Soil Testing Procedures
Soil Testing Procedures
Soil Testing Procedures
FIELD DOCUMEN I 3
Botswana
Part 2
Laboratory Procedure Manual
GABORONE, 1988
AG: BOT/85/011
Field Document 3
Botswana
by
Reinhard Breitbart
FAO Expert
Gaborone, 1988
TABLE OF CONTENIN
pH-DETERMINATION
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Preparation of saturated soil paste . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
Saturated paste extract . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . , . . 5
ELECTRICAL CONDUCTIVITY . . . . . . . . . . . . . . 6
Procedure . . . . . . . . ........ .
Calculations and data storage ..... .
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Temperature correction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
PHOSPHORUS DETERMINATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
Equipment. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
Reagents. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
Extracting solution for Bray and Kurtz I . . . . . . . . . . . . . . . . . . . . . . . . 11
Extracting solution for Bray and Kurtz II . . . . . . . . . . . . . . . . . . . . . . 11
Color reagent A . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Color reagent B . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
Standard solutions for calibration curve . . . . . . . . . . . . . . . . . . . . . . . . 12
Settings. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
Calculations . . . , . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
CEC-DETERMINATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
Equipment. . . . . . . . . . . . . . . . . . . . . . . . ..... . . . . . . . . , . . . . . . 18
Reagents. . . . . . . . . . . . . . . . . , . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
1 normal, neutral ammonium acetate solution . . . . . . . . . . . . . . . . . . . . . . 18
1 normal, acidified potassium chloride solution . . . . . . . . . . . . . . . . . . . 18
4% boric acid solution . . . . . . . . . . . . . . . 19
Mixed indicator .......... .
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50% sodium hydroxide solution . . . . . . . . .
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Sulfuric or hydrochloric acid 0.01 n . . . . . . . . . . . . . . . . . . . . . . . . . . 20
Procedure . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
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Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
EXCHANGEABLE CATIONS DElERMINATION ..... . . . . . . . . . . . . . . . . . 23
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lnterelement effects during Ca and Mg determination
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Preparation of Ca/Mg standard solutions (meq/litre) . . . . . . . . . . . . . . . . 24
Preparation of K/Na standard solutions (meq/litre) . . . . . . . , . . . . 25
Alternative K/Na standard solution in ppm ..... . . . . . . . . . . . . . . . 27
Ca/Mg and K/Na with Atomic Absorption Spectrometer . . . . . . . . . . . . . . 28
Preparation of the Varian AAl275 Atomic Absorption Spectrometer . . . . . 28
Calculations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
K/Na determination with 'CORNING 400' flamephotometer . . . . . . . . . . 3
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36
37
II
SAMPLE RECEPTION, GRINDIN(; AND STORA ;E
Sample reception:
Incoming samples must always be accompanied by a list of all sample numbers in the lot.
Check the samples against this list immediately after arrival.
Report any irregularities to the soil chemist.
The soil chemist or a senior laboratory technician decide which laboratory numbers are to be
assigned to the samples.
Record sample numbers and the respective lab numbers in the sample reception book and
enter them into the computer data base.
Sample grinding:
Before grinding most samples first have to be dried.
Spread each sample on a tray, together with the sample bag and sample number card. Place
in a wind protected spot until dry. Then till back into bag.
Write lab numbers on the sample containers with a permanent marker. Arrange sample bags
and sample containers in serial order to avoid any possibility of mixing up samples.
Fill an appropriate amount of soil from the sample bag into the 'llynucruste sample grinder.
Alter about 1 minute switch oft Fill the tine earth fraction which has passed into the receiver
through the 2 mm sieve at the bottom of the grinder into the sample container and discard
the reminder.
NOTE: Some samples, especially very clay rich samples, form extremely hard aggregates when
dry. These aggregates cannot be grinded successfully with the Dynacrush grinder, they might
even destroy it. Crush the aggregates first with a stone or a hammer before filling into the
grinder. Be careful not to crush any stones.
It no grinder is available crush the aggregates with u rounded piece of wood on a tlat tray
and pass the soil through a 2 mm sieve.
