This SOP is intended to serve as a field reference guide for the collection of water quality samples from CALOOSAHATCHEE river oxbows.

Sampling locations

* up = upstream (east) opening, dn = downstream (west) opening

** Coordinates locations are in the C-43 main channel, not in the oxbows .

Top of page

Chemical parameters and containers

Top of page

SWFRL personnel will measure a profile of temperature, pH, conductivity, and DO.

Instruments:

Fisher SCI Model 09-326-2 Meter for conductivity and temperature

OAKTON pHTester for pH

---

Lab/Office preparations (day before sampling trip)

Notify Lee County Environmental Lab to expect samples the next day.

Put 0.45 um 47 mm diameters membranes in clean dry Millipore filterholders.

Label all sample bottles with the oxbow location ID, duplicate number (if more than one duplicate), sample date, test parameters, and preservative.

Use pens or markers that are permanent. Write directly on the bottle or use a label that will not fall off when the container gets wet.

Gather five clean prelabeled empty sample bottles (one for each type of analysis) into one gallon size ZipLock Gripper Zipper Freezer Bags.

Prepare one bag for each sampling location, plus triplet of QA/QC samples, plus two spare bags.

Load supplies and chemicals into the transportation boxes.

Top of page

---

Boat preparations

Before trip:

• Make sure the boat is ready for the trip, make sure that gas tanks are full and all necessary sampling and safety gear is packed.

Before sampling:

• Anchor large boat at least 100' from downstream end of oxbow.
• Load skiff with equipment and bottles (see checklist, p. 11).
• Move skiff to downstream sampling location (maintain position with paddle)

---

Physical parameter measurement

• Position boat in sampling location as shown in the oxbow site map.


Avoid sediment disturbance, caused by the boat engine.

Instruments for field parameters:

pH tester

Dissolved oxygen meter

Conductivity meter

Top of page

---

Sample collection

Preparation for sample collection at the start of the sampling day.

• Confirm that all samples have been scheduled in the Lee County Lab.
• Calibrate instruments
• pH tester
• Dissolved oxygen meter
• Conductivity meter

• Load all the sample gear into the skiff.

Water collecting procedure

• Lower Niskin sampler into water 30 cm below surface.
• Swing it 5 times back & forth to rinse it.
• Stabilize sampler in non-turbid water and trigger the closure mechanism.
• Fill five (#1,3,4,5 and extra one to be filtered) containers to the top.
• Water from the additionally container should be filtered into bottle #2 (ortho-P).
• Retrieve collected sample and Niskin sampler to the clean processing area in the boat.
• Clean Niskin sampler for the next set of samples: rinse three times with DI or RO water.
• Put Niskin sampler in a plastic bag to prevent contamination during storage or transport to the field.

Filtering

Filtration must be completed within 15 minutes of sample collection.

Always use forceps and fresh latex gloves to prevent contamination.

For filtration use clean 60 cc syringes, clean Millipore 47 mm filterholders, and 0.45 um filter membranes.

Fill 60 mL syringe from bottles #1 or #3 completely.

Purge 10 mL sample through filtering equipment as a rinse for the filter system.

Filter sample via 0.45 um filter into the 250 mL ortho-P bottles (#2), if necessarily use a 1.0 um prefilter.

Rinse 3 times and fill bottle.

Fill 60 mL syringe from bottles #1 or #3 fully the second time.

Filter to the some bottle.

Secure sample container caps tightly.

Top of page

---

Preservation

• Sample preservation is performed on the boat within 15 minutes of sample collection.
• Preservation maintains the pH below 2 in bottles #1 and #4 after sample collection.
• Preservative for bottle #1 - 3 mL 50% sulfuric acid.
• Preservative for bottle #4 - 2 mL 50% nitric acid.
• The effectiveness of required pH adjustments must be checked for each sample.
• Narrow range pH paper model pHydrion part number 140 1-12 is used to test an aliquot of the preserved sample.
• Pour a small portion of the sample into the wastewater container over the pH paper.
• Compare the color with the manufacturer's color chart (bright red is required).
• Secure sample container caps tightly.

