TOC_Comments_Handling_phaseII-TG5

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Comments table TOC second consultation
MB
1
DIN
Cluster
Paragraph
0
Type of
comment
t
DIN
0
t
DIN
0
t
DIN
0
t
Comment (justification for
change) by the MB
Possibly validation data are
available from ISO 10694
The subtraction of quantified
amounts of elementary carbon is
permitted. This sentence is
important to handle the results of
the ongoing method development
on Elementary carbon (EC) in
waste (TC 292WG5). There has
to be an option to subtract EC
from TOC within the TOC
standard. This may be of
relevance for soil too.
Apart from classical techniques
for the determination of TOC in
solids there are currently systems
for TOC in water available, which
allow to analyze solids as
suspensions after ultra turrax
treatment. This should be
considered in the procedural
section.
In TC 292 any new standard
contains an annex “summary of
general requirements and
recommendations” which contains
a table with information especially
regarding the circumstances of
sampling, storage, sample
preparation and bottle material.
Proposed change by the MB
Project Horizontal observations
soil;validated;ISO 10694
Point taken to be evaluated Upps.
Recom.: validated data can be taken
as a references in the Foreword (see
table) The TG appricaites the work of
TC 292.
Change only if data are suitable.
The subtraction of quantified amounts
of elementary carbon from TOC
results is permitted.
Relevant instruction to be included. :
Upps. Recom.: The substraction of
Elementary Carbon will be added as
a note equal to EN 13137; The
substraction of EC shall be reported.
Either add sentences to permit new
techniques or broaden the procedural
description regarding this new option.
Would need validation: Upps. Recom.:
As the dicription of the method and
the validation data are not present at
the meeting the suspention will not be
included; Lab's can participate in the
validation with this method; In case of
satisfying results it will be added as an
annex.
Add an annex containing general
information.
Standard to be edited according to
fina lguideline for writing horizontal
standards
Comments table TOC second consultation
MB
1
DIN
Cluster
Paragraph
1
5.1 and
5.2
AFNOR
5.17
5.1 and
5.3
Type of
comment
e
Comment (justification for
change) by the MB
It is important to mention other
compounds here (for regulators)
even though they are mentioned
under “Interferences”.
te
The document allows the
determination of organic carbon
on fresh or dried soils. There is a
great risk that two laboratories
apply different pre-treatment and
in that case, the reproducibility of
the determination will decrease (R
will increase, if reproducibility is
assessed as required by
ISO 5725-2). Furthermore it is
more difficult to produce
homogeneous sample out of fresh
soil compared to dried soil.
Therefore test portions produced
from fresh soil are less
representative for the sample
than those made out of dried
soils.
We point out that organic carbon
content in soils is often in the
range of 10 g.kg-1 to 30 g.kg-1,
which is rather low compared to
the content of sludge or organic
wastes. The management of
organic C in agricultural soils
requires determination with low
uncertainty : a difference of a few
g.kg-1 in organic content can have
important consequences on the
diagnosis and on the
Proposed change by the MB
Project Horizontal observations
Coal, charcoal (elemental carbon)
and inorganic carbon compounds
except of carbonates will be
determined as organic carbon when
present in the sample.
We ask for a rewriting of the text to
ensure the use of dried samples pretreated according to ISO 11464 as the
only possibility for the determination
of TOC on soils.
…and inorganic carbon compounds
except of carbonates.. to be inserted
For soils, dry samples must be used
(as proposed for pH).The proposal is
to have separate standards for each
matrice.
text to be revised accordingly
text to be revised accordingly
Comments table TOC second consultation
MB
1
Cluster
Paragraph
Type of
comment
Comment (justification for
change) by the MB
management of the organic
carbon of the soils, in the field of
soil fertility as well as in that of the
soil function as a carbon source
or sink (global warming).
5.3
G
The use of method « A » when
TIC/TOC >10 lead to important
uncertainty on the TOC measure.
Method « B » must be more
accurate in this case than method
« A », since there is no error on
the determination of TIC. This is
not true for the tests presented.
The use of phosphoric acid to
eliminate carbonate should be
discussed. The kinetic of the
dissolving reaction may be much
longer. At least diluted chlorhydric
acid should be mentioned.
according to this standard
according to this standard
Note: not necessary and partly
not quite correct
7.13
T
AT
3.2
ed
AT
5.1
te
Proposed change by the MB
Project Horizontal observations
From previuos text
From previuos text
-revised earlier in desk study; to be
discussed.
Skip repetition
OK
Skip note
for discussion: Upps Recom: this note
has become irrelevant because of the
incorporation of ISO 10693 in this
standard (see other comment).