Store the samples in the sample store room with incrementing lab numbers.
pH-DETERM1NATION
Reagents:
Equippient:
Procedure:.
Close bottles tightly, put on shaker in horizontal position and shake for two hours. After
shaking retnove samples from shaker and let stand for one hour.
Switch the pH-meter into 'measuring' mode.
Place the electrode in the pll 7 buffer solution. Wait for stable reading.
(Less than 30 seconds should be required - if it takes much longer the electrode might
require cleaning.)
2
7. Alter calibration immerse electrode into upper part of sample suspension.
Do not stir the suspension.
Wait for a stable reading.
A change of 0.01 units in 10 seconds is considered a stable reading. Note the value,rinse the
electrode with distilled water from a wash bottle and continue with the next sample.
S. Alter pH4120 measurement also measure electrical conductivity of this extract.
(To decide whether or not preparation of saturated paste extracts for electric conductivit.
and/or soluble salts determination is required.)
SATURATED PASTE EXTRAC'T
Reagent:
distilled water
1(juif)ntenit:
spatuLt
4
Saturated paste extract:
For conductivity determination the extraction can be nade a few minutes after preparing the
saturated paste.
If the soil contains gypsum the conductivity can increase by 1 or 2 mS/cm upon standing.
Therefore it' gypsum is present allow the saturated paste to stand several hours (4-6 hours)
before extracting the solution.
If the solution is to be analyzed for its chemical constituents, the saturated paste should stand
for 12 hours or more (over night).
Place 9cm fine porous filter paper (i.e Whatman no 42,44 or 50) in extraction cups. Moisten
with few drops of water and press it on the bottom of cups.
Hang cups into extractor and connect syringes. Transfer samples into cups. Set extractor to
about 1 hour extraction time and start extraction.
5
ELECTRICAL CONDUCTIVITY
Procedure:
"Franskr saturated paste extract into small narrow vials. The cell constant of the conductivity
elretrode, presently in use is 1.00. If other electrode is used check cell constant usually either
engraved on electrode or on the connecting cable.
Switch the range of the Zeiss con 602 conductivity meter on 'cal' and set the display to 1000
with the 'cal' knob (calibration of cell constant).
Record the temperature of the solutions.
Switch 'range' into the lowest of the three mS/m positions (do no use the p.S/m range).
Insert electrode into extract.
NOTE: The two platinum electrodes inside the measuring chamber must be completely
immersed in the solution. If the extract is not enough prepare a new saturated paste extract
of this sample and combine the two extracts. (this can happen with very clay rich soils).
Record the reading and continue with the next sample. If the conductivity is out of the set
range, indicated by display of (1. ) switch to a higher range.
0-20.00 S/m
As already mentioned above only the three mS/m ranges (2-4) should be used.
II otherwise, it must be clearly indicated in the measuring protocol.
Calculations and data storage:
6
Temperature correction:
Soil survey data are calculated and stored with a Hewlett Packard HP 86B Micro computer.
7
Figure I Temperature correctilin table (US. Salinity Laborator Staff. 1954)
SOLUBLE SALTS DETERMINATION
PrOtled re:
l'ipette I nil saturated paste extract in to 0 oil volumetric flask up will: dc,ii111.:
and shake well tu mix.
\ Olt: it absorbance readings of simples are too I,. ..1 tt 445 can he
chosen.
The 'I, dilution' then is calculated:
Size of volumetric flask : nil saturated paste extract
Further procedure is exactly as for exchangeable
Calculations:
If linear regression curve is calculated concentration C of soluble cations in ntc:tsioring sointion is:
C =- a*E+b
a, b = regression coefficients
E = Extinction (absorbance reading')
If no linear regression curve is calculated concentration C ot° soluble cations in measuring solution
is:
E/e
E Extinction (absorbance reading)
e = Extinction coefficient
4)
Concentration I: of soluble salts in soil Imeq/11
K C ext rac: .
