Template for comments and secretariat observations
Date: 2006-03-28
Document:
6-16-1 Nutrients Kjeldahl
Horizontal 6-16-1 Nutrients Kjeldahl Nitrogen
Author of comments: ON/Austrian Standards Institute
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/N
ote
(e.g. Table 1)
Type
of comment2
Comment (justification for change) by the MB
Proposed change by the MB
Project Horizontal observations
on each comment submitted
AT
10.1
AT
10.1
AT
10.2
DE
Introduction
DE
Contents
last
paragraph
Table of p. 2
ed
The links to the chemicals and apparatus are wrong.
Corrected
ed
The last paragraph (The amount of….) should come before
10.1, so that it is valid for 10.1 and 10.2
changed
ed
The links to the chemicals and apparatus are wrong.
corrected
te
To my opinion, the proposed method is not applicable to
fertilized peat, because materials of this type can contain
large amounts of nitrates, which are not detected by the
method (see cl. 6)
Please proof the validation in EN 13654-1 and
eliminate this material in the table, if there are no
facts which contradict the experience given.
Fertilized peat is not in the
scope
Upps Recomm.: soil, treated
biowaste and sludge in the
title
ed
Referred numbers of pages are not correct always
Re-numbering
Corrected
DE
1
Scope
te
Nitrogen present in the form of nitrate or nitrite in
samples can not be determined by this method. This
should be stated more clearly
Replace
sentence by: “Nitrogen present in the
form of nitrate and nitrite can not be determined by
this method. Some nitrogen forms will not be
determined totally (see clause 6).”
Corrected
DE
1
1st sentence
ed
A word seems to be missing
This standard is applicable to…
Formal corrections are made
DE
3
ed
Singular correct?
… definitions apply:
See above
DE
3.1
ed
Definition can be given more concretely
Mass of nitrogen…
See above
te/ed
Better understanding
It condenses in the cooling system and rinses into
a conical flask, filled with boric acid solution. This
solution is titrated with sulfuric acid, using an
indicator to mark the endpoint.
Changed to proposal
ed
Improve english writing
Replace “Kjeldahltube” by “Kjeldahl digestion
vessel (flask or tube)”
Changed to proposal
ed
Better understanding
Nitrogen, bound by N-N and N-O linkages…
Changed to proposal
DE
5
DE
5
DE
6
4th
line
2nd sentence
2nd
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. CN for China; comments from the ISO/CS editing unit are identified by **)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 1 of 9
ISO electronic balloting commenting template/version 2001-10
Template for comments and secretariat observations
Date: 2006-03-28
Document:
6-16-1 Nutrients Kjeldahl
Horizontal 6-16-1 Nutrients Kjeldahl Nitrogen
Author of comments: ON/Austrian Standards Institute
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/N
ote
(e.g. Table 1)
Type
of comment2
Comment (justification for change) by the MB
Proposed change by the MB
Project Horizontal observations
on each comment submitted
DE
6
3rd sentence
te
Concretization
Furthermore, of the inorganic fraction nitrates and
nitrites are detected only partially
Changed to proposal
DE
6
4th sentence
ed
Fluctuations in water content?
Variation of water content?
“Fluctuations in water
content”
DE
6
4th sentence
ed
Fluctuations during titration (what does it mean?)
?
deleted
DE
6
last
sentence
ed
Meet this expression what it is really meant?
The amount of sulfuric acid needed, depends on
the composition of the sample which has to be
analyzed (see table 2).
Changed
DE
6
table
ed
Numbering and headline are missing
Use the information under the table as headline
and insert “Table 2:”.
Changed
DE
6
table,
headline of
column 2
ed
Better understanding
Consumption of sulfuric acid (36 mol/l) in ml/g
Changed
DE
7
Headline
ed
Headline is missing
7 Reagents
corrected
DE
7.2
ed
Potassium sulfate is only one component of the catalyst
mixture
“Catalyst mixture” (only) as headline
Changed
DE
7.3
ed
The information given is a concretization of 7.2, not a new
reagent.
Delete the number 7.3 and re-number all the
following reagents; check if they are cited in the
text correctly.
Formal mistakes corrected
DE
2nd 7
ed
Incorrect numbering
8
corrected
DE
2nd 7.1
ed
Number of the headline and cited number of the
apparatus are not correct
8.1…digestion stand (8.2)
s.a.
DE
2nd 7.1
te
The comment contradicts the information given before (is
the tube of 50 ml adequate for all analyses or not?).
Specify the information before or delete the
comment.
corrected
DE
8.2
ed
…evaporate the fume?
