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Standard

Operating Procedure for


Sentinel Landscapes (CRP6):
Soil Sample Processing at Regional
Laboratories using the:

Land Degradation Surveillance
Framework (LDSF)
Last updated February 2013
By Leigh Winowiecki
(adapted from the AfSIS-ICRAF-SOP)

I.

Introduction

This standard operating procedure is for processing soil samples collected using
the Land Degradation Surveillance Framework (LDSF) and is designed for use
by regional laboratories. The procedure covers sample reception and logging,
soil sieving and weighing, soil subsampling, soil sample storage, and shipping of
samples to the reference soil laboratory at the World Agroforestry Centre
(ICRAF) in Nairobi.
This SOP describes the laboratory processing procedure for the standard top
and sub soil samples collected from each plot and for the cumulative soil
mass (CM) samples, which are collected at the center of each plot.
All soil samples from the field are transported to regional laboratories for
processing and processed using this standard operating procedure.

II.

Soil sample reception and logging Sample Login Forms

Upon reception, all samples should be recorded on the sample login forms
(Tables 1-2) and checked for consistency against LDSF field sheets. Leigh
Winowiecki will send you the excel files and the completed forms should be
mailed to Leigh Winowiecki (l.a.winowiecki@cgiar.org) upon completion. Any
labeling discrepancies or problems due to damaged sample bags or lost samples
LDSF Standard Operating Procedure for Soil Sample Processing and Shipping
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should be noted on the form, and if possible resolved at this stage. This is
particularly important for cumulative soil mass samples, where complete recovery
of the sample is required.
Table 1: Sample login form for standard TOP and SUB soil samples.
Site

Sampling
date

Cluster

Plot

Depthcode

Total air dried soil


weight (g)

Bushbuck

21/02/2013

TOP

754.9

Coarse
fragment
(>2mm)
(g)
2.3

Bushbuck

21/02/2013

SUB

1100.9

15.9

Table 2: Sample login form for cumulative soil mass (CM) samples.
Site

Material

Samp
ling
date

Cluster

Plot

Depth_
top
(cm)

Depth_
bottom
(cm)

Total
air
dried
soil wt
(g)

Coarse
Frag (g)

Tin
ID*

Tin
wt
(g)*

Tin_air
dried
soil wt
(g)*

Tin_ove
n dried
soil wt
(g)*

Bushbuck

CM

21/02
/2013

20

543.1

4.5

9.8

59.8

42.3

* these fields are required only if you have oven-drying capabilities for gravimetric
moisture content. Otherwise, omit and make sure the samples are dry.

III.

Air drying of standard and cumulative mass soil samples

Air dry all the soil samples by spreading the soil sample out as a thin layer into
shallow trays or bowls. Drying can be done in large room, a custom-made solar
dryer, or a forced-air oven at 40 C. Break up clods as far as possible to aid
drying. It is important to ensure that no material from a sample is lost or
discarded, as weights of soil fractions are to be recorded. Contamination from
dust, plaster or other potential contaminants should be avoided as soils are
subjected to trace element analysis. Great care should be taken at all stages to
ensure sample labels remain with the samples. Drying time will depend on the
condition of the samples and ambient conditions, but the samples should be
thoroughly dry (i.e. constant weight).

IV.

Weighing and sieving of standard TOP and SUB soil


samples

NOTE: The ENTIRE sample must be weighed and processed!