C 2.dilution / 10
Dissolve 27.78 g NI-14F in approximately 500 ml distilled/deionized ateu dd 53.6 nil 11C1
(36%). Dilute to 1 litre in volumetric: flask, dilute to 25 liters in (from I)) 'adding 24
distilled/deionized vitter with measuring cylinders.
Close the drum and mix thoroughly.
Extracting solution for Bray and Kurtz U:
11
telor reagent A:
I. Dissole in a beaker 30 Aintrionintn-hepta-molybdat. in about 250 int 1190 dist.
Dksoke in a SeC0116 th'zti,Cr 0.727 g Antinomy- Potassium- tartrate.
Fill about 500m1 112(di. into a 2000m1 volumetric flask.
Add slowly 340 nil conc. 11.2SO4.
real.:( it4
Ot .
10 ppm P/1
Pipette 50 ml of 100 ppm solution into 500 ml volumetric llask.
Proceed as above.
1."
3. Standard series:
Pipette
10, 20, 30, 40, 50 ml
Settint:
A soil/extractant ratio of 1:7 is used.
Set Me dispenser for the extractant to 35ml. Using a AD 3 'three volumi -.three aliquut.
it must be made sure that all three syringes dispense precisel) the same dispenseltune.
Set the SUD 1 'combination diluter-dispenser' to dispense Sinl cok,7 15dul (list, water and
take u 01,11 extract.
'nit resulting dilution of 1:2 for samples and standards is found convenient
AsorlIanee for the highest standard is around 0.2-0.25.
Procedure:
1, Prepare the multi funnel rack. Fold double layers of filter paper and staple the edges that
hold their form. Put the titters into the funnels and place a tray of 33 bottles under the rack.
Prepare the color reagent 13. For one batch take 250-300m1 of reageo: Add 2.5-3 g Ascorbic
acid and stir with a magnetic stirrer until dissolved.
NOTE: Color reagent B is stable only for a t'ew hours and must always be prepared just
before the determination.
Weigh 5 g of the samples into the bottles of a tray. The last sample should be a standard!
sample which is repeated with every batch.
)iiiekly dispense 35 ml extracting solution to each of the samples.
Sdir for 1 minute with the multisample stirrer. (If the Bray and Kurtz II extraetant is used
stir for 40 seconds.)
Immediately after stirring filter by pouring simultaneously the contents of 1 1 bottles (one
bottle rack) onto one row of filters. It' the filtrates are not clear, filter again using the same
filters.
Put the tube connected to the syringe calibrated to 5 ml of the combination diluter-dispenser
into the color reagent B solution. (The syringe calibrated to 15 ml is permanently connected
with the water drum.) Pump at least 5 or more times and discard solution to make sure that
all tubes are filled with fresh solution.
13
S. Plao third bottle rack tras next tu the one with the tiltrates, Put tire double plastic tips uf
titc diluter-dispenser into eXtract. By pressing the lever take up 20 nd extract, 5 nil color
reagent and 15 ml water. Transfer this into the bottles of the third tray by run asing the lever.
l/ip the tips rIi t beaker with distilled water to clean the outside.
For the standards proceed vay. Eill a little wore tiran 20 ml Of tire stttiidards and
extracting solution t r the V of bottles and transfer with the diluter penser
itrio a econd ro','.
\TNT 1101(1, (0 hour the blue color of the m
1 ,bdate cmnplex is fu 11v developed
the spe-trophotometer determine the absorption standards and sato ples at 661 1101
w.;.% etengttL 1. Want°. fl11. Zen).
Calculations.
I t on coetlicient
E3 C
ulated:
n Extract r Weigh
NOTE: \\Atli dilution is not the initial dilution with the diluter-dispenser meant because [Itere the
standards are diluted too.
14
,
Digestion so ut
Sodinin tlichroinal
t5
Standartt
1.1iwculant .olution
superiloi 12- il,IC uit.t tcie,ltt 1)ívl\ltlssid. It IS highly
( ft(Iilt,Ill tul Itil, neon-,11 and
I 11'4 prl'ILIT1 t.11111Ct 110 11)0)1 mi beaker. Stii UI iuul ot 55111cr i,ith a magnetic
stirI VI 1/1 111111 ,1 1)11`,
OilitItt lit-f....
