132 North Lee Street, LaBelle, FL, 33935
tel: 863-674-5727, fax: 561-828-8458
www.SouthernDataStream.com
SOP compiled by: Anneline Petrequin
SOP FOR LAB SEDIMENT GRAIN-SIZE ANALYSES
1. List of the material
The lab equipment and apparatus:
One VWR Model 1305U Oven, 19" x 17" x 12"
One Fridge
One Mechanical Balance
One Adam Digital Scale, readings to 0.1g, max 3000g
One Sieve checker for a height 8” standard stainless steel sieves kit
Nest of height sieves, standard USGS Nb: 5; 10; 18; 35; 60; 120; 170; 200; (+ two sieves
with a finer mesh 1”; 3/8”; 270; 500)
One oven thermometer
One Computer
Pyrex evaporating dishes
A permanent marker
One Graduated baker
Magnifying glass
One nylon brush
Nylon scrub pads
One Stirring Rod
Freezing containers
One wash bottle
White Glazed Paper
Logbooks for the equipment
Long observation dish
One big plastic bowl
A white plastic basin
A flexible scale
cotton towels
Water bottles
Boots
Plastic spoons
Chemical:
Sodium Hexametaphosphate, 1 bottle of 500g, solid granular for preparation of solution
(present bottle, concentration in Assay (P2O5), 66.5% - 68%)
Protecting clothes and accessories
Nitrile Gloves
‘oven gloves’
Dust Masks
Dust Respirator
Laboratory coat
Splash googles
Safety kit:
Soap
Emollient
2. General Procedure for Lab work
2.1. logbooks
The use of the oven, the fridge and the computer must be kept into logbooks:
2.1.1. Oven Logbook:
Record:
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The start date and time of each use of the oven with the planned duration of the
heating process
The number and references of the samples placed into the oven
The temperature of the oven
The stop date and time of the heating process
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Cleaning dates
2.1.2
Fridge Logbook:
Record:
- The temperature
- The storage date of the sample
- The reference of each sample
- Cleaning dates
2.1.3. Computer Logbook:
Record:
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The references of the computer plots and reports done for each sample
2.1.4. Chemical use Logbook:
Record:
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The date of purchase of each chemical bottle, the name of the provider. Store a
photocopy of the Certificate of Analysis, and Material Safety Data Sheet into the
portfolio. The weight of the product and its concentration.
The date and time, interns name for each use
The weight used of each use
2.2. Safety
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Wear gloves for each manipulation of hot surfaces.
Wear a dust mask and a dust respirator when handling the dry sieving.
Store the sodium hexametaphosphate container in the fridge. Keep it away from
incompatible such as oxiding agents, acids.
Sodium hexamethaphosphate may have potential effects on health, they are:
- skin contact: may cause skin irritation, slightly hazardous
- eyes: causes eye irritation
- inhalation: may cause respiratory tract irritation. Symptoms may include
coughing and shortness of breath.
- ingestion: Phosphates are slowly and incompletely absorbed when ingested,
and seldom result in systemic effects. May cause gastrointestinal tract irritation with
nausea, vomiting, and diarrhea. May affect behavior/central nervous system/peripheral
nervous system (somnolence, convulsions, lethargy, flaccid paralysis), urinary system
(kidney- renal failure, acute tubular necrosis), may cause heart disturbances (fall in blood
pressure, slow pulse) and blood chemistry effects (reduction of serum level of calcium).
The toxicity of the phosphates is because of their ability to sequester calcium. Tetany
may also occur as a result of reduction in serum level of ionic calcium.
Please, follow the safety precaution:
- Do not ingest. Do not breathe dust. Avoid contact with eyes.
- Wear gloves when handling the product and the dilution
- Wear splash goggles when making the solution and handling it
- Wear a dust mask and a dust respirator when handling
- Wear long sleeves clothes and the laboratory coat
- Always keep bottles of cold water in the fridge.
- AVOID ANY SPILL. If spill occurs rinse with water and evacuate the flow
into the sanitary system.
- Wear boots (in case of large spill)
2.3. First Aid Measures
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Eye Contact: Check for and remove any contact lenses. In case of contact,
immediately flush eyes with plenty of water for at least 15 minutes. Cold water
may be used. Get medical attention.
Skin Contact: Wash with soap and water. Cover the irritated skin with an
emollient. Get medical attention if irritation develops. Cold water may be used.
Inhalation: If inhalator, remove to fresh air. If not breathing, give artificial
respiration. If breathing is difficult, give oxygen. Get medical attention.
Ingestion: Do NOT induce vomiting unless directed to do so by medical
personnel. Never give anything by mouth to an unconscious person. Loosen tight
clothing such as collar, tie, belt or waistband. Get medical attention if symptoms
appear. Seek medical advice immediately.
EMERGENCY INFORMATION:
- Phone given by the provider (Spectrum) in case of emergency:
CHEMTREC 1 - 800 - 424 - 9300
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There is a medical office close to the lab: If medical assistance is needed in
the evening or in the week-end, the health Department of the Hendry
County advised to go to the physician who may then decide if it’s needed to
go to Moore Haven or Leehigh Acres emergency center.
