biomass lab · page 3 the biomass lab the biomass lab of department d3a, università politecnica...

Analysis, quality monitoring,

research and development

activities

—- Biomass Lab Notebook —-

March 2015

Biomass Lab

UNIVERSITÀ POLITECNICA DELLE MARCHE

Department D3A

Via Brecce Bianche

60131 – Ancona – ITALY Tel: (+39) 071 220 4167 - 4297

Fax: (+39) 071 220 4167

Email: [email protected]

Web: www.biomasslab.it/eng/

Biomass Lab

mailto:[email protected]

http://www.biomasslab.it/eng/

Biomass Lab – Department D3A - Università Politecnica delle Marche

The Biomass Lab

The Biomass Lab of Department D3A, Università Politecnica delle Marche in Ancona

is a unit of research, service and release of scientific information on the field of solid

and liquid biomasses for energy and industrial use.

The work unit is made up of a group of young researchers and technicians and has

facilities, equipment and instruments to address the main topics of research and

development involving materials, processes and systems on the biomass field.

The focus of our efforts is the lab itself combined with the ten-year experience of the

staff gained within the initiatives and services with our customers and partners and

national and international research projects.

All the proposals contained in this brochure are designed thinking about the needs

and problems of the sector and are conceived to facilitate the access to services

and research to the widest number of operators.

Prof. Giuseppe Toscano

Biomass Lab Manager

Via Brecce Bianche – 60131 Ancona – ITALY - Tel/Fax: (+39) 071 220 4167

Web: www.biomasslab.it/eng/; email: [email protected]



Analytical activities on solid biomass 6

Analysis of pellet quality 8

Analysis of liquid biomass 9

Analysis of the ashes quality 10

Combustion test and emissions analysis 11

Biomass monitoring in plant 12

Setting up of biomass lab in plant 14

Pellet and densified engineering 16

Vegetable oil extraction tests 17

Biomass upgrade by torrefaction and hydrothermal treatment 18

Sustainability assessment of biofuels 20

Development of new methods of biomass analysis 22

Performance testing of innovative instruments for the biomass

rapid analysis 23

Summary






The lab

The Biomass Lab has instruments and sys-

tems for the characterization of solid and

liquid biomasses for energy and industrial

use.

The analyses are conducted in accordance

with the latest national and European stand-

ards of the energy sector.

Reference standards

The Biomass Lab checks regularly the up-

date of the international standards on the

biomass quality following the activities of the

groups ISO / TC 238 - Solid biofuels and

CEN / TC 335 - Biomass standards through

the Italian Heat Technology Committee.

To correctly evaluate the solid biomasses the Bio-

mass Lab has already implemented the package of

standards UNI EN ISO 17225. For the liquid biomass

the reference is UNI / TS 11163: 2009.

Analyses on solid biomass

The analyses of the different chemical and physical parameters of a biomass allow

to know its technical, energetic and environmental performance. In the following

table the main characterization analyses conducted by the lab on solid biomass are

listed. Thanks to the experience of the working group, the lab is able to support us-

ers in selecting the type of analysis to be

performed and the right analytical ap-

proach to be followed depending on the

different needs and contexts.

In order to verify the quality of their anal-

ysis protocols and reliability of the results

the Biomass Lab undergo verification

tests organized by specialized institu-

tions within specific round robin tests.

Analytical activities on solid biomass

Analyses

The results of the analyses

The analytical process is completed

in the production of a report

containing the results of the

analyses. The report contains

information of the sample, the

laboratory standards and, if it is

considered necessary, the notes of

the operators.

The Biomass Lab is also available to

evaluate the results of the analyses

and to discuss possible actions to

be taken.

How to request the analysis and

send the sample

To request a quote or information on

o t h e r p a r a m e t e r s w r i t e a t

[email protected] or call the numbers

(+39) 071-2204167 or 071-2204297.

In addition to the quote the Biomass

Lab will provide information on the

delivery method, the amount of sample

to be sent and the time to return

results.

