Date:
Document:
2006-09-30
Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
Comment (justification for change) by the MB
Proposed change by the MB
Secretariat observations
on each comment submitted
AT
ge
The conditions for Method B only provide a very “soft”
digestion with the risk of a large amount of undissolved
sample. Especially for the sample types (soil sludge,
biowaste and waste) a “stronger” digestion (which is
technical possible, see Annex 1 aquaregia for further
details) is strongly recommended.
That is true; the conditions of
microwave digestion will not
dissolve the sample totally or
to a great amount. The
conditions of method B
should lead to comparable
results according to method
A and not to the best
available dissolution. (see
data report 4.2.2.2, Figures
8-13) see Annex to answers
U: validation of additional
high temperature method
AT
2.1.1 ff
ed
The VWR art. Numbers of nitric acid and hydrochloric
acid are interchanged! This mistake is applied in the
whole document!
Will be checked
VWR art. Numbers removed
AT
8.2
te
Method B…(at least 100ml???): What is the reason tu
use such big vessels for a sample intake of 0,2 – 0,5 g
and 6 ml HNO3 and 2 ml HCl???
..suitable quartz or Teflon vessel…
accepted
AT
10.2.2
te
Raise the temperature of the reaction mixture slowly to
reflux conditions: Although the condensation zone will
differ between various digestion apparatus no minimum
temperature is defined!!! The temperature for Method B is
clearly defined!
Define temperature for Method A!
Boiling temperature is 103 °C
AT
10.3.1
ed
7.2 ≠ 8.2
…into the vessel (8.2).
accepted
AT
A.1.1. ff
ed
The VWR art. Numbers of nitric acid and hydrochloric
Will be checked
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page 1 of 16
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Date:
Document:
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
Comment (justification for change) by the MB
Proposed change by the MB
Secretariat observations
on each comment submitted
acid are interchanged! This mistake is applied in the
whole document!
AT
DE
A.1.2.
3.8
te
Te
VWR art. Numbers removed
Digestions performed at UBA Wien: Procedure 1: Added
reagents are of subboiled quality
2 ml HNO3, p.A., subboiled
Heating block or other equipment is missing
add
accepted
6 ml HCL, p.A., subboiled
Is explained in 8, no further
definition necessary
Not accepted
DE
3.10; 3.11
Te
Delete paragraphs no deeper information given
delete
accepted
DE
5
Te
Delete note
This is not an open standard
Should be discussed –see
NL comments
U: Delete note
DE
6.1, 8.1
Te
Cooking in 10 % nitric acid is not necessary
Standing several days is suficient
For trace metal analysis
cooking with acid should be
preferred
Not accepted
DE
6.1
Te
Particle size versus homogeneity and sample intake must
be addressed or related to a pre-treatment standard
Pb is not volatile under this condition.
accepted
DE
6.1
Te
“…. Some elements of interest can be lost because of
precipitation with some ions of the solution. It is the case
for insoluble chlorides, fluorides and sulphates for
example. In this case the precipitate can be analysed
separately.”
Aqua regia extraction is a conventional method
with regard to temperature, kind of chemicals used
and time. Only under strictly following the
prescribed procedure comparable results can be
achieved, which do not represent the totalcontent.
What shall be done with the precipitation?
Digestion with fluoric acid?
It is only mentioned in
interferences that this may
occur. The sentence:
Delete sentence
“In this case the precipitate
can be analysed separately.”
Will be deleted
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page 2 of 16
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
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Proposed change by the MB
Secretariat observations
on each comment submitted
DE
6.2
Ed
shift this § to10.3 ff microwave digestion
DE
8.1 to 8.9
Ed
Separate open digestion method A and pressurized
digestion in method B and all technical descriptions in
sub-clauses.
Include description of ISO 11466 for open reflux
method A
Should be discussed
accepted
Separation accepted
DE
8.5
te
modification of the text
microwave oven either temperature or power
controlled with temperature calibration in
combination with pressure measurement
accepted
DE
9.1
Te
“… Samples should be stored in suitable containers with
an appropriate closure material. Samples should be kept
cold (< 8°C). The sample pre-treatment should take place
within 1 month of sampling. Alternatively, samples may
be frozen (-18 °C) directly after sampling and kept frozen
before sample pre-treatment.”
There is no reason that aqua regia extracted
elements undergo any change at room
temperature conditions (e. g. volatilization ).
