This study is a summary of the complex odor proficiency testing method using the air dilution sensory method conducted for the last 7 years. Results of the homogeneity and stability test were obtained from the measurement of the standard sample for identifying the range of measurable concentration so that the complex odor proficiency testing method was established through processing the manufactured standard sample and distribution method. Standard samples were prepared using a large Teflon bag after being homogeneously mixed inside a Teflon bag. Also, a distributing container was selected with a polyester aluminum bag in order to avoid samples of the best condition from being contaminated during transport as well as being exposed to invasive odor from a sampling bag. Test results revealed that the mixture of toluene and m-Xylene was most appropriate for this proficiency testing method to the homogeneity and stability of the testing method. In addition, DMS and DMDS were the optimized samples at the outlet area. As a result, the standard method was established to address the analysis quality management to the mixed odor inspection agencies in Korea.

In this study, the homogeneity and stability of standard samples for proficiency testing in indoor air quality within the country (formaldehyde, benzene, toluene, ethylbenzene, p-xylene, styrene, TVOC) were evaluated. The procedures and statistical analysis methods applied in ISO/IEC 13528 (2009) and KS A ISO Guide 35 (2005) were applied as evaluation methods. The homogeneity evaluation was a statistical analysis of repeated measurements of each of the 11 ports and between the 11 ports concentration data. As a result, the coefficient of variation (CV) was within the range of 1.9%~5.9%. The difference between the ports was found to be insignificant and met the statistical standard specified in KS Q ISO 13528. The stability evaluation was assessed by the change in concentration over the long-term stability of the standard samples stored for 90 days. The coefficient of variation (CV), which was within the range of 2.6%~9.0%, exhibited changes in the concentration of the long-term stored standard samples. However, the results satisfy the statistical standard specified in KS A ISO Guide 35. Overall, there is no significant difference between the homogeneity of the standard samples by the port and the stability of the long-term stored samples. Therefore, it is considered to be an appropriate method to supply standard samples in an indoor air quality proficiency test.

The aim of this study is to analyze error cases induced during the proficiency test of certified odor measurement agencies. In the case of the homogeneity test performed in three panel groups, the geometric mean dilution factor of the site boundary PTMs(proficiency testing materials) was 1.4 ± 0.2, 1.7 ± 0.2, 1.8 ± 0.1 and that of the outlet PTMs was 3.7 ± 0.2, 3.7 ± 0.3, 3.7 ± 0.3, respectively. In the case of the stability test for 72 h, the geometric mean dilution factor of the site boundary PTMs was 1.6 ± 0.1 and that of the outlet PTMs was 3.6 ± 0.1. Among error cases induced during the proficiency test of certified odor measurement agencies, the proportion of error cases was in the order of case II(discontinuance of estimation)(40.0%) > case I(error on estimation procedure by panelist)(33.3%) > case III(miswriting of estimation result)(13.3%) > case IV(miswriting of dilution factor) and V(writing of wrong estimation result)(6.7%). Therefore, it seems likely that additional education related to error cases II and I is required.

2011년에 전국 79개 악취검사기관을 대상으로 공기희석관능법에 대한 숙련도 시험을 실시하였다. 악취방지법의 부지 경계선과 악취 배출원의 배출허용기준을 모사한 2개의 합성복합악취를 숙련도 시험물질(proficiency testing materials, PTM)로 사용 하였다. 부지 경계선 시료는 7ppm의 톨루엔과 7ppm m-자일렌의 복합악취로 구성하였으며, 배출구 시 료는 10ppm DMS (dimethyl sulfide)와 10ppm DMDS (dimethyl disulfide)의 복합악취로 구성하였다. 숙련도 시험 결과는 기준값으로 평균과 중간값을 사용하고, 목표표준편차로 일반 표준편차, 로버스트 표준편차 및 변동계수를 사용하여 Z-점수를 평가하였다. 시험결 과의 변동계수는 PTMs의 냄새강도가 증가함에 따라 감소하였다. 복합악취에 대한 숙련 도 시험 결과는 악취희석배율보다 로그 스케일의 악취지수를 사용하여 평가하는 것이 적 절했다. 두 PTMs에 대한 참여기관의 Z-점수를 변동계수, 표준편차, 그리고 로버스트 표 준편차를 사용하여 평가할 때, 참여기관의 95%가 숙련도 기준을 만족하였다. 목표 표준 편차를 변동계수의 20%로 설정하였을 때 참여기관의 만족도 비율은 부지경계와 출구 PTM 시료에 대해 각각 90%와 95%로 양호하였다. 이러한 결과들로부터 부지경계와 출 구의 복합악취를 모사한 두 합성 PTMs 모두 복합악취의 숙련도 시험물질로 적합하였다.

본 연구에서는 악취숙련도 시험을 위한 PTM 물질로 현장시료의 적용가능성을 평가하기 위하여 하수처리장에 채취한 현장시료의 안정성과 채취 균질성을 조사하였다. 또한 현장시료를 PTM으로 사용하여 71개 악취검사기관의 공기희석관능법의 숙련도 시험을 실시하였다. 다양한 설정값(참여기관 또는 기준기관의 악취지수 평균값이나 중위수)를 기준으로 3가지 Z-score 평가법(표준편차 이용한 Z-score, Robust 표준편차를 이용한 Z-score, 목표표준편차를 이용한 Z-score)으로 숙련도의 통계적 분석을 하였다. 하수처리장 농축조에서 채취한 현장시료는 2일 동안 희석배수의 변화 없이 안정적이었고, 참여기관을 4 그룹으로 나누어 순차적으로 채취한 현장시료가 균질한 것으로 평가되었다. 이는 현장악취시료가 악취 숙련도 평가를 위한 PTM 물질로 적용 가능함을 의미한다. 숙련도 시험결과의 통계적 분석을 통해 참여기관의 숙련도 만족비율은 Z-score 평가법이나 설정값의 기준(참여기관 또는 참고기관으로 선택한 3개 대학의 악취지수 평균값이나 중위수) 보다는 목표표준편차(S*ref)값에 의존하였다. 숙련도 만족비율은 S*ref 값이 증가함에 따라 증가하였으며, PTM 시료의 분석결과에 대한 변동계수(CV) 0.13에 해당하는 목표표준편차값에서 숙련도 만족비율은 약 93∼96% 수준이었다.

This study was carried out to provide the stable and homogeneous sample for the proficiency test which was applied for the olfactory dilution method of the offensive odor. For this purpose, the relationship between VOCs concentration and air dilution test results were analysed. As the results, the mixture of 7.1 ppm of toluene and m-xylene were suitable as a low level of PTM(proficiency test material) for air dilution olfactory method. In addition, time stability and homogeneity between samples were investigated through the time of 6 hr ~ 48 hr. As the results, the stability of sample concentration with GC analysis was shown as 5.1% RSD for toluene and 6.8 %RSD for xylene, respectively. The stability of sample was 5.4 %RSD in terms of air dilution olfactory method.

Since 2011, proficiency test for the air dilution olfactory method started in Korea for the evaluation of the authorized odor inspection agencies’ analysis skill. For this purpose, sulfur compounds of PTMs (proficiency test materials) were made and investigated for the application to the proficiency test as a complex malodor sample. Time stability and homogeneity between samples were analysed for the PTM which was made with 10 ppm of DMS and 10 ppm of DMDS. As the results, the stability of sample concentration with GC analysis was shown around 6%RSD through the time of 6~48 hr. In addition, dilution number during the same test period appeared almost stable, less than 6%RSD in air dilution olfactory method. The reproducibility results of four laboratories showed very similar results except one lab which was caused by the elder panel characteristics.