WOOD PELLETS

QUALITY CONTROL

Roger Mertens
10th of June 2010

WHO IS INSPECTORATE
A staff of over 5000 people.
Global inspection and testing in over
100 countries
countries.
A global network of laboratory and
sample preparation facilities.
A wide range of commodities.
commodities

ISO 17025 (Accreditation)

ISO 17025 (Accreditation)

ISO 17025 (Accreditation)

SUBJECTS
1 General requirements
1.
requirements.
2. Requirements for trace elements.
3. Pellets particle size requirements.
4. Sampling.
5. Theoretical approach - some terms from ISO 18283.
6. Sample preparation.
7. Analysis.
8. Repeatability reproducibility.
9. Size distribution.
10. Fiber particle size.
11. Mechanical durability.
y
12. Bulk density.
13. Visual aspect - conclusions.

General Requirements
Parameter

Norm M 7135

DIN 51731

Electrabel

Diameter D

4 10 mm

4 10 mm

< 10 mm

Length L

5 x D mm

< 50 mm

< 40 mm

Dust content
Moisture

< 10 %
< 10 %

< 12 %

< 10 %

Ash

< 0.50 %

< 1.50 %

< 1.50 %

Sulphur (S)

< 0.04 %

< 0.08 %

< 0.2 %

Nitrogen (N)

< 0.3 %

< 0.3 %

< 0.5 %

Fluoride (F)
Chloride (Cl)
Nett calorific value
Press aids

< 70 ppm
< 0.02 %

< 0.03 %

< 0.05 %

> 18 MJkg

17.5 19.5 MJkg

> 16 MJ/kg

<2%

Not allowed

Vegetable oils

AFT (DFT) red. atm.

> 1200 C

Phosphor (P)

< 300 ppm

Bulk density

> 600 g/l

Requirements for Trace Elements

Element

DIN 51731

Electrabel

A
Arsenic
i (A
(As))

< 0.8
0 8 mgkg
k

< 2 mg/kg
/k

Cadmium (Cd) + Titanium (Ti)

< 0.5 mgkg

< 1 mg/kg

Chrome (Cr)

< 8 mgkg

< 15 mg/kg

Copper (Cu)

< 5 mgkg

< 20 mg/kg

Lead (Pb)

< 10 mgkg

< 20 mg/kg

Mercury (Hg)

< 0.05
0 05 mgkg

< 0.10
0 10 mg/kg

Zinc (Zn)

< 100 mgkg

< 20 mg/kg

EOX
Benzo-a-pyrene
Penta-chlore-phenol

< 3 mgkg
< 0.5 mg/kg
< 3 mg/kg

Pellets Particle Size Requirements

Size

Electrabel

< 4 mm

100 %

< 3 mm

99 %

< 2 mm

95 %

< 1.5
1 5 mm

75 %

< 1 mm

50 %

Sampling
According CEN/TS 14778-1 (NTA 8202)
Size of increments (in liter):
V min = 0.5

for d 10 mm.

V min = 0.05 x d

for d 10 mm.

Sampling
From a falling stream

On stopped or moving conveyor

Sampling
Number of increments (n)

Sampling
Number of increments (n)

Stationary material

Moving material

Group 1

n = 5 + 0.025 x M lot

n = 3 + 0.025 x M lot

Group 2

n = 10 + 0.040 x M lot

n = 5 + 0.040 x M lot

Group 3

n = 20 + 0.060 x M lot

n = 10 + 0.060 x M lot

Sampling of Small Stock Piles (< 100 m3)

Increments in function of the volume (weight) per section.

section
If the material in the pile is segregated, move the material into
a new pile and take increments during the removal.

Sampling of Large Stock Piles

Visual inspection if there are regions containing significantly
different material.
pile formed?
How was the p
With a conical heap, coarser particles tend to collect at the
outside and at the base and finner particles collect in the
interior of the pile
pile.