…conduct away the fume
deleted
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. CN for China; comments from the ISO/CS editing unit are identified by **)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 2 of 9
ISO electronic balloting commenting template/version 2001-10
Template for comments and secretariat observations
Date: 2006-03-28
Document:
6-16-1 Nutrients Kjeldahl
Horizontal 6-16-1 Nutrients Kjeldahl Nitrogen
Author of comments: ON/Austrian Standards Institute
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/N
ote
(e.g. Table 1)
Type
of comment2
Comment (justification for change) by the MB
Proposed change by the MB
Project Horizontal observations
on each comment submitted
DE
9.1
DE
9.1
DE
9.2
te
To my opinion, the development of a standard which
covers sampling of all materials cited is nonsense. Either
it will be very voluminous or not concrete enough. The
same situation is given as with sample pretreatment (9.2).
Delete the information and refer to the special
sampling procedures.
Reference cited
3rd line
ed
What means “closure” material? PTFE is a very
expensive material. Its use is not necessary, if only total
nitrogen has to be analysed.
…containers of appropriate material, e.g. PE
Changed to “PE”
2nd section
ed
The information “During …avoided” concerns on 10.1
Delete in 9.2 and insert in 10.1
Added in 10.1
Ed/te
The terms “semimicro” and “macro version” are not
explained
explain
Not changed as these are
common expressions
ed
The information given concerns on 9.2
Delete it in 10 and insert it at the end of 9.2
correcetd
DE
DE
DE
10.1
DE
10
DE
10.1
1st
sentence
ed
Grinding is not referred before.
Omit “ground” (instead of “grinded”) or specify
grinding in cl. 9.2.
Changed to proposal
DE
10.1
1st sentence
ed
Better understanding
…, or the corresponding dry mass of undried
sample…
Changed to proposal
DE
10.1
ed
The referring numbers are not correct.
Check and correct them.
Corrected
DE
10.1
3 last
subsections
ed
The information given seem to be declarative to the
foregoing text
Make three notes.
DE
10.1
1st
subsection
ed
…adopted?
…adapted.
Changed
DE
10.1
3rd subs.
ed
What means “working instructions”?
Has to be specified, e.g. “in the manufacturers
manual.”
Changed to proposal
DE
10.2
ed
The referring numbers are not correct
Check and correct them.
s.o.
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. CN for China; comments from the ISO/CS editing unit are identified by **)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 3 of 9
ISO electronic balloting commenting template/version 2001-10
Template for comments and secretariat observations
Date: 2006-03-28
Document:
6-16-1 Nutrients Kjeldahl
Horizontal 6-16-1 Nutrients Kjeldahl Nitrogen
Author of comments: ON/Austrian Standards Institute
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/N
ote
(e.g. Table 1)
Type
of comment2
Comment (justification for change) by the MB
Proposed change by the MB
Project Horizontal observations
on each comment submitted
2 last subs.
ed
The information given seem to be declarative to the
foregoing text
Make two notes.
Note 10.2 rewritten
Upps. Recomm.: other
methods of detection should
be allowed
DE
10.2
DE
11
ed
Subdividing into two clauses seems to be appropriate.
Headlines: 11 Calculation and 12 Expression of
results
corrected
DE
11.1
ed
In the headline “Method” is redundant
Calculation
corrected
DE
11.1
Symbols in
the
equations
ed
mt means not a mass but a mass portion
wmd
corrected
DE
11.1
Explanation
of Symbols
ed
mt is …
wmd is the dry residue (mass portion of oven dry
matter) of the used material in %, determined
according to the standard procedure, which is
applicable to it
corrected
DE
11.1
Explanation
of Symbols
ed
The referring numbers are not correct
Check and correct them.
corrected
DE
13
and he whole
document
table
ed
The tables should be numbered
Give the tables numbers
yes
DE
13
table
Ed/Te
Express s rel with two decimal places
Express s rel with two decimal places
Not changed- format error,
during validation it should be
done.
Ge
Pretreatment of samples should possibly be equal to all
different parameters. This will save a lot of time.
Pretreatment of samples should therefore be
prescribed in cluster 1
Here dry and fresh samples
can be used
Upps. Recomm.: It should be
clear that liquid samples can
be used as well as dry and
NL
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. CN for China; comments from the ISO/CS editing unit are identified by **)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 4 of 9
ISO electronic balloting commenting template/version 2001-10
Template for comments and secretariat observations
Date: 2006-03-28
Document:
6-16-1 Nutrients Kjeldahl
Horizontal 6-16-1 Nutrients Kjeldahl Nitrogen
Author of comments: ON/Austrian Standards Institute
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/N
ote
(e.g. Table 1)
Type
of comment2
Comment (justification for change) by the MB
Proposed change by the MB
Project Horizontal observations
on each comment submitted
moist samples
NL
2
ed
Replace the WI number 29292030 with WI 292030 and
add the complete title.
