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