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Environmental Management Consolidated Business Center
Ash Fall Project
Dry Sieve/Sedigraph Process Procedure: AFP-SDG-01
Revision 0, 02/13/17
Dry Sieve/Sedigraph Process
Revision: 0
Effective Date is 3 days after the date of approval
Prepared By: Signature on File 02/07/17
Robert Hasson Date
Ash Fall Project QA Lead
Approved By: Signature on File 02/07/17
John April Date
ORP Ash Fall Project Engineer
Concurrence: Signature on File 02/10/17
Ken Armstrong Date
EMCBC Associate Deputy Director
Environmental Management Consolidated Business Center
Ash Fall Project
Dry Sieve/Sedigraph Process Procedure: AFP-SDG-01
Revision 0, 02/13/17
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1.0 PURPOSE
This procedure establishes the process for the measurement of the particle size distribution
of samples for the Ash Fall Project using the Dry Sieve/Sedigraph technique. Further, the
procedure describes the technique that will be used to prepare a subsample for analysis by
the Laser Diffraction method (Procedure AFP-LAS-01, Laser Diffraction Process).
2.0 SCOPE
This procedure is used for the samples submitted to the Ash Fall Project – Cascades
Volcano Observatory Sediment Laboratory (CVO) personnel for the Department of Energy
Environmental Management Consolidated Business Center (EMCBC) Ash Fall Project
supporting the Office of River Protection Program.
3.0 APPLICABILITY
This procedure applies to Ash Fall Project CVO personnel who analyze samples submitted
to the CVO Sediment Lab for the Ash Fall Project.
4.0 REQUIREMENTS and REFERENCES
4.1 Requirements
4.1.1 EM-QA-001, EM Quality Assurance Program (QAP)
4.1.2 ASME NQA-1-2008/2009a, Quality Assurance Requirements for Nuclear
Facility Applications
4.2 References
4.2.1 AFP-QAPP-01, Quality Assurance Project Plan (QAPP)
4.2.2 AFP-AP-03, Data Control
4.2.3 AFP-AP-05, Control of Electronic Management of Information
4.2.4 AFP-AP-06, Software Control
4.2.5 AFP-AP-09, Software Problem Reporting and Corrective Action
4.2.6 AFP-AP-18, Sample Control
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Dry Sieve/Sedigraph Process Procedure: AFP-SDG-01
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4.2.7 AFP-AP-19, Corrective Actions
4.2.8 AFP-AP-20, Quality Assurance Records
4.2.9 AFP-LAS-01, Laser Diffraction Process
4.2.10 Guy, 1969. Laboratory Theory and Methods for Sediment Analysis. USGS
TWRI Book 5 C1.
4.2.11 ASTM 2014. Test Sieving Methods, 5th Edition: Guidelines for Establishing
Sieve Analysis Procedures. Trent Smith, editor. ASTM Stock# MNL32-
5TH.
5.0 DEFINITIONS and ACRONYMS
None.
6.0 RESPONSIBILITIES
6.1 Ash Fall Project – CVO Sediment Laboratory Personnel
6.1.1 Responsible for maintaining sample control in the laboratory in compliance
with AFP-AP-18, Sample Control.
6.1.2 Responsible for conducting analysis in compliance with the analytical
procedures in this document.
6.1.3 Responsible for submitting results of the analysis to the Ash Fall Project –
CVO Sediment Laboratory Lead.
6.1.4 Responsible for submitting relevant Quality Assurance (QA) documentation
to Ash Fall Project – CVO Sediment Laboratory Lead.
6.2 Ash Fall Project – CVO Sediment Laboratory Lead
6.2.1 Responsible for reviewing laboratory results when they are received from
the Ash Fall Project – CVO Sediment Laboratory personnel.
6.2.2 Responsible for compliance with applicable procedures for physical records,
electronic records, QA records, and software for information received from
the Ash Fall Project – CVO Sediment Laboratory personnel.
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Dry Sieve/Sedigraph Process Procedure: AFP-SDG-01
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6.3 Ash Fall Project QA Lead
6.3.1 Responsible for the oversight of the sample controls and Sieve/Sediment
process.
7.0 GENERAL INFORMATION
The samples analyzed with this technique must have at least 3 grams of material finer than
0.063mm. Additionally, the samples must contain at least 10 grams of material between
4mm and 0.063mm sieve diameter.
8.0 PROCEDURE
8.1 Sample Receiving, Control, and Storage
8.1.1 The samples shall be provided to the Ash Fall Project – CVO Sediment
Laboratory personnel by the Ash Fall Project staff using the Chain of
Custody Form, AFP-AP-16, Sample Control. If the samples are shipped to
the Ash Fall Project – CVO Sediment Laboratory personnel, the shipping
labels will be retained along with the Chain of Custody Form and submitted
to the Ash Fall Project – CVO Sediment Laboratory Lead at the completion
of the analysis.