Changed to proposal
NL
2
ed
Add the sampling standard (as mentioned in chapter 9) in
chapter 2.
Refrence inserted by
Horizontal
NL
3
ed
Draft terms and definitions according to CEN rules.
yes
NL
3.1
Ed
Other analysis methods should be mentioned. Now this
test could only be done with titration as it is defined
NL
6
ed
Add table title and draft table according to CEN rules.
NL
7
Ed
Chapter header is missing
Insert the last word of chapter 6 Reagent as
chapter header 7
corrected
NL
7.3
Te
Other digestion mixtures, as potassiumsulfate,
coppersulfate and selenium or potassiumsulfate and
selenium should also be possible
Mention proposed mixtures in the text
Selenium should be avoided
due to its toxicity and due to
the fact , that it does not
increase digestion efficiency
Upps. Recomm.: The TiO2
CuSO4/KSO4 catalyst
should be the only catalyst
allowed unless another
expert group has stated,
that other catalysts are as
effective and safe
table
Spectrophotometric measurements, manual or
automatic
Modern Kjeldahl devices
generally contain a distillation
and titration unit,
Upps. Recomm.:other
analytical methods are
allowed. Note is added
corrected
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2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 5 of 9
ISO electronic balloting commenting template/version 2001-10
Template for comments and secretariat observations
Date: 2006-03-28
Document:
6-16-1 Nutrients Kjeldahl
Horizontal 6-16-1 Nutrients Kjeldahl Nitrogen
Author of comments: ON/Austrian Standards Institute
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/N
ote
(e.g. Table 1)
Type
of comment2
Comment (justification for change) by the MB
Proposed change by the MB
Project Horizontal observations
on each comment submitted
NL
7.7
Te
Sulfuric acid should replaced by hydrochloric acid
Sulfuric acid should be replaced by hydrochloric
acid
HCl is now mentioned as
alternative
NL
7
Ed
Chapter 7 Apparatus and 7.1 should be Chapter 8 en 8,1
Make changes to 8 and 8.1
Formal mistakes are
changed
NL
7.1
Ed
Reference to 6.2 is wrong
Reference should be to 8.2
Corrected
NL
10
Ed
Avoid hanging paragraphs. Add a subtitle to the first
paragraph.
NL
10
Ed
Replace 0.5 with 0,5 according to CEN rules/
NL
10.1
Ed
References in this chapter are wrong
Correct the references
NL
10.5
te
Standard now makes analysis of each sample in
duplicate obligatory. This is not something to be
determined in a standard
Remove this. Instead add a procedure of checking
the quality of the analysis by analyzing 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.
NL
11.1
ed
Draft formula and formula expression according to CEN
rules.
corrected
NL
13
table
ed
Add table title and draft table according to CEN rules.
s.o.
NL
Annex A
table
ed
Add table title and draft table according to CEN rules.
s.o.
NL
Bibliography
ed
Remove any duplicate ISO/EN standard already listed in
chapter 2.
s.o.
Corrected
Changed
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. CN for China; comments from the ISO/CS editing unit are identified by **)
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te = technical
ed = editorial
NOTE
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page 6 of 9
ISO electronic balloting commenting template/version 2001-10
Template for comments and secretariat observations
Date: 2006-03-28
Document:
6-16-1 Nutrients Kjeldahl
Horizontal 6-16-1 Nutrients Kjeldahl Nitrogen
Author of comments: ON/Austrian Standards Institute
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/N
ote
(e.g. Table 1)
Type
of comment2
Comment (justification for change) by the MB
Proposed change by the MB
Project Horizontal observations
on each comment submitted
GB
General
T
GB
Title
T
GB
Table of
applicability
T
GB
Scope
GB
Principle
This method is not fit for purpose because of its insistence on
using dried samples, which for some materials will mean loss
of ammoniacal-N and consequently underreporting the
agronomic fertilizer replacement value, which will lead to
excessive mineral fertilizer and risk of losses. In growing
media it could risk quality problems.
Sample homogenization and drying can improving laboratory
precision but if some of the analyte is lost in the process the
result could be precise but wrong.
Method 6162 stresses the importance of keeping soils cool and
not letting them dry out because of the risk of losing
ammoniacal-N but this method ignores that risk.
The title 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”
The use of fresh samples is
mentioned as alternative.