Should be discussed,
for some samples and
elements cooling may be
necessary
Not accepted
Delete sentence.
DE
DE
9.1
9.3
Te
Note
te
For element determination in soil samples cooling to 8 °C
or -18°C is not used
For soil an other inhomogenous material It is common to
grind < 2 mm fraction to < 150 µm prior to aqua regia
digestion (ISO 11466).
Should be discussed,
for some samples and
elements cooling may be
necessary
It is common to grind < 2 mm soil to < 150 µm
prior to aqua regia digestion.
Revise note related to method A and B
Reasons: more homogeneous sample and increased
There should be one grain
size for all types of samples,
therefore 250 µm was
proposed (according to the
discussion in the Workshop
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
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Proposed change by the MB
Secretariat observations
on each comment submitted
efficiency of acid attack by increasing the surface area of
the particles
Inorganic)
Not accepted
DE
9.3
NOTE
te
For soil samples it is more common to use the fraction
< 150 µm (see ISO 11466).
To be discussed.
There should be one grain
size for all types of samples,
therefore 250 µm was
proposed
DE
9.3
last
sentence
te
“The mass of laboratory samples shall be sufficient …”
Change to:
“The mass of test sample shall be sufficient …”
accepted
DE
9.4
te
For thermal heating (Method A; sample portion 3 g) the
material should contain less than 20 % (m/m) organic
carbon. Materials containing more than 20 % organic
carbon require treatment with additional nitric acid (see
10.2.2)
Method A) For thermal heating under reflux
conditions the material should contain less than
about 20 % (m/m) organic carbon according to EN
xxx. Materials containing more than about 20 %
(m/m) organic carbon require treatment with
additional nitric acid (see 10.2.2)
In this horizontal draft
standard an eventual need of
additional HNO3 is described
in 10.2.2
DE
9.4
te
For soil analysis, sample intake for method B should not
be smaller then 0,5 g. Fix this sample intake.
Delete note, combining parallel digestions is not
common. Address pre-oxidation of organic matter.
A mass of test portion of
about 0,5 g would be
preferable. Because of
manufacturers’ instructions of
different apparatus and the
need of taking into account
the organic content of the
sample this is not possible
Note
U: 0,5 g is fixed
DE
10.2.1
Note
Te
The relation 3 g to 28 ml aqua regia should be fixed
Delete note
A mass of test portion of
about 3 g would be
preferable. Because of
manufacturers’ instructions of
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
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on each comment submitted
different apparatus and the
need of taking into account
the organic content of the
sample this is not possible
U: The mass to volume ratio
is fixed.
DE
DE
10.2.2
10.2.2
te
Note
te
The absorption vessel should be filled with 15 ml 0,5 mol/l
nitric acid, not aqua regia.
fill the absorption vessel with 15 ml 0,5 mol/l nitric
acid
Should be discussed
The time of standing at room temperature should be 16 h
to allow a slow oxidation of the organic matter of the
material.
Ad 16 h standing over night, delete note
The experiments showed
that standing overnight
influence the results
evidently, therefore it was
necessary to delete this
sentence
U: accepted
U: add Note: The time
standing at room temp. may
have influence on the
digestion rate…
DE
10.3.1
te
The amount of the test portion should be constant by
0,5 g. The ratio sample / aqua regia is important.
Extraction efficiency depends on mass to volume,
T, p and time
A mass of test portion of
about 0,5 g would be
preferable. Because of
manufacturers’ instructions of
different apparatus and the
need of taking into account
the organic content of the
sample this is not possible
U: accepted, mass of test
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
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portion fixed at 0,5 g
DE
10.3.2
te
The microwave assisted digestion should be controlled
only by temperature and time not by power.
A procedure to establish the relationship between
microwave power and temperature for power-controlled
systems with pressure measurement has to be added.
See water standard….
A test portion of the sample mixed with aqua regia
is heated in a microwave oven to a temperature
beyond the boiling point (103 °C at 101.3 kPa) and
maximum 175 °C. Increase the temperature of the
digestion mixture with a rate of 6-10°C/min to a
temperature between the boiling point and 175 °C.
Maintain digestion for a period of at least 10 min
and at most 480 min. The duration of the digestion
depends on the final temperature.
