06Analysis of Wastes-2013

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Curso DoctoradoAnalysis of Wastes

September 2013

ABF-BOKU / Erwin Binner page 1

1 Erwin Binner LIMA 2013

Analysis of WastesAnalysis of Wastes

Institute of Waste Management

Erwin Binner MSc.Erwin Binner MSc.BOKUBOKU--UniversityUniversity / Vienna/ Vienna

Institute of Waste ManagementInstitute of Waste Management

Marion Huber-HumerGudrun Obersteiner

Peter BeiglErwin BinnerKatharina BhmRobert GlanzMarlies HradGnther KrausSandra LebersorgerPeter LechnerSabine LenzRoland LinznerPeter MostbauerFlorian PartAndreas PertlStefan SalhoferSilvia ScherhauferElisabeth Schmied

Felicitas SchneiderThomas EbnerReinhold OttnerJ ulia NowotnyZoricaStamenkovic

Mathias StiedlDavid WiederschwingerJ ulia Zeilinger


Outlook

Sampling of Wastes

Waste Composition

Sampling of Compost

Pretreatment of Samples

Analysis of Different Parameters (for Compost) from

Fresh Laboratory Sample

Dried Laboratory Sample

Analysis Sample

New Methods (FTIR, Thermogravimetry)

(Laboratory ABF-BOKU)

(Pilot Plant Station ABF-BOKU)


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Analysis ofAnalysis ofWastesWastes

WHY??WHY??


Waste AnalysisPurpose

survey of basic data for:

planning

determination of material flows

choice and dimension of waste treatmentfacilities and waste collection systems

optimisation, check of efficiency

assessment of the efficiency of existingcollection systems

identification of weak points and improvementpossibilities


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Waste AnalysisAims

waste prevention orientated

e.g. identification of preventable waste streams

recycling orientated

e.g. quality of separately collected recyclables,collection rates, waste potentials

disposal orientated

planning of routes and facilities, development of new

technologies, trend analysis in long-term planningsocio-scientific

consumer habits, identification of common disposalpatterns in certain socio-economic groups


Waste AnalysisAims

data needed for planning:

waste amount waste collection,design of treatment plants

design of treatment plants,potential of recovery

effects on environment,effects of already donemeasures

waste compositionpotential of hazardous comp.(heavy metals, organiccompounds, gas formationpotential)

waste compositionmaterial groups (paper,plastic, glass, metals, )


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Waste AnalysisAims

optimising waste treatment processes:

milieu conditions

degradability,possibility for recyclingcalorific value

degradability duringcomposting and MBT

rotting conditions,degradation status,emissions

characteristics of wastes

organic compounds,type of organic compounds


Waste AnalysisAims

assessment of products after wastetreatment:

compost qualitylandfill propertiesstabilityquality of products forrecycling

quality of products


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Waste AnalysisAims

assessment of landfill behaviour:

gas formation (degradability),leachate (solubility),odourmechanical stabilitysettlement

control atlandfill sites


Analysis of WastesAnalysis of WastesWHERE??WHERE??


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productio

n

use

recycling

residual

waste use?

biogasbiogas

Waste Management ConceptMunicipal Solid Waste (MSW)

recycling

compostinganaerobic treatment

soil

thermal treatment

thermal treatment

composting

MSW incineration landfill

landfill

anaerobic treatment

biogenous

resources

resources

con-sumption

productio

n

recycling

separate

collected

biowaste

separate

collection

SS

SS = sewage sludge

MBT = mechanical

biological pretreatment

excavated soil

construction anddemolition waste

reuse

recycling

landfill

landfill

MBT


Waste Collection in AustriaSeparate Collection (Definitions)

Municipal Solid Waste

(MSW)

Bio-Waste Paper

Residual Wastes

recycling

Recycling Banks

Glass Plastics Metals

composting

treatment

treatmentlandfill

Collection Centers

Hazardous

Household Wastes

Bulky Wastes

Electronic Wastes


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productio

n

use

recycling

residual

waste use?

biogasbiogas

Waste Management ConceptMunicipal Solid Waste (MSW)

recycling

compostinganaerobic treatment

soil

thermal treatment

thermal treatment

composting

MSW incineration landfill

landfill

anaerobic treatment

biogenous

resources

resources

con-sumption

productio

n

recycling

separate

collected

biowaste

separate

collection

SS

SS = sewage sludge

MBT = mechanical

biological pretreatment

excavated soil

construction anddemolition waste

reuse

recycling

landfill

landfill

MBT


Sampling of WastesMunicipal Solid Wastes (MSW) - Delivery

photo: Erwin Binner


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Sampling of WastesMunicipal Solid Wastes (MSW) - Delivery

photo: Binner, 2008


Sampling of WastesFractions for Recycling after Sorting

photo: Binner, 2008


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Sampling of WastesBiowaste Delivery

photo: Binner, 2008


Sampling of WastesBiowaste Compost

photo: Binner, 2010


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Sampling of WastesSewage Sludge Composting

photo: Binner, 2009


Sampling of WastesMechanical Biological Treatment

photo: Binner, 2009


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Sampling of WastesWastes from Abandoned Sites

photo: ABF-BOKU


Analysis of WastesAnalysis of WastesWHEN??WHEN??


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Sampling of WastesBefore Turning

if we want information about inhomogeneities

photo: Erwin Binner


Sampling of WastesAfter Turning

if we want information about average

photo: Binner, 2009


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Sampling of WastesAfter Turning

if we want information about effect of turning

e.g. water additionphoto: Binner, 2009

26 Erwin Binner LIMA 2013ABF BOKU Skripten\520-338-komp\Abb-englisch\MBA-OPUDO.cdr

MagneticSeparator

Magnetic Separator

Sewage Sludge

Oversized Particles>65mm

DANO - Rotary Drum24-36 hours

Flip-Flow Screen

Density Separator

Oversized Particles>25mm

Hard Inorganics

Pressure AeratedRotting Platform10 Weeks

Waste Air

Waste Air

Waste Air

Feedstock

Weak PressureAerated

Rotting Plattforn10-20 Weeks

Waste Delivery(bunker)

Landfill

Biofilter

Sampling of WastesDuring Movement of Material


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Analysis of WastesAnalysis of Wastes

HOW??HOW??


