Standard Operating Procedures
for DEP 319 Project at MAERC

1. Introduction

This SOP is intended to serve as a field reference guide for the collection of water quality samples from Buck Island Ranch surface water. 

2. QA/QC measures

2.1 In addition to standard samples, the field technicians collect equipment blanks (EB), field cleaned equipment blanks (FB), split samples (SS), and field duplicate samples (FD).

2.2 Overall care must be taken in regards to equipment handling, container handling/storage, decontamination, and record keeping. Sample collection equipment and non preserved sample containers must be rinsed three times with sample water before the actual sample is taken. Exceptions to this is any pre-preserved container.

2.3 If protective gloves are used, they shall be clean, new and disposable. These should be changed upon arrival at a new sampling point.

2.4 Highly contaminated samples shall never be placed in the same ice chest as environmental samples. It is good practice to enclose highly contaminated samples in a plastic bag before placing them in ice chests.

2.5 Ice chests or shipping containers with samples suspected of being highly contaminated shall be lined with new, clean, plastic bags.

2.6 If possible, one member of the field team should take all the notes, fill out labels, etc., while the other member does all of the sampling.

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3. ISCO sampling

3.1 Flow proportional sampling from streams and canals produces the most representative water quality samples by virtue of the sample number and size being proportional to flow volume or flow rate. The advantage of flow proportional sampling is more pronounced in the case of variable flow canals or streams. In sites where the sampling equipment is serviced once a week or less frequently, the design of a sampling scheme to determine sampling volumes for variable flow canals is essential.  Surface water samples are collected from each canal using an ISCO portable automatic water sampler interfaced with a programmable datalogger/controller (CR10x).

3.2 For each pre-determined sampling volume of flow, the CR10x controller triggers the auto sampler to collect a sample (aliquot).  Optimum sampling volume is desired to collect representative water quality samples throughout the week with minimum chance of filling all the bottles or leaving a lot of sampling bottles empty before the next service.

3.3 Flow proportional automatic sampling procedures are only applicable to long holding time (28 days) parameters: TKN, TP, NOx and NH4.

3.4 The ISCO 3700 autosamplers are supplied with 1000 mL plastic bag liners for the sample holders.

3.5 The 800 mL samples are collected at predetermined volumes of flow, as measured by an associated CR10 datalogger.

3.6 Each bottle/bag receives one sample.

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4. ISCO sample container cleaning

4.1  If auto sampler bottles are used in the ISCOs then the bottles must first be cleaned in the field laboratory using the standard EPA bottle cleaning procedure.  This procedure also applies to cleaning of other sampling equipment (buckets, dippers, etc.). Top of page

5. Preservation of samples

5.1  Proper sample preservation is the responsibility of the sampling team, not the lab providing sample containers.

5.2  It is the responsibility of the field team to assure that all samples are appropriately preserved.

5.3  When samples are analyzed for TKN, TP,  NH4 and NOx 1 mL of 50% Trace Metal grade sulfuric acid (Fisher Cat. No: LC25640-3) is preadded to the each discrete auto sampler bottles/bags (for 800 mL sample) in the field lab before sampling collection .  The preservative maintains the sample at 1.5<pH<2 after collection. To meet maximum holding time for these preserved samples (28 days), pull and ship samples every 14 days.

5.4  The effectiveness of required pH adjustments must be checked in the field (for grab samples) or in the ranch lab (for all ISCO samples).

5.5  Narrow range pH paper (test strips) shall be used to test an aliquot of the preserved sample.

5.6  Pour a small portion of the sample into disposable container.

5.7  Place the pH paper into the container and compare the color with the manufacturer's color chart.

5.8  Discard the aliquot. Do not pour back into sample container.

5.9  If the pH paper test shows inadequate acidification then more sulfuric acid solution should be added until the pH paper tests shows that the 1.5<pH<2 criteria is met.

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6. Bottle and tray labeling

6.1  Each ISCO sample bottle/bag must be assigned a unique label. The information to be entered on the label includes: 6.2 Merging Labels  from COC's

6.3  The labels must be affixed to the sample containers and look similar to the label below.
 

Filtered:

BIR
3456
W3-FG
ortho-P, NO3
Filtered
 
 

Preserved:

BIR
3457
S3-23
NOX, TP, TKN, NH3
Preserved
 
 


7. Sampler tubing

Tubing is replaced with new vinil tubings after three months.  The sampler is programmed to rinse the tubing twice with a sample before collection and then purge the tubing after the sample is taken.

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8. Analyte-free water containers

Analyte-free containers are defined by EPA to be glass containers. The DEP 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:

8.1 New Containers

8.1.1  Clean with tap water and lab grade soap (LiquiNox or equivalent) using a brush, if necessary, to remove particulate matter or surface film.

8.1.2   Rinse thoroughly with tap water.

8.1.3   Rinse thoroughly with DI water.  Enough water shall be used to ensure that all equipment surfaces are flushed with water.

