Flowchart for the Laboratory

Sampling

Sample

Subsample

Subsample

Subsample

Subsample

Subsample

Sub- suplying lab

LIMS Analyte A

Analyte B

Analyte C

Analyte D

Analyte Y

Result A

Result B

Result C

Result D

Result Y

Logistic Analyte D Result D

QC

QC

QC

QC

QC

LIM

S

Analytical report

Total Sampleresults

Other sample info and invoice data

Final approval & signiture

Customer

Invoice

Key parameters for the Laboratory

• Sampling

• LIMS

• Analytical methods

• Analytical selection

• Quality Assurrance & Control (QA/QC)

Sampling

• Sampling of waste water, drinking water, pool water, bathing water, slugde and soil

• Sampling plan - Approximary 70-80% of all samples are preordered for longer period.

• Sampling methods are Danish Standards orfrom technical papers.

• Waste water sampling – Momentary, time orflowproportional

LIMS - VAXLIMS

• Laboratory Information Management System – Information on sampling sites– Information on customers (orders)– Information on individual analytic programmes– Gives unique ID number to samples– Samples and subsamples are barcoded– Barcodes gives information to instruments and

instruments returns results to VAXLIMS– Sample information etc. can be accessed from

other ROVESTA departments (Holbæk, Næstved) – VAXLIMS produces final analytical reports and

data for invoices

Analytical Methods

• Almost every methods are Danish (DS) orEuropian/International EN/ISO Standards. A few US (”Standard Methods”) are in use.

• Most methods builds on long and well triedprinciples.

• Analytical principles are mostlyspectrofotometric (colourformation), titration, ionchromatography and physical/chemicalmeasurements like pH, conductivity etc.

Analytical Methods

• Many of the methods are automated e.g. withFlow injektion analysis, robotic oxygenemeasurement and titrators with autosampling.

• Automatisation of analysis is much more easy with ”clean” samples like drinking and fresh-/seawater

Analytical selection

• Waste water:

– pH– Suspended solids– Biochemical and chemical oxygen demand (BOD &

COD)– Nitrite, nitrate, ammonium, kjeldahl-N and total

nitrogen– Ortho phosphate and total phosphorus– Chloride– Sulfate

Analytical selection

• Fresh- and seawater:

– Suspended solids– Biochemical oxygen demand (BOD)– Nitrite, nitrate, ammonium and total nitrogen– Ortho phosphate and total phosphorus– Silicate– Chlorophyll

Analytical selection

• Drinking water:

– pH, conductivity, oxygen– Total solids, color, turbidity– Bicarbonate– Nitrite, nitrate, ammonium– Total phosphorus– Chloride, sulfate, fluoride– Hydrogen sulfide

Analytical selection

• Sludge:

– Total solids– Volatile solids– Total nitrogen– Nitrite+nitrate, ammonium, ortho-P (special)

Eksternal control of Quality System

• Government requirement for all environ-mental analyses to be performomed by accreditated laboratories

• DANAK inspection visit approx. every 15 mdr.

• Changes in akkreditation must be approvedby DANAK

• Obligation to participate in LaboratoryPerformance studies. Results are controlledby DANAK

Quality System – DS/EN ISO 17025

• Part 1: Management requirements – Organization– Quality System– Document control– Review of requests, tenders and contracts– Subcontracting of tests and calibrations– Purchasing services and supplies– Service to clients - complaints– Control of nonconforming tests– Corrective and preventive action– Internal audits– Management reviews

Quality System – DS/EN ISO 17025

• Part 2: Technical requirements– General– Personnel– Accommodation and environmental conditions– Test methods and method validation– Equipment– Measurement tracebility– Sampling– Handling of test items – Assuring the quality of test results– Reporting the results

Internal control (QC) of Quality System

• Blank and controlsamples in 2 concentrationlevels in all analytic runs

• Statistic surveillance of the results from above, to insure complience with eksternaldemands

• Regular extra control using certifided controlsamples (measurement traceability)

• Internal audits

QC of results

• Only results within measurementrange, and where control samples have been OK are approved be thetechnicians. The rest are reanalysed.

• The person autorizing the test reportchecks, if posible, for plausiblility ofresults (e.g. NO2+NO3 / TN, ion-balance)