Sampling of Wastes

wastes in most cases are

very inhomogeneous

particle size

water content content of hazardous compounds

the problem is to get athe problem is to get a

representative samplerepresentative sample


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Waste AnalysisSampling of MBT Wastes

same sampling procedure for all

possible parameters

representative samples

inhomogeneity of wastes

big particle size (up to 100 mm)


Sampling of WastesSampling Concept

first we need a plan (concept):

goal of investigation (why)

which parameters do we have to analyse

- needed sample amount

- adequate pre-treatment and stabilisation ofsamples

knowledge about properties of waste

- homogeneity

- bulk density

- maximum grain size, grain size distribution


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Sampling of WastesSampling Concept

first we need a plan (concept):

how to do sampling

- location and date of sampling

- proper tools for sampling

execution of sampling

- journal of sampling (note important items)

- taking sub-samples- mixing sub samples to field sample

- laboratory sample

- retain sample


Statistic Procedure: -NORM EN 14899Increment Sample Mixed Sample

Increment 1

Increment 2

Increment 3

Increment 4

Increment 5Increment 6

Mixed Sample

photo: Erwin Binner


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Statistic Procedure: -NORM EN 14899Sample Size (Amount)

94 l54 l43 l11.5 l3.5 l0.5 lvolume ofsample

66 kg38 kg30 kg8 kg2.4 kg0.3 kgamount ofsample

60 mm50 mm40 mm30 mm20 mm10 mmmax. grainsize (MBT)

pCV

pgDMsam

2

3

95

)1()(

6

1

Msam minimum amount for sample, in gD95 max. grain size (95-Perzentil), in cm density of particles, in g/cm3g factor for grain size distribution

p m/m percentage of particles with defined characteristic

CV wanted coefficient of variation


Sampling of WastesSimplification - Example MBT Wastes

statistical point of view for sampling:

total waste amount and maximum grain sizedetermine:

- number of qualified single samples resp. increments

- amount (volume) of qualified single samples resp. increments

7 to 10150 m3 to 2.200 m3100 to 1.500 t

4 to 615 m3 to 150 m310 to 100 t

2 to 35 m3 to 15 m33 to 10 t

1 qual. single samplesup to 5 m3up to 3 t

each qualified single sample consists of 6 to 10 increments


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Statistic Procedure: -NORM EN 14899Increment Size (Amount)

6

inc 101M

Minc minimum amount for increments, in kg

bulk density of waste, in kg/m3

for D95 < 3 mm

example: = 500 kg/m3 Minc = 0.5 g


Statistic Procedure: -NORM EN 14899Increment Size (Amount/Volume)

3

95

8395

9 107.2)3(10 DDMinc

Minc minimum amount for increments, in kg

D95 max. grain size(95-Perzentil), in mm (MBT 10 to 60)

bulk density of waste, in kg/m3 (MBT ~ 700)

for D95 > 3mm

6 l3.5 l2.0 l1.0 l0.2 l0.05 lvolume ofincrement

4.1 kg2.4 kg1.2 kg0.5 kg0.15 kg0.02 kgamount ofincrement



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Sampling of Wastes / Example MBT WastesIncrement Size (Amount/Volume)

5.1 l4.3 l3.4 l2.6 l1.7 l0.9 lvolume ofincrement

3.6 kg3.0 kg2.4 kg1.8 kg1.2 kg0.6 kgamount ofincrement


Minc minimum amount of increment, in kg

max. grain size, in mm

Minc = 0.06 x max. grain size


Sampling of WastesExample MBT Wastes Size Reduction

1,500 t MBTwaste

max. grain size

= 60 mm

10 qualifiedsingle samples,10 increments

(6 l) each< 20 mm

Coningand Quartering

10 qualified single samples 50 bis 100 l

100 lshredder

Coning

and Quartering

10l

laboratorysample


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costs

approx. 10,000

cutting area

850 x 350 mm

l:b:h =1,100 : 1,000 : 2,250 mm

Sampling of WastesExample MBT Wastes Size Reduction

photo: Binner, 2004


mix all the increments and build a cone

divide the cone into 4 similar parts

throw awaythrow away2 parts (1+3)2 parts (1+3)

mix the othertwo parts(2+4) carefully

divide again into4 similar parts

throw away 2 partsthrow away 2 parts

mix the other two parts carefully

repeat as often as necessary

Sampling of Wastes - Example MBT WastesConing and Quartering Procedure

coning and quartering procedure:


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Sampling of Wastes - Example MBT WastesConing and Quartering Procedure

photo: ABF-BOKU


Pretreatment ofPretreatment ofWaste SamplesWaste Samples


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Pretreatment of WastesPretreatment Concept

again we need the plan (concept):

goal of investigation



- adequate pre-treatment

- adequate stabilisation of samples


Oversized

Particles

Physical

Contaminants


pretreatment depends on parameters whichare to be analysed

fresh laboratoryfresh laboratory

samplesample (shredded < 20 mm):

dried laboratorydried laboratory

samplesample

(air dried, 45C, 105C):

prepared (milled)

Analysis sampleAnalysis sample


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Pretreatment of WastesPretreatment Concept - Stabilisation

depending on parameter:

biological parameters- + 4 C for max. 24 hours

- freezing - 22 C

NH4-N, NO3-N- freezing - 22 C as fast as possible

plant germination, water content, bulk density- + 4 C for 7-10 days

most other parameters- drying at 45 C resp. 105 C


Sampling of WastesPretreatment of Samples - Grinding

grinding samples happens step by step:

Shredder(for grinding of wet samples)

~ 10,000 photo: Binner, 2004


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Sampling of WastesPretreatment of Samples - Drying

temperature for drying depends on volatility:

105105CC (for water content andmost parameters)

4545CC (for volatile substances)

airair--dryingdrying (for humic acids becausechange of colour showshigher results using thephotometric method)

photo: Binner, 2003


J aw Crusher (to 1 mm) for hard and brittlewastes (slag, concrete)

AnalysisPretreatment of Samples - Grinding

photo: Binner, 2009


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Retsch SM 2000~ 10,000

Cutting Mill (for grinding of dried samples < 1 mm)

photo: Binner, 2009






Agate Vibratory Disk Mill(for further grinding < 0,5 mm)

dried at 45C (or air-dried)