Some Terms From ISO 18283

Primary increment variance VI

Some Terms From ISO 18283

Preparation and test variance VPT

Some Terms From ISO 18283

Overall precision PL

Sample Preparation
According CEN/TS 14780
Main purpose of the sample preparation:
Mass-reduction of the sample by division.
Particle size-reduction
size reduction of the sample.
sample
Keeping all the sub-samples representative for the original sample.

Sample Division
Manual cooning and quartering

Sample Division
Riffle dividers

Sample Division
Rotary dividers

Sample Division
Rotary dividers

Particle size-reduction
Cutter mill

Analysis
Total moisture (Mar):
Norm CEN/TS 14774-1 : reference method.
Drying at 105 C in air atmosphere till constant weight and
including a procedure for buoyancy effects.

Norm CEN/TS 14772-2 : simplified method.

Drying at 105 C
C in air atmosphere till constant weight
weight.
Sample
p weight
g in both cases minimum 300 g and p
preferably
y more than
500 g.
Thickness maximum 30 mm.
Loading of the dishes or trays about 1 g/cm2.

Analysis
An unusual expression:
Total moisture on wet basis ((Mar) and on dry
y
basis (Ud)
The reference method CEN/TS 14774-1 expresses the
relationship between moisture on dry and on as received
basis:
Ud = (Mar x 100) / (100 Mar)
Mar = (Ud x 100) / (100 + Ud)

Analysis
Moisture in the analysis sample (Mad):
Norm CEN/TS 14774-3
Drying at 105 C in air or nitrogen atmosphere till
constant
t t weight.
i ht
Particle size maximum 1 mm.
Loading of the dishes or trays about 0
0.2
2 g/cm2.
Sample weight minimum 1 g.

Analysis
Ash content (Adb):
Norm CEN/TS 14775
Heating at 550 C
C or 815 C
C (ISO 1171) till constant weight
weight.
Particle size maximum 1 mm.
Loading of the dishes or trays about 0.1 g/cm2.
Sample weight minimum 1 g.

Analysis
Ash content (Adb):
Possible differences between 550 and 815 C:
Loss of volatile inorganic compounds.
Further oxidation of inorganic compounds.
D
Decomposition
iti off carbonates,
b
t
fforming
i CO2.

Analysis
Volatile matter (Vd):
Norm CEN/TS 15148
Heating at 900 C
C for 7 minutes
minutes.
Particle size maximum 1 mm.
Sample weight between 0.9 1.1 g.
Oven temperature to be regained
within 4 minutes after insertion
of a cold stand and its crucibles.

Analysis
Total sulphur (S) and chlorine (Cl):
Norm CEN/TS 15289 (two steps or automatic equipment)
Two steps:
1. Digestion of the pellets and transfer of acidic gaseous
components into solution.
2. Determination of sulphate and chloride in the receiving
solution.
solution

Analysis
Total sulphur (S) and chlorine (Cl):
Automatic equipment:

Analysis
Total carbon (C) hydrogen (H) and nitrogen (N):
N
Norm
CEN/TS 15104 ((automatic
t
ti equipment)
i
t)
Burning the sample in pure oxygen.
Measuring the resulting gasses of CO2, H2O and N2

Analysis
Calorific value:
Norm CEN/TS 14918 (automatic equipment)
Gross calorific value (GCV) dry at constant volume (qV,gr,d).
Burning a pellet of the sample in a bomb calorimeter (add a
spike) and measuring the temperature rize
rize.

Analysis
Calorific value:
Net calorific value ((NCV)) at constant volume (qV,net,m
V net m)).
In cal/g or kcal/kg:
q V,net,m = [ q V,gr,d (49,2 x Hd) ] x [(100 MT) / 100 ] - 5,51 x MT

In J/g or kJ/kg:
q V,net,m = [ q V,gr,d (206 x Hd) ] x [(100 MT) / 100 ] - 23,0 x MT

Analysis
Calorific value:
Net calorific value (NCV) at constant pressure (qp,net,m).
In cal/g
q p,net,m = {q V,gr,d - 50,6 x w(H)d - 0,19 x [w(O)d + w(N)d ] } x [(100 - MT) / 100 ] - 5,83 x MT