4, lint ttofit
\tttu ì)!ninon- tiertliic 127 /loci 111:int silin ion
111t.
culations:
Soil Survc
- (-Mahon acc.-
cattiputcr,
NOTE:
,or aiiirÌeswith more than 6% tog (' different itple dry, 'hod)
must be applied,
I -1)1.TERMINATI
1..jcitee unit w \ k I
Reagents:
Volotoolow
\ceto acid
Xmoomi:t ,olOtioo
horic ;1C1d
' odiOto 11,ydroicie flake,
ohitlietric solution kit sidliiro ydrochlock'
Ethanol 95() (methylated spiric
Ethanol 50`k (methylated spir0;
Pluassitun chloride
Hvilrochloric acid ()%
Mixed indicator:
Dissolve
0.5 g res.)! green
and 0,1 g h1ìrtli t.('
water to about cm below time marl.. Put flask iii Nvaterbath temperate al 20°C for 3f, minutes.
Then till lo Mark.
Procedure:
1. Prepare sample extraction tubes by placing approxiii g 0 litter p u I p formed in to a ha
in a syrirt:;:. harrel.
Force it down tightly with plunger.
Weigh 2.5 g of soil sample. It' sample is rich in clay and/or salirme, inix well with one 10 nil
scoop sand Or edite. Fill mixture into tube.
NO'FF: A blank should be prepared with every batch. This is imperative if samples have been
mixed with sand or edite because both adsorb a certain amount of ammonim» which must
be subtracted from time result.
Place sample tubes in upper disk of extractor and connect tu inverted syringe. The plunger of
this syringe is inserted in slot of stationary disk Of extractor.
Fill sample tu he to the 15 itil mark with al11111011IUM acetate. Stir carefully to release all
enclosed air bubbles from the sample. Rinse the stirring rod and the sides of time tube with
ammonium acetate from a wash bottle not exceeding the 25 inI mark.
Set extractor to 2 hours extracting time.
Add about 45 nil ammonium acetate solution to reservoir tube, start extractor.
At the end of extraction the extractor stops automatically by a micro switch. Switch
off and pull plungers down as far as extractor will alloW.
Disconnect syringes from sample tubes (leaving (libber connector on Sanijile tubtfland fill
contents into numbered 100 ml volumetric flasks.
Fill syringes again tu 35-45 nil with ammonium acetate solution from a beaker ¡toil till also
imito volumetric flask. Fill up to volume with aminonium acetate from a wash bottle. Nlix well.
Keep for exchangeable cations determination.
Return upper 2-disc unit tu starting position.
20
\ttaih io sample tubes ,-11)e sides town. . 1, ethanol. fill .. marl.
15. ib s)rifles with acidified in potassium chloride solution and estrai.l. Collect eslract in
1
sultintetric flasks. Fill up to inark vv oh potassium chloride soliition mid shake N/A tO
I'll/01V I 50 ml aliquod KCI extract digestion tul)es.
16, Remove sitinple tubes and transfer samples lo the digestion tohes ot the distilling unit.
Fill 25 nil or the boric acid ,ilotom into 250 tol coin,.
^witcli distillitig unit on.
Place an empty digestion tube and a beaker in position.
(lose valve of steam generator outlet at the haek Id the (mil
Open steam salse. Open tap until water level reaches the electrodes in steam generator Close
tap.
When water starts boiling upen lap again. Regulate %vale,' current that the bin:knowing water
(coming from condenser as cooling Nvater) is just hand warm ;4-5 liters per minute,.
Distill about 150 nil into beaker. Close steam valve.
Place tithe with first sample and First conical flask with bori, acid in positi,,i, \aid 51)%
sodium livilroxide solution by puling; the lever of the 'alkali moor'
()pen steam valve and distill 4-5 minutes coiieet 125-150 nil Clo.m: steam salve.
Remove tu be and conical flask.