Retsch RS 1~ 10,000

for heavy metals: volatile (Hg, Cd) orcontamination by Centrifugal Mill (Cr, Ni, Mo, Fe)

for humic acids: change of colour whentemperature > 45C

photo: Binner, 2003


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Agate Vibratory Disk Mill(for further grinding < 0,5 mm)

dried at 45C (or air-dried)

for heavy metals: volatile (Hg, Cd) orcontamination by Centrifugal Mill (Cr, Ni, Mo, Fe)

for humic acids: change of colour whentemperature > 45C

for all

others

Retsch ZM 1000~ 3,500

RetschZM1

Centrifugal Mill(for further grinding < 0,5 mm)

samples dried at 105C

photo: Binner, 1989


Ultra-Centrifugal-Mill


photo: Binner, 2009


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Sampling of WastesPretreatment of Samples - Elution

elution procedure depends on parameterswhich are to be analysed

media for elutionmedia for elution

deionised water carboxylic acids, conductivity,soluable compounds (Landfill Ordinance)

CaCl2 NH4-N, NO3-N, pH (OE-NORM)pyrophosphate humic acidsCAL-Extract PCAL, KCAL

time of elutiontime of elution

1 hour NH4-N, NO3-N (OE-NORM)2 hours pH, PCAL, KCAL (OE-NORM)3 hours conductivity (OE-NORM)24 hours soluable compounds (Landfill Ordinance)



100 g solid

sample

+ 1,000 ml

deionised

water

photo: Binner, 2006


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photo: Binner, 2006


30 min. with 6,000 rpm

Centrifugation

photo: Erwin Binner, 2006


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Sampling and Pretreatmentof WastesConclusions

sampling concept

goal of investigation, parameters, location, time,needed equipment,

information about waste (max. grain size resp. itsdistribution, homogeneity, physical requirements)

calculation of minimum sample amounts, number

of increment samples, number of qualified mixedsamples, number and amount of laboratory

sample

sample stabilisation (cooling 4C, freezing -20C)


Sampling and Pretreatmentof WastesConclusions

sample pretreatment

which parameters should be analysed

stabilisation of samplesdrying, cooling 4C, freezing -20C

drying temperatureair drying, 45 C, 105 C

equipment for grinding (size reduction)Centrifugal Mill (contamination, heat), Agate Vibratory Disk Mill

elution media and perioddeionized water, CaCl2, pyrophosphate,


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Analysis ofAnalysis ofWaste CompositionWaste Composition


Waste AnalysisWaste Separation Analysis (WSA)

in order to obtain data on waste amounts andcomposition one possibility is to carry out aWaste Separation Analysis (WSA)

Austrian Standard (NORM S 2097) definition WSA: quantitative and qualitative

determination of waste fractions obtained bysorting of waste

a WSA consists of the sorting and an analysis ofspot samples


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Waste Separation Analysis (WSA)Procedure

motive / goal(accuracy)

sampling scheme(universal set, where to take samples and how many, which

fractions to analyse (products, materials) etc.)

sampling(and documentation)

sorting of samples

analysis of results

report


Scale

Sieving


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Waste Separation Analysis (WSA)Setting

photo: ABF-BOKUphoto: ABF-BOKU


Waste Separation Analysis (WSA)Sorting Table

photo: ABF-BOKU


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Waste Separation Analysis (WSA)Sieving

photos: ABF-BOKU


Waste Separation Analysis (WSA)

photo: ABF-BOKU


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Waste Separation Analysis (WSA)Sorting

Quelle: ABF

photo: ABF-BOKU


Waste Separation Analysis (WSA)Sorting

photo: ABF-BOKU


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Waste Separation Analysis (WSA)Fractions (e.g. 26 different fractions)

photos: ABF-BOKU


Examples: Food in Residual Waste and Bio-Bins in Food Retail Shops

photos: ABF-BOKU


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Waste Separation Analysis (WSA)Examples: Milk Products in Residual Waste

photos: ABF-BOKU

72 Erwin Binner LIMA 2013Photos: Lebersorger, Albrecht

Waste Separation Analysis (WSA)Examples: Meat in Residual Waste

photo: ABF-BOKU


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Waste Separation Analysis (WSA)Examples: Sweets in Residual Waste

Photos: Lebersorger, Albrecht

photos: ABF-BOKU


Waste Separation Analysis (WSA)Examples: Bread in Residual Waste

Fotos: ABF

photos: ABF-BOKU


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Analysis ofAnalysis ofCompostCompost


Sampling ofSampling ofCompostCompost


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Analysis of CompostSampling

sampling procedure:

compost piles never are homogenous -there are differences in:

water content

nutrient content

density

air supply temperature

degradation rate

pH-value

..


Analysis of CompostSampling

information aboutrotting (milieu)

conditions

sampling procedure depends on wanted

information:

analysis ofsingle samples

analysis of

mixed samples

information about

degradation rate or

content of harmful

substances


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Analysis of CompostMeasurements / Temperature

sampling procedure single samples:

to get information about homogeneity of milieuconditions

we need measurements (e.g. temperature, oxygencontent within the pores) at several points of the pile

photo: Erwin Binner


Analysis of CompostMeasurements / Temperature

Testotherm700

~ 600 photo: Erwin Binner, 2008


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Analysis of CompostMeasurements / Gas in the Pores

MLU LMSx~ 4,500



again we need the plan (concept):

goal of investigation



- adequate pre-treatment

- adequate stabilisation of samples


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Oversized

Particles

Physical

Contaminants


pretreatment depends on parameters whichare to be analysed


samplesample (shredded < 20 mm):

dried laboratorydried laboratory

samplesample

(air dried, 45C, 105C):

prepared (milled)

Analysis sampleAnalysis sample


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Analysis of CompostSampling / Mixed Samples

sampling procedure mixed samples:

to get information about whole pile

we need an average sample by mixing lots of increments

for each 200 m3 compost 1 profile

3 profiles minimum from each pile

from each profile 6 increments (~2 l)

mixing of all (minimum 18) increments

using cross mixing procedure


Analysis of CompostSampling / Mixed Samples

sampling procedure mixed samples:

example: volume of pile = 700 m3

we need an average sample by mixing

the 24 increments (~48 l)

4 profiles

6 points or

photo: Erwin Binner


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mix all the increments and build a cone

divide the cone into 4 similar parts

throw awaythrow away2 parts (1+3)2 parts (1+3)

mix the othertwo parts(2+4) carefully

divide again into4 similar parts

throw away 2 partsthrow away 2 parts

mix the other two parts carefully

repeat as often as necessary

Analysis of CompostSampling / Coning and Quartering Procedure

coning and quartering procedure:


