Temperature Calibration of Thermomechanical Analyzers: Part II—An Interlaboratory Test of the Calibration Procedure

Author(s):  
RJ Seyler ◽  
CM Earnest
2015 ◽  
Vol 8 (2) ◽  
pp. 779-792 ◽  
Author(s):  
P. Panteliadis ◽  
T. Hafkenscheid ◽  
B. Cary ◽  
E. Diapouli ◽  
A. Fischer ◽  
...  

Abstract. A comparison exercise on thermal-optical elemental carbon/organic carbon (ECOC) analysers was carried out among 17 European laboratories. Contrary to previous comparison exercises, the 17 participants made use of an identical instrument set-up, after correcting for temperature offsets with the application of a recently developed temperature calibration kit (Sunset Laboratory Inc, OR, US). Temperature offsets reported by participants ranged from −93 to +100 °C per temperature step. Five filter samples and two sucrose solutions were analysed with both the EUSAAR2 and NIOSH870 thermal protocols. z scores were calculated for total carbon (TC); nine outliers and three stragglers were identified. Three outliers and eight stragglers were found for EC. Overall, the participants provided results between the warning levels with the exception of two laboratories that showed poor performance, the causes of which were identified and corrected through the course of the comparison exercise. The TC repeatability and reproducibility (expressed as relative standard deviations) were 11 and 15% for EUSAAR2 and 9.2 and 12% for NIOSH870; the standard deviations for EC were 15 and 20% for EUSAAR2 and 20 and 26% for NIOSH870. TC was in good agreement between the two protocols, TCNIOSH870 = 0.98 × TCEUSAAR2 (R2 = 1.00, robust means). Transmittance (TOT) calculated EC for NIOSH870 was found to be 20% lower than for EUSAAR2, ECNIOSH870 = 0.80 × ECEUSAAR2 (R2 = 0.96, robust means). The thermograms and laser signal values were compared and similar peak patterns were observed per sample and protocol for most participants. Notable deviations from the typical patterns indicated either the absence or inaccurate application of the temperature calibration procedure and/or pre-oxidation during the inert phase of the analysis. Low or zero pyrolytic organic carbon (POC), as reported by a few participants, is suggested as an indicator of an instrument-specific pre-oxidation. A sample-specific pre-oxidation effect was observed for filter G, for all participants and both thermal protocols, indicating the presence of oxygen donors on the suspended particulate matter. POC (TOT) levels were lower for NIOSH870 than for EUSAAR2, which is related to the heating profile differences of the two thermal protocols.


2009 ◽  
Vol 43 (10) ◽  
pp. 1013-1021 ◽  
Author(s):  
Chin H. Phuah ◽  
Max R. Peterson ◽  
Melville H. Richards ◽  
Jay H. Turner ◽  
Ann M. Dillner

2005 ◽  
Vol 15 (2) ◽  
pp. 112-115 ◽  
Author(s):  
Thomas Schweizer

Abstract The calibration of the temperature control unit of a rotational rheometer with a hood oven is shown. The calibration technique shown for a Paar-Physica rheometer can be adapted to any rheometer with hood oven (indirect heating). The temperature of the bottom fixed plate and the air bearing suspended cone or plate are measured independently. By keeping the amount of venting gas constant, the set temperature of the hood oven is adjusted to reach a minimum gradient across the measuring gap. The calibration procedure is optimized to keep the oven as close as possible to the measuring position.


2014 ◽  
Vol 7 (8) ◽  
pp. 8697-8742
Author(s):  
P. Panteliadis ◽  
T. Hafkenscheid ◽  
B. Cary ◽  
E. Diapouli ◽  
A. Fischer ◽  
...  

