Health, Safety and Health, Safety and Environment (HSE) Environment (HSE)

regimeregime

Safe Job Analysis (SJA)Safe Job Analysis (SJA)

Safe job analysis must be made Safe job analysis must be made for all analytical operations for all analytical operations representing any dangerrepresenting any danger What can go What can go wrongwrong?? What can we do to What can we do to avoidavoid this? this? What can we do to What can we do to minimizeminimize the damage? the damage?

SJA must also be made for the Master SJA must also be made for the Master project as well as KJM2010 etc. project as well as KJM2010 etc.

Resources available on webResources available on web For Environmental analysis students: For Environmental analysis students:

See our internal group pages:See our internal group pages: https://www.mn.uio.no/kjemi/english/research/groups/

environmental-analysis/internal/ If SJA exists then this needs to be read If SJA exists then this needs to be read

and documented in the Lab protocol notebook and documented in the Lab protocol notebook and signed by staff (Grethe, Rolf, Cathrine, or and signed by staff (Grethe, Rolf, Cathrine, or Christian)Christian) The Lab protocol notebook is the property of UiO The Lab protocol notebook is the property of UiO

and must be handed in at end of stayand must be handed in at end of stay If SJA does not exist then one needs to make it If SJA does not exist then one needs to make it

and send it to me or Grethe. We will quality control and send it to me or Grethe. We will quality control and post it on the internal web and post it on the internal web

Safety rutinesSafety rutines

In the lab you must use gogglesIn the lab you must use goggles The doors to chemicals must be lockedThe doors to chemicals must be locked

Door to lab must be lockedDoor to lab must be locked Cabinets must be locked and key hiddenCabinets must be locked and key hidden

Analyses planAnalyses planModule 19Module 19

Conductivity and temperatureConductivity and temperature{H{H++} determined using pH electrode} determined using pH electrodeAlkalinity titration Alkalinity titration

UV/VIS MAS as a proxy for UV/VIS MAS as a proxy for DNOM and algae DNOM and algae

Phosphate- and possibly Aluminium Phosphate- and possibly Aluminium fractionationfractionation

Preparation of samples for anions and Preparation of samples for anions and cation analysis, heavy metals + DOCcation analysis, heavy metals + DOC

ConductivityConductivity

Conductivity meter Conductivity meter The instrument is calibrated using The instrument is calibrated using

1433 µS calibration solutions1433 µS calibration solutions The measurements are done for quality control The measurements are done for quality control

purposes in order to compare measured and purposes in order to compare measured and calculated conductivitycalculated conductivity

Determined as described in ISO7888 using Determined as described in ISO7888 using non-filtered water sample and preferably non-filtered water sample and preferably measured at 25measured at 25C. C.

The reading is presented as mS mThe reading is presented as mS m-1-1 (1mS m(1mS m-1-1 = 10µS/cm)= 10µS/cm)

{H{H++} determined } determined using pH electrodeusing pH electrode

Total Alkalinity titrationTotal Alkalinity titration Determined potentiometrically as described in ISO9963Determined potentiometrically as described in ISO9963 Titration with acid to pH 4,5Titration with acid to pH 4,5

and preferably measured at 25and preferably measured at 25CCCOCO33²²--+ HCO+ HCO33

-- + 3H + 3H33OO++ 2H 2H22COCO33+ 3H+ 3H22OO

Total alkalinity (=[HCOTotal alkalinity (=[HCO33--]+2[CO]+2[CO33²²--]) + H]) + H++ needed to change the pH needed to change the pH

from sample pH down to pH 4.5from sample pH down to pH 4.5Endpoint in the acid rangeEndpoint in the acid range

Also other weak acids (AAlso other weak acids (A--, Al(OH), Al(OH)nn3-n3-n))