Pretreatment ofPretreatment ofSamplesSamples


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Oversized

Particles

Physical

Contaminants

Analysis of CompostPretreatment of Samples

pretreatment depends on parameters which areto be analysed


samplesample (sieved


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Analysis of CompostPretreatment of Samples - Drying

temperature for drying depends on volatility:

105105CC (for water content andmost parameters)

4545CC (for volatile substances)

airair--dryingdrying (for humic acids becausechange of colour showshigher results using thephotometric method)

photo: Binner, 2003


Analyses ofAnalyses ofCompostCompost


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Analysis of CompostWater Content

Water Content (WC)


500 - 1,000 g (balance accurate to 0.1 g)

drying at 105 C until weight is constant (24 - 48 hours)

weighing again (warm, because material catches water fromatmosphere)

100 * (weight100 * (weight wetwet weightweight drydry))weightweight wetwetWC [% WM] =WC [% WM] =

result in: % WM (wet matter) accuracy: 1 decimal place (e.g. 25.4 %WM)

repetitions: 2 allowed difference: +2.5 %


Respiration Activity by SapromatExecution / Water Content

Balance BA 160B~ 2,300

photo: Binner, 2011


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Analysis of CompostWater Content

Memmert UML 800 ~ 3,500

Memmert UM 600 ~ 1,600

photo: Binner, 2011


Analysis of CompostWater Content / Calculation


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Analysis of CompostWater Capacity

Water Capacity (WCAP)

Fresh Laboratory Samplefilled in cylinder

compaction by falling 2 * 10 times 5 cm

cylinders in water bath, saturating over night

cylinders on sand bed for 3 hours (covering with plastic)

weighing, drying (105C), weighing

result in: % DM (dry matter) accuracy: no dec. place (e.g. 125 %DM)


weightweight capacitycapacityweightweight drydryWWCAPCAP [% DM] =[% DM] = -- 100100


Analysis of CompostWater Capacity

photo: Binner, 1989


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Analysis of CompostBulk Density

Bulk Density ()

weightweight wetwet [kg][kg]

volume [l]volume [l]Bulk DensityBulk Density [kg WM / l] =[kg WM / l] =

result in: kg WM / l accuracy: 2 dec. places (e.g. 0.75 kg WM/l)

repetitions: 3 (2) allowed difference: +5 %


filling in plastic cylinder (1,000 ml)

compaction by falling10 times 10 cm

weighing (balance accurate to 0.1 g)


Analysis of CompostBulk Density / Calculation


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Analysis of CompostBulk Density

Vol = 840 ml

photo: Binner, 1989


Analysis of CompostpH-Value

pH-Value (pH)

Analysis Sample< 0.5 mm

10 - 20 g (balance accurate to 0.1 g)

adding 100 - 200 ml (1:10) calcium-chloride (CaCl2*2H2O)for self monitoring use of deionised water is allowed

shaking for 2 hours

calibration of pH-meter (pH standards 4 / 7 or 7 / 10)keep standards in refrigerator (+ 4C)

measuring solution with pH-meter (compensated to 20C)result in: - comp. to 20C accuracy: 1 decimal place (e.g. pH = 7.5)



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range 7-10

range 4-7

Analysis of CompostpH-Value

WTW 532~ 1,150

temperaturePT 100

pH-unitE 56

photo: Binner, 2006


Analysis of CompostConductivity

Conductivity (Cond)

Analysis Sample< 0.5 mm

10 - 20 g (balance accurate to 0.1 g)

adding 100 - 200 ml (1:10) deionised watershaking for 2 hours

measuring solution with conductivity-meter (compens. to 20C)

if conductivity-meter compensates to 25C, the result is to bemultiplied with 0.905

result in: mS/cm (comp. 20C) accuracy: 1 decimal place (3.2 mS/cm)



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Analysis of CompostConductivity

WTW LF92~ 500

Seibold LTP

photo: Binner, 1998 photo: Binner, 2006


Analysis of CompostAmmonia-Nitrogen

Ammonia Nitrogen (NH4-N)

Fresh Laboratory Sample(stabilised - 22C)

50 g (balance accurate to 0.1 g)adding 200 ml calcium-chloride (1.84 g CaCl2*2H2O / l)for self monitoring use of deionised water is allowed

eluting for 1 hour (over head shaker)

filtration > 50 ml (SCHLEICHER & SCHLL 595 )

measuring as fast as possible (or stabilisation at - 22C)


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Analysis of CompostAmmonia-Nitrogen

distillation with steam (see nitrogen according to Kjeldahl)

Ionchromatograph

Test-Kits (Merckoquant 10024)

Photometer (adding chemicals, green colour, 655 nm)

0.78 * C [mg/l NH0.78 * C [mg/l NH44] * Dil. * 100] * Dil. * 100

2.5 * 1,000 * (1002.5 * 1,000 * (100 -- water content)water content)NHNH44--N [% DM] =N [% DM] =

result in: % DM (dry matter) accuracy: 3 dec. places (e.g. 0.050 % DM)

repetitions: 3 (1) allowed difference: not declared

methods:

C = concentration in the filtrate Dil. = factor of dilution0.78 = factor for calculation from NH4 to NH4-N


Analysis of CompostNitrate-Nitrogen

Ionchromatograph

Test-Kits (Merckoquant 10020 or 8032)

Photometer (2.6-dimethilenol, red colour, 324 nm)0,23 * C [mg/l NO0,23 * C [mg/l NO33] * Dil. * 100] * Dil. * 100

2.5 * 1,000 * (1002.5 * 1,000 * (100 -- water content)water content)NONO33--N [% DM] =N [% DM] =


repetitions: 3 (1) allowed difference: not declared

methods:

C = concentration in the filtrate Dil. = factor of dilution0.23 = factor for calculation from NO3 to NO3-N


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Analysis of CompostAmmonia and Nitrate-Nitrogen / Calculation


Analysis of CompostPhotometer

photo: Binner, 2006


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Analysis of CompostNH4-N and NO3-N - Ionchromatograph

Autosampler7,000

Dionex DX 12030,000

possible parameters:

NO3, NO2, PO4, Cl-, SO4,

NH4, Ca, K, Mg, Na,

photo: Binner, 2006


Analysis of CompostLoss of Ignition

Loss of Ignition (LOI) = Volatile Solids

Analysis Sample(< 0.5 mm)