8.1.2 Sample metadata will be recorded in the Sediment Laboratory
Environmental Database System (SLEDS), the Laboratory Information
Management System (LIMS) for the CVO Sediment Laboratory. SLEDS
will create a laboratory-specific unique sample identifier that will be
recorded on the sample container using a permanent marker or self-adhesive
label.
8.1.3 Samples will be stored in their original containers in the CVO Sediment
Laboratory until the analysis is performed. If the samples have perceptible
moisture when received, they will be dried in a convection oven set to 65°C
in their original containers until all perceptible moisture has evaporated.
The oven can be held at any temperature below 100°C.
8.2 Equipment Preparation
8.2.1 Balance
8.2.1.1 The Mettler Toledo SB32001 balance that will be used in the dry
sieve analysis will be verified to 0.1 gram using ASTM Class 1
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weights. Documentation of the balance verifications for the
project will be provided to the Ash Fall Project – CVO Sediment
Laboratory Lead as part of the QA records collected for the project.
8.2.2 Sieves
8.2.2.1 Before work on the sample batch begins, the working sieves used
for project samples will be checked against a set of ASTM-
certified sieves following the guidance in ASTM MNL32-5TH
.
Records of the verification test results for the working sieve set
will be provided to the Ash Fall Project – CVO Sediment
Laboratory Lead as part of the QA records collected for the project.
8.2.2.2 Before analysis of each sample, the working sieves will be visually
inspected by the analyst. If more than approximately 20% of the
openings are occluded after routine cleaning, the working sieves
will be cleaned in the ultrasonic bath. If more than 20% of the
openings remain occluded after ultrasonic cleaning, the working
sieve will be replaced, and the new set of working sieves checked
against the ASTM-certified sieves.
8.2.3 Sedigraph
8.2.3.1 Before each batch of sedigraph samples, the accuracy of the
sedigraph will be verified using Coarse Garnet Reference Material
supplied by Micromeritics. The Coarse Garnet verification process
recommended by Micromeritics will be followed. The check is
performed against the d10, d50, and d90 values provided as
recommended. The sedigraph must produce a value in the ranges
specified. Records of verification checks on Coarse Garnet will be
provided to the Ash Fall Project – CVO Sediment Laboratory Lead
as part of the QA records collected for the project.
8.2.3.2 Before each batch of sedigraph samples, an instrument baseline
will be recorded to document the background x-ray absorption of
the solution of dispersant and de-ionized water (DI) in the
instrument. Records of the baseline (blank) measurements will be
documented as part of the QA records for the project.
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Dry Sieve/Sedigraph Process Procedure: AFP-SDG-01
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8.3 Dry Sieving Gravels
8.3.1 Record the sample identification, analysis date, and analyst initials on the
Sieve Analysis Form (Attachment A).
8.3.2 Personnel should wear a dust mask. Place a pan on the balance and tare the
balance. Transfer the entire sample to the pan, and record its net weight to
the 0.1 gram on the Sieve Analysis Form. Save the original sample
container.
8.3.3 If requested by Ash Fall Project – CVO Sediment Laboratory Lead, gently
break up any clumps that may be present in the sample using a mortar and a
rubber-tipped pestle.
8.3.4 Pass the entire sample through a 4mm sieve. Record the mass retained on
the sieve as the gravel weight, and the mass passing the sieve as the sand
weight. Weights are recorded to the nearest 0.1 gram on the Sieve Analysis
Form.
8.3.5 If gravels are present, hand sieve the material coarser than 4mm and record
the weights retained on each sieve on the Sieve Analysis Form.
8.3.6 On one in ten samples, recombine the gravels, re-sieve, and record the
weights on the Sieve Analysis Form.
8.3.7 After gravel measurements are complete, place the gravels back in the
original sample container.
8.4 Subsampling Sand/Fine Fraction
8.4.1 The sand/fine fraction should be split into three representative subsamples.
One subsample will be delivered to other Ash Fall Project – CVO Sediment
Laboratory personnel to perform a laser diffraction analysis on the material
finer than 1.0mm (reference AFP-LAS-01, Laser Diffraction Process). The
second subsample will be used for the sieve/sedigraph analysis outlined in
the remainder of this procedure. The third subsample will be bagged,
labelled, and placed back in the original sample container. The third
subsample will only be retained if there is sufficient material present in the
sample. The purpose of the third subsample is to preserve an intact
subsample for physical archiving.
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8.4.2 A fourth subsample will be collected from up to one in ten samples based on
the availability of material. The fourth subsample will be used as a replicate
to assess the reproducibility of the sieve/sedigraph analysis. The
sieve/sedigraph analysis reproducibility is good when all reported values
agree to within 3 percent finer. The results are acceptable if all reported
values agree to within 5 percent finer. If values for the replicates agree to
within 5 percent finer, the results will have comments added noting that the
reproducibility is lower than the target. If values for the replicates do not
agree to within 5 percent finer, the procedure will be evaluated for any
potential errors, and the analysis will be re-run if physically possible.
