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Oxbow Sampling Project Standard Operating Procedures (SOP) John Capece, Benno Eidus, and Ed Rawlinson UF-IFAS Southwest Florida Research and Education Center, Immokalee FL Table of Contents C. Boat loading checklist 9 D. Skiff loading checklist 11 E. Example labels 11 F. Example chain of custody form 12 G. Analyte-free water containers 13 H Field data book 13 I. Example of physical parameters data sheet 15 J. Additional records 16 K. Sampling preparation inventory 17 L. Directory & contact information 20 M. Instruments calibration and field use 21
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| 1. Sampling locations | |||
|---|---|---|---|
| Oxbow ID* | River Bank | Coordinates in Minutes** | |
| Lat. (26 deg N) | Long. (81 deg W) | ||
| 2 up | North | 43.35 | 40.61 |
| 2 dn | North | 43.42 | 40.88 |
| 3 up | North | 43.30 | 40.26 |
| 3 dn | North | 43.31 | 40.36 |
| 9 up | South | 43.16 | 37.53 |
| 9 dn | South | 43.19 | 37.62 |
| 11 up | South | 42.89 | 36.22 |
| 11 dn | South | 42.93 | 36.46 |
| 13 up | North | 43.04 | 35.66 |
| 13 dn | North | 43.02 | 35.70 |
| 15 up | North | 43.26 | 34.93 |
| 15 dn | North | 43.23 | 34.98 |
| 18 up | South | 43.04 | 33.73 |
| 18 dn | South | 43.00 | 33.89 |
| 24 up | South | 43.62 | 31.47 |
| 24 dn | South | 43.53 | 31.53 |
| 26 up | North | 44.40 | 31.22 |
| 26 dn | North | 44.26 | 31.24 |
| 32 up | South | 44.98 | 28.42 |
| 32 dn | South | 44.96 | 28.54 |
| * up = upstream (east) opening, dn = downstream (west) opening ** Coordinates locations are in the C-43 main channel, not in the oxbows . | |||
2. Chemical parameters and containers | |||||||
|---|---|---|---|---|---|---|---|
| Bottle number | Bottle size | Method # | Parameter | Holding Time | Preservative | Filtration | Comments |
| #1 | 32 oz. | 353.20 | NOx | 28 days | H2SO4 | pH<2 | |
| 365.40 | total P | ||||||
| 350.10 | Ammonia | ||||||
| #2 | 32 oz. | 365.20 | Ortho P | 48 hr. | immediately, 0.45 um | ||
| # 3 | 1000 mL | 180.10 | turbidity | 48 hr. | |||
| 110.20 | color | 48 hr. | |||||
| AWWA 161002d | chlorophyll | 14 days (in dark) | |||||
| #4 | 32 oz. | 245.10 | Hg | 28 days | HNO3 |
pH<2 | |
| 220.10 | Cu | 6 mos. | |||||
| #5 | 100 mL (sterile) | 9221E | fecal coliform | 6 hr. | Na2S2O3 | prepreserved container | |
| 9230B | streptococcus | 6 hr. | |||||
3. Physical parameters
4. Lab/Office preparations (day before sampling trip)
Before sampling:
6. Physical parameter measurement
8. Filtering 9. Preservation 10. Labeling and recording 11. Storage and transportation 12. QA/QC samples
Field-cleaned Equipment Blanks (FB)
The field sampler is personally responsible for the care and custody of the samples until they are transferred to testing lab. The Chain of Custody form (Appendix F) includes:
15. Appendices Any sample from a natural source or source that may reasonably be expected to contribute pollution to or receive pollution from ground waters or surface waters of the state. Parent Sample A sample from which aliquots are taken for testing purposes. Subsample refers to any derivative of a parent sample. Sample Set The basic unit for analytical quality control. The analytical set is defined as samples that are analyzed (or sampled together) with the same method sequence, the same lots of reagents and with the same treatment common to all samples. The samples and QA/QC samples must have been collected within the same specified time period or in continuous sequential time periods. Quality Control Measures Blanks An artificial sample of an analytical matrix designed to monitor the introduction of artifacts into the system. Label all sample bottles with the oxbow description, duplicate number (if more than one duplicate), sample date, test ID, and preservative. Use a permanent pen or marker and write directly on the bottle or use a label that will not fall off when the container gets wet. Gather five clean empty sample bottles for all types of analyses in the one gallon size ZipLock Gripper Zipper Freezer Bag. Notify the personnel of Lee County Environmental Lab to expect samples. Load all Supplies and Chemicals in the transportation boxes. C. Boat loading checklist Liquid Detergents "Liqui-Nox" 1 bottle Five gal waterproof bags 25 bags 500 mL analyte free water squeeze bottles 3 bottles Paper towels 1 box 1:1 Hydrochloric Acid 500 mL Box # 2" Calibration & Preservation" Quantity pH buffers 4,7 and 10 8 packs each Conductivity Standards 100 and 1000 uS/cm, 4 bottles each Nitric Acid preservative 100 mL Sulfuric Acid preservative 100 mL Dropping Bottles 4 bottles Narrow range pH paper 2 rolls Box # 3 "Instruments" Quantity Dissolved oxygen meter 2 pH tester 2 Digital TDS Meter 2 Niskin Water Sampler 1 Extra Rope for Sampler 1 Water depth measuring tape 1 500 mL analyte free water rinsing 1 bottle Batteries for each instruments 1 complete for each Box # 4 "Filtration" Quantity Syringes, 60 mL 24 complete Syringe filter holders. 24 complete 0.45 um membranes, 2 boxes 1.0 um membranes 1 box Supplies without boxes Quantity Sample holding frame 1 frame 5 gal analyte free water 1 container Global Positioning System 1 Camera 1 Calculator 1 Tape Recorder 1 Microphone 1 Batteries for the Tape Recorder 2 Tapes 1 Floor mats 1 1 gal buckets to contain liquid wastes 1 Container for solid wastes 1 Transportation supplies Quantity Ice chests 3 coolers Ice 100 lb. Sealing tape 1 roll Protective clothing Quantity Gloves 2 boxes Goggles 2 Documentation supplies Quantity Notebooks/logs/field sheets 1 Pens, permanent markers, 10 p. 10 Bacteria Sample container tags 100 COC 10 Reference material: Quantity Site maps 1 SOPs 1 life jackets 3 Niskin bottle 1 sets of clean sampling bottles 2 water depth measuring tape 1 box # 3 "Instruments" 1 5 gal bucket 1 paddles 2 Sample ID Type EB FD FB Preservative H2SO4 HNO3 Testing parameters Sampling Date/Time Sampler initials Example COC form (Lotus file C:\benno\results\OXB_COC2.WK4) Analyte-free containers are defined by EPA to be glass containers. The DER QA Section will allow these containers to be made of Teflon, polypropylene, or high density polyethylene (HDPE). These containers should be filled up for a single sampling event and then emptied at the end of the sampling day. EPA's cleaning procedure for glass (Teflon and polypropylene) is as follows: 5.1 New Containers
5.2. Reused Containers
I. Example of PP data sheet (see next page) Example of PP form (Lotus file C:\benno\results\OXB_PHY2.WK4) All records and documentation required to trace a sampling event from point of origin. These records must include:
K. Sampling Preparation Inventory | |||||||
| Check | Equipment | Construction | Use | Parameter |
|---|---|---|---|---|
| 1. Decontamination equipment and supplies | ||||
| Liquid Detergents "Liqui-Nox" | N/A | Wash sampler | All parameter groups | |
| Five gal waterproof bags | Plastic | To contain wastes | All parameter groups | |
| 500 mL analyte free water rinser | Plastic | Wash sampler | All parameter groups | |
| Paper towels | Paper | Decontamination | All parameter groups | |
| 1:1 Nitric Acid Solution | N/A | Clean Container | Metals | |
| 1: 1 Hydrochloric Acid | N/A | Clean Container | Nutrients | |
| 5 gal analyte free water | N/A | Clean Container | All parameter groups | |
| 5 gal water container | Plastic | Clean Container | All parameter groups | |
| 2. Reagents for field calibration | ||||
| pH buffers (4,7 and 10), 8 packs each | N/A | Calibration | Physical properties | |
| Conductivity Standards 100 and 1000 uS/cm, 8 bottles | KCl | Calibration | Physical properties | |
| 3. Preservation supplies | ||||
| Acid preservative, 100 mL | Sulfuric Acid, ACS grade, 1:1 | Sample preservation | Anions, Inorganic Parameters | |
| Acid preservative, 100 mL | Nitric Acid,
ACS grade, 1:1 | Sample preservation | Metals | |
| Dropping Bottles | Glass | Sample preservation | Metals, Anions | |
| Narrow range pH paper | N/A | Sample preservation | Metals, Anions | |
| 4. Sample transportation supplies | ||||
| Ice chests | Plastic | Transporting samples | All parameter groups | |
| Sealing tape | Plastic | Transporting samples | All parameter groups | |
| Shipping labels and forms | Paper | Transporting samples | All parameter groups | |
| Ice | Water | Transporting samples | All parameter groups | |
| Sample container tags | Paper | Documentation | All parameter group | |
| 5. Protective clothing | ||||