10 g (balance accurate to 0.01 g) into ceramic pot (DIN 12904)

drying at 105 C for 3 hours (determination of ResidualWater)

weighing again after cooling in desiccator (otherwise materialcatches water from atmosphere)muffling at 350C for 3 hours in order to prevent

temperatures > 550C by Calorific Value of the sample

after 3 hours muffling at 550C for 5 hours

or muffling by heating to 550C over a period of 5 hours


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time [hours]

sampletemperature[C]

300

600

100

200

400

500

550C

stop at 350Cfor 3 hours

3

quick heating to 550C

ignition of

sample

calorific value of

sample



Loss of Ignition (LOI)

after muffling (in most cases over night)

weighing again (cooling in desiccator!)

keeping residue of ignition for determination of carbon

100 * (weight100 * (weight drydry weightweight 550550CC))

weightweight drydryLOI [% DM] =LOI [% DM] =

result in: % DM (dry matter) accuracy : 1 dec. place (e.g. 35.7 % DM)

repetitions: 3 (2) allowed difference: +2.5 %


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AND FA 200~ 2,500

photo: Binner, 2006



Naber L9~ 1,400

photo: Binner, 2006


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Naber L9~ 1,400

photo: Binner, 2006


Analysis of CompostLoss of Ignition / Calculation


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Analysis of CompostTotal Organic Carbon

Total Organic Carbon (TOC)


0.5 g (balance accurate to 0.0001 g) into steel pot

putting on auto-sampler

incineration at 900C, measuring CO2 (and N) byheat conductivity detector

result = total carbon = TCresult = total carbon = TC (% DM)

repeating procedure with 0.5 g residue of ignition at 550C

result = inorganic carbon = TICresult = inorganic carbon = TIC (% LOI)



Total Organic Carbon (TOC)

calibration by L-glutamin-acid (C = 40.78 and N = 9.52 %DM)

calculating difference: TC TIC = TOC

result in: % DM (dry matter) accuracy: 1 dec. place (e.g. 15.4 % DM)

repetitions: 3 allowed difference: +5 %

CCTCTC * 100* 100

(100(100 content of Residual Water)content of Residual Water)TC [% DM] =TC [% DM] =

CCTICTIC * (100* (100 Loss of Ignition)Loss of Ignition)

100100TIC [% DM] =TIC [% DM] =


61/102


September 2013




VARIO MAXCNS

41,000

Balance3,000 photo: Binner, 2006



VARIO MAXCNS

41,000

photo: Binner, 2006


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September 2013



Analysis of CompostCarbonate

Carbonate (CaCO3)

calculated by using TIC



CCTICTIC [%] * (100[%] * (100 Loss of Ignition)Loss of Ignition)

0.120 * 1000.120 * 100CaCOCaCO33 [% DM] =[% DM] =

C = measured concentration TIC0.12 = factor for calculation from C to CaCO3




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September 2013



Analysis of CompostTotal Nitrogen

Nitrogen according to Kjeldahl (NKj)

by heating to 650C for 2-4 hours (until solution looks likemilk) Nitrogen is transformed into Ammonia

adding: 50 ml H2O70 ml NaOH (33 % sodium hydroxide)one drop of Tashiro-indicator (in boron sol.)


1 g (balance accurate to 0.01 g) into glass tube (250 ml)

adding: 15 ml H2SO4 (95 % sulphuric acid)+1Kjeldahl pastille

5 minutes steam distilling into 30 ml solution of boron (2 %)



Nitrogen according to Kjeldahl (NKj)

by steam distilling, Ammonia is transformed into Ammonia-boron

Ammonia-boron is titrated with HCl (0.1n hydrochloric acid)colour changes from violet into dark green

amount of HCl is measured

0.14007 * (amount of HCl) * 1000.14007 * (amount of HCl) * 100

samplesample--weightweightdrydry** (100(100 cont. ofcont. ofResidResid. Water). Water)NNKjKj [% DM] =[% DM] =




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September 2013






Total Nitrogen (NTOT)

is calculated by:

NNTOTTOT

==NNKjKj

+ NH+ NH44--N + NON + NO

33--NN

measured directly by VARIO MAX as:

NDUMAS

or

CCNN * 100* 100

(100(100 content of Residual Water)content of Residual Water)NNDUMASDUMAS [% DM] =[% DM] =


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September 2013




Gerhardt SMA 12/HT~ 5,200 photos: Binner, 2006



Gerhardt WD 12~ 5,000

photos: Binner, 2006


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September 2013



Analysis of Wastes(Heavy) Metal Analysis

digestion for heavy metal analysisAnalysis Sample(< 0.5 mm)

2.0 g (balance accurate to 0.001 g) into digestion glass

adding: 40 ml of aqua regia (HNO3 : HCl = 1:3)and boiling stones

apply water cooler and cooling trap (filled with diluted HNO3)

boiling for 2 hours, afterwards cooling to room temperature

washing cooler with: HNO3 from cooling trapand deionized water

filtering digestion solution into volumetric flask

filling up with deionized water to 100 ml



measuring the solution by AAS

AAS = Atomic Absorption Spectrophotometera hollow-cathode lamp (one lamp for each element) sends

light beam, with spectrum of the element (e.g. Chromium)which is to be measured

molecules in sample-solution are atomized by nebulizer andburner(acetylene + air or acetylene + nitrous-oxide (N2O) as fuel)

Cr atoms absorb light, by this the intensity of the light beamis reduced (the more Cr atoms the merrier reduction)

by measuring standard solutions (e.g. 10 mg Cr/l) andsample solutions, the concentration of Cr in the samplesolution can be calculated [In mg/l]


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September 2013




sample

air or N2O

acetylene

discharge

bluff bodies

Flame

nebulizer

light beam

source:



Cr [mg/kg DM] =Cr [mg/kg DM] =

C [mg/l Cr]C [mg/l Cr] * Dil. ** Dil. * 1,0001,000 ** 1001001010 * sample* sample--weightweightdrydry [g][g]** (100(100 Residual Water)Residual Water)

result in: mg/kg DM (dry matter) accuracy: depends on amount

repetitions: 3 allowed difference: 5 20 %

calculation of heavy metal content in waste:

C = concentration in the solution Dil. = factor of dilution

1,000 = g kg 10 = ~2 g solids in 100 ml l


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September 2013




accuracy: depends on amount

1,00050010050

1051

0,1

accuracy

7,5005,000 - 10,0003,6001,000 5,000

270100 - 500

650500 1,000

15,000> 10,000

6550 - 100371 - 500,5


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September 2013



Analysis of Wastes(Heavy) Metal Analysis / Digestion

fume hood

heaterphotos: Binner, 2006


Analysis of Wastes(Heavy) Metal Analysis / Digestion

aqua regia

cooling trap(filled with HNO3)

water cooler

heater

filtration

filling up to100 ml



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September 2013



Analysis of Wastes / (Heavy) Metal AnalysisAtomic Absorption Spectrophotometer (AAS)

flowmeterfor acetylene

+ air (orN2O)

sample

mixingchamber

burner

hollow-cathodelamp

light beam

Perkin Elmer20,000 photos: Binner, 2006



measuring the solution by ICP-AES

ICP-AES =inductive coupled plasma atomic emissions spectrometry

molecules in sample-solution are atomized by nebulizer andArgon-plasma-gas (5,000 to 10,000K)

by atomization, atoms (e.g.: Cr) emit (send out) light of (forCr) specific wave length,(the more Cr atoms the merrier emission)

by measuring standard solutions (e.g. 10 mg Cr/l) andsample solutions, the concentration of Cr in the samplesolution can be calculated [in mg/l]

advantage of ICP is, that many elementscan be measured in one step


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September 2013



Analysis of Wastes(Heavy) Metal-Analysis (ICP-AES)

inductive coupled plasma - atomic emissions spectrometry



Analysis of CompostPhysical Contaminants

Physical Contaminantsoversized particles > 25 mm

glass in fraction > 2 mm

plastics in fractions > 4 mm and > 20 mm

ferrous metals and non ferrous metals in fraction > 6.3 mm


repetitions: 1 allowed difference: not determined

~ 500 - 1,000 g dried laboratory sample(105C)

sieved according DIN 4198 (0,63/2/4/6,3/8/11,2/16/20/25mm)

sorting contaminants by hand

total sample weight + weight of the different contaminants


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September 2013



Analysis of CompostPhysical Contaminants

Prfgertegesellschaft RT405-7~ 2,500



Analysis of CompostPlant Germination Test

Plant Germination Test


mixing sample to Standard Substrate (0/15/30/45% sample)

Standard Substrate = Fruhstorfer Soil : brick-powder= 1:1applying in Neubauer glass pots (120 mm * 60 mm)

silica sand (100-200 g)

sample mixture (~200 g)

test-plants: 0.4 g Lepidiumsativum= cressor 0.3 g Phleumpratense = grass, accurate to 0.01 g

silica sand (100 g)

50-100 ml water, until sample mixture is saturated


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September 2013




each mixture is tested in triplicate

covering pots by plastic until plants germinate (~2 days)

notice germination delay against 0 % compost variant (days)

plants remain in a bright room (green house) at ~20C

every 1-2 days irrigating of plants

harvesting after 9-11 days (cress) and 18-20 days (grass)

weighing plant massassessment of germination rate (how many seeds havegerminated)



100 * (germination100 * (germination mixturemixture))

germinationgermination blancblancplant germ. [% of blanc]plant germ. [% of blanc]

==



for assessment:

average of the 3 repetitions is to be compared to the

average of the 3 blank (100% standard substrate / 0%compost) which define 100%100 * (weight100 * (weight mixturemixture))

weightweight blancblancplant mass [% of blanc] =plant mass [% of blanc] =

result in: % from blank accuracy: no decimal place (e.g. 99 %)


germ.germ. mixturemixture germ.germ. blancblancgermination delay [days] =germination delay [days] =


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September 2013



Analysis of CompostPlant Germination Test Cress Test




sample

15 %

30 %

45%blank

(100% substratephotos: Binner, 2010


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September 2013




20C - light 16 hours / dayphotos: Binner, 2010





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September 2013






Analysis of CompostPlant Germination Test (ON S 2023)


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September 2013



ReactivityReactivityof Wastesof Wastes


Self HeatingSelf HeatingTestTest


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September 2013



Reactivity of WastesSelfheating Test Status of Rotting





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September 2013



Reactivity of WastesSelf Heating Test Status of Rotting

Self Heating Test in Dewar-Bottle

Sample 425/8-12

0

10

20

30

40

50

60

70

80

0 1 2 3 4 5 6 7 8 9 10 11 12 13 14

test duration [days]

temperature[C]

repetition 1

repetition 2



Finished

CompostTmax = 20 - 30 C

Rottegrad V

Rotting Status V

Finished

CompostTmax = 30 - 40 C

Rottegrad IV

Rotting Status IV

Fresh CompostTmax = 40 - 50 CRottegrad III

Rotting Status III

Fresh CompostTmax = 50 - 60 CRottegrad II

Rotting Status II

FeedstockTmax = 60 - 70 CRottegrad I

Rotting Status I


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September 2013



New MethodsNew Methods


Infrared-Spectroscopy

Thermal Analysis

New Methods for Waste AnalysisWhat s New?

photos: Smidt, 2009


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September 2013



New Methods for Waste AnalysisHow to Characterize

source: Smidt, 2009


physical characterization:

color: green

length: 45 cm

width: 55 cmheight: 105 cm

chemical characterization:

LOI: 28,8 %

TOC: 14,9 %

TN: 1,62 %AT4: 2,3 mg O2 / g DM

New Methods for Waste AnalysisHow to Characterize

FTIR-spectrum


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September 2013



emission

diffuse Reflection

(DRIFT)

transmission

reflection

attenuated totalreflection (ATR)

FTIR: Fourier Transform Infrared SpectroscopyPrinciples of Infrared Measurement

source: Smidt et al., 2009


4000 cm-1

400 cm-1

sample spectrum

wavenumbe

r

FTIR: Infrared-Spectroscopy(Fourier Transform Infrared Spectroscopy)

Principle: Transmission



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September 2013


166 Erwin Binner LIMA 2013elektrial vector

+

-

dipole-moment

H

d-Cl

d+

Cl

H d+

d-

E

FTIR: Infrared-SpectroscopyInteraction of Infrared-Light and Molecules



400900140019002400290034003900

Wellenzahl (cm-1)

Absorbanz

R C N - R

O H

FTIR: Infrared-SpectroscopyInfrared Induces Vibration of Molecules

wave number [cm -1]

absorbance



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September 2013



Wellenzahl (cm-1)