8.4.3 The subsamples are created by passing the sand/fine fraction through the
vane splitter in the CVO Sediment Laboratory Ro-tap room. Pour the
sand/fines through the vanes with an even back-and-forth motion directly
onto the center line of the splitter.
8.4.4 Split the sand/fines as many times as required to produce an appropriate size
subsample for sieve analysis. The subsample should be large enough to
produce a detectable mass on each sieve without overloading any single
sieve (ASTM 2014, p.21). Record the subsample (“split”) weight to the
nearest 0.1 gram and the number of splits on the Sieve Analysis Form.
8.4.5 Continue splitting the sand/fine fraction until a mass of 5 to 10 grams is
achieved. Transcribe sample identifiers, metadata, and subsample mass onto
a plastic bag with permanent marker. Place the entire subsample in the
plastic bag and seal. Transfer control of the subsample to the Ash Fall
Project – CVO Sediment Laboratory personnel responsible for the laser
diffraction analysis.
8.4.6 Retain the remaining sand/fine fraction in a labelled container until sieve
analysis is complete. The third subsample for archiving will be taken from
this material when the sieve analysis is complete.
8.5 Dry Sieving Sand/Fine Fraction
8.5.1 Construct the stack of working sieves at phi intervals from 2.00mm to
0.063mm, plus the catch pan.
8.5.2 Place the stack on the Ro-tap machine. Introduce the first subsample onto
the top sieve. Cover the stack, lower the arm, set the Ro-tap machine to 10
minutes, and lower the cover. The Ro-tap will automatically turn off when
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Dry Sieve/Sedigraph Process Procedure: AFP-SDG-01
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the timer expires. Sieve duration from 8 to 12 minutes is acceptable.
8.5.3 When the Ro-tap is finished, take the sieve stack out of the machine.
Transfer the material on the sieve to a tared container. Invert the sieve over
the container and brush the underside to dislodge any particles that may be
held in the openings. Record the net weight retained on each sieve on the
Sieve Analysis Form to the neared 0.1 gram. Record the net weight of fines
in the catch pan.
8.6 Preparing for Sedigraph Analysis
8.6.1 The sedigraph requires 1.5 to 3 grams of fine (<0.063mm) material for a
reliable analysis. If sufficient mass for a sedigraph analysis is present in the
catch pan, transfer the fines from the catch pan to a sedigraph cup. The
sedigraph cup must be labelled with the sample identifier using a self-
adhesive label.
8.6.2 If insufficient mass is present in the catch pan, fines can be taken from any
remaining material retained in step 8.4.4. The remaining material can be
hand sieved at 0.063mm until sufficient fines mass is recovered. If
sufficient material is present, split the remaining material and hand sieve the
fines from a subsample. This will preserve an intact subsample of the
sand/fine fraction for archiving.
8.6.3 Record the dry fines mass in the sedigraph cup to the nearest 0.1 gram in the
comments section of the Sieve Analysis Form.
8.7 Sample Preservation
8.7.1 If an intact subsample has been retained in steps 8.4.4 or 8.6.2, it will be
transferred to a clearly labelled plastic bag. The bag will be labelled with
the sample identifiers, sample metadata, the words “INTACT SPLIT
<4mm”, the date, the analyst name, and the mass of the material in the bag.
The bag will be sealed and placed in the original sample container along
with the gravels. When the batch is complete, the Chain of Custody
procedure AFP-AP-18, Sample Control will be used to transfer control of
the preserved samples to the Ash Fall Project – CVO Sediment Laboratory
Lead.
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8.8 Sedigraph Analysis
8.8.1 Add 50-80ml of DI to the sedigraph cup with the dry fines. Add 1ml of
dispersing agent to the cup and stir. The dispersing agent is a buffered
sodium hexametaphosphate solution prepared according to the instructions
in Guy (1969, p.29). If requested by the Ash Fall Project – CVO Sediment
Laboratory Lead or other investigators, further disperse the suspension by
sonicating for 30 seconds at a 90% duty cycle with the sonic probe.
8.8.2 Create a new sample information file on the sedigraph. Add the analyst
name and sample identifiers in the appropriate fields. Use the USGS
Standard Silt-Clay Analysis default file to set up the sedigraph run.
8.8.3 Start the analysis routine on the sedigraph. When prompted, add the sample
to the sedigraph mixing chamber. The first step in a sedigraph analysis is a
‘full scale’ scan of the sample, measuring the total X-ray occlusion. The full
scale scan must be between 15% and 30%. If the full scale scan value is too
high, the material in the mixing chamber can be diluted to bring the value
into the correct range.