1. Log sample onto sample login form (Table 1) (Leigh Winowiecki will send you
the excel file).
2. Weigh the entire air-dried soil sample to 0.1 g using a calibrated
top-pan balance. Record the weight of the entire sample onto the sample
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login form. (Make sure to tear the weight of the bowl or tray, to record only
the weight of the soil sample, not the weight of the drying bowl.)
3. Mix the dry sample thoroughly while still in the drying tray or bowl.
4. Spread the sample onto a plastic sheet on a solid table.
5. Using a wooden rolling pin, crush the sample to pass through a 2 mm mesh
size certified sieve. While crushing, remove any plant materials (e.g. roots)
and any possible pieces of gravel (making sure they are gravel and not soil
aggregates) and place in a separate pile (the coarse fraction pile).
6. Pass the crushed sample through the 2 mm sieve. DO NOT use the sieve as
a grinder; i.e. do not rub or mash the soil on the sieve, but shake the sieve
gently to allow the soil to pass through. If a large amount of soil needs to be
sieved, it is easier to do it in small batches rather than all at one time.
7. Place whatever remains on the sieve back onto the plastic sheet and crush
again gently. Then pass again through the 2 mm sieve. Make sure that all
soil materials are crushed, but do not attempt to crush gravel and rocks.
8. Transfer anything that now remains on the sieve into the coarse fraction pile.
9. Record the weight of the coarse fragments (>2mm) onto the login form.
10. Clean off the bench with a damp cloth to remove soil dust, so as to prevent
contamination from one sample to another.
The whole sample is now processed and no material should be discarded.
You will remain with two fractions:
a. The coarse fraction (>2 mm), which cannot pass through the sieve.
b. The soil fines (<2 mm), which have passed through the sieve.

V.

Weighing and sieving of cumulative mass (CM) soil


samples

NOTE: The ENTIRE sample must be weighed and processed!


1. Log each cumulative mass soil sample onto the Cumulative Soil Mass
Sample Login Form (Table 2) (Leigh Winowiecki will send you the file).
2. Ensure that cumulative soil mass samples are COMPLETELY air-dried and
that no sample has been lost during transport!!

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3. Weigh the entire air-dried cumulative soil mass sample to 0.1 g using a
calibrated top-pan balance.
4. Record the weight of the entire sample onto the sample login form. (Make
sure to tear the weight of the bowl or tray, to record only the weight of the soil
sample, not the weight of the drying bowl.)
Note: If you have access to an oven, follow the procedure outlined in Figure 1.
This procedure is used to calculate the gravimetric water content of the soil, e.g.,
any residual moisture in the air-dried sample, in order to calculate the total ovendried weight of the cumulative soil mass samples. If you do not have access to
an oven, you must make sure the samples are completely air-dried before
recording the total air-dried weight.
5. Spread the sample onto a plastic sheet on a solid table.
6. Using a wooden rolling pin, crush the sample to pass through a 2 mm mesh
size certified sieve. While crushing, remove any plant materials (e.g. roots)
and any possible pieces of gravel (making sure they are gravel and not soil
aggregates) and place in a separate pile (the coarse fraction pile).
7. Pass the crushed sample through the 2 mm sieve. DO NOT use the sieve as
a grinder; i.e. do not rub or mash the soil on the sieve, but shake the sieve
gently to allow the soil to pass through. If a large amount of soil needs to be
sieved, it is easier to do it in small batches rather than all at one time.
8. Place whatever remains on the sieve back onto the plastic sheet and crush
again gently. Then pass again through the 2 mm sieve. Make sure that all soil
materials are crushed, but do not attempt to crush gravel and rocks.
9. Transfer anything that now remains on the sieve into the coarse fraction pile.
10. Record the weight of the coarse fragments onto the login form.
11. Clean off the bench with a damp cloth to remove soil dust, so as to prevent
contamination from one sample to another.

The whole sample is now processed and no material should be discarded.


You will remain with two fractions:
c. The coarse fraction (>2 mm), which cannot pass through the sieve.
d. The soil fines (<2 mm), which have passed through the sieve.

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Figure 1: Cumulative soil mass processing procedure, including oven-drying a subsample


for gravimetric water content calculations.

VI.

Subsampling soils to be shipped to ICRAF Soil and Plant


Spectroscopy Laboratory in Nairobi, Kenya

Due to the high cost of shipping, only ~200-250 g of the standard TOP and SUB
soil samples and ~50-75 grams of the CM samples will be sent to the laboratory
in Nairobi. Therefore, we need a subsample of the entire soil sample. This
subsample must be representative of the entire sample collected from the field,
so much care is needed when following the below procedure.
To subsample the fine fraction (soil < 2 mm diameter)
If the weight of the soil fines is much greater than 200 g, subsample the soil fines
using coning and quartering technique (see below box and Figure 2) to give
about 200 g of soil for each TOP and SUB and ~ 50-75 g of each CM sample.