ANALYSES METHODOLOGY

Solid biomass sampling UNI EN 14778

Sample preparation UNI EN 14780

Moisture content UNI EN 14774

Ash content UNI EN 14775

Gross calorific value UNI EN 14918

Net calorific value UNI EN 14918

Carbon, hydrogen and nitrogen content

UNI EN 15104

Sulphur and chlorine content UNI EN 15289

Water soluble chloride and potas-sium

UNI EN 15105

Minor elements UNI EN 15297

Major elements UNI EN 15290

Bulk density UNI EN 15103

Particle size distribution UNI EN 15149-2

Content of volatile matter UNI EN 15148

Ash melting behaviour UNI CEN/TS 15370

Mechanical durability (pellet) UNI EN 15210-1

Diameter and length (pellet) UNI EN 16127

Fine particles (pellet) UNI EN 15210-1

Particles bulk density (pellet) UNI EN 15150






In the adjacent table the set of crite-

ria important to complete the analyti-

cal framework required by the stand-

ards on pellet and determine the

quality class are listed.

However, it is also possible to opt for

a partial characterization of the prod-

uct, selecting only the parameters

that are absolutely necessary to con-

trol the essential aspects of quality.

Aim

The aim is to enable the manufacturer or retailer, to provide guarantees about the

energy performance, the heating behaviour and the environmental aspects of the

product.

Biofuels of standard quality

In recent years the use of pellet and

densified biofuel has shown an in-

crease. The success is due to the qual-

ity standards, relatively high for this

category of products.

On the basis of different criteria UNI

EN ISO 17225-2 and 6 define the qual-

ity classes of pellets and densified.

The Biomass Lab could return a com-

plete characterization of these prod-

ucts and is able to verify compliance

with the quality classes provided by

law.

Analysis of pellet quality



Diameter and length (pellet) UNI EN 16127

Bulk density UNI EN 15103

Moisture content UNI EN 14774-1


Mechanical durability UNI EN 15210-1

Calorific value UNI EN 14918

Nitrogen content UNI EN 15104

Sulphur and chlorine content UNI EN 15289

Minor elements UNI EN 15297


Analyses

Analysis of liquid biomass

The list of the available anal-

yses is shown in the adjacent

table.

Aim

The aim is to provide a compre-

hensive quality framework,

useful both to verify compliance

with the specifications written

in energy recovery systems

which are intended and to have

guarantees about the energy

performance and the environ-

mental aspects.

Oil and natural fats

The main liquid biomass are vegetable

oils. They can be removed mechanical-

ly and/or chemically from oil crops

seeds or can derive from other produc-

tion processes (catering wastes or

residues of the food industry).

The main standard for the energy use

of oils and fats is UNI /TS 11163:

2009.

The Biomass Lab is able to character-

ize the liquid biomass and to verify the

compliance with the quality standards

of the energy conversion plants.


Ash content ISO 6884

UNI EN ISO 6245

Gross calorific value ASTM D240

Calorific value ASTM D240

Carbon, hydrogen and nitrogen CEN/TS 15104

Sample preparation Fats composition analysis

ISO 5509 ISO 5508

Content of volatile matter UNI EN ISO 662 UNI EN ISO 665

Thermogravimetric analysis Method in TGA – DTA

Density ISO 6883

UNI EN ISO 3675

Viscosity (between 20°C and 90°C) UNI EN ISO 3104

Acidity UNI EN ISO 660

Iodine value UNI EN ISO 3961

Water content UNI EN ISO 12937 UNI EN ISO 8534

Phosphorus ISO 10540-3

Sodium and Potassium UNI EN 14108 UNI EN 14109

Analyses






Chemical-physical characterization of

the ashes

The Biomass Lab can analyse both the ash

content and the quality of a biomass. In fact

the lab is equipped with instruments for chemi-

cal characterization and thermal behaviour of

the ash.

To perform this determination the Biomass Lab

uses analytical methodologies according to the

current technical standards (see table).

The ash issue

The presence of inorganic ashes in biofuels repre-

sents a very critical aspect for all energetic conver-

sion technologies. Besides being a combustion resi-

due which needs to be constant-

ly removed, the ashes are re-

sponsible for technical (fouling,

slagging, corrosion, fly ashes)

and environmental problems

(fine particles).

These critical issues are strictly linked to the chemi-

cal composition of the ashes, which is also respon-

sible for their thermal behaviour (fusion and volati-

lization temperatures).

Analysis of the ashes quality

Analyses





Mineral fraction UNI EN 15297

Water soluble chloride, sodium and potassium content

UNI EN 15105

Combustion test

and emissions analysis

Combustion test and emissions measurement

The Biomass Lab is equipped with portable instru-

ments for the emissions measurement (solids and

gases) released by biomass combustion devices,

allowing to perform in-situ emission sampling on

existing plants.