---

Labeling and recording

• Each bottle must be assigned a unique label prior to placing in cooler.
• Bottles are labeled using black fine point permanent marker.
• Sample labels include the sample type (EB, FD, or FB), plot location ID (number of oxbow and location in oxbow), preservative type, sampler initials, testing parameters, and sampling date.
• Record sampling time on the 100 mL bacteria bottle label.
• Register sampling information on COC.

---

Storage and transportation

• Check sample bottles for leaks by squeezing tightly.
• Check accuracy of labeling twice before storage.
• The labeled bottles are stored and transported in coolers with ice.
• Samples are transported to the analytical laboratory by courier.
• Samples should be delivered to the laboratory before 3 PM.


Top of page

---

QA/QC samples

• Precleaned Equipment Blanks (EB) ...one per day
• Field Duplicates (FD) ...one per ten samples
• Field-cleaned Equipment Blanks (FB) ...one per day

Precleaned Equipment Blanks (EB)

• Fill the Niskin bottle completely with analyte-free water.
• Process this water as if it were an actual sample (add appropriate preservative, filter, etc.).
• These samples are labeled as EB.
• Complete the chain of custody.

Field Duplicates (FD)

• These samples are collected starting from the second sampling location as the fourth and fifth sample sets. FD are required once per ten sample.
• They are collected at the same time from the same sourse to check the correctness of the sampling process.

Field-cleaned Equipment Blanks (FB)

• these blanks should be prepared during the middle to end of a sampling trip.
• the laboratory requires one field blank for each set of samples.
• collect this sample after the Niskin bottle has been cleaned in the field.
• fill the Niskin bottle completely with the DI or RO water.
• fill four bottles from Niskin.
• filter and fill the fifth bottle for ortho-P.
• add appropriate preservatives.
• these samples are labeled as FB.
• complete the chain of custody.

Top of page

---

Sample delivery and sample custody

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 includes:

• Sampling date and time
• Sample ID
• Bottles type
• Number of Bottles
• Preservative
• Analyses required
• Comments
• Signature

---

Lab/office post-processing

clean bottles/equipment

store instruments

order re-supply items

0.45 and 1.0 membranes

bottles

acids

pH papers

napkins

markers

labels

gloves

syringes

pH buffers

conductivity standards

DO-meter sensor membranes

DO-meter sensor filling solution

• photo copy and file field notes
• enter the physical measurements in database


Top of page

Appendices

Definitions

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.

Top of page

---

Preparation checklist

• Put 0.45 um 47 mm diameter filter membranes in clean dry Millipore filterholders
• 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 six clean empty sample bottles for all types of analyses in the one gallon size ZipLock Gripper Zipper Freezer Bag.
• Notify the personell of Lee County Environmental Lab to expect samples.
• Load all Supplies and Chemicals in the transportation boxes.

---

Boat loading checklist

Box # 2" Calibration & Preservation"

Item	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

Top of page

Box # 3 "Instruments"

Item	Quantity
pH tester	2
Dissolved oxygen meter	2
Digital TDS Meter	2
Niskin Water Sampler	1
500 mL analyte free water rinser	1 bottle
Batteries for instruments	1 complete for each

Box # 4 "Filtration"

Item	Quantity
Syringes, 60 mL	24 complete
Syringe filter holders	24 complete
1.0 um membranes	1 box
0.45 um membranes	2 boxes

Supplies without boxes

Item	Quantity
Sample holding frame	1
Camera	1
Tape Recorder 1	1
Batteries for the Tape Recorder	2
Floor mats 1	1 gal
Container for solid wastes	1
5 gal analyte free water	1 container
Global Positioning System	1
Tapes	1
Calculator	1
Buckets to contain liquid wastes	1
Microphone	1