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Coning and Quartering Technique for Subsampling the Soil


1. Spread the soil sample onto a plastic sheet on a solid table.
2. Thoroughly mix the soil sample using a spoon, spatula or plastic ruler.
3. Configure the soil into a conical pile.
4. Further mix the soil by circumventing the cone symmetrically, repeatedly
taking soil from the base and transferring it to the apex of the cone. Do
this at least twice.
5. Flatten the cone to a height of 1 cm.
6. Divide the pile into four quarters (along two lines intersecting 900 to each
other).
7. Select one pair (e.g., two quarters) as the sample to be retained.
8. If this sample is still too large, repeat the procedure from the beginning
using these two quarters.

Figure 2: Example of coning and quartering of the soil sample to create a representative
subsample for shipping to Nairobi.

Packaging the subsample for shipping to Nairobi


200-250 g of the TOP and SUB soil subsample
Place at least 200 g of the TOP and SUB soil fines sample into a strong Ziploc
plastic bag, labeled with the site, cluster, plot, depthcode, and date, both on the
bag and a paper label placed inside the bag. Excess soil fines should be stored
in a labeled bag in case further analyses are done later.

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Example Label: TOP and SUB soil samples be sure to label both the plastic
bag and a paper label placed inside the bag:
BUSH.1.1.TOP
21/02/2013

BUSH.1.1.SUB
21/02/2013

50g of the Cumulative Soil Mass (CM) subsample


Place ~50 g of the Cumulative Soil Mass (CM) fines sample into a strong Ziploc
plastic bag, labeled with the site, cluster, plot, material, depth and date both on
the bag and a paper label placed inside the bag. Example label: Bush1.1.CM.020. 12-March-2013. Excess soil fines should be stored in a labeled bag in case
further analyses are done later.
Example Label: Cumulative Soil Mass samples be sure to label both the plastic bag
and a paper label placed inside the bag:
BUSH.1.1.CM.0-20
21/02/2013

BUSH.1.1.CM.20-50
21/02/2013

BUSH.1.1.CM.50-80
21/02/2013

BUSH.1.1.CM.80-110
21/02/2013

Subsampling the coarse fraction


The coarse fraction of the samples (i.e. the fraction > 2 mm diameter) will also
need to subsampled and shipped to the ICRAF laboratory for carbon and multielemental analysis.
Use coning and quartering to obtain a 20 g subsample of the coarse fraction.
Place the subsample in a zip-lock polythene bag labeled with the site, cluster,
plot, depthcode, coarse, and date. Example: Bush.1.1.TOP.Coarse
21/02/2013. If you have less than 20 g of coarse, ship the entire labeled coarse
fragment sample.

VII.