2(). Place tube with new sample and new conical flask in position. Add sodium hydroxide, upen
steam valvc,
During second distillation Wrote first sample vvith 0.01 nD2S0, or 1 and so on.
At tire endpoint of the titration the green color disappears completely. lile solution looks gre
One drop more gives pink. (If an automatic titrator is used, set the end point to pli 1.4»
21
z
( t tr4ct/a1iquot
Equipment:
olunietric flasks
SD-1 diluter
SO nil polyethylene cont,iiiier, ,ir
Absorptioa
lical);Nii is,
or
dissonc I 338,7 g LitC13*711"0 in 5 liters dist. water. (For better solubility
EaC1,'7(10 37.-rf) La)
distilled water,
Preparation or ( standard solutions
f 0.090 Cir('()
anii 6 It): 7H
!. kndard series
24
--t;3;3;1.irti 2 ineti : 3 tic 3
4 met! /
i,31.3(1/1 K
t`10,
"1110
--)pper
Store
01111iVO
C in
Fir ;mil- 30 13-3
25
\iternative K/Na standard solution in ppiii:
hit() 1000
1 \ 11)11(%
Piocilc _ill la
Standard series
Pipette;
Proceed as
Connect the SI)-1 diluter set to a dilution ratio of 1:50 to the 2000 ppm lanthanum chloride
solution. (1 ntI sample uptake + 49 inl dispension.)
Connect the diluter set to a ratio of 1:10 to a drum with (I°, died water. (5 ml sample uptake +
15 inl water.)
lit the literature a 1000 ppin cesium chloride solution is recommended to sup ss partial
ionization of K and Na, Tests showed that the etree: lies within the erroi range ol the
determination. The costs tot the er3 expensive chentii,il pu n- cesium chloride can lw save&
Dilute ammonium acetate extracts from the CE( deternuir.,;1011 and standards inti»o yethlene
containers. For blanc dilute ammonium acetate solution. Sv -ontainers tr mix Then 1111 olution
into vials Milne, the automatic sample changer.
b. Check that iman pressure is inorc than 700 kpa II piessori. is bt...ioo
because acetone ma be formed and can come into the sstent.z
c Check that gas pressure olto svsleo:
not get started!
2. ()iterating_ modes:
The Varian Atomic Absorption Spectrometer can be operated in se'
Fully automatic with automatic sample changer and the t icwlc t 11.118613 micro
computer as controller and receker of the dal::
Half automatic without sample changer but controlling and ,andling by the
computer.
Half autotnatic with sample changer but without computer.
Manual without sample changer and computer.
28
a. Full automatic operating mode:
Switch system on in the following sequence:
I, Uninterruptable power supply
Spectrometer
Compressor and exhaust fan
Sample changer
Printer (make sure that printer is connected to .p ectr4otteter and not to eomputer
Monitor
Disc drive
Insert I-IP86 AI275 - system disc into drive O and datitsk into drive i
computer
I lic Ainostart' program %will start up computer. For
lisplayed on monitor.
Index' section
7,istrumer
Set: t '3 -waNcleligtil 422,6 tool
Mg-wavelength '285.2 Diu.
I. -wavelength i "O) 5 ii in i
\a-viaveiengt li ..t.s9.0 mu k
29
Half automatic (wet, IIOUt but with uoiui r as cou tt. .
'I he saint ,=)ib1i11,T which controls the full automatic operi mode alSO handles
automatic mode without sample changer. Time setting of the s nneter
manualk or by software using the same recommended param abokc.
Loop through pzirameters nressing repeatedly Programin set up', change parameters
using numeric he hoard.
spect irameters. (Spectrometer must be in 'AliS'-niode.)
Loni sample changer with
'Start' to start run.
ENtinction (alkorptimu
e = Extinction coullimot
Extrao = 100 ml
11eivli1 =- 2.5 g
K= * dimwit!
KiNa determination with 'CORNING a ephotometer
Ube corkentr:ition of the Na-standards is low enough to stay in the linear range of the
entissioniciincentration function.