Dr Caignet, 50 Belmont Street, Labelle, FL 33935, 863 - 675 - 7272
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Police / Fire / Medical Emergencies: Dial 911. Dial 211 for information.
2.4.Cleanliness
Clean the cold oven with a humid scrub after each use.
Clean the fridge monthly with bleach.
Clean tables and dishes after each use, for each sample. Use cotton towel or paper towel
for drying.
Clean the sieves after each use. Use the magnifying glass to check the finest meshes
before using them and just after having cleaned them.
3. Grain-size analysis
Follow the steps bellow:
3.1. Samples Preparation
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Note the field sample reference into the analysis logbook
Prepare the sample analysis summary spreadsheet: indicate the field trip date and
time, the lab analysis date and time, your name, and the reference number of the
sample.
Prepare two freezing containers and write on them the reference number of the
sample with the permanent pen
Remove the sediment from its tube and display it onto a long dish on the
manipulating table
Observe the sediment carrot. Measure its lengths and write it into the sample
summary spreadsheet. Observe it and note down each relevant geological
information: geological layer change, change into the visible grain size
constitution, presence of big size organic constituents. Measure the depth of any
visible change. Enter the results into the computer Sample datasheet and make a
drawing as bellow.1
Boring Log Description
1
See Soil Description Summary in Appendix
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Place the sample into the big plastic bowl and mix it softly
Fill one freezing container with the mixture and store it in the fridge for further
reference or for repeating the grain size analysis for accuracy test. Write ‘wet’ on
the container.
Note into the reference of the sample into the fridge log book.
Remove the sediment from the table and through it away
Clean the table with a pad
Store the tube outside for cleaning it after the analysis
3.2.Wet Weighting
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Prepare a sticky label with the reference number of the sample and cling it to an
evaporating dish
Place a dry and empty evaporating dish on the numerical scale.
Note down the dish weight, it may be helpful in case of error. Tare.
Fill the dish with the wet sediment and read results
Note the results into the sample summary spreadsheet and in the analysis logbook
Place the sample on the oven table or counter
3.3.1st Evaporation
The water-sediment mixture is poured into the evaporating dish, and the sample is
dried and weighed.
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Prepare and weight as many samples as disposable in the oven.
Evaporating dishes are aligned sequentially on the oven table.
- Compare sample data on the worksheet with data on the field notebook and with
the bottle tare value.
- Check the dish-identification number against the container-identification number
on the sample to ensure agreement.
- Place the evaporating dishes in the oven.
- To avoid any loss of sediment from boiling, the dishes are dried at 85 to 95°C for
24 hours.
- Note down the date and start time of the heating process with the samples numbers
in the oven logbook and the sample summary spreadsheet.
3.4.Dry Weighting
Samples are dried.
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Wear gloves and a dust mask before opening the oven. Take the samples out
from the oven.
Place the sample on the laboratory table.
Make the scale on zero and weight a dish. Tare.
Carefully transfer the dry sediment (use a sieve brush) from the evaporating dish
to the weighting dish.
Empty the evaporating dish; clean it with the wash bottle. Dry it carefully with a
cotton towel
Weight the dry evaporating dish
Make the difference of the weight of the full dish with the empty dish. Note the
dry weight of the sediment into the sample summary spreadsheet and in the
analysis logbook.
3.5. Preparation of the Sodium Hexametaphosphate solution
We want a 20 g.L-1 solution. Prepare the solution if the solution bottle is empty.
- Wear lab coat, appropriate clothes, boots, splash goggles, dust respirator and
gloves. Have a cold water bottle near you in case of skin/eye contact.
- Calculate the weight of sodium hexametaphosphate needed for dilution using the
Certificate of Analysis of the chemical, placed in the chemical logbook, to know the
sodium concentration.
- Prepare a clean plastic bottle and a clean weighting dish
- Dispose the chemical containers, the bottle, the weighting dish, the graduated
backer, the stirring rod and a plastic spoon on the desk close to the sink.
- Weight the dish. Tare. Place the sodium hexametaphosphate granular in the
weighting dish with the plastic spoon. Fill up to the wanted weight. Close the chemical
container immediately after use.
- Measure the needed quantity of water with the measuring backer.
- Add little water in the measuring backer and mix gently the granular with the
stirring rod till dilution. If necessary repeat the operation till dilution is complete.
- Carefully transfer the solution into the bottle. Rinse softly the dish with the wash
bottle and direct the flow into the bottle.
- Transfer the water from the backer into the bottle, little by little in several steps.
For each step, close the bottle and stir gently to homogenize.
Finally rinse with plenty waters all the apparatus in the sink. Dry with paper
towels. Wash the gloves, the sink and the desk.
Ensure the PH of the solution is between 8 and 9.
3.6.Wet Sieving
Wet Sieving is commonly use to separate the Sand and fine fractions of a sample. The
goal is to determine the amount of material that is less than or greater than sand size.
