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Standard
Operating Procedures
for DEP 319 Project at MAERC |
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.
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.
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.
6.3 The labels
must be affixed to the sample containers and look similar to the label
below.
Filtered:
|
Preserved:
|
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.8.2 Reused Containers8.1.2 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.
Tubing is used for 3 months at and then discarded. Do not reuse tubing.
New tubing is pre cleaned as follows:
| 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 |
3
|
enter |
| enter head manually |
no
|
enter |
| retry up to 1 times |
yes
|
enter |
| programming mode |
basic
|
enter |
| calibrate sample |
disable
|
enter |
| start time delay |
0
|
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 |
| 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 |
| 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] |
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.
14.2 The following supplemental information is recorded in the Field Data Book :
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.
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.
| Sample Type |
| ISCO |
| Filtered Grab Samples |
| Preserved Grab Samples |
| Split Samples |
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.
| Samples | Code | When are they collected? |
| Pre cleaned equipment blanks | (EB) | one per set of ISCO or grab samples |
| Field duplicates (-FD1 & -FD2) | (FD) | one per every ten samples |
| Field cleaned equipment blanks | (FB) | one per set of grab samples |
| Split samples (-SS1 & -SS2) | (SS) | one per ten samples |
18.2 These records must include:
| 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 |
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.
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.
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).
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.