Absorbanz

compost 23 days

compost 260 days

sewage sludge compost

biogenic material

amines

nitrate

carbonate

fingerprint region

wave number [cm -1]

absorbance

Quality of Compost / FTIR-AnalysisCharacterization of the Rotting Process

aliphatic methyl

bands

amides / aromatic amines

= easy degradable

org. compounds

inorganic compounds

silicates / carbonates



Infrared spectroscopic characteristics of thebiowaste composting process

400900140019002400290034003900

Wavenumber (cm-1

)

Absorbance 2850

140 d

56 d

1 d

280 d

2920

13841640

1540

1740

1420

12601320

1030

875

I IIIII

source: Bhm, 2009


85/102


September 2013



Quality of Compost / FTIR-AnalysisCharacterization of the Rotting Process

C-Ocarbonates875

Si-O, Si-O-Siclay-minerals1030

C-O-C, C-Opolysaccharides1250-900

() C-N(aromatic) amines1320

N-Onitrate1384

COO-

C-O

carboxylates

carbonate

1420-1430

amides II1570-1540

C=OC=C

amides I, carboxylatesalkenes, aromatic vibrations

1630-1650

aliphatic methylene groups2850

C-Haliphatic methylene groups2920-2925

O-Hbound and free

hydroxyl groups (water)3400

development

during rotting

process

vibrationsfunctional groups,

rsp. compounds

wave number

(cm-1)


Statistical ToolsPrinciple of Multivariate Data Analysis

??

J

I

data X

unmanageablepack of data

multivariatedata analysis

0.017

0.015

0.018

0.020

400

0.0270.026100

0.0280.0273

0.0270.0262

0.0230.0231

38993900samples

J

I

matrix of data

400900140019002400290034003900

Wellenzahl (cm-1

)

Absorbanz

source: Bhm, 2009


86/102


September 2013



0

0.5

1

1.5

2

2.5

3

3.5

0 0.5 1 1.5 2 2.5

distance to model "MBT"

dista

ncetomodel"compost"

MBT-Model

Compost Model

Classification of FTIR-Spectra by SIMCA(Compost MBT)

0

0,5

1

1,5

2

2,5

3

3,5

0 0,5 1 1,5 2 2,5


distancetomodel"compost"

MBT-Model

Compost Model

"unknown samples"

0

0,5

1

1,5

2

2,5

3

3,5

0 0,5 1 1,5 2 2,5


distancetomodel"compost"

MBT-Model

Compost Model

sewage sludge 1

anaerobic digestion 1

anaerobic digestion 2

sewage sludge 2

sewage sludge 3

both

none

source: Bhm, 2009


PLS-RegressionPrediction of Extractable Humic Acids (HA)

MODELL - PARAMETER:

number of samples =269

R2 = 0,87RMSEP =2,6 % oDM(=medium error)

advantage:

time

lower amount of chemicals

PLS-R = Partial Least Squares Regression

0

5

10

15

20

25

30

35

40

0 5 10 15 20 25 30 35 40

HA measured (% ODM)

HApredicted(%

ODM)

source: Bhm, 2009


87/102


September 2013



Prediction of the loss on ignition (LOI) and theTOC by FT-IR spectra

0

10

20

30

40

50

60

70

0 10 20 30 40 50 60 70

LOI measured (% DM)

LOIpredicted(%

DM)

0

5

10

15

20

25

30

0 10 20 30

TOC measured (% DM)

TOCpredicted(%

DM)

n =188n =427

source: Bhm, 2009


Prediction of total nitrogen (TN) andrespiration activity (RA4) by FT-IR spectra

0

0.5

1

1.5

2

2.5

3

0 0.5 1 1.5 2 2.5 3

TN measured (% DM)

TNpredicted(%

DM)

0

10

20

30

40

50

60

70

0 10 20 30 40 50 60 70

O2 uptake measured (mg g-1

DM)

O2uptakepredicted(m

gg-1D

M) n =115n =187


88/102


September 2013



thermal behavior depends ontemperature

measurement of different parametersis possible

Thermal AnalysisPrinciple


thermogravimetry

differential scanningcalorimetry (DSC)

mass-spectrum of allproducts ofcombustion

Thermal AnalysisPrinciple

photos: Smidt, 2009


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September 2013



rising temperature

ThermogravimetryPrinciple


ThermogravimetryEquipment

photo: Binner 2012


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September 2013



physical parameters are changed because of chemicalreactions during composting process change of energy-amount

different thermal behaviour (oxidative or pyrolytic) shows degradation rate, reactivity, stability

thermogram loss of weight during combustionDSC-curve energy-amount (heat-flow)mass-spectrum gaseous products of combustion

characteristic of ionic current

control of process and quality (e.g. composting),reactivity and effect of remidiation,combustion behaviour

ThermogravimetryPrinciple


Thermogravimetry ThermogramsQuality Controll of Composts

20

30

40

50

60

70

80

90

100

110

0 100 200 300 400 500 600 700 800 900

Temperatur (C)

Masseverlust(%

)

Frischmaterial

ReifkompostHS 45,8%oTM


Klrschlamm-kompost

temperature [C]

mass-loss[%

]

sewage sludgecompost

biogenic material

compostHA =45.8 %oDM

compostHA =19.7 %oDM

source: Smidt, 2009


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September 2013



Quality Control of CompostsDynamic Difference-Calorimetry (DSC)

-25

0

25

50

75

100

125

150

175

200

0 100 200 300 400 500 600 700 800 900

Temperatur (C)

DSC(mW)

Frischmaterial



Klrschlamm-kompost

temperature [C]

DSC[mW]

sewage sludgecompost

biogenic material

compost (humification)HA =45.8 %oDM

compost (mineralisation)HA =19.7 %oDM

source: Smidt, 2009


LaboratoryLaboratory


92/102


September 2013



Laboratory ABF-BOKUDigestion Laboratory

fume hoods

storage for bases

storage for acids

storage for solvents

balance

NKJ -distillation

NKJ -digestion

photos: Binner 2006


Laboratory ABF-BOKUDigestion Laboratory

storage for solventsstorage for waste chemicals photos: Binner 2006


93/102


September 2013



Laboratory ABF-BOKUMeasuring Laboratory

Ionchromatograph

balance samples forWater Content

pH-meter

photo: Binner 2006


Laboratory ABF-BOKUCleaning / Gas-Distribution

storage for deionised water

deioniser

dish washer storage for gasphotos: Binner 2006


94/102


September 2013



Laboratory ABF-BOKUSample Storage

freezer -22C

storage for Analysis Samples

photos: Binner 2006


Equipment forEquipment forLaboratory TestsLaboratory Tests


95/102


September 2013



Laboratory TestsComposting System

.

