Segundo Taller de la Red Latinoamericana de Laboratorios de Suelos (LATSOLAN) 12-14 marzo 2019 Ciudad de México

1. Item 7:
Comparison of SOPs between
LATSOLAN and SEALNET
Sra. Floria Bertsch, Costa Rica
Sra. Nopmanee Suvannang, Thailand

2. What we need to
standardization/harmonization
- The structure of SOP/template format
- The method?
Qué necesitamos para
estandarizar/armonizar los SOPs
- El formato del SOP
- El método del SOP

3. Template format of SOP
1.Foreword 1. Application 1. Introduction to soil organic carbon
Why do we analyse Exchange K
2.Scope and Application 2. SCOPE or EXTENT 1. Scope 2.SCOPE 2. Summary of Method 2. Scope and field of application
3.Principle 1. PRINCIPLE 3. Principle 1.PURPOSE 4. Principle
What do we really analyse
4.Materials and Equipment 4. REAGENTS 4. Reagents 6. Reagents 5. Materials and equipment
3. EQUIPMENT AND MATERIALS 5. Aparatus and Glassware 5. Equipment Reagents
6. Laboratory sample 6. Sample preparation
5.Procedure 5. PROCESS 7. Procedure 7. PROCEDURE 7. Procedure 7. Procedure
6. Quality Assurance/Quality Control 10. Precision and Accuracy 9. Quality assurance / Quality control
6.1 Precision test 9. Repeatability
6.2 Accuracy Test
6.3 Control Chart
7. Health and Safety Health and Safety 4. Safety 10. Health and Safety
8. Calculation 6. CALCULATIONS 8. Calculation 8. Calculation 8. Calculation
9. Reference 7. BIBLIOGRAPHY 2. Normative References 6. REFERENCES 11. References 3. Reference documents (if any)
10. appendix 10. Test report 9. report 11. Appendix I
11.1 Results Of Interlaboratory Comparison
10.1 preparation of reagent 11.2 Flowchart
3. Interferences
11.3 Others that need and too long to put in the
content
3. RESPONSIBILITIES
3.FORMS
USDA
Waginagen
(Winnie)
SEALNET LATSOLAN ISO
British Geological Survey
(BGS)

4. Do we agree on criteria to accept
the method to use
¿Estamos de acuerdo con los criterios de
aceptación el método a utilizar?
-The method that we use need
to be able to tracibility to the
international method : ASTM,
SSSA, ISO etc
-Follow the majority practices?
(most labs have done)
-Follow the standard method?
-Inhouse method? Need
validation
El método que utilizamos debe poder
ser rastreable al método
internacional: ASTM, SSSA, ISO,
etc.
¿Se seguien las prácticas dominantes?
(lo que la mayoría de los labs hacen)
¿Sigue el método estándar?
¿Método interno? Necesita validación

5. Region Amount
of soil
volume
of water
ratio type of water particle
size
(mm)
type of
agitation
Agitation
time
resting time again shake
and read in
the
suspension
electrode immersion depth Form of
expression
of the
result
SEALNET 10 g 25 ml 1:2.5 Deionized/distilled
water The pH of
the water should
be between 5.6
and 7.0
2 mm shaker 30 min 60 min yes insert the electrode into the
suspension
1 decimal
LATSOLAN 10 g 25 ml 1:2.5 at least Type III of
ASTM 1193: 2001
or Grade 3 of NC-
ISO 3696: 2004.
2 mm shaker 10 min at least 30
minutes
yes insert the electrode into the
suspension
1 decimal
pH water 1:2.5