Moreover, the lab has a test bench for flue meas-

urement, consisting of:

a pellet stove (ca. 12 kWt) used to perform com-

bustion tests on pelletized material

a total flow dilution tunnel employed to measure

the total particulate, including the condensable

fraction (as required by Ministerial Thermic De-

cree December 28th, 2012), and the emissions

in non-steady state combustions.

Biomass domestic heating

The combustion of woody biomasses for do-

mestic heating (wood log, chips and pellet)

represents 14.5% of the total thermal energy

produced in Italy (ISTAT 2014) and is obtained

almost in low heat power domestic devices

(<35 kWt) such as fireplaces, stoves and boil-

ers.

Even though the biomasses are viewed with

particular interest due to their renewability

(directive 2009/28/CE) and cheapness com-

pared with fossil fuels, the high emission of

toxic compounds (e.g. fine PM, PAHs, CO, VOC)

associated to biomass combustion restricts their diffusion.

This issue is mainly associated with medium-low heat power appliances where the

combustion process is not well controlled and flue gas treatment devices are no

present.





Steps of the “monitoring plan”


Biomass monitoring

The monitoring of a biofuel produc-

tion process or energy production

process is dealt with a periodic sam-

pling of the biomass using methods

defined by appropriate normative.

The analytical characterisation in

laboratory of all the samples allows to

create a temporal database of those

chemical and physical parameters

related to the biomass quality.

The use of statistical tools such as control charts permits to verify whether the quali-

ty parameters fall within intervals of acceptability which are defined by the norma-

tive or by the producer itself. The use of control charts allows also to predict in ad-

vance a possible over limit and to take prevention actions.

Biomass monitoring in plant

Finding plant information

Selection of parameters

to be analysed

Sampling method

Laboratory analyses

Creation of control charts

The Biomass Lab proposes to:

create specific monitoring plans to reach the targets of the quality control with

low analytical costs

take representative biomass samples to be analysed or to train the operators in

the plant

analyse the samples for the selected parameters in accordance with current

normative

create specific control charts in order to monitor the process

Key targets for the plant

The results of the monitoring plan allow to:

keep the energy conversion process in efficiency and/or to assure the biomass

quality thanks to a preventive and planned control of the raw materials quality

control and classify the suppliers on the basis of the biomass quality delivered to

the plant

identify the biomasses that demonstrate to be more critical for a use in plant

demonstrate how to pursue targets about process quality or biomass quality.

Solutions






Why to install a biomass lab in plant?

Fast results of the analyses

Cost reduction of the analyses

Best monitoring of biomass quality

More effective environmental monitoring

and possibility to carry out self-

certification protocols

Arrangement for high level control sys-

tem promoting the technical support of

a specialized lab

Best decision-making capacity in the

field of biomass supply

Setting up of biomass lab in plant

The four step of Biomass Lab

intervention

1) Visiting plant: context analysis,

definition of objectives

2) Planning: identifying possible

technical solutions

3) Implementation: selection of sys-

tems and equipment and configura-

tion of the lab

4) Training: training of technical staff

Biomass Lab

Lab in plant

Analyses

The main analyses to im-

plement in plant

The lab in plant is set up to analyse only some of the analytical parameters of the

solid biomass, the ones most useful to provide a synthetic overview of the biomass

quality. The table shows some important parameters that can be easily determined

by a lab in plant.

The results of the analyses represent the most important information of the biomass

quality and allow to evaluate the product from a technical and economical point of

view.

ANALYSES INSTRUMENTS

Moisture Ventilated oven and balance

Particle size

distribution

Sieves, vibrating screen and

balance

Bulk density Cylindrical bin and balance

Ash content Muffle and precision balance

Durability (pellet) Pellet durability machine,

sieve, balance

Example of lab in plant and

possible synergy with the

Biomass Lab

Analyses of the parameters not

considered in those performed in the

laboratory in plant.

Biomass sample

Lab in plant

Analysis of the biomass as received, evaluation and data storage.

Option: possibility to send a small quantity of sam-ple to Biomass Lab.





Pelletizing test

The Biomass Lab has several solu-

tions to densify lignocellulosic mate-

rials of different origin, both pure

and in mixture.

The pellet obtained is immediately

analysed in order to verify the com-

pliance to the required characteris-

tics.

Biofuels upgrade

Biofuels upgrade is the set of lab

activities that aims to improve the

biomass quality with respect to ash

fusibility and the behaviour in boiler.

The proper biomass mixture and the

use of inorganic additives allow the

production of a biofuel with less

problems of encrustation and fusi-

bility.