Top of page

---

Protective clothing

---

Documentation supplies

---

Reference material

Top of page

---

Example Labels

Sample ID 2UP

Type FD

Preservative H2SO4

Testing parameters NH3, TP, NOx

Sampling Date 8/25/98

Sampler initials ___________

---

Example COC form

---

Analyte-Free Water Containers

New Containers

• Clean with tap water and lab grade soap (Liquinox or equivalent) using a brush, if necessary, to remove particulate matter or surface film.
• Rinse thoroughly with tap water.
• If trace metals are to be sampled, then rinse with 10-15% reagent grade nitric acid (HNO3). The acid rinse should not be used on steel sampling equipment (bailers, augers, trowels, etc.).
• Rinse thoroughly with tap water. Enough water shall be used to ensure that all equipment surfaces are flushed with water.
• Rinse thoroughly with analyte-free water and allow to air dry as long as possible.
• Clean sampling equipment shall be wrapped in a plastic bag to prevent contamination during storage or transport to the field.
• If no further sampling is to be performed, equipment must be rinsed with tap water immediately after use.
• Wash per instructions, cap with Teflon film, aluminum foil or the bottle cap.
• The bottle cap shall be equipped with a teflon liner. Aluminum foil or teflon film may be used as liner material.


Top of page

Reused Containers

• Immediately after being emptied, cap with aluminum foil, teflon film or the container cap.
• Wash container exterior with lab-grade detergent solution and rinsed with DI water.
• Rinse interior twice with isopropanol (delete if containers are plastic).
• Rinse interior thoroughly with analyte-free water.
• Invert and allow to drain and dry.
• Fill container with analyte-free water and cap tightly with aluminum foil, Teflon film or the container cap.
• The bottle cap shall be equipped with a teflon liner. Aluminum foil or teflon film may be used as liner material.
• Water shall not be stored for more than 3 days prior to a sampling trip.

---

Field Data Book

• Field location/GPS data
• Sample numbers
• Date/time collected

---

Physical parameters

• temperature in grad. C
• conductivity in uS/cm
• DO in mg/L
• pH

Top of page

---

Example of PP data sheet

---

Additional records

All records and documentation required to trace a sampling event from point of origin.

• These records must include:
• Field notebooks.
• Calibration and quality control data associated with a sample set.
• Preservative preparation logs.
• Instrument maintenance logs.
• Sample disposition logs.
• Final reports.

Directory & contact information

Phone 278-7070 Fax 939-4850

Mr. Kibbey Keith - Director

Tarpow Bay Lall, Florida for Environmental Studies

Phone # 472-3776 Fax 939-4850

Dr. Ken Cummins

Dr. Peggy Wilzbach

Tarpon Bay Environmental Lab

900 A. Tarpon

Sanibele, FL 33957

The Spirit

Phone # 941-675-0533

Mr. Richard Neely

12255 Anchor Ln. SW.

Moore Haven, FL 33471

University of Florida SWFREC

Phone 658-3400 Fax 658-3469

Dr. John Capece, Asst. Professor 998-8321 (pager) 860-6341 (cell)

Mr. Benno Eidus, Chemist 658-3417 (office)

Ms. Angela Alexander, Secretary 645-0780 (cell)

Mr. Ed Rawlinson, Technician 279-5918 (pager) 370-6912 (cell)

Top of page

Instruments calibration and field use

SPECIFICATIONS

Conductivity Range:

• .01 to 19.99 uS (micromhos)
• 1 to 1999 uS (micromhos)
• .01 to 19.99 mS (mhos)
• .1 to 199.9 mS (mhos)

• 0.3% of reading

• Automatically temperature compensated to the international standard of 25 degrees Celsius, temperature may also be compensated manually.

• 0.0 to 50.0 Celsius

• Default value set at 2 % per degree Celsius.

