standard operating protocol (sop) on water chemistry

This project has received funding from the European Union’s Horizon 2020 research and innovation programme under grant agreement No 731065

Project Title: AQUACOSM: Network of Leading European AQUAtic

MesoCOSM Facilities Connecting Mountains to Oceans from

the Arctic to the Mediterranean

Project number: 731065

Project Acronym: AQUACOSM

Proposal full title: Network of Leading European AQUAtic MesoCOSM Facilities

Connecting Mountains to Oceans from the Arctic to the

Mediterranean

Type: Research and innovation actions

Work program topics

addressed:

H2020-INFRAIA-2016-2017: Integrating and opening research

infrastructures of European interest

Standard Operating Protocol (SOP) on Water Chemistry

Version: V1.0; 29 May 2020

Main Authors: Christian Preiler (WCL), Robert Ptacnik (WCL), Deniz Başoğlu (METU), Meryem

Beklioğlu (METU), Henrik Larson (UMF), Sébastien Mas (CNRS-MARBEC)


Abstract 4 Water

Chemistry

This deliverable contains Standard Operating Procedures (SOP) that describes the methods for sampling and storing samples for the analysis of water chemistry from mesocosm experiments carried out in all aquatic environments (fresh and marine waters). It gathers best practice advice with a focus on sampling and pre-analytical processing and provides an overview of analytical methods used by project partners.

This SOP points out relevant considerations regarding planning and execution of sampling mesocosms. The listing of analytical methods used by partners allows to identify frequently used methods as well as differences in analytical procedures in the AQUACOSM community.

Keywords • Water Chemistry, Sample Storage


Table of Contents

I. Cross References ....................................................................................................................................... 5

II. Dissemination activities related to the Deliverable .................................................................................. 5

1. Water Chemistry ........................................................................................................................................ 6

1.1 Definitions and Terms........................................................................................................................ 6

1.2 Health and Safety Indications ............................................................................................................ 7

1.2.1 General Information .................................................................................................................. 7

1.2.2 Safety Instructions ..................................................................................................................... 8

1.2.3 Working and Personal Protection (Safety) Equipment ............................................................. 8

1.2.4 Use, Storage and Disposal of Reagents and Chemicals ............................................................. 8

1.2.5 Use, Storage and Disposal of the Equipment ............................................................................ 9

1.3 Environment Indications ................................................................................................................... 9

1.4 Sampling ............................................................................................................................................ 9

1.4.1 Introduction ............................................................................................................................... 9

1.4.2 Sampling Strategy/ Sampling Plan ........................................................................................... 10

1.4.3 Equipment for Sampling .......................................................................................................... 11

1.4.4 Techniques for representative sampling ................................................................................. 12

1.4.5 Quality Assurance Considerations ........................................................................................... 13

1.5 Filtration .......................................................................................................................................... 14

1.5.1 Introduction ............................................................................................................................. 14

1.5.2 Vacuum Filtration .................................................................................................................... 14

1.5.3 Pressure Filtration ................................................................................................................... 15

1.5.4 Filter Types .............................................................................................................................. 15

1.5.5 Cleaning procedure for glass fibre filters ................................................................................ 16

1.5.6 Cleaning procedure for synthetic membrane filters ............................................................... 17

1.5.7 Volume for filtration ................................................................................................................ 17

1.6 Sample Storage ................................................................................................................................ 17

1.7 Auxiliary measurements .................................................................................................................. 19

1.7.1 Water transparency (aka Secchi depth) .................................................................................. 19

1.7.2 Light measurements ................................................................................................................ 19

1.7.3 Standard physical parameters (Temperature, Oxygen concentration, Conductivity) ............ 20

1.8 Methods applied by Project Partners .............................................................................................. 21

1.8.1 Aarhus University (AU) ............................................................................................................ 21

1.8.2 Centro de Biodiversidade e Recursos Genéticos – Universidade de Évora (CIBIO)................. 22

1.8.3 MARine Biodiversity, Conservation and Exploitation (CNRS-MARBEC) .................................. 24


1.8.4 Ecole Normale Superieure (ENS) ............................................................................................. 26

1.8.5 GEOMAR Helmholtz Centre for Ocean Research Kiel (GEOMAR) ........................................... 28

Hellenic Center for Marine Research (HCMR) ......................................................................................... 32

1.8.6 Ludwig-Maximilians-Universität Munich (LMU) ...................................................................... 35

1.8.7 Middle East Technical University (METU) ............................................................................... 37

1.8.8 Netherlands Institute of Ecology (NIOO) ................................................................................. 39

1.8.9 Umweltbundesamt (UBA) ........................................................................................................ 40

1.8.10 University of Helsinki, Tvärminne Zoological Station (UH) ...................................................... 46

1.8.11 University of Bergen (UIB) ....................................................................................................... 48

1.8.12 Umea Marine Science Center (UMF) ....................................................................................... 51

1.8.13 WasserCluster Lunz (WCL) ....................................................................................................... 54

1.9 References 1 – Water Chemistry ..................................................................................................... 56

Co-funded by the European Union D4.1 Standard Operating Procedures| I Cross References

AQUACOSM – INFRA-01-2016-2017- N. 731065 of 56

I. Cross References

The SOPs that will be provided by AQUACOSM will be listed here in the following versions when the different

SOPs are completed.

The SOPs that will be provided by AQUACOSM will be for:

1. Phytoplankton (this SOP)

2. Zooplankton (Deliverable 4.1.2)

3. Microbial Plankton (Deliverable 4.1.3

4. Periphyton (Phytobenthos) (Deliverable 4.1.4)

5. Water Chemistry (Physical and Chemical Elements of Water) (Deliverable 4.1.5)

6. High-Frequency Data Collection (Deliverable 4.1.6)

7. QA/QC (Deliverable 4.1.7)

A general description for water sampling will be covered under the Water Chemistry SOP.

II. Dissemination activities related to the Deliverable

The SOPs will be made available to all users of TA in AQUACOSM, and will also be publicly available for any

user through the AQUACOSM webpage (https://www.aquacosm.eu/project-information/deliverables/)

https://www.aquacosm.eu/project-information/deliverables/

Co-funded by the European Union D4.1 Standard Operating Procedures| 1 Water Chemistry


1. Water Chemistry

1.1 Definitions and Terms

Alkalinity capacity of water to resist changes in pH that would make the water more acidic

Analyte The constituent or characteristic of a sample to be measured

Aphotic Zone Zone within a water body where photosynthetic production is not possible (gross

primary production < respiration)

Blank A blank contains little to no analyte of interest. It is included in measurements to

trace contaminations or signal drift.

Conductivity Inverse of electrical resistivity, increases with ions in solution and is temperature

dependent

Detritus Dead particulate organic material

Euphotic Zone Zone within a water body where photosynthetic production is possible (gross

primary production > respiration), it roughly corresponds to 2-2.5-times of the

transparency (Secchi depth) [1]

Macrophytes Water plants

Matrix Components of a sample other than the analyte

Phytoplankton Community of free-floating, predominantly photosynthetic protists and

cyanobacteria in aquatic systems, (in limnological analysis commonly excluding

ciliates). [1]

Seston Organisms and non-living matter swimming or floating in water

Standard (analytical) Standardized reference material containing a known amount of the analyte, used to

calibrate measured signal against analyte concentration

Stratification Formation of a vertical temperature gradient within a water column that due to

differences in density avoids vertical mixing

Turbidity Cloudiness or haziness of a fluid

Zooplankton Community of free-floating, heterotrophic organisms



1.2 Health and Safety Indications

1.2.1 General Information

In this section, general guidance on the protection of health and safety while sampling and analysing water

samples from mesocosm experiments will be provided to minimize the risk of health impacts, injuries and

maximize safety. The users of this SOP are expected to be familiar with the Good Laboratory Practice (GLP)

of World Health Organization (WHO) [4] and Principles on GLP of Organisation for Economic Co-operation

and Development (OECD) [5]. Health and Safety Instructions of the mesocosm facility, if there are any, shall

be followed properly to protect the people from hazardous substances and the harmful effects of them.

According to preventive employment protection measures to avoid accidents and occupational diseases (on-

site or in the laboratory), the work should be practiced consistent with national and EU regulations (see the

OSH Framework Directive 89/391/EEC, [6]). Other regulations and guidelines can be found on the EU – OSHA

website (European directives on safety and health at work [7]). All necessary safety and protective measures

shall be taken by the users of this SOP and the scientist-in-charge shall ensure that those measures comply

with the legal requirements.

The table below summarizes the hazards, risks and safety measures for laboratory studies on water

chemistry.

Table 1-1: Hazards and risks associated with laboratory work

Occupations at

risk

Hazards/Risks Preventive Measures

Laboratories o Exposure (skin, eye,

inhaling) to harmful

chemicals

o Ingestion of harmful

chemicals

o Appropriate personal protection equipment

(gloves, goggles, lab coat)

o Ventilated working area

o Being informed about risks of applied

chemicals and providing SDSs in the facility

o Clear labelling of all chemical containers

o No eating or drinking in the lab

o Washing hands after leaving the lab

o No storage of sample/ chemicals in empty

food containers

o Keeping solvents away from heat sources

(ovens, open flame, autoclave)

http://www.who.int/tdr/publications/documents/glp-handbook.pdf

http://www.who.int/tdr/publications/documents/glp-handbook.pdf

https://ntp.niehs.nih.gov/iccvam/suppdocs/feddocs/oecd/oecd_glpcm.pdf

http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:31989L0391&from=EN

https://osha.europa.eu/en/safety-and-health-legislation/european-directives



o Flame/ Explosion

o Hot surfaces/ steam

o Vacuum/ Implosion

o Overpressure

o Accidental release of

substances harmful to

the environment

o Use of tightly closed boxes to store solvents in

refrigerators

o Using heat – insulating gloves

o Using autoclaves with safety interlock

o Using exclusively thick-walled containers

approved for vacuum applications

o Using autoclaves with safety interlock

o Collection of chemicals and samples and

disposal according to national and local

regulations

1.2.2 Safety Instructions

Personnel involved in practical work, i.e. installation, sampling, analysis at an AQUACOSM facility has to

receive a safety instruction of the respective institute. The safety instruction summarizes rules, information

and advices related to work safety based on legislation and experience. The safety instruction needs to be

completed prior to practical work.

