parafilm membrane and, thus, too much water is pressed out. Increase vacuum only slowly from 0 to   0.33 bar. With this procedure the water starts to emerge. Suction to be used until dripping off speed is only approx. 1 drop/ 15 minutes ( at least, however, 2 hours, attention to be paid to tightness of the parafilm).

6) Balance of the low pressure to be established and parafilm removed.

7) The funnels with the partially wet soils to be weighed.

8) Soil is dried in the Buchner funnels.