.

valve

water

airdistribution

temperature

plasticscreen

airsupply

feedmixturevolume~7l

Laboratory reactor system

.

.

.

.

.

valve

water

air distribution

temperature

plastic screen

air supply

feed mixturevolume ~7l


.

.

.

.

.


Laboratory TestsComposting System / Climate Chamber

photos: Binner 2006


96/102


September 2013



Laboratory TestsComposting System / Rotting Reactor

photos: Binner 2006


Laboratory TestsComposting System / CO2-Measurement

CO2-measuring unit (infrared)

switch for 6 test cellsphotos: Binner 2006


97/102


September 2013



0,0

0,5

1,0

1,5

0 2 4 6 8 10 12 14 16 18 20

Duration of the composting process [days]

C-degradationrate[gC/kgC

Input.h]

Aceticacid[%D

M]

4,0

5,0

6,0

7,0

8,0

9,0

C-degradation rate

pH-Value

pH-Value

C-Degradation Rate, Acetic Acid and pH-ValueTest s eries 2 / Batch 1

0,0

0,5

1,0

1,5

0 2 4 6 8 10 12 14 16 18 20



Input.h]

Aceticacid[%D

M]

4,0

5,0

6,0

7,0

8,0

9,0

C-degradation rate

pH-Value

pH-Value


Laboratory TestsComposting System / Calculation

0,0

0,5

1,0

1,5

0 2 4 6 8 10 12 14 16 18 20



Input.h]

Aceticacid[%D

M]

4,0

5,0

6,0

7,0

8,0

9,0

C-degradation rate

Acetic acid

pH-ValuepH-Value


lag -

phase

exponential

ph

ase

end of intensivedegradation phase


Laboratory TestsOdour Emissions

0

200

400

600

800

1.000

1.200

1.400

1.600

0 2 4 6 8 10 12 14 16 18 20


NH4-N[mg/kgDM

].

4,0

5,0

6,0

7,0

8,0

9,0

NH4-N

pH-Value

pH-Value[-]

Ammonia Nitrogen and pH-ValueTest s eries 6 / Batch 2


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September 2013



0

2.0004.000

6.000

8.000

10.000

12.000

14.000

16.000

18.000

0 2 4 6 8 10 12 14 16 18 20


[ppmDM]resp.

[mg/10.m

3wasteair.

h]

0

200

400

600

800

1.000

1.200

[Odourunits/m

3wasteair]

Olfactometer [OU/m3 ]

Odor EmissionsTest ser ies 2 / Batch 2

0

2.0004.000

6.000

8.000

10.000

12.000

14.000

16.000

18.000

0 2 4 6 8 10 12 14 16 18 20


[ppmDM]resp.

[mg/10.m

3wasteair.

h]

0

200

400

600

800

1.000

1.200

[Odourunits/m

3wasteair]

Acetic acid - waste air

[mg/10m3 waste air . h]



Laboratory TestsOdour Emissions

0

2.0004.000

6.000

8.000

10.000

12.000

14.000

16.000

18.000

0 2 4 6 8 10 12 14 16 18 20


[ppmDM]resp.

[mg/10.m

3wasteair.

h]

0

200

400

600

800

1.000

1.200

[Odourunits/m

3wasteair]Acetic acid - waste air

[mg/10m3 waste air . h]

Acetic acid - solid matter [ppm DM]




0,0

0,5

1,0

1,5

2,0

2,5

0 2 4 6 8 10 12 14 16 18 20

Duration of the Composting Process [days]


Input.h]

4,0

5,0

6,0

7,0

8,0

9,0

Degradation rate, high O2

pH-Value

C-Degradation Rate and pH-ValueTest series 2 / Batch 1 and 4

0,0

0,5

1,0

1,5

2,0

2,5

0 2 4 6 8 10 12 14 16 18 20



Input.h]

4,0

5,0

6,0

7,0

8,0

9,0


Degradation rate, low O2

pH-Value


Odour Emissions - Laboratory TestsInfluence of Oxygen Supply

0,0

0,5

1,0

1,5

2,0

2,5

0 2 4 6 8 10 12 14 16 18 20



Input.h]

4,0

5,0

6,0

7,0

8,0

9,0


Degradation rate, low O2

pH-value, high O2

pH-value, low O2

pH-Value



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September 2013



Odour Emissions - Laboratory TestsInfluence of pH-Value

Without lime

0,0

0,5

1,0

1,5

2,0

2,5

0 2 4 6 8 10 12 14 16 18 20

Duration of the Com posting Process [days]

C-deg

radationrate[gC/kgC

Input.h]

Without lime

Carbon Degradation RateTest ser ies 2 / Batch 4 to 6

without lime

0,0

0,5

1,0

1,5

2,0

2,5

0 2 4 6 8 10 12 14 16 18 20



Input.h]

Without lime

0.2% lime


0.2% lime

without lime

0,0

0,5

1,0

1,5

2,0

2,5

0 2 4 6 8 10 12 14 16 18 20



Input.h]

Without lime

0.2% lime

0.4% lime


0.4% 0.2% lime

without lime


Laboratory TestsComposting System

.

.

valve

water

airdistribution

temperature

plasticscreen

airsupply

feedmixturevolume~7l


.

.

.

.

.

valve

water

air distribution

temperature

plastic screen

air supply

feed mixturevolume ~7l


.

.

.

.

.


100/102


September 2013



Laboratory TestsComposting System / Climate Chamber

photos: Binner 2006


Laboratory TestsComposting System / Rotting Reactor

photos: Binner 2006


101/102


September 2013



Laboratory TestsComposting System / CO2-Measurement

CO2-measuring unit (infrared)

switch for 6 test cellsphotos: Binner 2006


Laboratory TestsLandfill Simulation / Leachate / Temperature

photos: Binner 2006


102/102


September 2013


Thank Youfor YourAttention

Thank Youfor YourAttention

[email protected]://www.wau.boku.ac.at

Documents

06Analysis of Wastes-2013