Upps. Recomm.: It should be
clear that liquid samples can
be used as well as dry and
moist samples
Determination of Kjeldahl Nitrogen in soil, treated
biowaste and sludges
Changed to proposal given in
Uppsala
What is “domestic sludge” and what is “industrial sludge”
“fertilized peat” in EN 13654 was a growing medium
“sediment” is outside the scope of HOR
“bark humus” in EN 13654 was actually “composted bark”
and it was a growing medium constituent or a soil
improver, it was not a waste
Improve the precision of this table – the current
terminology is inadequate, misleading or wrong.
Restrict the table to the Scope of HOR, i.e. soils,
sludges and treated biowastes
Table deleted
T
The wording in EN 13654 is better
The Scope of HOR is Soils, sludges and treated
biowastes” - “related waste” is outside the Scope of HOR
The Kjeldahl method determines ammonium-N,
nitrate-N, nitrite-N and organic-N … Nitrogen in NN linkages, N-O linkages and some heterocyclics
(especially pyridine) is only partially determined.
Nitate and nitrite-N is not
determined in the proposed
method. Other terms are
used as proposed
T
If samples are dried there is a risk of losing ammoniacal-N,
especially from digestates; it is preferable to kepp samples cool
between collection and the time that they are analysed and then
to extract the sample in its “as received” condition.
Is titanium dioxide/copper sulphate [note dioxide spelling]
really needed? EN 13654 uses potassium sulphate/copper
sulfate
Delete the restriction to “dried” samples
Fresh and dry samples can
be used
A detailed survey on catalyst
mixtures , which are as
effective as the used mixture
Should be subject of a
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. CN for China; comments from the ISO/CS editing unit are identified by **)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 7 of 9
ISO electronic balloting commenting template/version 2001-10
Template for comments and secretariat observations
Date: 2006-03-28
Document:
6-16-1 Nutrients Kjeldahl
Horizontal 6-16-1 Nutrients Kjeldahl Nitrogen
Author of comments: ON/Austrian Standards Institute
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/N
ote
(e.g. Table 1)
Type
of comment2
Comment (justification for change) by the MB
Proposed change by the MB
Project Horizontal observations
on each comment submitted
research work in future and
exceeded the proposal of the
desk study, which aimed at
comparing the effectivity of
A mixture containing
selenium or TiO2
GB
Interferences
and sources of
errors
T
GB
9.1
T
GB
9.2
T
10
T
Like the Scope this is also erroneous about the limitations of
the method
Is PTFE really necessary? It is expensive. Isn’t polyethylene
or polypropylene good enough?
This repeats the Scope error of not qualifying biowaste with
“treated” and including “related waste”
It also repeats the error of requiring dried samples
Homogenising the sample improves laboratory precision but if
the real material is heterogeneous the act of homogenizing
might lose some N – the result could be a precise but wrong
answer
Rewrite
digestion temperature and
impurities as sources of error
added
Check necessity for PTFE
Changed to “PE”
Rewrite
Changed to “ treated waste”
GB
Procedure
FIN
7
tec
Header is missing:7 Reagents
All formal mistakes corrected
FIN
8
tec
7 Apparatus should be 8 Apparatus
See above
FIN
7.1
tec
Corrected
FIN
10.1
7.1 should be 8.1 and in the same sentence
…suitable for digestion stand (6.2) should be
(8.2)
In the first sentence …flask or tube (5.2)
should be (8.1).
Para1
tec
A homogeneous test sample
is ment, which means e.g.
manual homogenising not
milling, which will result in
ammonium losses due to
temperature increase
Corrected
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. CN for China; comments from the ISO/CS editing unit are identified by **)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 8 of 9
ISO electronic balloting commenting template/version 2001-10
Template for comments and secretariat observations
Date: 2006-03-28
Document:
6-16-1 Nutrients Kjeldahl
Horizontal 6-16-1 Nutrients Kjeldahl Nitrogen
Author of comments: ON/Austrian Standards Institute
1
2
(3)
4
5
(6)
(7)
MB1
Clause No./
Subclause No./
Annex
(e.g. 3.1)
Paragraph/
Figure/Table/N
ote
(e.g. Table 1)
Type
of comment2
Comment (justification for change) by the MB
Proposed change by the MB
Project Horizontal observations
on each comment submitted
Para1
tec
FIN
10.1
In the second sentence ..Add 10 ml sulfuric
acid (7.1) should be (7.1)
Corrected
1 MB = Member body (enter the ISO 3166 two-letter country code, e.g. CN for China; comments from the ISO/CS editing unit are identified by **)
2 Type of comment: ge = general
te = technical
ed = editorial
NOTE
Columns 1, 2, 4, 5 are compulsory.
page 9 of 9
ISO electronic balloting commenting template/version 2001-10