The term fine fraction refers to particles that pass through a 0.062-mm mesh sieve and
sand fraction refers to particles large enough to be retained on a sieve. We use the same
method to separate the silt clay fraction with a sieve diameter of 0.00075mm as requested
by the Department of Environmental Protection (DEP).
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Break up gently any clumps in the material using the stirring rod. Because this
may generate dust, you should wear a dust mask.
Disperse the sand sample in sodium hexametaphosphate (this helps to separate the
fine particles): Add 250ml of hexametaphosphate solution (20g per liter), then 50
ml of hot distilled water and stir for 20 minutes.
Using a 0.075 mm mesh sieve and a white plastic basin, puddle the sediment
sample in the sieve immersed in water/sodium hexametaphosphate in the basin.
The coarser fraction will remain on the surface of the sieve and the silt/clay
fraction will pass through, remaining in suspension in the basin.
Wash periodically the sample onto the sieve with the water. The screen is rinsed
with a gentle stream of water (gravity flow) to wash the particles through and into
the assigned dish and stir gently the immersed sieve.
Finally, rinse until no visible fines pass through the screen.
Once sieving is complete, dry the coarser fraction on the surface of the sieve by
placing the sieve and sediment in a drying oven at 80-100ºC for 24 hrs. Note the
drying starting and end dates and time in the oven logbook and in the sample
summary spreadsheet. Don’t forget to wear gloves, dust mask and dust
respirator before opening the oven.
After drying, carefully transfer the dried sediment fraction from the sieve (using a
sieve brush) to a weighting dish to obtain dry weight of sand fraction. The weight
of the silt/clay fraction is obtained by difference.
Note the weight of the silt/clay fraction in the sample summary spreadsheet and in
the analysis logbook
3.7. Dry Sieving
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Transfer carefully the dried and weighed sediment to the uppermost (coarsest) of
a stacked series of graded sand sieves, taking care to gently brush all of the
material from the container using a fine sieve brush. A 75 µm sieve will be at the
bottom of the stack of sieves and care should be taken to use a pan below this
finest sieve to catch the last of any fine material which may still pass.
Mount carefully the sieve column to the automatic sieve shaker for a period 12-15
minutes.
If necessary, use a sieve brush to move material about on the sieve. This sieve
may then be detached and any doubts about the finality of the sieving may be
checked by agitating and tapping over a sheet of white glazed paper. Any material
passing through should be immediately transferred to the next finer sieve.
If the sediment is at all damp, particles will stick together. If possible, collect the
sample back together and replace it in the 70°C oven to dry properly, or freeze
until the next occasion for practical work. Otherwise, use the method in step 3 to
encourage particles to pass through the sieves.
When the finality of sieving has been checked, the material on each should be
emptied on to a sheet of glazed paper and any grains lodged in the sieve should be
removed with a sieve brush.
Weight a dish
The fraction can then be transferred to the same dish for weighing.
Repeat the weighting for each fraction
Note down the results of the analysis in the sample summary spreadsheet and in
the analysis logbook.
Clean the sieves with water and a brush. The finer sieve meshes might be clogged
with sediment. Periodically inspecting the sieve with the magnifying glass is
helpful.
3.8. Waste storage
The ‘Florida handbook for small quantity waste generator’ and the ‘40 CFR part 261 –
Identification and listing of hazardous waste’ are used as reference.
Our waste generator Category: Conditionally Exempt Small Quantity
Generators (CESQG) -100 kg/month (220 pounds) or less.
Notifying the Department of Environmental Protection (DEP) of our
waste production id not necessary.
As a Conditionnally Exempt Small Quantity Generator, we are allowed
to store on-site up to 1,000 kilograms (2,200 pounds.) of hazardous waste
with no accumulation time limit.
Procedure:
- Place the waste into containers and maintain them close.
- Record of the first date of accumulation, and the amount, type and number of
containers of each hazardous waste generated
- Mark each container with the date that storage began and with the words
"Hazardous Waste.
- Inspect containers at least weekly to check for leaks and signs of corrosion.
3.9.Analysis of the Results
Calculate fraction weight percentage and create a cumulative chart with a logarithmical
scale. The software Excel possesses all the necessary features. Use the sample summary
spreadsheet.
Logarithmic Grain-Size Cumulative Chart
APPENDIX
- Soil Classification, literature :Black file “Soil
information ”
- Soil Description procedure For SouthWest Florida
:Black file “Soil information ”
- Sieve care and cleaning.
Sieve care and cleaning
Test sieves, like any other piece of analytical laboratory equipment require regular
car to maintain their performance standards. Sieves should be kept clean and dry at all
times.
To clean-up, brushing of the mesh, sizes 125 and coarser is recommended. For
best results, use a nylon bristle paint brush (or toothbrush). The sieve openings should be
brushed from the underside only with a gentle circular motion.
Vigorous brushing will distort the sieve openings and reduce the effective life of the
sieve.
Particles lodged in the sieve never should be removed with a sharp object.
With proper care and cleaning procedure, any test with sieves should provide
many years of consistent service.