1.2.3 Working and Personal Protection (Safety) Equipment

Personal protective equipment (gloves, safety glasses, lab coat) has to be provided in the labs and must be

used for handling chemicals.

Gloves should be chosen according to permeation time which depends on material and thickness of gloves

and type of chemical to be used. Check lists of permeation time provided by the distributor of gloves to

choose the type of glove offering best protection. Still, some chemicals easily penetrate any kind of available

glove material. In this case gloves need to be changed immediately after contact with the chemical. Consult

the SDS for recommendations on which material of glove to use.

1.2.4 Use, Storage and Disposal of Reagents and Chemicals

Before using a chemical the first time the Safety Data Sheet (SDS) needs to be consulted to be informed about

the hazard potential of the substance. For each chemical a SDS in its most recent version has to be provided

by the distributor. In addition, SDS for all chemicals used in a lab should be made available to all users, i.e.



hard copies collected in a folder. The SDS provides information on safe handling, storing and disposing of a

chemical. Based on the hazard classifications the user has to apply appropriate personal protective

equipment and needs to work under the chemical fume hood if required to eliminate the risk of exposure.

Chemicals should be stored in original containers if possible. Other containers than original, including

samples containing chemicals need to be labelled clearly. The label should indicate name and concentration

of chemicals as well as date and person responsible. All containers need to be closed tightly and stored in a

ventilated area. Hazardous chemicals have to be stored in specific cabinets separated from other chemicals

and meeting the safety requirements of the respective hazard class. This applies for flammables, explosives,

oxidizing chemicals, acids, bases, and toxic chemicals.

Only the quantities of daily consumption should be stored directly at the working area. Corrosive chemicals

must never be stored above eye height.

Collection vessels for disposal must be clearly labelled with a systematic description of their contents. To

avoid dangerous chemical reactions, consult the SDS before mixing chemicals. Entrust waste chemicals to the

appropriate authorities for disposal.

1.2.5 Use, Storage and Disposal of the Equipment

Consult your local head of the lab about rules for disposal of equipment.

1.3 Environment Indications

A plan for the disposal of chemical waste needs to be prepared prior to the experiments. The plan must be

in competence with the EU Waste Legislation ([8]) and The List of Hazardous Wastes ([9]) provided by the

European Commission. The SDS needs to be revisited for the disposal of reagents and chemicals prior to

waste disposal.

1.4 Sampling

1.4.1 Introduction

Good quality of analytical data relies on (1) representative sampling, (2) suitable storage conditions, and (3)

accurate and precise measurements.

“Progress in analytical protocols results in the taking of samples increasingly becoming quality-determining

step in water quality assessment. Poor sampling design or mistakes in sampling technique or sample handling

during the sampling process inevitably lead to erroneous results, which cannot be corrected afterward.”

(Handbook of water analysis, Nollet, L., M., L., De Gelder, L., S., P., 2014)

http://ec.europa.eu/environment/waste/legislation/a.htm

http://eur-lex.europa.eu/legal-content/EN/TXT/PDF/?uri=CELEX:32000D0532&from=EN



1.4.2 Sampling Strategy/ Sampling Plan

Prior to a sampling event a sampling strategy has to be defined in consideration of selected analytes and aims

of the study. This includes specification of analytes, spatial aspects (surface sample or depth-integrated

sample), sampling frequency, sampling equipment, volume and number of samples, type and size of sample

containers, processing and storage of sample, sample coding, and standardized documentation.

Figure 1-1: Elements of Sampling Strategy (from: Practical guidelines for the analysis of seawater [2])

A. Mixed mesocosms

In case mesocosms are mixed continuously, one water sample can be considered representative for the

entire mesocosm. Here, samples should be taken near the centre of the mesocosm. Care should be taken to



avoid macrophytes, if present, while sampling. If it is unclear whether the whole water volume is efficiently

mixed, an initial series of samples can be taken in transects across the mesocosm and along the vertical axis.

B. Stratified mesocosms

If mesocosms waters are stratified or partially mixed, the sampling procedure must be determined after

careful considerations on the water layer(s) to be sampled (e.g., sampling discrete water layers; sampling

multiple depths with subsequent pooling to one combined representative sample; utilization of tube

sampler). The absence of vertical temperature profiles indicates vertical mixing, but NOT necessarily

homogenous distribution of motile organisms like (micro-) zooplankton. Hence, especially particulate matter

(chlorophyll-a, particulate nutrients) may be non-homogenously distributed even in the absence of a

thermocline, and require careful consideration of the appropriate sampling design.

1.4.3 Equipment for Sampling

The following specific pieces of equipment are suggested for collecting water samples from mesocosms

✓ Appropriate water sampler, depending on the type of sampling (stratified or integrated), and (e.g.

Schroder/Schindler/Ruttner sampler for single strata; tube sampler for depth integrated samples)

✓ As an alternative to a water sampler a sample can be retrieved by pumping, i.e. by a silicone tube

connected to a carboy which in turn is connected to a vacuum pump. Land based mesocosms can be

equipped with sampling ports, avoiding the risk of contamination from sampling equipment.

✓ Clean & rinsed sampling containers in the field

✓ Sampling containers needs to be labelled properly in the laboratory prior to sampling. The labels on

the sampling bottles need to be standardized and provide information on name of the experiment,

sampling date, mesocosm ID, and possibly depth with appropriate abbreviations of the treatments

of the experiments. Labels can be either printed or written using a permanent waterproof marker

Figure 1-2: Devices for water sampling - Ruttner Sampler, Schindler Patalas, and Tube Sampler



1.4.4 Techniques for representative sampling

Representative sampling – samples need to be representative for the mesocosm unit of interest. In case

multiple parameters (e.g. dissolved & particulate nutrients, chlorophyll-a) are sampled on the same event, it

is mandatory that all parameters are analysed from the same water sample (multiple sub-samples from one

water sample). This implies that homogenous distribution of particles (phytoplankton, bacteria, detritus) is

ensured whenever a sub-sample is taken from the sampling container.

A. Mixed mesocosms

In case mesocosms are mixed continuously, one water sample can be considered representative for the

entire mesocosm. Here, samples should be taken near the centre of the mesocosm as stated in both [10] and

[12]. Care should be taken to avoid macrophytes, if present, while sampling. If it is unclear whether the whole

water volume is efficiently mixed an initial series of samples can be taken in transects across the mesocosm

and along the vertical axis (see point 6.4.B below).

B. Stratified mesocosms

If mesocosms waters are stratified or partially mixed, the sampling procedure must be determined after

careful considerations on the water layer(s) to be sampled (e.g. sampling discrete water layers; sampling

multiple depths with subsequent pooling to one combined representative sample; utilization of tube

sampler). Absence of vertical temperature gradients indicates vertical mixing, but NOT necessarily

homogenous distribution of motile organisms like (micro-) zooplankton. Heterogeneous distribution of

phytoplankton must also be assumed if mesocosms contain structuring elements (such as macrophytes), and

has not been proven to be (practically) homogenous (see 6.4.A). C. Composite and discrete sampling

Careful consideration of the sampling design is required in case the mesocosms are stratified and include an

aphotic zone (mesocosm depth > Zeu1). In this case the integrated water sample would typically be taken from

the euphotic zone (Zeu).

For shallow mesocosms containing sediment and possibly macrophytes, a detailed sampling design for

collecting samples at multiple horizontal and vertical positions might be needed [12]:

Best Practice Advice: “The entire water column, from the surface to approx. 5 cm above the sediment, is

sampled from three positions in each enclosure: 10, 30 and 60 cm from the enclosure wall. Two samples are

prepared: one to be used for chemical and phytoplankton analyses where water is sampled without touching

the plants – and one to be used for zooplankton analysis, where water is sampled also close to the plants.”

“The best way to sample from the entire water column is by using tube samplers which sample from top to

bottom. The diameter of the tube should not be too small to avoid zooplankton escaping during sampling (>

6 cm). If it is not possible to use a tube sampler, samples can be taken with a Ruttner water sampler from the

surface (20 cm below the water surface), middle and the bottom (20 cm above the sediment). The sample in

the middle should be adjusted according to the enclosure type and actual water depth [11].

1 Zeu corresponds to 2-2.5 x Secchi depth



1.4.5 Quality Assurance Considerations

Any treatment of a sample, like transfer into another container, preservation, filtration, dilution may

introduce a contamination or alter the sample in another way. Consequently, the ideal procedure would be

to transfer the sample directly into the container for storage and analyse it immediately.

Sampling Technique

Already the technique of sampling can alter the quality of a sample. Pumping or temperature change may

already affect concentration of dissolved gases.

Sampling Sequence

Following sequence is recommended for subsampling water from a water sampler:

O2, pH/DIC/Alkalinity/ Nutrients

Contaminations

Potential sources for contamination of samples throughout the entire sampling procedure need to be

identified and avoided. Problematic contaminations can be either the chemical compound of interest or any

other substance interfering with the chemical analysis.

Sources for contaminations may be:

• Water Sampler/ Tube: Make sure it is clean and the materials suite your purpose.

• Sample Vials: Materials may release/ adsorb compounds into/ from your sample. Use clean

containers of appropriate material and consider rinsing them with sample first.