Sample shipping procedures

The following will be shipped to the ICRAF-Nairobi lab from each sentinel site:
~200 g sample of soil fines ( < 2mm) for all standard TOP and SUB a
~50 g of soil fines ( < 2mm) for all CM soil samples.
The corresponding ~20 g subsample coarse fraction ( > 2mm). If there are
no coarse fragments, that is fine.
ICRAF Laboratory can facilitate shipment through DHL. Good
communication with the ICRAF laboratory and SL Scientists prior to shipping is
essential to ensure legal requirements are met and to ensure the safety of the
samples.
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1. In advance of shipment, send the details of your samples to the ICRAF SoilPlant Spectral Diagnostic Lab at ICRAF Headquarters to: Tor Vagen
(t.vagen@cgiar.org) and Samuel Gaturu (s.gaturu@cgiar.org) and Leigh
Winowiecki (l.a.winowiecki@cgiar.org). This includes the sample login forma
from Section The information required is (a) a description of the material (e.g.
air-dried 2 mm-sieved soil samples), (b) the number of soil samples, (c) the
total weight of the soil in the batch, and (d) name, institutional address and
fax number of the scientist shipping the samples.
2. Obtain a phytosanitary certificate from your country's plant inspectorate
authorities or, if this is not possible, a letter from the relevant government
authority indicating that the soils are specifically meant for research purposes
only and have no commercial value. Send the phytosanitary certificate or
letter to the ICRAF laboratory.
3. Based on the above documentation, the ICRAF laboratory will obtain a Kenya
import permit for the samples from the Kenya Plant Health Inspectorate
Service. The ICRAF laboratory will email you a scanned copy of the permit1.
The samples should be shipped together with a copy of the KEPHIS permit
and your phytosanitary certificate or government letter. Failure to do so may
result in the samples being destroyed by KEPHIS!
4. The soil samples to be shipped should be carefully double-packed into strong
polythene bags that cannot be easily ripped or damaged in transit, and
packed into strong shipping cartons. Also have the shipping agent repack the
consignment again. Secure packing is critical because if the package arrives
damaged the samples will be destroyed by KEPHIS and our agreement may
be revoked. Do not underestimate what airlines can do to a package!
5. The shipping address is:
World Agroforestry Centre (ICRAF)
UN Ave, Gigiri
P. O. Box 30677-00100
Nairobi
KENYA
Tel: +254 20 7224000
Fax: +254 20 7224001
Remember that the shipment must be accompanied by the import permit
and your phytosanitary certificate. Invoice must indicate a minimal
value and include the words: FOR CUSTOMS PURPOSES ONLY OF
NO COMMERCIAL VALUE to facilitate clearing.
6. On shipping you must immediately fax or email the shipping details (e.g.
airway bill number) to Leigh Winowiecki (l.a.winowiecki@cgiar.org) and Tor
Vagen (t.vagen@cgiar.org) and Samuel Gaturu (s.gaturu@cgiar.org). This
will allow us to alert the shipping agent's Nairobi office about the arrival of the
quarantine shipment.
1

KEPHIS also issue a quarantine (Q) label that the ICRAF Soil Lab will retain for clearance purposes.

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Collection and treatment


The ICRAF Laboratory will arrange clearance of the shipment and inspection of
the soils by KEPHIS. Upon clearance by KEPHIS, ICRAF will arrange for
collection of the soils and their transport to ICRAF House.
ICRAF have specified procedures for handling foreign soils in their laboratory as
part of their agreement with KEPHIS. Essentially, the soils will be logged as
foreign soils, stored in a dedicated foreign soils store, and destroyed after use.
Cost of permits
The ICRAF laboratory charges 100 USD to cover all the expenses involved in
sample clearance protocols, including KEPHIS fee, visits to the KEPHIS office,
and clearance when the samples arrive.
________________________________________________________________
ANNEX Explanation of LDSF soil sample labeling
Each LDSF site has 16 clusters and 10 plots per cluster. If there are no depth
restrictions, there should be 160 TOP SOIL samples and 160 SUB SOIL
SAMPLES and 480 Cumulative Soil Mass Samples (~800 soil samples per site).
The labeling of each soil sample should follow the below outline:
Site.Cluster.Plot.Depthcode.Date
Standard Top and Sub Soil Samples Cluster 1 Plot 1
Long.1.1.TOP 26-June-2013
Long.1.1.SUB 26-June-2013
Cumulative Soil Mass Samples Cluster 1 Plot 1
Long.1.1.CM.0-20 26-June-2013
Long.1.1.CM.20-50 26-June-2013
Long.1.1.CM.50-80 26-June-2013
Long.1.1.CM.80-110 26-June-2013
Standard Top and Sub Soil Samples Cluster 1 Plot 2
Long.1.2.TOP 26-June-2013
Long.1.2.SUB 26-June-2013
Standard Top and Sub Soil Samples Cluster 1 Plot 2
Long.1.2.CM.0-20 26-June-2013
Long.1.2.CM.20-50 26-June-2013
Long.1.2.CM.50-80 26-June-2013
Long.1.2.CM.80-110 26-June-2013

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