Densified biofuels

The biomass densification for the pro-

duction of pellet and briquettes for

energy use is a strategic step of the

biofuel production chain.

The improvement of this technique to

a wider range of raw materials sets

new needs in order to achieve stand-

ards of biofuel quality which have to

guarantee the best possible perfor-

mance.

For this reason the activities of the

Biomass Lab aim to raise the standards of the biomasses quality, in particular the

agricultural and agro-industrial ones, through pelletizing tests of mixtures and the

use of inorganic additives.

Pellet and densified engineering

Mechanical extraction

The production of vegetable oil by means of mechani-

cal extraction from oleaginous seeds represents a good

opportunity for small and medium agricultural farms.

The products, crude vegetable oil and extraction cake,

can be employed in different applications - food,

energy, zootechny, agronomy, etc. - according to

the starting seed type.

The Biomass Lab has carried out several tests on

different seeds employing some models of extrac-

tion press, with the aim of enhancing the process

knowledge and increasing the product quality.

The most important studied parameters affecting

the process yield and the product quality are seed

typology, extraction temperature and pressure.

Vegetable oil extraction tests

Mechanical press

Currently the Biomass Lab owns a mechanical press with a working capacity of 50-

60 kg/h employed to evaluate the vegetable oil extraction yields from different seed

typologies.

In recent years tests were mostly focused on seeds from experimental crops (e.g.

Brassica carinata), from extra-European crops (i.e. Jatropha) and seeds recovered

from agro-industry residues

(i.e. grapeseeds, tomato

seeds).

Soxhlet method

To assess the process yields

of mechanical extraction it is

fundamental to know the

potential seed oil content. To

this aim the Biomass Lab

performs chemical extraction

(with solvent) following the

Soxhlet Method. Reference

standard: UNI EN ISO 659.






Biomass upgrade by torrefaction and

hydrothermal treatment

Biomass upgrade

Since some years the Biomass Lab

is studying the biomass thermal

treatments and is carrying out

experimental tests on residuals of

solid biomasses from the food and

forestry sectors.

Thermal treatments of inter-

est

The torrefaction process consists

in subjecting the biomass at condi-

tions of temperature within 200-

300°C, inert environment and

atmospheric pressure. The pro-

cess upgrades the raw biomass

into a biofuel with a higher energy

content, a hydrophobic behaviour

and a higher resistance to the microbial degradation.

The hydrothermal treatment consists of a biomass carbonization performed in wa-

ter, at a relatively high pressure and temperatures within 180 and 260°C. This pro-

cess combines the torrefaction upgrades to the ash content reduction related to the

water leaching effect.

Biomass Lab systems and approach

The Biomass Lab owns the appropriate devices to

perform the biomass treatments and to measure the

properties of the products obtained.

The thermogravimetric analyser (TGA/DTA) studies the

biomass thermal behaviour and is useful to set suita-

ble experimental plans for the following reactor tests.

The Biomass Lab has two bench reactors, one to per-

form lab-scale tests and the other one bigger, express-

ly constructed to treat enough quantities of raw mate-

rials in order to analyse some special parameters on

the torrefied products.

Torrefied biomass: upper class biofuel

By means of the biomass thermal treatment it is possible to obtain an upper class

biofuel, with a higher energy density, a hydrophobic behaviour, biologically stable,

easy to grind and standardisable.

Wood hydro-treatment

The thermal treatments in an aqueous medium can find interesting applications as

a pre-treatment of woody biomass for the production of high quality pellets and

briquettes.

On a poor biomass (e.g. wood chips rich in bark or soiled) this process can

determine a calorific value increase as well as an ash content decrease that can

make possible the production of an upper class pellet.

Analysis of physicochemical parameters

Analyses are carried out follow-

ing the national and European

standards of the energy sector.

The overall efficiency of the

treatments is estimated through

the analysis of mass and energy

balances while the biomass

quality upgrade is evaluated by

means of specific charts. The

results are collected in a specific

database and then compared

with the reference materials.

Upgrade





Sustainability

The sustainability concept involves

mostly environmental, economic,

social and institutional aspects, often

interrelated. Currently energy produc-

tion is one of the most important ac-

tivities where the application of the

sustainability concept is a priority.

The assessment of energy and envi-

ronmental sustainability, in particular,

is a useful tool to different aims, from

the optimization of processes and

production chains to marketing, from

the verification of compliance to limits

defined in specific standards to the

enhancement of the social acceptabil-

ity of a product.