• Skin: Wear gloves to avoid contaminations with sweat, remains of soap, sun screen, etc.

• Boat Exhaust/ Cigarette Smoke: Rich in ammonia

Best Practice Advice: Use silicone tubing for O2, pH, DIC

Sample Matrix

The matrix of a sample (turbidity, salinity, colour, alkalinity, other chemical constituents) can affect the

chemical analysis in various ways. Optical characteristics of the sample can influence measurements based

on absorbance and fluorescence or may interfere with the signal-producing reaction. If sample and standard

do not share the same matrix, the calibration is incorrect.

Turbidity: If possible, turbidity should be removed by filtration. Alternatively, the chemically untreated

sample can be used as blank to correct for turbidity.

Salinity: Sea salt may suppress analyte absorbance in spectrophotometric measurements like phosphate,

silicate and ammonia. This problem can be addressed by preparing reference solutions of standards with



nutrient-free or low-nutrient sea water, or artificial sea water. The salinity should be equal to that of the

samples. If salinity varies a lot, a mathematical correction of salt effects can be applied by establishing a

correction function for each analyte showing salt effects.

1.5 Filtration

1.5.1 Introduction

By means of filtration, the water sample is separated into a particulate and dissolved fraction for separate

analysis. The water sample can be forced through the filter material either with vacuum or over-pressure.

The filter type affects minimal particle size retained and filtering capacity. Filter material needs to be chosen

to minimize interaction with the analyte and to allow required cleaning procedures (see 7.5 and 7.6). Any

meaningful analysis of a set of filtered samples must include at least 4 blanks. Blank filters should be cleaned

according to established procedures and from the same batch as the filters used for the samples.

1.5.2 Vacuum Filtration

The circulate filter is placed between the filter support and the funnel held in place with a clamp. Filtrate is

collected in the receiving flask while particles are retained on the filter. Applied vacuum should not exceed

200 m bar to avoid rupture of cells and leaching of particulate material [13].

Figure 1-3: Vacuum filtration (from: Practical guidelines for the analysis of seawater [2])



1.5.3 Pressure Filtration

As an alternative to vacuum filtration a sample can be pressurized and passed through a filter. Filtration with

syringe and filter holder may be an optimal procedure if samples need to be filtered immediately. Required

equipment is small and filtration does not depend on infrastructure, hence filtration with a syringe can be

easily performed in the field. Still it is only appropriate when rather small volumes of sample need to be

filtered.

To minimize sample carry-over syringe and filter need to be flushed with new sample, especially because

filter holders contain some dead volume.

Figure 1-4: Disposable filter discs and reusable filter holders used for filtration with the syringe

1.5.4 Filter Types

Glass fibre filters are best choice for organic carbon (DOC/POC), nitrogen (DON/PON), and phosphorus

(DOP/POP). Glass fibre filters have a poor uniform pore size, but they can be easily cleaned by baking at high

temperature (typically 450°C) for several hours to produce low blanks for these elements and at the same

time they provide good flow rates for high-volume samples. Glass fibre filters are the classical filter material

for the determination of chlorophyll pigments and are also suitable for the filtration of nutrient samples

except silica, in which polycarbonate filters are mostly used [2].

Besides glass fibre filters (GF/F ~ 0,7µm and GF/C ~ 1,2µm) membrane filters of 0,45 and 0,2µm pore size are

used to separate particulate and dissolved phases of water samples [3].



Best practice advice:

● For efficient retention of seston including cyanobacteria GF/F filters should be used.

● Filters used for quantification of particulate carbon should be pre-combusted at 450°C

● Filters for quantification of particulate phosphorus should be acid washed.

Table 1-2: Filter Materials and their characteristics (from: Practical guidelines for the analysis of seawater [2])

1.5.5 Cleaning procedure for glass fibre filters

To assure glass fibre filters are free of organic traces they have to undergo a cleaning procedure.

Bake filters at 450°C for 4 hours. Place filters in a glass beaker and cover them with diluted acid (i.e. 10-15%

Hydrochloric Acid). Rinse filters repeatedly with analytical grade water and dry them at 60°C.



✓ Best practice advice: Apply the above cleaning procedure (acid washing/ baking) to all glass fibre

filters even if not required for the subsequent analysis (i.e. chlorophyll). This will assure identical

filtration results/ comparability of chemical parameters since the high temperature and washing can

affect the effective pore size of the filters.

1.5.6 Cleaning procedure for synthetic membrane filters

Rinse with analytical grade water (i.e. MilliQ) and allow the filters to stand soaked in MilliQ for 30 minutes,

rinse again with MilliQ and press out the remaining water with air. A test tube rack can be used as support.

Always discard the first millilitres of sample to waste.

✓ Best practice advice: Use syringes with plastic plungers, avoid syringes with rubber plungers. The

rubber or the grease on the rubber is a potential source for contamination.

1.5.7 Volume for filtration

The water volume required in order to collect sufficient material on a filter depends both on the parameter,

the sensitivity of the methodology, and esp. on the density of particles in the water, which in turn depends

on the trophic state of the experimental system.

✓ As a rule of thumb, a clearly visible coloration on the filter (well visible against the white background

of a glass fibre filter) ensures reasonable quantity of material for most common analytical protocols

(PON/C/P, Chlorophyll-a).

✓ A careful documentation of filtered volume is mandatory in order to calculate concentrations (e.g.

µg Chl-a L-1).

1.6 Sample Storage

The biological activity in water does not stop with sample collection, since bacteria and micro- and nano-

plankton continue to digest and excrete material [13].

Nutrients are subject to rapid changes in their concentration within a few hours in unpreserved samples [2].

Sample preservation is needed whenever measurements cannot be performed immediately or when a

backup for potential reanalysis is required.

Each analyte has its own reaction chemistry and consequently different requirements for storage in solution.

Therefore, no general procedure can be recommended for the storage of water samples [3].

Optimum storage conditions differ largely among parameters (see Table 1-3 below).



Table 1-3: Best Practice Advice for Storage of Water Samples

Analyte Container Preservation Notes

Soluble Reactive

Phosphorus

Glass, acid washed

LDPE, acid washed

Filter and measure immediately or store ≤4°C in the dark if

analysed within 24hrs.

For longer storage freeze filtered samples at -20°C.

Calcareous water (Ca2+ > 100mgL-1)

must be acidified with 1ml

concentrated hydrochloric acid L-1

before freezing to prevent co-

precipitation of phosphate

Particulate Phosphorus Plastic petri dish or

Eppendorf tube

Filter immediately, freeze filters at -20°C

Total Phosphorus Glass, acid washed

LDPE, acid washed

Store in containers and volumes desired for digestion ≤4°C in

the dark.

For long term storage freeze samples at -20°C.






Total Dissolved

Phosphorus

Glass, acid washed

Store filtered samples in containers and volumes desired for

digestion ≤4°C in the dark.

For long term storage freeze filtered samples at -20°C.






Total Reactive

Phosphorus

Glass, acid washed

Measure immediately, or store at 4°C in the dark if analysed

within 24hrs.

Ammonia Plastic or Glass Measure immediately, if necessary filter and store at 4°C for

up to 24hrs, or filter and freeze unacidified at -20°C for up to

28d

Note that samples that have been

measured immediately are not

necessarily comparable with

samples that have been filtered and

frozen. this is especially true for

ammonia.

DOC (NPOC) Polycarbonate or

cell culture flasks

Filter through combusted GF/F or 0,2µm membrane filter into

combusted glass vial and preserve immediately with H3PO4,

store in the dark at 4o C.

Nitrate Plastic or Glass Measure immediately, if necessary filter and store at 4°C up to

2d. For longer storage filter and store at -20°C.

In samples preserved with acid, NO3-

and NO2- cannot be determined as

individual species.

Nitrite Plastic or Glass Measure immediately, or filter and store at -20°C for longer

storage

Never acidify for storage.

Total Nitrogen Plastic or Glass Acidified to pH 1-2 with H2SO4 samples can be stored 1 month

Chlorophyll a Plastic petri dish or

Eppendorf tube

Filter immediately after sampling and freeze at -20C Protect from light, ideally store at -

80°C

Dissolved Inorganic

Silicate

Plastic Filter immediately. Store at 4°C for up to 1 month. Do not acidify, silicate precipitates

under acidic conditions. Avoid

freezing.

Total alkalinity Glass, acid washed Filter immediately after sampling and store at 4°C up to 24h or

up to a month if the samples is poisoned.

Samples can be poisoned with HgCl2

solution.

Oxygen, dissolved Plastic or Glass Cool, protect from air and light, store up to 6hrs On-site measurement preferable



pH Plastic or Glass Cool, protect from air (fill bottle to cap) On-site measurement preferable

Alkalinity Plastic or Glass Cool, protect from air (fill bottle to cap), store up to 24h On-site measurement preferable,

especially for samples high in

dissolved gases

Best practice advice: Samples preserved by acidification should be neutralized prior to analysis. Acid and

base may introduce background to the sample, hence standards used in subsequent measurements must

undergo the same treatment.

1.7 Auxiliary measurements

Here we briefly outline measurements that are often conducted in combination with sampling for water

chemistry. Transparency and basic physical parameters are often taken alongside water sampling for water

chemistry and phytoplankton.

Best practice advice: The relevance of measuring irradiation and transparency depends on the depth of the

mesocosms. In shallow mesocosms (d < 2m), light very likely will not be limiting during the growing season.

Moreover, the influence of the suspended particles including phytoplankton on under water light climate is

very limited in shallow water columns.

1.7.1 Water transparency (aka Secchi depth)

Water transparency is a key parameter in limnology and oceanography, informing especially about the optical

depth of the water column, which affects e.g. the vertical structure of biota and biological processes, such as

primary production, but also vertical migration of the zooplankton.