Power:

• One 9 volt alkaline battery

• uS/cm microsiemens or micromhos per centimeter
• mS/m millisiemens or mhos per meter
• ^oC temperature

• Use very clean beakers/flasks.
• Avoid cross-contamination between measurements by rinsing the probe in deionized/distilled water and by rinsing the probe in the solution to be tested.
• 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.
• 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

• Connect the probe by placing the connector plug into the keyed instrument socket.
• Press the ON/OFF key to turn the unit on.
• Place the unit in the MODE required (conductivity or temperature) by pressing the MODE key.
• Place the probe in the sample solution.
• Read the answer on the digital display while stirring the probe in the solution.

• If the unit has already been calibrated on that day, then "CAL" will appear in the top left corner of the display.

• Press the CHECK key, "CHK" will appear on the top right corner of the display.
• 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.

• 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.
• Erase any existing calibration data.
• Insert the probe into a known solution (in a range of 100 and 1000 uS/sm).

• Press the MODE key to place the unit in the measurement function desired: Conductivity (uS/cm), Resistivity (MQ/cm) or Concentration (c).
• 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.
• With correct value on the display, press ENTER key to enter the value as a calibration point.

CONDUCTIVITY MEASUREMENT

• Micromho is a measurement of conductance.
• A micromho is the same as a microsiemens (1 micromho = 1 microsiemens).

• Press the MODE key four times until you enter the temperature mode indicated by ^oC on the display.

• BAT Indicates that the battery needs to be replaced.
• E6 or E7 Calibration point error. Clear all calibration data and start calibration over. Make certain that the value you are calibrating to is correct.
• Sc or Oc Temperature probe (thermistor) short or open probe.
• -L or -H Salinity measurement is below or above the measurement range.

• 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.

• 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.


Top of page

---

DO-meter YSI Model #51B

Calibration

• Turn the meter's selector knob to "Zero".
• 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.
• 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.
• 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, for it to work properly.
• 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.
• 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.
• 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.

• Open the battery compartment lid
• Remove old batteries and replace with four fresh C size batteries noting polarity as shown in the battery compartment.
• After changing batteries, recalibration is necessary.

• Make sure that probe cap has wet tissue inserted in top to ensure that the membrane inside the probe remains moist.
• Turn on and let warm up for at least five to fifteen minutes
• Calibrate the meter before every sampling location.
• 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.
• 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.
• 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.
• 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

• 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.
• 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.

• 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.

• 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.


Top of page

---

Model 1010 Series 2.5 l Niskin Sampler

Field Use

• Tie the end of the rope to the boat to secure the Niskin Sampler.
• Place top-plug lanyard loop over bottle cap release pin (the longer pin).
• Release pushrod cap and snap bottom plug lanyard between top plug lanyard ball and pin. Do not put into loop.
• Simultaneously (with one hand) depress thumb block, and hold pushrod in place (at base of lower mounting block).
• Put Niskin Sampler in the sampling area 30 cm down into water to the color band.
• Wave the Niskin Sampler back and fourth five times.
• Pull the rope to make the caps shuts to collect water sample.
• Extract Niskin Sampler from river.
• Open the valve and draw water to four sampling bottles.
• Open the tops and dump out the left over water.
• Rinse the Niskin Sampler three times in the inside with deionized water.
• Put the Niskin Sampler in a clean plastic bag.

Maintenance

• Wash bottle with fresh water and DO water after use and before storage.
• Store bottles with valves in final closed position.
• After extended storage, especially before every deployment, make sure that all moving parts and seals are free to perform.
• Replace black power cord (spring) when its force drops 25% below initial values
• In high sediment-laden water, do not grease working parts.
• Grit trapped in grease scours sealing surfaces.
• Inspect O rings for damage.
• Adjust knots in latex tubing to control any leakage.

 

 

Top of page
Back to WQ page

Created 09/03/98
WebMaster Benno Eidus