8.1.4   Rinse twice with isopropanol. One rinse may be used AS LONG AS all equipment surfaces are thoroughly wet with free flowing solvent.

8.1.5  Rinse thoroughly with analyte-free water and allow to air dry as long as possible.

8.1.6  Clean sampling equipment shall be wrapped in plastic bags to prevent contamination during storage or transport to the field.

8.1.7  If no further sampling is to be performed, equipment must be put in plastic bags.

8.1.8  Wash per instructions, delete solvent rinse if plastic (HDPE or polypropylene) containers are being cleaned.  Cap with teflon film, aluminum foil or the bottle cap.

8.2 Reused Containers Top of page

9. ISCO samplers cleaning

9.1 ISCO samplers shall be cleaned on a quarterly (3 months) as follows: 9.2 ISCO Automatic Sampler Distributor Arm 9.3 ISCO Sampler Metal Tube 9.4 Sampler Suction Intake 9.5 Sample Tubing Decontamination

Tubing is used for 3 months at and then discarded. Do not reuse tubing.
New tubing is pre cleaned as follows:

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10. ISCO configuration

Option Settings press
set clock
time 
enter
bottles and sizes
portable, 24 bottles 
enter
bottle volume
1000 
enter
suction lane
3/8, vinyl, 25 ft 
enter
liquid detector
enable 
enter
rinse cycle
enter
enter head manually
no
enter
retry up to 1 times
yes 
enter
programming mode
basic 
enter
calibrate sample
disable 
enter
start time delay
enter
enable pin
no 
enter
sample upon disable
no 
enter
sample upon enable
no 
enter
reset, sample interval
no 
enter
inhibit countdown
no 
enter
event mark
no 
enter
purge counts
yes 
enter
pre sample
150 
enter
post sample
922 
enter
tubing life
enter 
enter
reset pump counter
no 
enter
pump count to warning
500,000 
enter
program lock
disable 
enter
sampler ID
ID number 
enter
run diagnostic
run 
enter
exit configuration
exit 
enter
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11. ISCO programming

Option Settings Button 
to press
Basic
paced sampling flow enter
sample every pulse 1 enter
multiplex samples no enter
sample volume 800 enter
suction head 25 enter
enter start time no enter
Extended
load program none enter
save current program none enter
flow mode sampling enter enter
take sample at start time no enter
take sample at time switch no enter
non uniform time no enter
sampling stop/resume enable enter
sample at stop no enter
sample at resume no enter


11.1 Recording Sample Collection Date and Time

Prior to servicing the ISCO sampler and collecting filled bottles, it is necessary to record the date and time each sample bottle was filled by the ISCO. These data can be extracted from the ISCO and transcribed to the COC form in the field by following the instructions provided on page 134 of the ISCO 3700 Instruction Manual.
see in Acrobat format
Option Display Status
11.1.1 Press display status to view the results of the sampling program. DONE 24 SAMPLES 
16 -JUN-91
11.1.2 select "REVIEW." [REVIEW PRINT] PROGRAM 
 INFORMATION
11.1.3 select "RESULTS." REVIEW PROGRAM [NO, 
 SETTINGS, RESULTS]
11.1.4 This display reports the start time and date of the program. Press enter/program to advance to the next display. PROGRAM STARTED AT 
 5:30 19-JUN-91
11.1.5 This display reports the nominal sample volume. Press enter/program to advance to the next display. 200 ml SAMPLES 
11.1.6 This display reports the bottle number(s) for each sample event. It also reports the source of the event; in this case, the sample was taken at the start time. Press enter/program to advance to the next display SAMPLE: 1, BOTTLE: 1 
SOURCE: START 
TIME: 5:30 19-JUN-91
11.1.7 This display reports the initiation time of the sample and the number of pump counts to liquid detection in the sample delivery cycle. These values indicate changes in the sampling conditions - head changes, for example. 
Press enter/program to advance to the next display
TIME: 5:30 19-JUN-91 
 I COUNTS: 280
11.1.8 Press enter/program to continue to review the information for the remaining sample events.
11.1.9 Press enter/program to return to the "REVIEW PROGRAM" display. PROGRAM FINISHED AT 
 12:00  20-JUN-91
11.1.10 Select "NO" to return to standby. REVIEW PROGRAM [NO 
 SETTINGS, RESULTS]
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12. ISCO SERVICE AND RESETS

12.1 When the resets are working do:
12.1.1 When water is covering the suction intake 12.1.2 When water is not covering the suction intake 12.2 If resets are not working then:
12.2.1 When water is not covering the suction intake 12.2.2 When water is covering the suction intake Top of page 
13. Sample transfer to ranch lab
13.1   At time of sample collection the bottles/bags are immediately capped.

13.2   Samples are transported to the ranch lab while the bottles are still in the ISCO autosampler tray.  The clean bottles from extra tray of bottles/bags is exchanged for the field tray at each ISCO unit. Clean bottles are rotated to get the first clean bag to position number 2.