Transparency is typically measured by lowering a white disk vertically into the water until it is not visible

anymore. Now the disk is slowly lifted, until it becomes visible. The depth where the disk just becomes visible

is defined Secchi depth. A detailed outline is given in

http://www.helcom.fi/Lists/Publications/Guidelines%20for%20measuring%20Secchi%20depth.pdf.

1.7.2 Light measurements

Light is a key resource for primary production. In aquatic ecology, it is commonly measured as photo-

synthetically active radiation (PAR; https://www.licor.com/documents/liuswfuvtqn7e9loxaut ). For proper

quantification of light, irradiation needs to be measured by an appropriate probe at various positions inside

the mesocosm, taking the optical structure (illuminated vs. shaded side etc.) and day-time into account.

Especially in narrow mesocosms with opaque walls, a proper quantification of irradiation may be very

difficult.

https://www.licor.com/documents/liuswfuvtqn7e9loxaut



If light intensity is a key parameter and e.g. manipulated by shading, comparing irradiance at a fixed position

(e.g. middle of water column) may be a good proxy. An example for light-manipulation inside mesocosms

can be found here https://www.nature.com/articles/srep29286

1.7.3 Standard physical parameters (Temperature, Oxygen concentration, Conductivity)

Standard physical parameters, especially water temperature, conductivity, pH and oxygen concentration are

often measured using handheld probes. For measuring all of these parameters, the same recommendations

regarding representativeness apply, as outlined above (→ 1.4.4 Techniques for representative sampling). If

mesocosms are stratified, layers must be sampled separately. Measurements of physical parameters using

submersible probes are described in section Fehler! Verweisquelle konnte nicht gefunden werden. Fehler!

Verweisquelle konnte nicht gefunden werden. (High Frequency Measurements).



1.8 Methods applied by Project Partners

1.8.1 Aarhus University (AU)

Parameter

Detection Mode

Method Name Reference Comments Manual Automated

Alkalinity X Titration DS 253, 1977

Chlorophyll a X

Spectrophotometric determination in ethanol

extract

DS 2201, 1986

X Chlorophyll a sensors - Turner designs - Cyclops 7F

Conductivity X YSI 6600 Xylem Analytics

Nitrogen

NH4

X

Photometric method, ammonia-nitrogen

(indophenol blue)

DS 224, 1975

NO3

X

Automated Hydrazine Reduction method with FIA

Star 5000 Foss FIA Star 5000

TN

X

Automated Hydrazine Reduction method with FIA

Star 5000, digestion with peroxodisulfate/NaOH

DS 221/Foss FIA Star 5000

Oxygen X Oxygen probe Oxyguard

pH X pH probe Oxyguard

Phosphorus



SRP

X

Orthophosphate photometric method (ascorbic

acid/molybdate) DS 291, 1985

TP

X

Total Phosphorus photometric method (ascorbic

acid/molybdate), digestion with peroxodisulfate DS 292, 1985

Silica X Photometric method, molybdosilicate DMU T.A. nr. 22

1.8.2 Centro de Biodiversidade e Recursos Genéticos – Universidade de Évora (CIBIO)

Parameter

Detection Mode Method Name

Reference

Comments

Manual Automated

Conductivity X Digital rugged conductivity probe CDC40105, Hach

Oxygen X

Digital, luminescent/optical dissolved

oxygen (LDO) probe LDO101, Hach

pH X

Digital combination pH electrode with

built-in temperature sensor PHC101, Hach

Chlorophyll a X Handheld Fluorometer /Chlorophyll in vivo Aquafluor®, Arar 1997 (EPA Method 445.0)

No cell disruption and

acidification is applied

Nitrogen

NH3 X Indophenol Blue Method Ivancic & Deggobis 1984

NO2 X Automated Hydrazine Reduction Method ISO 13395:1996




TN X

Persulfate Digestion, Hydrazine Reduction

Method

Clesceri 1999 (4500-P, chapter J);

ISO 13395:1996

Phosphorus

TP/ TDP X

Persulfate Digestion and Ascorbic Acid

Method Grasshoff 1999 (chapter 10.2.13)

References

Arar, E. J., & Collins, G. B. (1997). Method 445.0: In vitro determination of chlorophyll a and pheophytin a in marine and freshwater algae by fluorescence.

Cincinnati: United States Environmental Protection Agency, Office of Research and Development, National Exposure Research Laboratory.

Clesceri, L. S., Greenberg, A. E., & Eaton, A.D. (1996). Standard methods for the examination of water and wastewater. APHA, AWWA and WPCF, Washington DC.

DIN EN ISO 15681-2, Water quality - Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA) - Part 2: Method by

continuous flow analysis (CFA), 06-2001



1.8.3 MARine Biodiversity, Conservation and Exploitation (CNRS-MARBEC)

Parameter

Detection Mode


Chlorophyll a X Fluorometric Detection Strickland and Parson 1972

Acetone extraction

Ultrasonic cell disruption

Pigments X High-Performance Liquid Chromatography Method Zapata et al. 2000

Suspended

particulate matter

(SPM)

X Gravimetric Strickland and Parson 1972

Nitrogen

NH4 X Ortho-phthaldialdehyde fluorometric Method (OPA) Holmes et al. 1999

NO2

X

CFA-based photometric detection, diazotization of

NO2 (Gries-Ilosvay reaction) with sulphanilamide

produce a reddish-purple colour, which is measured

at 540 nm.

ISO 13395:1996

NO3

X

CFA-based photometric detection, nitrate reduction

to nitrite by use of coppered Cd-granules and

detection as nitrite (see above)

ISO 13395:1996

Oxygen (dissolved) X Titration – Winkler method Strickland and Parsons 1972

- use of a silicone tube for sampling

to avoid air bubbles

- use of calibrated bottles/flasks.



pHT (total scale) X

Spectrophotometric method (based on the

absorption ratio of the sulfonephthalein dye, m-

cresole purple

Byrne 1993

Liu et al 2011

- use of a silicone tube for sampling

to avoid air bubbles

Phosphorus

SRP

X

CFA-based photometric detection, reduction to

molybdenum blue complex by use of ascorbic acid.

The complex is measured at 660 nm.

ISO 15681-2

Salinity X

Silica X


molybdenum blue complex by use of ascorbic acid ISO-16264

Oxalic acid is added to avoid

phosphate interference

Temperature X

References

Byrne R.H. (1993). Spectrophotometric seawater pH measurements: total hydrogen ion concentration scale calibration of m-cresol purple and at-sea results.

Deep-Sea Research, Vol. 40, No 10, pp 2215-2129.

Holmes, R. M., Aminot, A., Kérouel, R., Hooker, B. A., & and Peterson, B. J. (1999). A simple and precise method for measuring ammonium in marine and freshwater

ecosystems. Can. J. Fish. Aquat. Sci., 56, 1801–1808

ISO 13395:1996, Water quality -- Determination of nitrite nitrogen and nitrate nitrogen and the sum of both by flow analysis (FIA and CFA) and spectrometric

detection.

ISO 15681-2, Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA), Part 2: Method by continuous flow analysis (CFA).

ISO-16264: Determination of soluble silicates by flow analysis (FIA and CFA) and photometric detection.



Liu X., Patsavas M.C and Byrne R.H. (2011). Purification and characterization of meta-cresol purple for spectrophotometric seawater pH measurements. Environ.

Sci. Technol., 2011, 45 (11), pp 4862–4868.

Strickland, J.D.H., & Parsons, T.R. (1972). A Practical Handbook of Seawater Analysis. 2nd Edition, Fisheries Research Board of Canada Bulletin, 167, 310 p.

Zapata, M., Rodriguez, F., & Garrido, J. (2000). Separation of chlorophylls and carotenoids from marine phytoplankton: A new HPLC method using a reversed

phase C-8 column and pyridine-containing mobile phases. Mar. Ecol. Prog. Ser., 195, 29–45, doi:10.3354/meps195029

1.8.4 Ecole Normale Superieure (ENS)

Parameter

Detection Mode


Alkalinity,

total

X Potentiometric automated titration with open cell

method

Dickson et al. 2007

Chlorophyll a X Fluorometric Detection after Acetone Extraction Jespersen and Christoffersen 1987

Dissolved oxygen X Optical method (optode sensor)

Nitrogen

NO2

X Colorimetric with Sulfanilamide and NEDD Grasshoff et al. 1983 N° G-173-96 Rev. 10 Seal analytical AA3

autoanalyzer method

X Colorimetric Strickland and Parsons, 1972 UV VIS

spectrophotometer



NO3 X

Colorimetric with Sodium salicylate Strickland and Parsons, 1972 UV VIS

spectrophotometer

X Cd reduction and colorimetric method with

Sulfanilamide and NEDD

Grasshoff et al. 1983 N° G-392-08 Rev. 5 Seal analytical AA3

autoanalyzer method

NH4+ X Ortho-phthaldialdehyde (OPA) fluorometric Method Kerouel and Amniot 1997 NH4+

TN

X Persulfate digestion, Cd reduction and colorimetric

method

Grasshoff et al. 1983

N° G-392-08 Rev. 5

Seal analytical AA3

autoanalyzer method

pH X

Potentiometric with glass/reference electrode cell

(total scale)

Dickson et al. 2007

Phosphorus

SRP X Colorimetric with molybdate and ascorbic acid Strickland and Parsons, 1972 UV VIS

spectrophotometer

X Colorimetric with molybdate and ascorbic acid Murphy and Riley 1962

Drummon and Maher 1995

N° G-175-96 Rev. 15 (Multitest MT 18)

TP/TDP

X Persulfate and sulfuric acid digestion then molybdate

and ascorbic acid method

Grasshoff et al. 1983 N° G-393-08 Rev. 4 Seal analytical AA3

autoanalyzer method

Silicate X Ascorbic Acid - Molybdenum – Oxalic - Blue Complex Grasshoff et al. 1983 N°. G-177-96 Rev. 11

(Multitest MT19)

Seal analytical AA3

autoanalyzer method



References

Dickson A.G., Sabine, C.L. and Christian, J.R. (Eds.) 2007. Guide to best practices for ocean CO2 measurements. PICES Special Publication 3, 191 pp.