6. Reference Amount
of soil
volume
of water
ratio type of water particle
size (mm)
type of
agitation
Agitation
time
resting
time
again shake
and read in
the
suspension
electrode immersion depth
Thomas G.W. in Spark et al 1996
SSSA Book Series 5: Method of
Soil Analysis, Part 3, Chemical
Methods, Chapter 16
10 g 10 ml 1:1 deionized water not
mention
stirring stick
or stirring
machine
not mention 10 min entire
suspension
may be
stirred
during the
pH
determinatio
n
either
1.insert to the suspension
2. place electrode in the clear
solution
3. direct to the sediment soilar
supernatant above the soil
ASTM D4972-13 Standard Test
Method for pH of Soils (2013).
ASTM International. United States
10 g 10 ml 1:1 ASTM type III or
better (D1193)
(0.25 -4.0 US/cm,
pH 5.0-8.0)
2 mm
sieve (No.
10)
stirring stick
or stirring
machine
not mention 1 hour - place the electrode into the
partially settled suspension to
mitigate the suspension effect
Peech M, 1965 Hydrogen -Ion
Activity, Chaper 60 in Black C.A
et al. 1965. Methods of Soil
Analysis Part 2 Chemical and
Nicrobiological Properties, No 9
Agronomy Am. Soc. Of Agr.
Wisconsin, USA
20 g 20 ml 1:1 distilled water not
mention
stirring stir the
suspension
several
times
during the
next 30 min.
1 hour - glass electrode will be immerse
well into the partly settled
suspension and the calomel
electrode will be immerse just
deep emough into the clear
supernatant solution to
establish a good electrical
contact through the ground-
glass joint or the fiber -capillary
hole
insert the electrode into theHandbook of Reference Methods.
Soil and Plant Analysis Council ,
2002. Soil Analysis Handbook of
Reference Methods. Soil and
Plant Analysis Council Inc. CRC
Press Washinton, DC
5 g 5 ml 1:1 not mention 2 mm
sieve (No.
10)
stirring 5 sec. 10 min stirr while
reading
into soil water slurry
Donald and Thomas, 2009. in
Northeastern United States
Cooperative Bulletin No 493.
Recommended Soil Testing
Procedures for the Northeastern
United States.chapter 3
5 g 5 ml 2 mm
sieve (No.
10)
15 sec 30 min swirl
carefully
before read
the pH
soil water slurry
Jones, J Benton 2001. CRC Press
LIC.Laboratory Guide for
Conducting Soil Tests and Plant
Analysis
10 g 10 ml 1:1 2 mm
sieve (No.
10)
glass rod or
mechanical
5 sec. 30 min stirr with
glass rod or
mechanical
Rayment and Lyon 2011. Soil
Chemical
Methods_AustraliaCSORO
publishing
20 g
50
10
100 ml
50
25
1:5 (4A1)
1:1 (4A.2)
1:2.5
(4A.4)
< 1.5 *10-3
dS/m
pH ≥6.5 but ≤ 7.5
< 2 mm
sieve (No.
10)
mechanical
shake end
over end at
25 ͦC
1 hour 20-30
min
mechanical
stirred
during the
measuremen
t
FAO Soils Bulletin 38/2, 1980.
Soil and Plant Testing as a basis
of fertilizer recommendations
250 p
10 g 50 ml 1:5 distilled water or
deionized water
2 mm
sieve (No.
10)
stir the
suspension
not mention 18 hour not mention
ISO 10390-2005. Soil quality-
Determination of pH, second
edition 2005-02-15
5 ml 25 ml 1:5
(volume
fraction,
volume to
volume
using the
spoon or
balance)
0.2 US/cm (mS/m)
at 25C, pH >5.6)
2 mm
sieve
shaking by
mechanical
shaker or
mixer
60 min ± 10
min
1 hour
not
longer
than 3
hour
in the suspension at 20 ͦC ± 2 ͦC
immediately after or whilst being
stirred

7. Do any lab can provide work
on difference condition for
method validation?
¿Algún laboratorio puede
proporcionar datos de validación
(en diferentes condiciones) para
este método?

8. Region
Mass range
of soil
sample
analyzed, in
g (minimum-
maximum)
Particle
size of
the soil
sample
(mm)
Molarity of
Potassium
Dichromate
that uses
ml of
dichromate
used
(range,
according
to the soil
mass used)
ml of
Sulfuric
Acid
used
(range,
according
to the
mass
used)
ratio
Add
external
heat?
If yes, how
long, what
temperature
(° C) and
by what
means?
Time
(min) of
rest of
the
reaction
amount
of water
use
(ml)
Type of water
used,
according to
ASTM
need addition
filtration
Does your
method
require
adding
Phosphoric
Acid?
If you use
Phosphoric
Acid, how
many mL?
How do you
evaluate the
excess of
Dichromate?
SEALNET 0.5 -1.0 g of
air dry soil
(adjust if
necessary,w
ith colour
of soil)
0.5 mm
sieve
0.167 M
or 1 N
10 ml 20 ml 1:2 no - 30 min 200 ml deionized/
distilled water
filter the
suspension
using an acid
resistant filter
paper (e.g.
Whatman No.
540), if
experience
shows that the
end point of
the titration
cannot
otherwise be
clearly
discerned.
yes
if
diphenylami
ne
indicator is
used
10 mL of
85% H3PO4.
titration
LATSOLAN A variable
amount of
the test
sample is
weighed
according
to the
estimated
organic C
content and
placed in
the
Erlenmeyer
0.5 mm
sieve
5 ml 10 ml 1:2 no - 30 min 15 ml Distilled or
demineralized
water Type
III (ASTM
1193: 2001)
or Grade 3
(ISO 3696:
2004)
no yes 1 ml titration
OC (WB)