Comments table TOC second consultation
MB
1
NL
Paragraph
5.1
Type of
comment
ed
Comment (justification for
change) by the MB
A remark should be placed to
warn for high inorganic carbon
concentrations; in that case
method B is preferred
Proposed change by the MB
Project Horizontal observations
Remark: in samples with relative high
inorganic carbon concentrations,
method B is preferred if possible
AT
6
te
Amendment for clarification
AT
7
ge
AT
7.1
te
This document describes partly
procedures for specific apparatus.
But this document should only
focus on procedures which have
a directly influence on the result.
All other steps should be used as
an informative annex.
Specific calibration reagents are
specified; other ways of
calibration should be allowed.
Depending on the experience of the
lab with high carbonate contents the
procedure may lead …
The precise instruction for sample
pre-treatment, calibration and
measurement is part of the
informative annex. Some of the
described procedures are only for
specific apparatus.
Proposal included - To be discussed.
Upps Recom.: Method B is only
applicable if the lab is well
experienced; Separate determination
acc. To ISO 10693 is to be preffered.
OK - clarification to be inserted
AT
7.2
ed
CaC03 - not 0  O
CaCO3
to be discussed; Upps. Recom.: the
calibration must be done with well
known substances that are stable and
pure. the substances used for
calibration cannot be the same as
those for control or as sample.
ok
AT
7.3
ed
Na2C03 - not 0  O
Na2CO3
ok
AT
7.10
ed
A12O3 - not 1  l
Al2O3
ok
AT
9
te
Sampling and sample pretreatment should be the same as
for other standards. –
… as homogeneous as possible
 of course!
Relationshiop with sampling / pretreatment standard is not
mentioned
The whole number can be
abbreviated
To be coordinated with standard on
pre treatment
NL
Cluster
9.1
Te
Additional sentence: other
substances, which guarantee correct
calibration (e.g. tested flour), are
allowed.
Ad this relationship (standard for
pretreatment is still under construction
in Horizontal, but shoild be mentioned
here in 9.1)
?
Comments table TOC second consultation
MB
1
Cluster
5.17
AT
5.17
Paragraph
9.2
Type of
comment
te
9.2
te
10.1.1
11.1.1
te
Comment (justification for
change) by the MB
Permission to use dried soils is
given at the beginning of the
document in the Principle (subclauses 5.1 and 5.2).
However, in other part of the draft
standard, i.e. at least in the Scope
(clause 1) and in the sample pretreatment (clause 9.2), only “undried” (i.e. fresh) soil can be used.
The determination of the water
content shall be performed on a
separate sub-sample
The draft standard specifies that
“measurements are made at least
twice”. The inclusion of this
statement is probably a
consequence of the expected
poor reproducibility of the results
obtained from the test portion,
due to the fact that only fresh
samples are used. As a sufficient
accuracy might as well be
reached with only one analysis especially if the test portion is
homogenous, as is mostly the
case using dried samples - it
should not be requested to
duplicate analyses. It should be
left to the quality management of
the laboratory to proof the
accuracy of its determinations,
especially as there are
possibilities for quality control of
the process without double
Proposed change by the MB
Project Horizontal observations
We ask for a rewriting of the text to
assure the use of dried samples pretreated according to ISO 11464 as the
only possibility for the determination
of TOC on soils.
do
For soils it is not necessary to
determine the water content. The
result refers to air-dried samples.
We ask that the determination of TOC
should be undertaken on dried soil
(according to ISO 11464) and to leave
the decision on the proof of accuracy
to the performing laboratory (see also
ISO 10694).
Sentence changed to accommodate
possibility for results based on air
dried samples
General question for more standards general decision to be taken. Upps.
Recom.: refer to pretreatment
standard (in progress).
Comments table TOC second consultation
Cluster
Paragraph
Type of
comment
Comment (justification for
change) by the MB
analysis as well. Obligatory
duplicates will again increase the
cost of the determination.
5.17.2
10.1.2
G
10.1.3
te
The description of the methods of
measurement of TOC and TIC is
very brief. The use of a system
such as micro-analysis with CHN
should be specified. The methods
of determination of TIC should be
specified more accurately.
The determination of the TIC by
using ISO 10693
AFNOR
MB
1
AFNO
R
AT
10.1.3
G
AT
10.2
te, ge
Abbreviation – skip the first part of
the sentence
The possibility to measure
simultaneously total nitrogen
should be stated.
Calibration
The function shall be linear.
Otherwise the working range
must be restricted to the linear
Proposed change by the MB
Project Horizontal observations
to be discussed: Upps. Recom.: given
the materials in this standard the use
of micro systems is not recommended
but can be used if proven to be equal.
TIC may alternatively be determined
by using ISO 10693. The
concentration of MgCO3 has no
influence.
For discussion Upps Recom: see
above :accepted.