Jespersen, A-M. & K. Christophersen, 1987. Measurements of chlorophyll- a from phytoplankton using ethyl alcohol as extraction solvent. Arch.Hydrobiol. 109:

445-454.

Kerouel, R.and Amniot, A. Marine Chemistry Vol. 57, no 3-4, pp.265-275, Jul 1997.

Strickland, J. D. H., and Parsons, T. R. (1972). A practical handbook of seawater analysis. B. Fish. Res. Board Can. 167, 311.

K. Grasshoff et al., Methods of Seawater Analysis, 2nd edition, Verlag Chemie, 1983.

Murphy, J. and Riley J.P., 1962. A modified single solution method for the determination of phosphate in natural waters. Analytica Chimica Acta 27:31-36.

Drummon, L. and Maher, W., 1995. Re-examination of the optimum conditions for the analysis of phosphate. Analytica Chimica Acta 302: 69-74.

1.8.5 GEOMAR Helmholtz Centre for Ocean Research Kiel (GEOMAR)

Parameter


Reference

Comments

Manual Automated

Alkalinity,

total X Potentiometric titration, open-cell method Dickson et. al., 2003

Carbon

DIC X Acidification, gas stripping, Infrared absorption e.g. Goyet & Snover, 1993



POC X

Treated with fuming HCL in a desiccator for 2h,

elemental analysis accomplished by combustion

analysis

Sharp 1974, Hansen and Koroleff 1999;

Grasshoff “Methods of seawater

analysis”, 1999

TPC X

Elemental analysis accomplished by combustion

analysis



analysis”, 2001

Chlorophyll a X Fluorometric Detection after acetone extraction Welschmeyer 1994

Pigments X

Reverse-phase high-performance liquid

chromatography Barlow et al., 1994

Nitrogen

DON X Determination by alkaline persulphate oxidation Hansen and Koroleff, 1999

NH4 X Determined fluorometrically Holmes et. al. 1999

NO2 X

Automated Camium Reduction Method,

photometrically

Murphey and Riley et.al., 1962; Hansen

and Koroleff, 1999; Grasshoff “Methods of

seawater analysis”, 1999; NIOZ –

Nederlands Instituut for Onderzoek der

Zee (Royal Netherlands Institute ), Den

Hoorn (Texel), The Netherlands

NO3 X

Automated Cadmium Reduction Method,

photometrically


and Koroleff, 1999, modified by Keroul

and Aminot 1997, Grasshoff “Methods of





Zee (Royal Netherlands Institute for Sea

Reserach), Den Hoorn (Texel), The

Netherlands

PON


analysis



analysis”, 2000

TPN

X


analysis



analysis”, 2002

pH T (total

scale) X

Spectrophotometric method (based on the

absorption ratio of the sulfonephthalein dey, m-

cresole purple Clayton and Byrne, 1993

Phosphorus

DOP X Determination by alkaline persulphate oxidation Hansen and Koroleff, 1999

SRP X Automated Cadmium Reduction Method










Netherlands

TPP X Spectrophotometrically

Hansen and Koroleff, 1999; Holmes et al.,

1999

Silica

Biogenic

silica X

Spectrophotometrically, leaching method (135

minutes, 85°C with 0.1M NaOH) Hansen and Koroleff, 1999

Silic acid X Automated Cadmium Reduction Method








Netherlands



Hellenic Center for Marine Research (HCMR)

Parameter


Reference

Comments

Manual Automated

Carbon X

POC X

CHN analyzer Hedges and Stern (1984)

TOC

X

high-temperature catalytic oxidation

method Sempéré et al. (2002)

Chlorophyll a X

Fluorometric Detection after acetone

extraction Holm-Hansen et al. (1965)

Nitrogen

NH3

X

Vis/UV spectrophotometric

determination Ivancic & Deggobis 1984

NO2

X


determination Strickland and Parsons (1972)

NO3

X



PON X

CHN analyzer Hedges and Stern (1984)

TN

X

Wet-oxidation

Pujo-Pay & Raimbault (1994) and

Raimbault et al. (1999)

Oxygen,

dissolved X Winkler Carpenter (1965a, b)



Phosphorus

SRP

X


determination Strickland and Parsons (1972) micromolar level

SRP X

MAGIC method Rimmelin and Moutin, 2005 nanomolar level

TP

X

Wet-oxidation

Pujo-Pay & Raimbault (1994) and

Raimbault et al. (1999)

Silica X



References

Carpenter, J. H., 1965(a). The accuracy of the Winkler method for the dissolved oxygen analysis. Limnology and Oceanography, 10, 135-140.

Carpenter, J. H., 1965(b). The Chesapeake Bay Institute technique for dissolved oxygen method. Limnology and Oceanography, 10, 141-143.

Hedges, J. I., and Stern, J. H. (1984). Carbon and Nitrogen determination of carbonate-containing solids. Limnol. Oceanogr. 29, 657–663.

Holm-Hansen, O., Lorenzen, C. J., Holmes, R. W., and Strickland, J. D. H. (1965). Fluorometric determination of chlorophyll. J. Cons. Perm. Int. Explor. Mer. 30, 3–

15.

Invancic, I., and Degobbis, D. (1984). An optimal manual procedure for ammonia analysis in natural waters by the indophenol blue method. Water Res. 18, 1143–

1147.

Kirchmann, D. L., Newell, S. Y., and Hodson, R.,E. (1986). Incorporation versus biosynthesis of leucine: implications for measuring rates of protein syntheis and

biomass production by bacteria in marine systems. Mar. Ecol. Prog. Ser. 32, 47–59.



Lin, P., Chen, M., and Guo, L. (2012). Speciation and transformation of phosphorus and its mixing behavior in the Bay of St. Louis estuary in the northern Gulf of

Mexico. Geochim. Cosmochim. Acta 87, 283–298.

Miyazaki, Y., Kawamura, K., Jung, J., Furutani, H., and Uematsu, M. (2011). Latitudinal distributions of organic nitrogen and organic carbon in marine aerosols

over the western North Pacific. Atmos. Chem. Phys. 11, 3037–3049. doi:10.5194/acp-11-3037-2011.

Pujo-Pay, M., Raimbault, P., 1994. Improvement of the wet-oxidation procedure for simultaneous determination of particulate organic nitrogen and phosphorus

collected on filters. Mar. Ecol. Prog. Ser. 105, 203-207.

Raimbault, P., Pouvesle, W., Diaz, F., Garcia, N., Sempere R., 1999. Wet oxidation and automated colorimetry for simultaneous determination of organic carbon,

nitrogen and phosphorus dissolved in seawater. Marine Chemistry, 66, 161-169.

Sempéré, R., Panagiotopoulos, C., Lafont, R., Marroni, B., and Van Wambeke, F. (2002). Total organic carbon dynamics in the Aegean Sea. J. Mar. Syst. 33–34,

355–364.

Smith, D. C., and Azam, F. (1992). A simple, economical method for measuring bacterial protein synthesis rates in seawater using 3H-leucine. Mar. Microb. Food

Webs 6, 107–114.

Steeman-Nielsen, E. (1952). The use of radio-active carbon (C14) for measuring organic production in the sea. Journal du Cons 18, 117–140.

Strickland, J. D. H., and Parsons, T. R. (1972). A practical handbook of seawater analysis. B. Fish. Res. Board Can. 167, 311.

Rimmelin, P., and Moutin, T. (2005). Re-examination of the MAGIC method to determine low orthophosphate concentration in seawater. Anal. Chim. Acta 548,

174–182.



1.8.6 Ludwig-Maximilians-Universität Munich (LMU)

Parameter

Detection Mode


Alkalinity X Acidic titration DIN ISO 9963-1/2

Carbon (POC) X Elemental analyser DIN 38409-46; Hedges & Stern 1984

Chlorophyll a X

In vitro: fluorometric detection after acetone

extraction DIN 38412-16

X

In vitro: fluorometric detection after ethanol

extraction DIN 38412-16

X

In vivo: fluorometric detection (Algal lab

analyser, Turner, AquaPen)

Chlorophyll content is excited

by coloured LEDs and allocated

to the different algal classes

Cl- X Ion chromatography DIN ISO 10304-1; Smith & Chang 1983

Nitrogen

NO2 X Ion chromatography DIN ISO 10304-1; Smith & Chang 1983

NO3 X Ion chromatography DIN ISO 10304-1; Smith & Chang 1983

NH4 X Fluorometrical Holmes et al. 1999

PON X Elemental analyser Hedges & Stern 1984

Oxygen, dissolved X Winkler Carpenter (1965a, b)

Phosphorus

PP X Photometric with ammoniummolybdate DIN ISO 6878:2004; Grasshoff et al. 1999



SRP X Photometric with ammoniummolybdate DIN ISO 6878:2004; Grasshoff et al. 1999

TP X Photometric with ammoniummolybdate DIN ISO 6878:2004; Grasshoff et al. 1999

Salinity X 2 graphite electrodes WTW multi probe

SiO2 X Photometric detection DIN ISO 15923-1

SO4 Ion chromatography DIN ISO 10304-1; Smith & Chang 1983

References

Carpenter, J. H., 1965(a). The accuracy of the Winkler method for the dissolved oxygen analysis. Limnology and Oceanography, 10, 135-140.