Evaluation method

The sustainability assessment of products is more and more linked to LCA approach

(Life Cycle Assessment) taking into account the entire production chain, from extrac-

tion and production of raw ma-

terials to the production and

use of products. This approach

has become the standard one

when dealing with liquid biofu-

els (e.g. biodiesel and bioetha-

nol) and other biofuels (e.g.

pellet, agri-pellet, woodchip,

briquette, biogas). LCA analyses

are based on many information

related to the production chain,

a specific software for data

elaboration and updated data-

bases to convert input data in

impacts.

Sustainability assessment of biofuels

Solutions

Results

CO2eq saving and

energy balance have

been calculated for

d i f ferent b iofuel

production chains, in

particular for crop

residues and agro-

industry residues.

These evaluations are

usefu l a lso a t

enterprise level to

enh anc e en ergy

efficiency and to limit

e n v i r o n m e n t a l

impacts.

The Biomass Lab uses

the most updated LCA

software and database.

The research activity

conducted on biomass

and biofuels has pro-

duced many data and

reliable information,

useful to the LCA study

development.

Biomass Lab staff took part in technical standardization development at national

and international level on biomass and biofuels sustainability issues. The team thus

can properly deal with these topics.

0

10

20

30

40

50

60

70

80

90

SCENARIO A SCENARIO B RIFERIMENTO FOSSILE

Global Warming Potential (g CO2eq/MJ)

0,0

0,2

0,4

0,6

0,8

1,0

1,2

1,4

SCENARIO A SCENARIO B RIFERIMENTO FOSSILE

Cumulative Energy Demand (MJX/MJ)

Sustainability of pellet from vineyard pruning

CO2eq Savings 75% Energy balance 1:5






Development of new methods of biomass

analysis

Instruments for fast biomass analysis

The Biomass Lab, being for years close to industries and their issues, is equipped

with instruments suitable for developing fast

biomass quality analyses, in particular:

a Fourier Transform Infrared Spectrometer

(FT-IR) for analysis of solids in mid- and near-

infrared

devices for rapid measure of moisture

content in solid biomasses

a thermogravimetric/differential thermal

analyser

Furthermore, the lab offers a calibration ser-

vice of analytical methods by means of com-

parison with the standard methodologies.

Analysis of the biomass quality

The energetic biomass market is facing

a rapid expansion in response to the

increasing global energy demand and

the simultaneous needing to reduce

greenhouse gases emissions. In this

context, the determination of biofuel

quality, according to technical stand-

ards, is a fundamental requirement to

protect the final users and the environ-

ment. At present, the quality control of a

biomass is performed by specialized

laboratories and requires the determina-

tion of different physical-chemical pa-

rameters obtained with analytical methodologies which are time- and money-

consuming, often incompatible with industrial needs. For this reason it is important

to develop fast analytical techniques, preferably non-destructive, which not require

skilled operators.

Experience for innovation

The Biomass Lab offers its wide experience in the field of the biomass analysis to

identify and test innovative analytical solutions and to develop new methods of anal-

ysis, more rapid, cheap and efficient than the reference ones.

The interest about systems and devices for rapid analysis is increasing in order to

meet the growing need of the

biomass plants, as well as of the

biofuels industry, to quickly ana-

lyse certain quality parameters

(such as moisture, ash and ener-

gy content) just after the feed-

stock delivery.

In consideration of that, the Bio-

mass Lab aims to identify, devel-

op or simply test new analysis

instruments designed to meet

the specific needs of the opera-

tors.

Some examples of alternative analytical methods

The Biomass Lab has recently developed a simplified method for the analysis of the

ash melting point of the pellets. The analysis protocol has been developed by the

Lab thanks to the experience acquired

during the participation to the International

r e s e a r c h p r o j e c t A s h M e l T

(www.ashmelt.eu).

The Biomass Lab has also collaborated

with known companies of the national en-

ergy sector to identify and test some devic-

es for the rapid moisture content analysis

of the biomass. Different kind of instru-

ments have been tested to measure many

types of biomass at different moisture

degrees. The results were then compared

with those obtained with the reference

method to check their reliability.

Performance testing of innovative

instruments for the biomass rapid analysis





Department D3A Via Brecce Bianche – 60131 Ancona – ITALY

B iomass Lab

Tel: (+39) 071 220 4167 – (+39) 071 220 4297

Fax: (+39) 071 220 4167

Email: [email protected]

Web: www.biomasslab.it/eng/



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