Set the S1)-1 diluter to a dilution ratio of 1:5 (8 tul solution + 32 ml dist. water).
Open th,. i.ta tap. Switch 'Fuel - on'. ()pen window to the burner chamber and press
until llame is burning.
Set the filter t 'K' (for potassium).
1. Insert tiibt: into Mane and set to O wtth 'blanc' regulator. Then insert 1u1ic into highest
staliday-f. and set to 100 with '5ensqivit3 - coarse - tine'. Repeat Wane setting, repeal sensitivity
setting until reading,- arc constant.
7, \l:uir stwdirit curve, then measure samples. Record, tite values on the appropriate form.
8. NV hen all samples are determined set filter to 'Na' (for sodium) and Catibrak he instrumenl.
as above f.point Nleasure standard curve and samples und record the
9, For ch. - g down first cios;., gas tap, then switch 'fuel - otr, then 'power-ofr
PARTICLE SIZE DETER N
o quipment
Stopwatch
iteATAB:
Pretreatment of Samples:
34
Removal of soluble salts:
pH>8.2 EC> 4 mS/cm (400 mS/m)
If no carbonates are present but the electrical conductivity exceeds 4 rnSicm, respec ve %
InSim soluble salts should be washed out:
Add approximately 200 ml Water to the samples, let stand for about two hours, stir
occasionally.
For precipitation add few ml saturated sodium chloride solution or acetone.
Centrifuge excess water, then continue with normal procedure.
35
Procedure:
Close the first cylinder with rubber stopper. Shake vigorously end over end for about 1 minute.
Make sure that the sample is completely dispersed.
Put cylinder back into waterbath, start stopwatch insert hydrometer carefully take 1. reading
after 41) Sec
('lose second cylinder, shake and put back into waterbath after precisely 2 min total time on
stopwatch. Insert hydrometer and read after 2 min 40 sec total time.
Wait until 4 min take 2. reading of 1. sample. Wait until 6 min take 2. reading of second
sample. During waiting shake third cylinder already. Put cylinder back into the bath after 8
min total time. Take 1. rea-ding after 8 ruin 40 sec.
Shake fourth cylinder and insert at 10 min, read at 10 min 40 sec, wait until 12 min, take
2. reading of third sample ,wait until 14 mm, take 2. reading of fourth sample, and so on.
Take the third reading after 4 hours settling time.
Starting I reading times for 24 samples see table 2.3.
Place a 53 micron test sieve in a large funnel into a sink equipped with a 'soil trap' to avoid
blockage of the drainage pipes.
Transfer sample from ineasuring cylinder on to sieve and rinse thoroughly with water until all
clay and silt fraction is washed out. (The water jet should not be too strong to avoid loss
of sand fraction due to splashing).
Wash sand fraction from sieve into beaker.
Place beaker on hot plate or drying oven to evaporate water.
36
4. Dry sieving of sand fraction:
Stack five test sieves 53, 106, 250, 500, 1000 p.m meshsize and a receiver pan.
Transfer sand fraction onto the top sieve (1000 p.m) and put onto sieve shaker.
Shake for about 5 min at an amplitude of 2.5-3 (amplitude scale is on sieve head).
Brush the fractions on separate large sheets of paper with smooth surface.
Clean sieves thoroughly.
(Do not use brass or steel brushes for sieves with nteshsize smaller than 500 micron).
Tare beaker then add fractions starting with receiver, then 53 jun. I:4;
Record each weight.
Lalculittions:
Sand Fraction:
37
This correction factor is based on the assumption that the determination of the sand fraction by
sieving is 'correct', no sand is lost during the procedures. It equalizes minor reading or rounding
errors since it is difficult to read a hydrometer more precisely than one unit.lf no soil hydrometers,
calibrated in g soil / liter are available, only hydrometers calibrated in specific gravity (g / liter)
the factor corrects the readings to % soil.
The correction factor using soil hydrometers should be in the range of 0.9 to 1.1,
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Table 2: Time table for hydrometer readings
Start stopwatch
Time : 0:00'00" hr:min'sec"
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