Carpenter, J. H., 1965(b). The Chesapeake Bay Institute technique for dissolved oxygen method. Limnology and Oceanography, 10, 141-143.

Grasshoff, K., Kremling, K., & Ehrhardt, M. (Eds.). (1999). Methods of seawater analysis. John Wiley & Sons

Hedges, J. I., & Stern, J. H. (1984). Carbon and nitrogen determinations of carbonate‐containing solids. Limnology and oceanography, 29(3), 657-663.

Holmes, R.M., Aminot, A., Kérouel, R., Hooker, B.A & Peterson, B.J. (1999) A simple and precise method for measuring ammonium in marine and freshwater

ecosystems. Can.J.Fish.Aquat.Sci. 56: 1801-1808.

Smith, F. C., & Chang, R. C. C. (1983). The practice of ion chromatography. Wiley.

DIN EN ISO 9963-1:1996-02: Wasserbeschaffenheit - Bestimmung der Alkalinität - Teil 1: Bestimmung der gesamten und der zusammengesetzten Alkalinität

(ISO 9963-1:1994); Deutsche Fassung EN ISO 9963-1:1995

DIN EN ISO 9963-2:1996-02: Wasserbeschaffenheit - Bestimmung der Alkalinität - Teil 2: Bestimmung der Carbonatalkalinität (ISO 9963-2:1994); Deutsche

Fassung EN ISO 9963-2:1995

DIN 38409-46:2012-12: Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammuntersuchung - Summarische Wirkungs- und Stoffkenngrößen

(Gruppe H) - Teil 46: Bestimmung des ausblasbaren organischen Kohlenstoffs (POC) (H 46)



DIN 38412-16:1985-12: Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammuntersuchung; Testverfahren mit Wasserorganismen (Gruppe L);

Bestimmung des Chlorophyll-a-Gehaltes von Oberflächenwasser (L 16)

DIN EN ISO 10304-1:2009-07: Wasserbeschaffenheit - Bestimmung von gelösten Anionen mittels Flüssigkeits-Ionenchromatographie - Teil 1: Bestimmung von

Bromid, Chlorid, Fluorid, Nitrat, Nitrit, Phosphat und Sulfat (ISO 10304-1:2007); Deutsche Fassung EN ISO 10304-1:2009

DIN EN ISO 6878:2004-09: Wasserbeschaffenheit - Bestimmung von Phosphor - Photometrisches Verfahren mittels Ammoniummolybdat (ISO 6878:2004);

Deutsche Fassung EN ISO 6878:2004

DIN ISO 15923-1:2014-07: Wasserbeschaffenheit - Bestimmung von ausgewählten Parametern mittels Einzelanalysensystemen - Teil 1: Ammonium, Nitrat, Nitrit,

Chlorid, Orthophosphat, Sulfat und Silikat durch photometrische Detektion (ISO 15923-1:2013)

1.8.7 Middle East Technical University (METU)

Parameter


Reference

Comments

Manual Automated

Alkalinity X Titration

Standard Methods, 22. Edition. American

Health Association, 1996.

Chlorophyll a X

Spectrophotometric Detection after dissolving in

ethanol

Jespersen, A-M. & K. Christophersen,

1987.

Nitrogen

NH3 X The Skalar Autoanalyzer method

San++ Automated Wet Chemistry

Analyzer, Skalar Analytical,



B.V., Breda, The Netherlands

X Indophenol Blue Method Chaney, A. L. and Morbach, E. P., 1982.

NO2 X The Skalar Autoanalyzer method




X Spectrophotometric method (pink dye)

Mackereth, F.J., H. J. Heron & J. F. Talling,

1978.

NO3 X The Skalar Autoanalyzer method




X Spectrophotometric method (pink dye)


1978.

TN

X The Skalar Autoanalyzer method




Phosphorus

SRP X Ascorbic Acid Method


1978.

TP/ TDP X Persulfate Digestion, Ascorbic Acid Method


1978.

Silica X

Molybdosilicic Acid Method/ Heteropoly Yellow

Method

Golterman, H., L. Clymo & M. A. M.

Ohnstad, 1978.)



References

Chaney, A. L. and Morbach, E. P., 1982. Modified reagents for the determination of urea and ammonia. Clin. Chem. 8, 130-132.

Golterman, H., L. Clymo & M. A. M. Ohnstad, 1978. Methods for chemical and physical analyses of freshwaters. 2nd edition. Blackwell Scientific Publishers, Oxford.

Jespersen, A-M. & K. Christophersen, 1987. Measurements of chlorophyll a from phytoplankton using ethyl alcohol as extraction solvent. Arch.Hydrobiol. 109:

445-454.

Mackereth, F.J., H. J. Heron & J. F. Talling, 1978. Water analyses: some methods for limnologists. Freshwater Biological Assoc. Scientific Publication No: 36.

Standard Methods, 22. Edition. American Health Association, 1996.

San++ Automated Wet Chemistry Analyzer, Skalar Analytical,B.V., Breda, The Netherlands.

1.8.8 Netherlands Institute of Ecology (NIOO)

Parameter


Reference

Comments

Manual Automated

Alkalinity X Si Analytics Titroline-7000, Titrasoft software 3.1 Si Analytics,

Carbon

Shimadzu TOC-L

Shimandzu Benelux, Den Bosch, The

Netherlands

DOC/ DIC X

TOC/ TIC

Chlorophyll a X HPLC ultimate 3000

Nitrogen



NH3 X Quaatro method 541502714000

Quaatro Applications, Beun de Ronde,

Abcoude, The Netherlands

NO2 X Quaatro method 5415028714100



NO3 X Quaatro method 5415028714100



TN X Flash CN analyser Interscience, Breda, The Netherlands.

Phosphorus

TP/ TDP X Quaatro method Q-031-04 Rev. 1



Silica X Quaatro method Q-038-04 Rev 1



1.8.9 Umweltbundesamt (UBA)

Parameter


Reference

Comments

Manual Automated

Alkalinity X Acidic titration by robotic titrosampler

Endpoints: DIN EN ISO 9963-1, optional:

Gran-Plot-titration acc. Sigg & Stumm

1989

Coupled with major

anion and cation

analyses (TitrIC-System)

(incl. ion mass balance)



Carbon

DOC/ DIC

TOC/ TIC X

Combustion and IR-detection by through-flow or

automatic sampler DIN EN 1484

Chlorophyll,

total (chl-a +

pheophytin) X

Photometric detection after cell disruption and

subsequent hot ethanol extraction

Endpoints: Total chlorophyll acc. Parsons

& Strickland 1963, chl a + pheophytin acc.

DIN 38412-16

Ultrasonic cell

disruption

Filterable dry

matter X Gravimetric DIN 38409-2

Major

anionic

components:

F, Cl, Br, SO4,

PO4, NO2,

NO3 X

IC-automated detection by electric conductivity,

incl. inline dialysis, chemical and CO2-surpression DIN EN ISO 10304-1

Coupled with titration

and major anion



Major

cationic

components:

Li, Na, K, Mg,

Ca, NH4 X

IC-automated detection by electric conductivity

incl. inline dialysis DIN EN ISO 14911

Coupled with titration

and major anion



Nitrogen

NH3 X

CFA-based photometric detection, indophenol blue

method (Berthelot’s reagent)

Chaney & Marbach 1962, Bucur et al.

2006, DIN EN ISO 11732, Skalar Kat Nr.

155-002w/r



NO2 X

CFA-based photometric detection, diazotization of

NO2 (Gries-Ilosvay reaction) with sulphanilamide

Bendschneider & Robinson 1952, acc. to

DIN EN ISO 13395, device specific: Skalar:

Katnr. 461-031

NO3 X


nitrite by use of coppered Cd-granules and

detection as nitrite (see above)

Wood et al. 1967, Nydahl 1976

TN/TDN

X

Pressure digestion by use of persulfate oxidation to

nitrate and subsequent detection as nitrite (see

above)

Koroleff 1983b

Joint digestion of

nitrogen + phosphor

feasible

Phosphorus

SRP X


molybdenum blue complex by use of ascorbic acid

and antimonyl tartrate

Murphy & Riley 1962, Walinga et al. 1995,

acc. to DIN EN ISO 15681-2: Skalar: Kat Nr.

503-010w/r, a + b

Optional: Low-level-

phosphate module used

below 2 µg/L PO4-P

TP/ TDP X

Pressure digestion by use of persulfate oxidation

and subsequent photometric detection as

phosphate (SRP) (see above)

Koroleff 1983a

Joint digestion of

nitrogen + phosphor

feasible

Silica X


molybdenum blue complex by use of ascorbic acid

Mullin & Riley 1955, DIN EN ISO 16264,

Skalar: Katnr. 563-052

CFA-based photometric

detection, reduction to

molybdenum blue

complex by use of

ascorbic acid



References

Bendschneider, K., Robinson, R.J. (1952): A new spectrophotometric method for the determination of nitrite in sea water. J. Mar. Res. 11, 97-96.

Bucur, B., Catala Icardo, M., Martinez Calatyud, J. (2006): Spectrometric determination of ammonia by an rFIA assembly. Revue Roumaine de Chimie 51, 101-108.

Chaney, A.L., Marbach, E.P. (1962): Modified reagents for determination of urea and ammonia. Clin. Chem. 8, 130-132.

DIN 38409-2: Summarische Wirkungs- und Stoffkenngrößen (Gruppe H), Bestimmung der abfiltrierbaren Stoffe und des Glührückstandes (H 2).

German standard methods for the examination of water, waste water and sludge; parameters characterizing effects and substances (group H); determination of

filterable matter and the residue on ignition (H 2).