H2CO3HCO3

CO3

2−

0

0,1

0,2

0,3

0,4

0,5

0,6

0,7

0,8

0,9

1

3 4 5 6 7 8 9 10 11 12

pH

UV/VIS MASUV/VIS MAS Measurement of absorbency @ Measurement of absorbency @ 254 and 400 nm254 and 400 nm Absorbency at UV 254 nm is commonly used as a proxy Absorbency at UV 254 nm is commonly used as a proxy

for Dissolved Natural Organic Matter (DNOM)for Dissolved Natural Organic Matter (DNOM) Strongly correlated with TOC due to Strongly correlated with TOC due to

conjugated double bonds chromophores conjugated double bonds chromophores Algae adsorb light at UV 254 nm, Algae adsorb light at UV 254 nm,

but more than DNOM at VIS 400 nm but more than DNOM at VIS 400 nm

Nutrient fractionationNutrient fractionationPDI = Orthophosphate PDO = Dissolved organic PPR = Reactive pool of PPIP = Inorganic particulate PPChl = Alga P

Major anions to be determined Major anions to be determined by Ion Chromatograph (IC)by Ion Chromatograph (IC)

PrinciplePrinciple• The sample is injected The sample is injected

in a flow of eluentin a flow of eluent• The analyte ions are The analyte ions are

separated by different separated by different degree of binding to the degree of binding to the active sites on the ion active sites on the ion exchange materialexchange material

• Cations are exchanged Cations are exchanged with Hwith H++

• The activity x specific The activity x specific conductivity of the conductivity of the analyte along with analyte along with HH++ in the eluent stream in the eluent stream are measured by are measured by means of a means of a conductometerconductometer

Major cations to be determined by Major cations to be determined by ICP-AES/OES or MSICP-AES/OES or MS

Ohmic heating Ohmic heating The heat arises from interaction between the ions and The heat arises from interaction between the ions and

electrons and a fluctuating magnetic field which electrons and a fluctuating magnetic field which causes the charged particles to move in circular orbits causes the charged particles to move in circular orbits

Atomization: PlasmaAtomization: Plasma Detection technique: Detection technique:

Atomic/Optic emission spectroscophy; AES

Problems with analysis of Problems with analysis of major anions and cations in water major anions and cations in water

Anions are analyzed in raw waterAnions are analyzed in raw water Cations are analyzed in water digested Cations are analyzed in water digested

in acid (HNOin acid (HNO33))

Colloidal material is Colloidal material is detected in the detected in the cation analysis cation analysis but not in the but not in the anion analysisanion analysis

Total organic carbonTotal organic carbon Analytical chemistry lab Ø 104Analytical chemistry lab Ø 104 High temperature (680High temperature (680ººC) catalytic C) catalytic

combustion analysis on a combustion analysis on a Shimadzu TOC-5000A instrumentShimadzu TOC-5000A instrument

Principle:Principle: The organic carbon is combusted The organic carbon is combusted

to COto CO22 by high temperature and by high temperature and catalysis. catalysis. The amount of COThe amount of CO22 produced produced is measured using is measured using an IR detectoran IR detector

Analytes measured may include: Analytes measured may include: TC, IC, TOC, NPOC, and POC TC, IC, TOC, NPOC, and POC

P determinationP determination Orthophosphate reacts with ammoniummolybdate to a Orthophosphate reacts with ammoniummolybdate to a

yellow-colouredyellow-coloured phosphorousmolybdate acid, that is phosphorousmolybdate acid, that is reduced with ascorbic acid in the presence of antimony reduced with ascorbic acid in the presence of antimony to a strongly to a strongly blue colouredblue coloured complex complex

This colour is measured photometrically as described in This colour is measured photometrically as described in Norwegian Standard (NS 4724)Norwegian Standard (NS 4724)

At higher concentrations (soil extracts) P conc. is At higher concentrations (soil extracts) P conc. is determined by ICP-OESdetermined by ICP-OES Detects higher cons. then the colorimetric method due to Detects higher cons. then the colorimetric method due to

inclusion of non-labile species (org.-P etc)inclusion of non-labile species (org.-P etc)

QC of dataQC of data After the analysis After the analysis

the data must be the data must be compiled and quality compiled and quality controlled by controlled by

ion balance and ion balance and agreement between agreement between

measured and calculated measured and calculated conductivityconductivity

For this purpose you may For this purpose you may use the Data compilation use the Data compilation and QC worksheet and QC worksheet available at available at http://folk.uio.no/rvogt/KJhttp://folk.uio.no/rvogt/KJM_MEF_4010/M_MEF_4010/