The conditions of method B
should lead to comparable
results according to method
A. The theoretical relation
between temperature and
time proved not to be
applicable. (see data in
chapter 4.2.2.2 of report,
Figures 8-13, table 17 )
U: validation of additional
high temperature method
controlled by temperature
DE
10.3.2
Te
“…. NOTE If a temperature controlled microwave unit is
used the appropiate temperatures of 110 to 120°C should
be obtained for about 5 minutes. These are the
temperatures that should be reached with the power
programme of table 1, otherwise the power should be
adjusted to reach these temperatures.”
As it is written a sample would only be heated for 5
min at 110 to 120 °C. This definitely woulld not
lead to comparable results with reflux extraction, at
which samples are heated for 2 h at a specified
temperature.
Delete or re-write sentence.
The experiments and the
validation data for sludge in
EN 13346 prove that these
conditions lead to better
comparable results than the
theoretical ones.The
conditions of method B
should lead to comparable
results according to method
A. The theoretical relation
between temperature and
time proved not to be
applicable. (see data in
chapter 4.2.2.2 of report,
Figures 8-13, table 17 )
Note rewritten to normative
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
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Proposed change by the MB
Secretariat observations
on each comment submitted
text with temp. 115±5°C for
temperature controlled
microwave digestion.
U: validation of additional
high temperature method
DE
7.5, 8.4,
10.2.1, 10.2.2,
10.3.1, 10.3.2
ed
wrong reference numbers
DE
10.3
ge
Waste and biowaste may be rather heterogeneous
materials and require significantly more time and effort
for homogenization than soil samples. If the mass of test
portion is limited to less than 0,5 g there is a high
probability that it is not representative for the laboratory
sample. That´s why the question:
Is the proposed microwave assisted digestion method
really appropriate for such materials?
To be discussed.
Thie time and power settings in table one are only
exemplary, different models of microwave systems use
different programs. The temperature calibration of the
system is to be integrated in this chapter.
Table 1: Example of Power/Time Programm
DE
10.3.2
Table 1
te
Accepted and corrected
This depends on the quality
of test portion preparation.
Therefore an additional
reference to EN 15002 was
made.
U: mass of test portion fixed
at 0,5 g
Add the description of the temperature calibration
Temperature/power
calibration is in annex A
According to the ruggedness
study the temperature /power
programme has to be fixed to
the extend possible (taking
into account that different
apparatus are used all over
Europe) in order to achieve
comparable results.
U: validation of additional
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
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comment2
Comment (justification for change) by the MB
Proposed change by the MB
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on each comment submitted
high temperature method
controlled by temperature
DE
Annex A
Power calibration is only useful if related to temperature
under same constellation as sample digestion used
delete
Temperature/power
calibration in annex A is
necessary
Deleting the power control
method as proposed by TG 6
cannot be followed by the
author as many labs in
Europe have no temperature
controlled microwave oven
and this method has proven
to be applicable alt least for
sludges ( EN 13346)
DE
Annex B
This can only be used for open thermal heating method
A, method B should be checked for conditions used
Microwave digestion should be adapted to the
procedure of US EPA 3051A: 175 °C, 10 min time
or longer if temperature is lower (same energy
transfer)
For this round robin test the
conditions used for method B
were according to Table 1 of
horizontal draft standard. But
some more precise
conditions as prescribed in
the new horizontal standard
were at this time not
prescribed, therefore the
data are rather scattered.
The EPA method will not
lead to comparable results as
shown in report 4.2.2.2
U: validation of additional
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
Comment (justification for change) by the MB
Proposed change by the MB
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high temperature method
DE
Annex B
DS
Report Fig 3 4
DS
Table 7 and 9
ge
Data for microwave assisted digestion in a semi-open
vessel are of no concern to this draft standard.
Revise Annex B.
Will be replaced in the final
version by the actual
validation data
It is not clear if the temperature/pressure represents the
inner oven or a sample. As the temperature governs the
dilution process and as the temperature of pressurized
digestion does not exceed 100 – 110 similar temperature
curve for the open digestion would be similar?
Temperature is usually
measured within the sample
CV % (repeatability variations) for closed microwave
digestion are larger than 10 % for 12 out of the 17
elements in the table, which indicate that the ruggedness
of the described digestion is questionable, and
reproducibility CV (between different ovens, laboratories)
are expected very high.
In this table variations of
digestion procedures are
included
Temperature of open
digestion usually is
performed at the boiling point
of aqua regia (103°C)
as a consequence
performance characteristics
are fixed in more detail and
open microwave digestion
has been deleted from the
horizontal draft standard
(see report 4.2)
Will be replaced in the final
version by the actual
validation data
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
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Proposed change by the MB
Secretariat observations
on each comment submitted
DS
Table 7
DS
Table 11
Open microwave digestion seem more robust that the
described closed, however yields for 9 out of 17 elements
are lower which indicate that methods are not
comparable.