9. Regional
pH of
Ammonium
Acetate
mass of
soil
sample
analyzed
in g
Particle
size of
the soil
sample
(mm)
Total
volume of
extractor
solution
ratio
How do you
performthe
extraction?
With what type
of equipment
does the
agitation?
How do you
separate
the phases?
Agitation
time and
number
of times
If you filter,
what # of
filter paper
do you use?
What conc
do you
use for K
calibration?
calculatio
n base
on air dry
soilor
oven dry
SEALNET ammonium
acetate
(pH=7, N=1)
2.5 g 2 mm 25 ml 1:10 reciprocating
shaker for 30
minutes
reciprocating
shaker
filter 30 min
only 1
time
Whatman
No. 2 filter
paper
contain 0,
5, 10, 15,
20, and 40
ppmK
air dry
soil
LATSOLAN ammonium
acetate
(pH=7, N=1)
5 g 2 mm 100 ml
(33 ml* 3
time
shaking)
1:20 reciprocating
shaker for 10
minutes
reciprocating
shaker
centriguge
and filter
10 min
repeat 3
time
Whatman 2,
41 or similar
paper.
contain 0,
5, 10, 20,
30, and 40
ppmK
air dry
soil
Exch K (NH4OAc)

11. Item 8:
Sugerencias de nuevos SOPs para incluir
en el Ring Test LATSOLAN-SEALNET

12. SEALNET 18 Labs
pH water 1:2.5 (16)
OC (WB) (15)
Exch K (NH4OAc) (16)
Total C (3)
Avail P (Olsen) (16)
,
LATSOLAN 20 Labs
pH water 1:2.5 (16)
OC (WB) (16)
Exch Ca, Mg, K (NH4OAc) (16)
Total C (2)
Total N (5)
Total N (Kj) (12)
CaCO3 (6)
Lo que se hizo en el primer RING TEST

13. Propuestas adicionales para el Segundo
RING TEST (SEALNET-LATSOLAN)
SEALNET
pH water 1:2.5
OC (WB)
Exch Ca,Mg,K (NH4OAc)
Total C
Total N
Avail P (Olsen, Bray)
EC 1:5
LATSOLAN
pH agua 1:2.5
COx (WB)
Ca, Mg, K Interc (NH4OAc)
C total
N total
N total (Kj)
CaCO3
P intercambiable (Olsen?, Bray?)
CE 1:5?

14. Region Amount
of soil
volume
of water
ratio type of water particle
size
(mm)
type of
agitation
Agitation
time
resting time again shake
and read in
the
suspension
electrode immersion depth Form of
expression
of the
result
SEALNET 10 g 25 ml 1:2.5 Deionized/distilled
water The pH of
the water should
be between 5.6
and 7.0
2 mm shaker 30 min 60 min yes insert the electrode into the
suspension
1 decimal
LATSOLAN 10 g 25 ml 1:2.5 at least Type III of
ASTM 1193: 2001
or Grade 3 of NC-
ISO 3696: 2004.
2 mm shaker 10 min at least 30
minutes
yes insert the electrode into the
suspension
1 decimal
CE 1:5
La propuesta es usar el mismo de pH y agregarle más
agua al final para alcanzar esa relación

15. Metodos para P disponible
o Bray P1: 0.03 M ammonium fluoride + 0.025 M HCl
o Bray P2: 0.03 M ammonium fluoride + 0.1 M HCl
o Olsen-P: 0.5 M sodium bicarbonate pH 8.5