8.8.4 The standard sedigraph routine performs two runs on each sample to assess
the repeatability of the analysis. After both runs, the average cumulative
percent finer at each target phi size is reported. Print the standard sedigraph
report for each sample. A copy of the printed report will be submitted to the
Ash Fall Project – CVO Sediment Laboratory Lead along with the analytical
results.
8.9 Data Analysis, Computations, and Reporting
8.9.1 Create a new tab for each sample and replicate in the project spreadsheet by
copying the Sieve-Sedigraph Template. Re-name the tab with the sample
identifier. Fill in the required data from the Sieve Analysis Form and the
sedigraph report. The spreadsheet will compute the resulting percent finer
at each phi size according to the following calculations.
8.9.1.1 The sample net weight is the sum of the gravel weight and the sand
weight recorded on the Sieve Analysis Form.
8.9.1.2 For sieve sizes 4mm and larger, add the masses retained on gravel
sized sieves finer than the target size plus the sand weight. Divide
the mass finer by the total sample weight and multiply by 100 to
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compute the percent finer.
8.9.1.3 For sieve sizes from 2mm to 0.063mm, the retained masses must
be scaled to the whole sample mass. The scaling factor is the ratio
of the sand weight to the split weight. Multiply each mass times
the scaling factor, and compute the percent finer based on the
scaled masses as above.
8.9.1.4 For sizes below 0.063mm, multiply the cumulative percent finer
from the sedigraph report by the 0.063mm percent finer from the
sieve analysis to compute the overall percent finer for each
reported size in the silt/clay fraction.
8.9.2 Transcribe the same data into the SLEDS Dish Assignment Form for the
sample, including any replicates. Use SLEDS to produce a Size Distribution
report for each sample and replicate. Check the values produced by SLEDS
against the values computed in the spreadsheet. The values must match to
the 0.1 percent finer. SLEDS is used to verify the computations and data
entry into the spreadsheet. The printed Size Distribution reports will be
submitted to the Ash Fall Project – CVO Sediment Laboratory Lead to
document the software testing for the project in accordance with, AFP-AP-
06, Software Control, Section 8.9.3.
9.0 RECORDS
9.1 The spreadsheet containing the computed results is an Automated Calculational
Application (ACA) as defined in AFP-AP-06, Software Control. An ACA package
will be submitted by the Ash Fall Project – CVO Sediment Laboratory personnel to
the Ash Fall Project – CVO Sediment Laboratory Lead when the analytical work is
complete. The package will contain the information required by AFP-AP-06,
Software Control, Section 8.9.2.1.2. The dual data entry into SLEDS will fulfill the
requirements to test the ACA. The ACA will be reviewed by the Ash Fall Project –
CVO Sediment Laboratory Lead, and that review documented in accordance with
AFP-AP-06, Software Control, Section 8.9.4. After review, any changes that are
identified as necessary by the CVO Sediment Lab, the Ash Fall Project – CVO
Sediment Laboratory Lead, or the QA Lead will be documented in compliance with
AFP-AP-06, Software Control, Section 8.9.6.
9.2 The approved document in its entirety shall be submitted by the EMCBC
Coordinator to records in accordance with AFP-AP-20, Quality Assurance Records.
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9.3 The following are considered Lifetime QA Records:
Mettler Toledo SB32001 Balance verification results relevant to the Ash Fall
Project samples
Sedigraph verification and background results relevant to the Ash Fall
project samples
Verification testing of working sieve sets.
10.0 FORMS USED
10.1 Sieve Analysis Form
11.0 ATTACHMENTS
11.1 Attachment A – Sieve Analysis Form
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Attachment A – Sieve Analysis Form
SIEVE SIZE ANALYSIS
Sample Identification: Gross Wt. (g): Location: Tare Wt. (g): Date, Time: Net Wt. (g): Analysis Requested By, Date: > > Gravel/Sand break at 4.00 mm Gravel Wt. (g): Sand Wt. (g): Analysis By, Date: Computation By, Date: # of Sand Splits: Check By, Date: Split Wt. (g):
SIEVE SIZE (mm)
PHI SIZE NET WT.
(g) % FINER THAN
128.0 -7.0
64.0 -6.0
32.0 -5.0
16.0 -4.0
8.00 -3.0
4.00 -2.0
2.00 -1.0
1.00 0.0
0.500 1.0
0.250 2.0
0.125 3.0
0.0625 4.0
pan material >4.0
Comments:
Environmental Management Consolidated Business Center
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Dry Sieve/Sedigraph Process Procedure: AFP-SDG-01
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Form 12-1 – Record of Revision
DOCUMENT: AFP-SDG-01, Dry Sieve/Sedigraph Process
Revision Number Description of Changes Revision on Pages Effective Date
0 Initial Issue All 02/13/2017