| Gloves | Latex | Sampling | All parameter groups | |
| Clothing and goggles | N/A | Protection | All parameter groups | |
| 6. Documentation supplies | ||||
| Notebooks/logs/field sheets | Paper | Documentation | All parameter groups | |
| Pens, permanent markers, 10 p. | N/A | Documentation | All parameter groups | |
| Sample container labels | Paper | Documentation | All parameter groups | |
| Custody labels/tags | Paper | Documentation | All parameter groups | |
| Custody/transmittal forms | Paper | Documentation | All parameter groups | |
| Camera | N/A | Documentation | All parameter groups | |
| Calculator | N/A | Documentation | All parameter groups | |
| Tape Recorder | N/A | Documentation | All parameter groups | |
| Microphone | N/A | Documentation | All parameter groups | |
| Batteries for the Tape Recorder | N/A | Documentation | All parameter groups | |
| Tapes | N/A | Documentation | All parameter groups | |
| 7. Reference material: | ||||
| Site maps | Paper | Locate positions | All parameter groups | |
| SOPs | Paper | Documentation | All parameter groups | |
| 8. Filtration equipment | ||||
| Syringes, 60 mL, 24 p. | Polypropylene | Field filtration | Inorganic anions | |
| Syringe filter holders, 24 comp.. | Stainless Steel | Field filtration | Inorganic anions | |
| 0.45 um membranes, 2 boxes | Polyester | Field filtration | Inorganic anions | |
| 1.0 um membranes 1 box | Polyester | Field filtration | Metals in GW | |
| Sample holding/frame | wood/PVC | Hold bottles | All parameter groups | |
| Floor mats | PE | Protection from contamination | All parameter groups | |
| 1 gal buckets to contain liquid wastes | PE | Protection from contamination | All parameter groups | |
| Container for wastes | PE | Protection from contamination | All parameter groups | |
| 9. Field Test Instruments | ||||
| Global Positioning System | N/A | Positioning | ||
| Total depth sensor/scale | N/A | Positioning | Total depth | |
| Dissolved oxygen meter | N/A | DO | Dissolved Oxygen | |
| pH tester | N/A | pH | Physical Properties | |
| Digital TDS Meter | N/A | Conductivity, Temperature | Physical Properties | |
| Niskin Water Sampler | SS | Sampling | All parameter groups | |
| Extension pole for Sampler | Wood | Sampling | All parameter groups | |
| Water depth measuring tape | Fiberglass/Ceramic | Depth measuring | Sample location depth | |
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Tarpow Bay Lall, Florida Center for Environmental Studies
The Spirit
University of Florida SWFREC
M. Instruments calibration and field use Conductivity MeterSPECIFICATIONSConductivity Range:
Accuracy
Temperature Compensation:
Temperature Compensation Range:
Temperature Coefficient:
Power:
DISPLAY SYMBOLS
GENERAL OPERATING TECHNIQUES 1. Use very clean beakers/flasks. 2. Avoid cross-contamination between measurements by rinsing the probe in deionized/distilled water and by rinsing the probe in the solution to be tested. 3. Make certain to sustain flow through the probe (or move the probe through the solution in a stirring motion) while making your readings. Stirring helps prevent polarization, ensures that the solution is well mixed, and helps to maintain a uniform, temperature within the solution. 4. When finished using the probe, always rinse it in distilled water and store dry or in distilled water. Solutions which are allowed to dry on the probe will eventually block out active sites on the internal platinum electrode, the surface area will be reduced, and a new probe will be required. Do not touch the internal platinum electrode, if the surface is damaged linearity will be affected, specifically in the high conductivity readings, and difficulty may be found in achieving high readings. MAKING MEASUREMENTS
