Experiences on the TCDDTCDF emission measurement at a hazardous waste incinerator

1
Experiences on the TCDD/TCDF emission measurement
at a hazardous waste incinerator
Conference on POP Inventory Brno, May 2003
2
Introduction

• The Ministry of Environment and Water assigned
  the Department of General and Analytical
  Chemistry of The Technical University of Budapest
  at 2002, to improve the reliability of TCDD/TCDF
  emission measurements in Hungary.
• The department has organised an inter-laboratory
  comparison measurement with the participation of
  four sampling and four analytical laboratories.

3
Sampling laboratories

• Environmental Protection Inspectorate, Gyor
• Environmental Protection Inspectorate, Veszprém
• Department of General and Analytical Chemistry of
  The Technical University of Budapest
• Palota Environmental Protection Ltd, Budapest

4
Analytical laboratories

• Central National Public Health Laboratory,
  Budapest (FJOKK)
• Metropolitan National Public Health Laboratory,
  Budapest (ÁNTSZ)
• Bálint Analitika Ltd., Budapest
• National Agricultural Laboratory, Budapest (OMMI)

5
Sampling

• Problems
• contamination of samples by the sampling
  equipment
• sealing problems (filter-cooler type samplings
  are better than dilution type ones)
• not sufficiently cold temperature (to be below
  dew point)
• not suitable placing of the sampling point

6
Sample preparation

• Problems
• short extraction time, minimum 24h is
  necessary, (during 8 h toluene extraction, 50
  efficiency)
• lack of precise sample clean up.

7
Analysis

• Problems
• long sample storing before analysis
• using one chromatography column only
• Lack of regular calibration of the analytical
  equipment

8
Conclusions

• There were no accredited laboratory for TCDD/TCDF
  emission measurement from 2001to 2002
• The emission measurement of dioxins needs
  coordinated, cautious and professional work
• It is advised to take min. 6m3 sample
• Taking into consideration the sophisticated
  nature of the applied equipment, it seems that
  the sampling may result smaller errors compared
  to the sample clean up and analysis
• .

9
Conclusion cont.

• the extraction standard solution should be given
  to the sample immediately after arriving to the
  laboratory.
• it is advised to accept concentration below 0.05
  ng/Nm3 and not to expect above 0.15 ng/Nm3
  between these too values, another three samples
  to be taken on consecutive two days to form an
  average.

10
Conclusion cont.

• In case of installing new the TCDD/TCDF source,
  the form of sampling point to be discussed with
  the authority
• For proper separation of all 17 congeners, it is
  advised to apply at least two different polarity
  columns
• Concerning the low concentration range of the
  emissions (from 0.0010 to 0.003 I-TEQ ng/Nm3),
  the deviation of the measurements is good.