DIN 38412-16: Testverfahren mit Wasserorganismen (Gruppe L), Bestimmung des Chlorophyll-a- Gehaltes von Oberflächenwasser (L16)

German standard methods for the examination of water, waste water and sludge; test methods using water organisms (group L); determination of chlorophyll a

in surface water (L 16)

DIN EN 1484: Wasseranalytik - Anleitungen zur Bestimmung des gesamten organischen Kohlenstoffs (TOC) und des gelösten organischen Kohlenstoffs (DOC);

Deutsche Fassung EN 1484-1997

Water analysis - Guidelines for the determination of total organic carbon (TOC) and dissolved organic carbon (DOC)

DIN EN ISO 11732: Wasserbeschaffenheit - Bestimmung von Ammoniumstickstoff - Verfahren mittels Fließanalytik (CFA und FIA) und spektrometrischer Detektion

(ISO 11732:2005); Deutsche Fassung EN ISO 11732: 2005.

Water quality - Determination of ammonium nitrogen - Method by flow analysis (CFA and FIA) and spectrometric detection (ISO 11732:2005)

DIN EN ISO 13395: Wasserbeschaffenheit. Bestimmung von Nitritstickstoff, Nitratstickstoff und der Summe von beiden mit der Fließanalytik (CFA und FIA) und

spektrometrischer Detektion (ISO 13395: 1996). Deutsche Fassung EN ISO 13395: 1996.

Water quality - Determination of nitrite nitrogen and nitrate nitrogen and the sum of both by flow analysis (CFA and FIA) and spectrometric detection (ISO 13395:

1996)



DIN EN ISO 15681-2: Wasserbeschaffenheit. Bestimmung von Orthophosphat und Gesamtphosphor mittels Fließanalytik (FIA und CFA). Teil 2: Verfahren mittels

kontinuierlicher Durchflussanalyse (CFA) (ISO 15681-2: 2003). Deutsche Fassung EN ISO 15681-2: 2004.

Water quality - Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA) - Part 2: Method by continuous flow analysis

(CFA) (ISO 15681-2: 2003)

DIN EN ISO 16264: Wasserbeschaffenheit. Bestimmung löslicher Silicate mittels Fließanalytik (FIA und CFA) und photometrischer Detektion (ISO 16264:2002).

Deutsche Fassung EN ISO 16264: 2004.

Water quality - Determination of soluble silicates by flow analysis (FIA and CFA) and photometric detection (ISO 16264: 2002)

DIN EN ISO 9963-1: Wasserbeschaffenheit-Bestimmung der Alkalinität, Teil 1: Bestimmung der gesamten und der zusammengesetzten Alkalinität (ISO 9963-1):

1994, Deutsche Fassung EN ISO 9963-1: 1995

Water quality - Determination of alkalinity - Part 1: Determination of total and composite alkalinity (ISO 9963-1: 1994)

DIN EN ISO 10304-1: Wasserbeschaffenheit- Bestimmung von gelösten Anionen mittels Flüssigkeits- Ionenchromatographie, Teil 1: Bestimmung von Bromid,

Chlorid, Fluorid, Nitrat, Nitrit, Phosphat und Sulfat (ISO 10304-1:2007), Deutsche Fassung EN ISO 10304-1:2009

Water quality - Determination of dissolved anions by liquid chromatography of ions - Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite,

phosphate and sulfate (ISO 10304-1:2007)

DIN EN ISO 14911: Wasserbeschaffenheit- Bestimmung der gelösten Kationen Li+, Na+, NH4+ , K+, Mn2+, Ca2+, Mg2+, Sr2+ und Ba2+ mittels

Ionenchromatographie, Verfahren für Wasser und Abwasser (ISO 14911:1998), Deutsche Fassung EN ISO 14911: 1999

Water quality - Determination of dissolved Li⁺, Na⁺, NH₄⁺, K⁺, Mn²⁺, Ca²⁺, Mg²⁺, Sr²⁺ and Ba²⁺ using ion chromatography - Method for water and waste water (ISO

14911: 1998)

Koroleff, F. (1983a): Determination of phosphorus by acid persulphate oxidation. - In Grasshoff, K. (ed.): Methods of sea water analysis (2nd ed.), p. 134-136.

Weinheim: Verlag Chemie.

Koroleff, F. (1983b): Determination of total and organic nitrogen after persulphate oxidation. - In Grasshoff, K. (ed.): Methods of sea water analysis (2nd ed.), p.

164-168. Weinheim: Verlag Chemie.



Mullin, J.B., Riley J.P. (1955): The colorimetric determination of silicate with special reference to sea and natural waters. - Anal. Chim. Acta 12, 162-176.

Murphy, J., Riley J.P. (1962): A modified method for the determination of phosphate in natural waters. - Anal. Chim. Acta 27, 31-36.

Nydahl, F. (1976): On the optimum conditions for the reduction of nitrate to nitrite by cadmium. Talanta 23: 349-357.

Parsons T.R. & Strickland J.D.H. (1963): Discussion of spectrophotometric determination of marine-plant pigments, with revised equations for ascertaining

chlorophylls and carotenoids. J. Mar. Res. 21: 155-63.

Skalar Kat Nr. 155-002w/r, Analyse: Ammonium, Bereich: 2 - 100 ppb P, Matrix: Abwasser. - Issue 102197/MH/97202624 97-0411.

Skalar Kat Nr. 461-031, Analyse: Nitrat + Nitrit, Meßbereich: 2 - 100 ppb P, Matrix: Seewasser. - Issue 0690899/MH/99207147. 990728 Institut

für Meereskunde

Skalar Kat Nr. 503-010w/r, a: Analyse: Phosphat, Meßbereich: 2 - 100 ppb P, Matrix: Seewasser. - Issue 060899/MH/99207147.

Skalar Kat Nr. 503-010w/r, b: Analysis: Phosphate, Range: 5 - 100 ppb P, Matrix: Surface- & drinking water. - Issue 0690803/MH/99226559.

Skalar Kat Nr. 563-052: Analyse: Silikat, Meßbereich: 0.02 - 1 ppm Si, Matrix: Wasser. - Issue 111397/MH/97202944 97-0541.

Sigg, L. & Stumm, W. (1989): Aquatische Chemie. - 396 S., 128 Abb., 37 Tab. Zürich: Verlag der Fachvereine 1989.

Walinga, I., Van Der Lee, J.J., Houba, V.J.G., Van Vark. W & Novozamsky, I. (1995): 1.7.2 Determination of phosphorus by colorimetry (automated, by flow

analyzer). - In: Walinga, I., Van Der Lee, J.J., Houba, V.J.G., Van Vark. W & Novozamsky, I. (eds.) (1995): Plant analysis manual: PANA-A1/34 - 39. Dordrecht:

Kluwer.

Wood, E.D., Armstrong, F.A.J. & Richards, F.A. (1967): Determination of nitrate in sea water by cadmium-copper reduction to nitrite. J. mar. biol. Ass. U.K. 47, 23-

31.



1.8.10 University of Helsinki, Tvärminne Zoological Station (UH)

Parameter


Reference

Comments

Manual Automated

Carbon

DOC X

High-temperature catalytic oxidation and

infrared detection

Grasshoff et al. (1999) (chapter

15)

POC X


mass spectrometric detection


17)

Chlorophyll a X

Fluorometric detection after ethanol

extraction

Baltic marine environment

protection commission (1988)

Nitrogen

NH3 X Indophenol Blue Method

Modification of Grasshoff et al.

(1999) (chapter 10.2.10);

Grasshoff (1976) (chapter 9.2)

Dichloroisocyanuric acid

as hypochlorite donor

NO2 X Automated Colorimetric Method


(1999) (chapter 10.2.8);


NO3 X

Automated Colorimetric Method, Vanadine

Chloride Reduction Method


(1999) (chapter 10.2.9);




PON X


chemiluminescence detection


17)

TDN

X


chemiluminescence detection


15)

TN X

Persulfate Digestion, Vanadine Chloride

Reduction Method


(1999) (chapter 10.2.16);

Grasshoff (1976) (chapter 9.8.3)

Phosphorus

SRP X Automated Ascorbic Acid Method


(1999) (chapter 10.2.5);


PP

X

Dry Ashing, Ascorbic Acid Method

Solorzano 1980a; Modification

of Grasshoff et al. (1999)

(chapter 10.2.12); Grasshoff

(1976) (chapter 9.1.2)

TP X

Persulfate Digestion, Automated Ascorbic

Acid Method


(1999) (chapter 10.2.13);


Silica X Automated Molybdosilicate Method


(1999) (chapter 10.2.11);




References

Guidelines for the Baltic monitoring programme for the third stage (1988). Part D. Biological determinands. Baltic Sea Environment Proceedings No. 27 D. Baltic

Marine Environment Protection Commission – Helsinki Commission.

Grasshoff, K. (Ed.) (1976). Methods of seawater analysis. Verlag Chemie.

Grasshoff, K., Kremling, K., & Ehrhardt, M. (Eds.). (1999). Methods of seawater analysis. John Wiley & Sons.

SOLORZANO, L., SHARP, J. H. (1980a). Determination of total dissolved phosphorus and particulate phosphorus in natural waters. Limnol. Oceanogr., 25(4), 754-

758.

1.8.11 University of Bergen (UIB)

Parameter


Reference

Comments

Manual Automated

Carbon

POC X Flash elemental analyses Pella & Colombo 1973

TOC1 X

High temperature catalytic

oxidation Børsheim 2000

Chlorophyll a X

Fluorometric Detection after

Acetone Extraction Parsons et al. (1984)

X

Fluorometric Detection after

Methanol Extraction Holm-Hansen and Riemann (1978)



Nitrogen

NH4+ X

Ortho-phthaldialdehyde

fluorometric Method (OPA)

Holmes et al. 1999

Adapted for microwell plate according

to Poulin & Pelletier 2007

NO3 X2

Cadmium reducing column

(nitrate to nitrite)

Parsons et al. (1992) adapted to an

autoanalyzer (San1 Segmented Flow

Analyser, Skalar Analytical B.V., The

Netherlands) as described in Rey et al.