Repeatabilities of Hg 20 %, B 70 %, Cd 11 %, Cr 23 %
etc. for closed MV are very high.
Similar for thermal heating – for e.g. B, Co, Cu, Na, Pb
should be remarked as such figures indicate that very
high reproducibility standard deviations are expected.
Therefore it was deleted in
the new version of horizontal
draft standard
In this table variations of
digestion procedures are
included
- as a consequence
performance characteristics
are fixed in more detail (see
report 4.2)
Will be replaced in the final
version by the actual
validation data
DS
Table 16
XRF methods results to be quoted with care – may not
represent the “true contents”.
These data have been taken
from the characterisation
study of JRC, they are the
reference values for this
study.
In order to check the
methods two certified
reference materials were
analysed in addition (results
in annex 2)
Will be replaced in the final
version by the actual
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
Comment (justification for change) by the MB
Proposed change by the MB
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validation data
DS
Conclusion
DS
Clause 8.5
DS
General
Couldn’t it be questioned if the digestion time can be
reduced from hours in the thermal heating method to 30
minutes in the microwave oven methods, without setting
strict control of the temperature in the digests during
digestion and raising the “mean” temperature?
Method B – a focused microwave ….
This has be done (See report
4.2.2.2 and 5)
Incert option for using oven controlled by
temperature (new generation ovens)
It is not possible to draw conclusions on the effect of
Treatements due to the rather big scatter in the data.
accepted
More detailed analysis of the
data in the report show that
some conclusions can be
drawn, especially that the
performance characteristics
have to be fixed in detail.
(see report 5)
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
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GB
General
GB
General
T
T
This method is not fit for purpose because it does not
refer to the need for additional nitric acid when samples
have large amounts of organic matter. Sludges and
treated biowastes can contain more than 60% organic
matter. EN 13650 notes that samples containing
>28%OM will require additional nitric acid. In the
classical aqua regia extraction this was assessed visually
from the colour of the residue.
Lime stabilization of sludge is a frequent type of
treatment; this type of material will have a large
neutralizing capacity and presumably need more aqua
regia, but it is not mentioned in the text.
Change the method to fit the Scope of materials
Do we really need aqua regia? Evaluation_nitricacid
appears to show that there is not much difference in
extractability between aqua regia and nitric acid digestion
overall, except maybe less “noise” with nitric acid. Some
elements are extracted a bit more in one and some in the
other. Nitric acid is less hazardous than aqua regia and it
is more fit for purpose for high thoroughput automated
analytical service providing laboratories. “Pseudo-totals”
are operationally defined, Evaluation_nitricacid has
shown the methods are more or less equivalent so why
not settle on the less hazardous, less noisy nitric acid?
Recommend dropping aqua regia because it is
intrinsically more hazardous than nitric acid and no
advantage over nitric acid extraction.
In this horizontal draft
standard an eventual need of
additional HNO3 is met by
reducing the mass of test
portion in case of high
organic amount or
Carbonates in the sample
See chapter 9.4 “mass of
test portion” and validation
data of EN 13346 and 13657,
where it was proven that
these methods are fit for
purpose even for samples
with high organic amount
In Europe, 4 international
standards are broadly used
for digestion with aqua regia
of similar matrices, EN 13657
is prescribed by European
Landfill Directive
Could be discussed - See
German comments
U: Aqua regia method will be
validated
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Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
Comment (justification for change) by the MB
Proposed change by the MB
Secretariat observations
on each comment submitted
GB
Evaluation_Aq
uaregia
T
Why is there no reference to:
EN 13650:2001 Soil Improvers and growing media –
aqua regia extraction?
Include this standard in the consideration
This has be done in the first
horizontal desk study
(reference1), EN 13650 can
be added in the references of
the Evaluation study too
GB
Title
T
The title was corrupted in the file on the website. It
should reflect the Scope of HOR which is “soils, sludges
and treated biowaste” [not necessarily in that order] it is
not “biowaste” and it is not “sewage sludge”. Aqua regia
is a pseudo-total extract – not total
Determination of aqua regia extractable elements
in soil, treated biowaste and sludges
Should be discussed
GB
Table of
applicability
T
The descriptions are imprecise – does the method really
purport to be applicable to all of these?
