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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


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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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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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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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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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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:


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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

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