(2000).

PON X Flash elemental analyses Pella & Colombo 1973

Phosphorus

SRP X

Ascorbic Acid - molybdenum

- tartrate blue complex Koroleff 1983

Salinity X

Direct measurement with

SAIV SD204 CTD -

Silicate

Ascorbic Acid - Molybdenum

– Oxalic - Blue Complex Valderrama 1995

1 No routine analysis

2 Performed by Institute of Marine Research (IMR) in Bergen



References

Børsheim, K. Y. 2000. Bacterial production rates and concentrations of organic carbon at the end of the growing season in the Greenland Sea. Aquat. Microb.

Ecol. 21: 115– 123. doi:10.3354/ame021115

Holm-Hansen O, Riemann B (1978). Chlorophyll a determination: improvements in methodology. Oikos 30: 438-447.

Holmes RM, Aminot A, Keroul R, Hooker AH, Peterson BJ (1999). A simple and precise method for measuring ammonium in marine and freshwater ecosystems.

Aquat Sci 56: 1801-1808.

Koroleff F (1983). Determination of nutrients. In: Grasshoff K, Ehrhardt M, Kremling K (eds). Methods in seawater analyses. Verlag Chemie: Weinheim/Deerfield

Beach, Florida. pp 125-131.

Parsons, T. R., Y. Maita, and C. M. Lalli. 1984. A manual of chemical and biological methods for seawater analysis, p.

Pergamon Press.

Pella E, Colombo B (1973). Study of carbon, hydrogen and nitrogen determination by combustion-gas chromatography. Microchimica Acta 61: 697-719.

Rey, F., T. T. Noji, and L. A. Miller. 2000. Seasonal phytoplankton development and new production in the central Greenland Sea. Sarsia 85: 329–344. doi:10.1080/

00364827.2000.10414584

Valderrama JC (1995). Methods of nutrient analysis. In: Hallograeff GM, Anderson DM, Cembella AD (eds). Manual of harmful marine microalgae. IOC manuals

and guides. UNESCO: Paris. pp 262-265.



1.8.12 Umea Marine Science Center (UMF)

Parameter


Reference

Comments

Manual Automated

Alkalinity X Potentiometric Titration

SS-EN ISO 9963-

1:1994 modified

HC-B-B151

Carbon

DOC X

High temperature combustion with NDIR

detection

HC-C-C21 / SS-EN

1484 ed. 1

modified

Chlorophyll a X Spectrofluorometry, ex 433nm/em 673nm ICES / HC-C-C21 Ethanol extraction

C and N X

Elemental analysis: High temperature

combustion with IR-detection

LECO

Corporation5

Nitrogen

NH4 X CFA (QuAAtro, Autoanalyzer ) ”Grasshoff”2 Photometric Phenol method



NO2 X CFA (QuAAtro, Autoanalyzer ) ”Grasshoff”2

Photometric

sulfanilamide/Ethylenediamine

NO3 X CFA (QuAAtro, Autoanalyzer ) ”Grasshoff”2

Photometric CD-reductor,


TN X

Simultaneous N and P Oxidative digestion

with peroxodisulfate using the borate buffer

system followed by CFA (QuAAtro,

Autoanalyzer ). ”Grasshoff”2



TDN X







Oxygen X Winkler Titration SS-EN 25813:1992

pH

HC-B-B141 / SS-EN

ISO 10523:2012 pH 7 – 10

Phosphorus

PP X Photometric Dry combustion

Solarzano3 S-EN

ISO 6878:20054

Photometric Molybdate-

ascorbic acid



TP X






ascorbic acid

TDP X






ascorbic acid

Silica X CFA (QuAAtro, Autoanalyzer) ”Grasshoff”2

Photometric Molybdate-Oxalic

acid

References

1HELCOM Combined Manual for Marine Monitoring (2015) Letters B or C refers to actual part and annex

2K. Grasshoff et al, Methods of Seawater Analysis, 2nd edition, Verlag Chemie, 1983, page 125-187; 347-376

3L.Solarzano, J. H. Sharp, Limnol. Oceanogr.., 25(4) 1980 754-758,

4SS-EN ISO 6878:2005, Water quality—Determination of phosphorus - Ammonium molybdate spectrometric method

5LECO Corporation, Thru Spec CHN/CHNS Micro Carbon/Hydrogen/Nitrogen/Sulfur Determinators. Instruction Manual Version 2.7X. Part Number 200-716, July

2015



1.8.13 WasserCluster Lunz (WCL)

Parameter


Reference

Comments

Manual Automated

Alkalinity X Titration Schwoerbel (chapter 1.2.5)

Carbon

DOC/ DIC X Oxidation and Conductometric Detection U.S. Patent No. 5,132,094

TOC/ TIC X Oxidation and Conductometric Detection U.S. Patent No. 5,132,094

Chlorophyll a X Fluorometric Detection after Acetone Extraction Arar 1997 (EPA Method 445.0)

No cell disruption and

acidification is applied

Nitrogen

NH3 X Indophenol Blue Method Ivancic & Deggobis 1984

X Indophenol Blue Method ISO 7150


X Colorimetric Method ISO 13395:1996


X Sodiumsalicylate Method Schwoerbel (chapter 1.2.14)

TN

X Persulfate Digestion, Hydrazine Reduction Method

Clesceri 1999 (4500-P, chapter J);

ISO 13395:1996

Phosphorus

SRP X Ascorbic Acid Method Grasshoff 1999 (chapter 10.2.5)

X Automated Ascorbic Acid Method ISO 15681-2



PP

X

Dry Ashing and Ascorbic Acid Method

Solorzano 1980a; Grasshoff 1999 (chapter

10.2.5)

Digestion modified from

Solorzano

TP/ TDP X Persulfate Digestion and Ascorbic Acid Method Grasshoff 1999 (chapter 10.2.13)

Silica X Molybdosilicate Method or Heteropoly Blue Method Clesceri 1999 (4500-SiO2, chapter C or D)

References

Arar, E. J., & Collins, G. B. (1997). Method 445.0: In vitro determination of chlorophyll a and pheophytin a in marine and freshwater algae by fluorescence.

Cincinnati: United States Environmental Protection Agency, Office of Research and Development, National Exposure Research Laboratory.

Clesceri, L. S., Greenberg, A. E., & Eaton, A.D. (1996). Standard methods for the examination of water and wastewater. APHA, AWWA and WPCF, Washington DC.

DIN EN ISO 15681-2, Water quality - Determination of orthophosphate and total phosphorus contents by flow analysis (FIA and CFA) - Part 2: Method by

continuous flow analysis (CFA), 06-2001

Grasshoff, K., Kremling, K., & Ehrhardt, M. (Eds.). (1999). Methods of seawater analysis. John Wiley & Sons

ISO 7150-1: 1984, Water quality—Determination of ammonium, manual spectrometric method

ISO 13395:1996, Water quality—Determination of nitrite nitrogen and nitrate nitrogen and the sum of both by flow analysis (CFA and FIA) and spectrometric

detection.

Ivančič, I., & Degobbis, D. (1984). An optimal manual procedure for ammonia analysis in natural waters by the indophenol blue method. Water Research, 18(9),

1143-1147.

R. Godec, et. al., “Method and apparatus for the determination of dissolved carbon in water” U.S. Patent No. 5,132,094)

Solorzano, L., & Sharp, J. H. (1980). Determination of total dissolved phosphorus and particulate phosphorus in natural waters. Limnology and Oceanography,

25(4), 754-7



1.9 References 1 – Water Chemistry

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“Guidance on the Monitoring of the Biological Quality

Elements Part B2 - Phytoplankton,” Vienna, 2015.

[2] WURL, Oliver (Hg.). Practical guidelines for the analysis of

seawater. CRC press, 2009.

[3] NOLLET, Leo ML; DE GELDER, Leen SP (Hg.). Handbook of

water analysis. CRC press, 2000.

[4] WHO, Handbook: Good Laboratory Practice (GLP): Quality

practices for regulated non-clinical research and

development, 2nd ed. Switzerland: TDR/WHO, 2009.

[5] OECD, OECD series on principles of good laboratory

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[6] Council Directive, “89/391/EEC of 12 June 1989 on the

introduction of measures to encourage improvements in the

safety and health of workers at work,” Off. J. Eur.

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[7] OSHA, “European directives on safety and health at work

- Safety and health at work.” [Online]. Available:

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[9] European Commission, “COMMISSION DECISION of 3 May

2000 replacing Decision 94/3/EC establishing a list of wastes

pursuant to Article 1(a) of Council Directive 75/442/EEC on

waste and Council Decision 94/904/EC establishing a list of

hazardous waste pursuant to Article 1(4) of Council Directive

91/689/EEC on hazardous waste (notified under document

number C(2000) 1147) (Text with EEA relevance)

(2000/532/EC),” Off. J. Eur. Communities, vol. 69, 2000.

[10] U. Mischke et al., “EU FP7 226273, WISER deliverable

D3.1-4: guidance document on sampling, analysis and

counting standards for phytoplankton in lakes,” pp. 1–51,

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[11] UNESCO/IOC, MICROSCOPIC AND MOLECULAR

METHODS FOR QUANTITATIVE PHYTOPLANKTON ANALYSIS.

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[12] Aarhus Universitet – National Environmental Research

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experiments and monitoring along a climate gradient in task

2,” 2014.

[13] GRASSHOFF, Klaus; KREMLING, Klaus; EHRHARDT,

Manfred (Hg.). Methods of seawater analysis. John Wiley &

Sons, 2009.

standard operating protocol (sop) on water chemistry

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