13.3   Confirm that the first bottle of the clean replacement tray contains an equipment blank (analyte-free water with preservative and with bottle cap removed).

13.4   The field notes should reflect the any problems with the sample bottles, including empty bottles or low sample volumes (less than 800 mL).  For samplers where low sample volumes are noted repeatedly, the ISCO sample delivery system (pump, hose, timer, etc.) should be inspected and tested to resolve the problem.

13.5   In the lab samples are thoroughly mixed by inverting three times, transferred to the pre-cleaned 250 ml bottles, labeled, and stored at 4o C.

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14. Field data book

14.1   Field data sheets must be completed at the time and location of each site inspection, bottle tray or battery change, and data download.

14.2   The following supplemental information is recorded in the Field Data Book :

14.3  Information from the field data sheets is entered to the online data sheet submission forms (datalogger and/or ISCO) within 24 hours of data collection.

14.4  Significant problems, comments, and abnormalities should be noted in the field data book.

14.5  The field data sheets and copies of field book entries are stored in the project files at the ranch office.

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15. Sample custody

15.1  All shipments are accompanied by Chain Of Custody Form . These forms identify contents of the sample shipment. The information to be entered on the chain of custody form includes: 15.2  Samples are transported to the analytical laboratory at 4oC covered with ice in sealed coolers.

15.3   Samples are submitted to the analytical laboratory within two weeks of the day the ISCO was serviced.

15.4   The field sampler is personally responsible for the care and custody of the samples collected until they are transferred to the analytical Lab.

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16. Chain of custody forms

16.1  Examples of Chain of Custody (COC) forms:
 
Sample Type
ISCO 
 Filtered Grab Samples
Preserved Grab Samples
  Split Samples
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17. Grab sampling procedure

17.1.1  Technicians should view and study the SFWMD water sampling training video prior to first attempt at sample collection.  Technicians should review the video quarterly to confirm adherence to proper procedures.

17.1.2  Short holding time parameter samples  are collected manually as grab samples on a weekly basis depending of flow at tray replacement time. These samples should be delivered to the receiving laboratory within 24 hours of collection.

17.2  Equipment.

17.3  Collecting Procedure 17.4  Filtering (for ortho-P and NOx samples). 17.5  Preservation (for TKN, NH3 and TP grab samples) 17.6  QA/QC Samples. All QC samples must remain with the sample set until they have been received by the laboratory. 17.7  Sample Custody Top of page

18. Documentation

18.1  All records and documentation required to trace a sample from point of origin through delivering to testing Lab.

18.2  These records must include:

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19. Physical parameter measurement

Parameter Field SOP (html) Field SOP (pdf) Instrument Model Reference SOP (html) Reference SOP (pdf)
19.1 pH ph.html ph.pdf pHTestr 2 AOAC Method #973.41 aoac-ph.pdf
19.2 Dissolved Oxygen do.html do.pdf YSI 55 USGS Method #6.2 usgs-do.pdf
19.3 Conductivity cond.html cond.pdf TDSTestrs 3 AOAC Method #973.40 aoac-cond.pdf
19.4 Temperature temp.html temp.pdf YSI 55 USGS Method #6.1 usgs-temp.pdf
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20. Definitions

20.1 Field cleaned equipment blanks

Blanks of analyte-free water that are prepared on-site by filling appropriate sample containers with the water, adding appropriate preservatives, sealing the containers, and completing the appropriate documentation. These blanks should be prepared during the middle to end of a sampling event by filling sample containers with water from the equipment decontamination water transport containers. They are to be treated, stored, transported, and analyzed in the same manner as the sample group for which it was intended. These blanks may be submitted for all water parameter groups. Field blanks are containers of Millipore DI water that are filled at the sampling station, then labeled, packaged, sealed and shipped to the laboratory like other samples. They check for contamination in the laboratory and for cross contamination during the collection and shipment of the samples. The laboratory requires one field blank for each set of sampling.

20.2 Equipment blanks

Equipment blanks of analyte-free water are prepared on-site by pouring the equipment decontamination water through decontaminated field equipment. Appropriate sample containers, for each analyte group must be used, preservatives added, if required, and appropriate documentation must be completed.  At least one equipment blank is required for each water sample set, and it must be collected at the beginning of the sampling episode.

20.3 Field duplicate

Samples that have been collected at the same time and from the same source. This requires two distinct sampling operations using the appropriate equipment and procedures. The analytical results from duplicates are used to determine the precision of a system.  Duplicates are submitted to be analyzed as separate samples (analyst does not know they are duplicates).

20.4 Split samples

Replicates of the same sample that are given to two independent laboratories for analysis. This involve one single sampling/ filtering operation from which the sample is divided between two laboratory submission containers

20.5 Sample

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.

20.6 Sample set

The basic unit for analytical quality control. The analytical set is defined as samples which 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.
 

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