In J/g
q p,net,m = {q V,gr,d - 212 x w(H)d - 0,8 x [w(O)d + w(N)d ] } x [(100 - MT) / 100 ] 24,43 x MT

Analysis
Major, minor and trace elements:
Depending on the element to be measured:
Digestion of the sample in a closed vessel.
Fl i off the
Fluxing
th ashes
h iin Pt di
dishes.
h
Measurement:
Flame atomic absorption (FAA).
Graphite furnace atomic absorption (GFAA).
Inductive coupled plasma (ICP)

Repeatability - Reproducibility
Parameter

Repeatability

Reproducibility

Total moisture

Not applicable

Not applicable

Ash content < 10 %

0.2 % absolute

0.3 % absolute

3 % of the mean result

4 % of the mean result

Sulphur or chlorine 500 mg/kg

50 mg/kg

100 mg/kg

Sulphur or chlorine > 500 mg/kg

10 % of the mean result

20 % of the mean result

Carbon

0.5 % absolute

1.5 % absolute

Hydrogen

0.25 % absolute

0.5 % absolute

Nitrogen 0.5 %

0.05 % absolute

0.1 % absolute

Nitrogen > 0
0.5
5%

10 % of the mean result

20 % of the mean result

120 J/g

300 J/g

Volatile matter

GCV - NCV

Size Distribution
Norm CEN/TS 15149-1
Oscillating screen method using sieve apertures > 3.15 mm.
A minimum sample size of 8 liter.
Round holes.
Moisture content < 20 %.
Manual or mechanical sieving allowed.
Horizontally oscillating (one or two dimensial).

Size Distribution
N
Norm
CEN/TS 15149
15149-2
2
Vibrating screen method using sieve apertures < 3.15 mm.
A minimum sample size of 50 g.
Combination of round and square holes.
Moisture content < 20 %.
M
Manual
l sieving
i i nott allowed.
ll
d
Recommended for sawdust:
3.15 mm round, 2.8 2.0 1.4 1.0
0.5 and 0.25 mm square wire cloth.

Size Distribution
N
Norm
CEN/TS 15149
15149-3
3
Rotary screen method

Fiber Particle Size (Meal Spectrum)

Grinding finer produces better quality pellets.
The following spectrum should be approached:

>3

mm Up to

1%

23

mm Up to

5%

12

mm Around

20 %

0,5 1

mm Around

30 %

0,25 0,5 mm Around

24 %

< 0,25

mm Not less than 20 %

Fiber Particle Size (Meal Spectrum)

Fib particle
Fiber
ti l size
i

Mechanical Durability DU
N
Norm
EN 15210
15210-1
1
Collision against each other and the walls of a specified
rotating test chamber.

Test portion 500 10 g > 3,15 mm round holes .

500 rotations at 50 2 rpm.
DU = (mA / mE) x 100
Electrabel requirement: > 94 % and < 98 %.

Bulk Density
N
Norm
EN 15103
Cylindric bucket of 5 l or 50 l.
A ratio height to diameter between 1,25 and 1,50.
Free falling from a height of 15 cm for the settling of the pellets.
Bulk densities:
# Pellets about 650 kg / m3.
# Fraction < 3,15 mm about 400 kg / m3.
g / m3.
# Fraction < 1,00 mm about 320 kg

Visual Aspect - Conclusions

The visual aspect of the wood pellets is the first quality control.
The colour is an indication if more than one type of wood has been
used.
Due to the big difference in bulk density is it hard to estimate the
undersize visually.
visually
Wet spots are easy to detect, due to colour difference or
g
of the p
pellets.
desintigration
Wood pellets have to be concidered as dangerous, due to possible
CO gas formation in closed spaces.

Visual Aspect - Conclusions

Check for free water in barges, because this can accelerate the
danger of self combustion.
Tempeature monitoring is strongly advised:
20 40 C Enzymatic heat.
40 75 C Microbiological heat.
> 75 C

Chemical heat.

SELF COMBUSTION AT..?