16. Reference
mass of
soil sample
analyzed in
g
Particle size
of the soil
sample
(mm)
Total volume
of extractor
solution
ratio add chacoal
How do you
perform the
extraction?
Agitation
time
time to
develop
colour
wavle
length
used
Expression
of results
(units)
Kuo. in Spark et al 1996
SSSA Book Series 5: Method of Soil Analysis, Part 3,
Chemical Methods, Chapter 32
2 g < 2 mm 40 ml 1:20 1/2 tea spoon
no need to use if use
ascorbic acid
mechanical shaking 30 min 30 min 882 nm mgP/kg
Olsen and Dean, 1965
Phosphorus, Chaper 73 in
Black C.A et al. 1965. Methods of
Soil Analysis Part 2 Chemical and Nicrobiological
Properties, No 9 Agronomy Am. Soc. Of Agr. Wisconsin,
USA p 73-4.4
5 g < 2 mm 100 ml 1:21 1 tea spoon
add more if necessary
mechanical
shaking end over
endreciprocating
shaker
25 ͦ C ± 1 ͦ C
30 min 10 min 660 nm mgP/kg
Handbook of Reference
Methods. Soil and Plant
Analysis Council , 2002. Soil
Analysis Handbook of Reference Methods. Soil and
Plant Analysis Council Inc. CRC Press Washinton, DC
2.5 g < 2 mm 50 ml 1:22 no reciprocating
shaker
30 min 15 min 880 nm kg P/ha
Jones, J Benton 2001. CRC Press
LIC.Laboratory Guide for Conducting Soil Tests and
Plant Analysis
2.5 g < 2 mm 50 ml 1:23 no mechanical
shaking end over
endreciprocating
shaker
30 min 20 min 880 nm mgP/kg
Rayment and Lyon 2011. Soil
Cheical Methods_AustraliaCSORO publishing
Method 9C1
5 g < 2 mm 100 ml 1:24 no mechanical
shaking end over
end
30 min
at 25 ͦC
30 min 882 nm mgP/kg
FAO Soils Bulletin 38/2,
1980. Soil and Plant Testing as a basis of
fertilizer recommendations 250 p
5 g 2 mm 100 ml 1:25 1 tea spoon shaking at 200 rpm 30 min 10 min 660 nm
ISO 10390-2005. Soil quality-
Determination of pH, second edition 2005-02-15
5 g ±
0.01 g
2 mm 100 ml
± 0.5 ml
1:26 1.0 g shaking 30 min
at 20 ͦC ±
1 ͦC
60 min

17. Region
massofsoil
sample
analyzeding
Particle size of
the soil
sample (mm)
extractant
Totalvolume
ofextractor
solution
ratio addchacoal
How do
you
perform
the
extraction?
Agitationtime
andnumberof
times
Ifyoufilter,
what#offilter
paperdoyou
use?
time to
develop
colour
wavle
length
used
calculation
base onair
dry soilor
ovendry
SEALNET 5g 2mm 0.5M
NaHCO3 at
pH8.5
100ml 1:20 Addahalf
teaspoonofP-
free carbon
black(approx.
0.5g).
shaking 30min
at25 ͦC
whatmanNo
42
60min 882nm ovendry soil
basis
LATSOLAN
P (Olsen)

18. Core questions to be answered
Preguntas para ser respondidas
- EC??
- Olsen P??
- P (BRAY 1 and BRAY 2)
- Quién va a desarrollar el SOP de cada uno???

19. Test Item for PT
2018 2019 2020 2018 2019 2020 2018 2019 2020
pHwater 1:2.5 × × × × ×
OC (WB) × × × × ×
OC (dry combustion) × × ×
Avail P (Olsen) × × × ×
Exch K × × × × ×
Exch Ca × × × ×
Exch Mg × × × ×
Exch Na × × ×
CEC × × ×
EC 1:5 × × ×
Avail P (Bray 1) × × ×
Avail P (Bray 2) × × ×
Total N (DUMAS) ×
GLOSOLAN SEALNET LATSOLAN

20. SEALNET 18
LATSOLAN (11 Central America + 9 South America) 20
PACIFIC 3
EUROPE and EURASIA : 8
AFRICA 5
NENA 4
NORTH AMERICA 1
TOTAL 43
Region Participating Laboratory
no of labs participate
2019