Abstract. A comparison exercise on thermal-optical elemental carbon/organic carbon (ECOC) analyzers was carried out among 17 European laboratories. Contrary to previous comparison exercises, the 17 participants made use of an identical instrument set-up, after correcting for temperature offsets with the application of a recently developed temperature calibration kit (Sunset Laboratory Inc, OR, US). Five filter samples and two sucrose solutions were analyzed with both the EUSAAR2 and NIOSH870 thermal protocols. z Scores were calculated for total carbon (TC) and nine outliers and three stragglers were identified. Three outliers and eight stragglers were found for EC. Overall, the participants provided results within the warning levels with the exception of two laboratories that showed poor performance, the causes of which were identified and corrected through the course of the comparison exercise. The TC repeatability and reproducibility relative standard deviations were 11.4 and 14.6% for EUSAAR2 and 9.2 and 11.7% for NIOSH870; the standard deviations for EC were 15.3 and 19.5% for EUSAAR2 and 19.9 and 25.5% for NIOSH870. TC was in good agreement between the two protocols, TCNIOSH870 = 0.98 · TCEUSAAR2 (R2 = 1.00, normalized means). Transmittance (TOT) calculated EC for NIOSH870 was found to be 20% lower than for EUSAAR2, ECNIOSH870 = 0.80 · ECEUSAAR2 (R2 = 0.96, normalized means). The thermograms and laser signal values were compared and similar peak patterns were observed per sample and protocol for most participants. Notable deviations of plotted values indicated absence or inaccurate application of the temperature calibration procedure and/or pre-oxidation during the inert phase of the analysis. Low or no pyrolytic organic carbon (POC), as reported by a few participants, is suggested as an indicator of pre-oxidation. A sample-specific pre-oxidation effect was observed for filter G, for all participants and both thermal protocols, indicating the presence of oxygen donors on the suspended particulate matter. POC (TOT) levels were lower for NIOSH870 than for EUSAAR2, which is related to the heating profile differences of the two thermal protocols.


2014 ◽  
Vol 7 (4) ◽  
pp. 3321-3348 ◽  
Author(s):  
J. Pavlovic ◽  
J. S. Kinsey ◽  
M. D. Hays

Abstract. Thermal-optical analysis (TOA) is a widely used technique that fractionates carbonaceous aerosol particles into organic and elemental carbon (OC and EC), or carbonate. Thermal sub-fractions of evolved OC and EC are also used for source identification and apportionment; thus, oven temperature accuracy during TOA analysis is essential. Evidence now indicates that the "actual" sample (filter) temperature and the temperature measured by the built-in oven thermocouple (or set-point temperature) can differ by as much as 50 °C. This difference can affect the OC-EC split point selection and consequently the OC and EC fraction and sub-fraction concentrations being reported, depending on the sample composition and in-use TOA method and instrument. The present study systematically investigates the influence of an oven temperature calibration procedure for TOA. A dual-optical carbon analyzer that simultaneously measures transmission and reflectance (TOT and TOR) is used, functioning under the conditions of both the NIOSH 5040 and IMPROVE protocols. Application of the oven calibration procedure to our dual optics instrument significantly changed NIOSH 5040 carbon fractions (OC and EC) and the IMPROVE OC fraction. In addition, the well-known OC-EC split difference between NIOSH and IMPROVE methods is even further perturbed following the instrument calibration. Further study is needed to determine if the wide-spread application of this oven temperature calibration procedure will indeed improve accuracy and our ability to compare among carbonaceous aerosol studies that use TOA.


2014 ◽  
Vol 7 (9) ◽  
pp. 2829-2838 ◽  
Author(s):  
J. Pavlovic ◽  
J. S. Kinsey ◽  
M. D. Hays

Abstract. Thermal–optical analysis (TOA) is a widely used technique that fractionates carbonaceous aerosol particles into organic and elemental carbon (OC and EC), or carbonate. Thermal sub-fractions of evolved OC and EC are also used for source identification and apportionment; thus, oven temperature accuracy during TOA analysis is essential. Evidence now indicates that the "actual" sample (filter) temperature and the temperature measured by the built-in oven thermocouple (or set-point temperature) can differ by as much as 50 °C. This difference can affect the OC–EC split point selection and consequently the OC and EC fraction and sub-fraction concentrations being reported, depending on the sample composition and in-use TOA method and instrument. The present study systematically investigates the influence of an oven temperature calibration procedure for TOA. A dual-optical carbon analyzer that simultaneously measures transmission and reflectance (TOT and TOR) is used, functioning under the conditions of both the National Institute of Occupational Safety and Health Method 5040 (NIOSH) and Interagency Monitoring of Protected Visual Environment (IMPROVE) protocols. The application of the oven calibration procedure to our dual-optics instrument significantly changed NIOSH 5040 carbon fractions (OC and EC) and the IMPROVE OC fraction. In addition, the well-known OC–EC split difference between NIOSH and IMPROVE methods is even further perturbed following the instrument calibration. Further study is needed to determine if the widespread application of this oven temperature calibration procedure will indeed improve accuracy and our ability to compare among carbonaceous aerosol studies that use TOA.


2015 ◽  
Vol 601 ◽  
pp. 29-32 ◽  
Author(s):  
Emiel J. Kappert ◽  
Michiel J.T. Raaijmakers ◽  
Wojciech Ogieglo ◽  
Arian Nijmeijer ◽  
Cindy Huiskes ◽  
...  

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