CLEARING CALIBRATION DATA If the unit has already been calibrated on that day, then "CAL" will appear in the top left corner of the display. 1. Press the CHECK key, "CHK" will appear on the top right corner of the display. 2. Press and hold the ENTER key for 10 seconds, "0" zero will be displayed to the far left of the display to indicate that all calibration data has been cleared. CALIBRATION The unit may be calibrated to known solutions. Calibration is achieved by using the arrow keys to adjust the display to read to a known value. The ENTER key is used to store a value as a calibration point. Four calibration points may be entered to ensure accuracy over the entire measurements range. 1. Erase any existing calibration data. See "Clearing Calibration Data" 2. Insert the probe into a known solution (in a range of 100 and 1000 uS/sm). 3. Press the MODE key to place the unit in the measurement function desired: Conductivity (uS/cm), Resistivity (MQ/cm) or Concentration (c). 4. Press the arrow keys to adjust the value on the display to the value of the solution. "CAS" will blink on the display. Each press of the arrow key increases/decreases the display by 1 digit. To rapidly increase/decrease the display, press and hold down the arrow key, the least significant digit is changed until ten digits have been counted, then the next significant digit, etc. 5. With correct value on the display, press ENTER key to enter the value as a calibration point. The instrument is now calibrated. This procedure may be repeated three (3) additional times (total of four calibration points) using different solutions to insure accuracy over the entire measurement range. CONDUCTIVITY MEASUREMENT Micromho is a measurement of conductance. A micromho is the same as a microsiemens (1 micromho = 1 microsiemens). TEMPERATURE MEASUREMENT Press the MODE key four times until you enter the temperature mode indicated by oC on the display. DISPLAY MESSAGES
BATTERY REPLACEMENT Erratic readings, no display, or "BAT" on the display are all indications that the battery needs to be replaced or that the battery is not making proper contact. Place your thumb against the word "OPEN" on the back of the unit and slide the battery cover up and off. Replace the battery with a new 9 volt alkaline battery. Make certain that the battery is inserted properly and that proper contact is made. Low battery power can occasionally cause any number of "apparent" operational difficulties. Replacing the batteries will solve most difficulties. MAINTAINING CALIBRATION For calibration contact:
ACCESSORIES One-Shot Traceable Conductivity Calibration Standards (Model 4175-4179) . Single-use standards eliminate concerns about external container contamination. Calibration is made in the standard vial. Opening the standard container to 1 3/4" diameter and depth 3 1/2" allows the probe calibration to take place in the standard's polyethylene container. Supplied as a pack of six One Shot standards. Each standard contains 100 mL. Calibration: 1. Turn the meter's selector knob to "Zero". 2. Observe the display to see if the needle registers exactly 0.0 mg/L (top scale of the display). If not, twist the zero knob (left hand set of dials) until the needle does register 0.0 mg/L. Make sure that the needle is exactly lined up with its mirror image to avoid parallax. This warrants that you are reading the display properly. 3. Turn the right hand dial to "Full Scale". Observe the display to see if red needle registers on 15.0 mg/L (top scale of the display). If not, then twist the Full Scale knob (left hand set of dials) until the needle does register 15.0 mg/L. If the meter will not calibrate to full scale, the batteries are probably weak. Open the back by removing the screws at the four corners. Insert two alkaline D cell batteries and re-test for full scale calibration. Be sure that the polarity of the positive and negative poles of the battery are correctly matched with the poles of the battery holder, otherwise the machine will not work properly. If the machine posts are corroded, use sodium bicarbonate (baking soda) or fine sandpaper to remove corrosion. If successful, replace the back of the meter and proceed. If this fails, the unit is probably in need of repair. 4. Remove cap from probe and inspect for bubbles under the membrane or damage to the membrane itself. Replace the membrane if either are present. Bubbles that are present are indicative of a probe with a leaky diaphragm or one that has been overexposed to dry conditions. Caution: If a probe has gone completely dry, you will not see any bubbles. Probe solution must then be added, and bubbles bled off (by gently pressing a pencil eraser into the plunger hole), for it to work properly. 