Improve the precision of this table – the current
terminology is inadequate, misleading or wrong.
This table is in all horizontal
standards,
“sediment” and “waste” are outside the scope of HOR
Restrict the table to the Scope of HOR, i.e. soils,
sludges and treated biowastes
The methods were validated
for these matrices as cited in
the table
U: scope limited only to
sludge, treated biowaste and
soil
GB
Scope
T
GB
4 Safety
remarks
E
NL
Whole doc
Ed
The Scope of HOR is Soils, sludges and treated
biowastes” - “waste” is outside the Scope of HOR
Restrict the Scope of the method to the Scope of
HOR
Should be discussed
“has to be” “have to be” are not standards terminology
Rewrite as “shall”
“Have to be” is a normative
wording too
All references should be checked; an addition chapter
has been introduced and not taken care of in the
references
change
Has been checked and
corrected
U: scope limited only to
sludge, treated biowaste and
soil
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. FR for France; comments from the CMC editing unit are identified by ***)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 13 of 16
CEN electronic balloting commenting template/version 2001-10
Date:
Document:
2006-09-30
Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
Comment (justification for change) by the MB
Proposed change by the MB
Secretariat observations
on each comment submitted
NL
1
scope
Ge
Waste is part of the scope; overlap is imminent.
Prevent overlap
Has to be discussed
U: scope limited only to
sludge, treated biowaste and
soil
NL
3.11
Ed
NL
4
safety
Ge
NL
5
Principle
Te
Focused microwave is not a common instrument for
closed vessel digestion
Toxic is not true for these chemical; the general
description is harmfull
The fixed 20 min period for digestion in closed vessel is
not common practice in the lab; several other studies
(see work for ie ISO TC 147) show other relations
between time and temperature that can be applied.
remove
accepted
Change in harmfull.
accepted
The conditions of method B
should lead to comparable
results according to method
A. (see data in chapter
4.2.2.2 of report, Figures 813, table 17 )
U: validation of additional
high temperature method
NL
5
note
Te
What other heating devices are meant?
Specifiy ie autoclave etc
Should be discussed
see DE comments (delete
this sentence)
U: Delete note
NL
6
Ge
NL
8
Te
Part of the information is (or should be) part of other
standard like sample containers etc.
Method B: Quarts vessels are not suitable for these
matrices. The nominal volume of the vessel is set at
100mL. A very commonly used microwave has vessel of
nominal 50 mL and is excluded by this criteria.
Make a reference to other standards
accepted
Remove quartz and nominal vessel volume.
Partly accepted, quartz
proved to be suitable in some
labs, 100 ml deleted
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. FR for France; comments from the CMC editing unit are identified by ***)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 14 of 16
CEN electronic balloting commenting template/version 2001-10
Date:
Document:
2006-09-30
Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
Comment (justification for change) by the MB
Proposed change by the MB
Secretariat observations
on each comment submitted
NL
8.5
Te
Focused microwaves are not common equipment.
NL
9.3
Ge
The grain size is fixed at 250 um; refer to sample prep
standard but can not be achieved by mixing of sludge
Remove focused
accepted
Partly accepted
Sewage Sludge is usually
totally dissolved by aqua
regia even without particle
size reduction (see EN
13346)
NL
9.4
Te
The amount of C is also linked to the amount of nitric acid
used.
Yes, the amount of HNO3 is
fixed
NL
10.3.2
Te
The described method deviates from other studies on
MW digestion (water, EPA etc); the prescribed
temperature is to low for the time stated. The relation
between temperature and time has been investigated
before and is missing.
The conditions of method B
should lead to comparable
results according to method
A. The theoretical relation
between temperature and
time proved not to be
applicable. (see data in
chapter 4.2.2.2 of report,
Figures 8-13, table 17 )
U: validation of additional
high temperature method
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. FR for France; comments from the CMC editing unit are identified by ***)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 15 of 16
CEN electronic balloting commenting template/version 2001-10
Date:
Document:
2006-09-30
Digestion of solid matrices.
Part 1:Digestion with aqua regia
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/
Note
(e.g. Table 1)
Type
of
comment2
Comment (justification for change) by the MB
Proposed change by the MB
Secretariat observations
on each comment submitted
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. FR for France; comments from the CMC editing unit are identified by ***)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 16 of 16
CEN electronic balloting commenting template/version 2001-10