Upps Recom.: not very common for all
of these matrices but can be done.
The calibration is device-specific. It is
not always possible to achieve a
linear function. It has to be possible to
use a function of 2nd or 3rd order.
The calibration should be part of the
informative annex
for discussion: Upps. Recom.: the
calibrationshould be a lineair function.
Comments table TOC second consultation
MB
1
Cluster
Paragraph
Type of
comment
Comment (justification for
change) by the MB
range.
Proposed change by the MB
Project Horizontal observations
10.2 et
10.3
T
The use of a sample based on
EDTA is forbidden, because it is
used in the control sample. There
is no reason to forbid EDTA in
sampling. Soils or sludge
samples, … may also be used as
control samples.
Standard now makes analysis of
one sample per batch in duplicate
obligatory. This is not something
to be determined in a standard
Allow the use of EDTA as
sample.Allow also the use of real
samples (sludge, soil, etc. ) as control
sample.
to be discussed: Upps. Recom.: see
above; not accepted.
Remove this. Instead add a
procedure of checking the quality of
the analysis by analysing a reference
sample in each batch of samples.
This may be a home made sample or
a certified reference material. Results
should be controlled with a control
chart.
The coefficient of variation should be
known an made available to
customers if required. It is not
necessary to report it with each
sample!
Remove this. Instead add a
procedure of checking the quality of
the analysis by analysing a reference
sample in each batch of samples.
This may be a home made sample or
a certified reference material. Results
should be controlled with a control
chart.
The coefficient of variation should be
known an made available to
customers if required. It is not
necessary to report it with each
General question to be solved
NL
10.3
te
NL
10.4
te
The relevant coefficient of
variation “shall be reported”. This
is not common practice!
NL
11.3
te
Standard now makes analysis of
one sample per batch in duplicate
obligatory. This is not something
to be determined in a standard
NL
11.4
te
The relevant coefficient of
variation “shall be reported”. This
is not common practice!
General question to be solved
General question to be solved
General question to be solved
Comments table TOC second consultation
MB
1
Cluster
Paragraph
Type of
comment
Comment (justification for
change) by the MB
Proposed change by the MB
Project Horizontal observations
sample!
NL
Annex
A
GB
General
T
GB
General
T
GB
Title
T
GB
Table of
applicab
ility
T
% of outliers and SR% for method
B are rather high!
As method B has rather high
reproducibility % (20-25%) with rather
high % of outliers it is questionable if
this method is a suitable method!
to be discussed: Upps. Recom.:
Validation of the method B should
prove that it is applicable for these
matrices.
The authors appear to have missed
the point that the objective of
determining TOC is to estimate the
non-coal (and non-charcoal) organic
matter content.
That is the reason that dichromate
digestion and titration is the classic
benchmark (ISO 14235:1998 Soil
quality –
Determination of organic carbon by
sulfochromic oxidation) though it
does not appear to have been used
by the authors of Evaluation_DMLOI-TOC.
At the EU level we are concerned
about loss of soil organic matter, we
therefore need a method that does
not measure coal, lignite or charcoal
as organic matter.
This method is totally unfit for
purpose because it would
erroneously report coal, charcoal,
etc. as organic carbon.
The title extends beyond the Scope of
HOR – delete sediment and waste
Revise Evaluation_DM-LOI-TOC with the
objective in mind of estimating noncarbonised organic matter.
The object of Project Horizontal was to
develop horizontal methods based on the
existing vertical methods - to the extent
possible. The proposed TOC method is
based on the existing method for TOC in
sludge and waste.
No budget for development of a “new”
principle for determination of organic
carbon was set aside to full fill the need as
now expressed by UK.
Develop a fit for purpose method that
does not include coal, charcoal, etc. as
organic carbon
-
Soil, sludges and treated biowaste –
Organic constituents - Determination of
total organic carbon (TOC)
Changed.
The title is changed according to the
discussions at the Uppsala meeting
Revise the table so that it is consistent
with the Scope of HOR, i.e. soils, sludges
and treated biowastes
Changed.
The table is changed according to the
discussions at the Uppsala meeting
“sediment” “soil improvers” “growing
media” and “waste” are outside the
Scope of HOR, which is sludges,
soils and treated biowastes.
Comments table TOC second consultation
MB
1
Cluster
GB
Scope
Paragraph
Type of
comment
Comment (justification for
change) by the MB
Proposed change by the MB
Project Horizontal observations
T
The Scope extends beyond the
Scope of HOR and it explicitly states
that it is not restricted to “total
organic carbon” because it would
include coal and charcoal in its
estimate
When a fit for purpose method is
produced it should conform to the Scope
of HOR
Changed.
The scope is changed according to the
discussions at the Uppsala meeting
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