5. Loosely replace the probe cap and allow the temperature and humidity within it to stabilize (normally a minute or two). Turn selector to "Read Temp and Set Dial". Read the temperature on the lower scale of the display. Adjust the "O2 Solubility Factor" Placing the cap loosely on the probe creates an environment saturated with water (=100% humidity), which is necessary for calibration. 6. Turn selector to "Calib O2". Using the gauge in the upper right corner of the display, twist the "Calib" knob until the needle corresponds with the appropriate altitude for the area. If the test site is at sea level, the gauge should register on the bottom line of the scale. 7. Using the mercury thermometer, read the temperature of a "test blank" for comparison with that of the probe. Turn the selector to "Read Temp and set Dial". Insert probe into the blank and gently agitate until the needle stabilizes. Record both readings in °C. Even though both should match, there may be a difference of up to ± 1 °C. If the difference is greater, the meter may be in need of repair and the dissolved oxygen readings are suspect. CHANGING BATTERIES
Make sure that probe cap has wet tissue inserted in top to ensure that the membrane inside the probe remains moist. 1. Turn on and let warm up for at least five to fifteen minutes 2. Calibrate the meter before every sampling location. 3. Remove cap from probe and lower into sample medium to the desired depth. The minimum depth must be sufficient to fully immerse the probe. Make CERTAIN that the probe is immersed fully in the medium, or the meter will not register properly. 4. Turn selector to "Read Temp and Set Dial". Gently agitate the probe throughout the medium while the needle stabilizes. Read the lower scale of the display and record the temperature (°C). Let the display reach an equilibrium (usually takes less than a minute) before you go to the next step. Make sure that the needle is exactly lined up with its mirror image to avoid parallax. This ensures that you are reading the display properly. 5. Set O2 Solubility Factor dial to the correct temperature. Make CERTAIN that the lines on the dial connect, i.e., if the medium is freshwater and is 25 °C, then the freshwater (top) line and the line from 25 should connect. 6. Turn selector to "Read O2". Gently agitate the probe while the needle stabilizes. Read the upper scale of the display and record the dissolved oxygen in mg/L. CAUTION: to AVOID CROSS CONTAMINATION BETWEEN SAMPLES, NEVER IMMERSE THE ELECTRODE ABOVE COLOR BAND. SPECIFICATIONS Range 0 to 14 pH extended range Resolution 0.01 pH Accuracy ±0.02 pH at normal room temperature; Operating Temperature, 0 to 50 C, 32 to 122 F Temperature Compensation, Automatic CALIBRATING Calibrate to pH 4, 7 and 10. For best accuracy, calibrate to all 3 pH at field temperature, starting with pH=7. Turn on the tester and press the "CAL" button to enter CALibration mode. Immerse the electrode into the buffer about 1", stir gently and wait 2 minutes for the displayed value to stabilize. Press "HOLD/CON" button to CONfirm and complete the calibration. Repeat with pH 4 buffer, and finally pH 10 buffer to complete the slope adjustment. Field Use: Remove cap and press ON/OFF button on the keypad to turn on the pHTester. Dip the electrode ½" to 1" into the test solution. Never dip the electrode above the color band. Stir once, let the display stabilize. Allow a couple of minutes for the ATC to correct for temperature change. Note the pH. Press "HOLD/CON" button if you wish to hold the reading. Press it again to release it. Press the ON/OFF button to shut off. MAINTENANCE Rinse the electrode with DI or RO water after using. To maximize electrode life, place a small piece of clean paper or sponge in the cap, moisten with tap water and replace cap. CHANGING BATTERIES Flip up the battery compartment lid Remove old batteries and replace with four fresh DA675 or model 303 battery noting polarity as shown in the battery compartment. After changing batteries, recalibration is necessary. Operating Instructions Field Use
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