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MEASUREMENT OF NITROUS OXIDE IN A NITROGEN MATRIX USING GAS

CHROMATOGRAPHY WITH MICROELECTRON CAPTURE DETECTION:
VALIDATION OF ANALYTICAL METHOD

Article  in  The Journal of Engineering and Exact Sciences · March 2017

DOI: 10.18540/jcecvl3iss3pp381-394

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 The Journal of Engineering and Exact Sciences - JCEC
ISSN: 2446-9416

Vol. 03 N. 03 (2017) 381–394 doi: https://doi.org/10.18540/2446941603032017381

OPEN ACCESS

MEASUREMENT OF NITROUS OXIDE IN A NITROGEN

MATRIX USING GAS CHROMATOGRAPHY WITH
MICROELECTRON CAPTURE DETECTION: VALIDATION
OF ANALYTICAL METHOD

O. ZUAS1, M. R. MULYANA1, N. HAMIM2, H. BUDIMAN1

1Gas Analysis Laboratory, Metrology in Chemistry Research Group, Research Centre for
Metrology, Indonesian Institute of Sciences (RCM-LIPI)
2Electrochemistry Laboratory, Metrology in Chemistry Research Group, Research Centre for

Metrology, Indonesian Institute of Sciences (RCM-LIPI)

E-mail: [email protected]

ABSTRACT: Atmospheric nitrous oxide (N2O) as one of the most potent greenhouse gases
significantly contributes to the global warming effect. Therefore, an accurate and valid measurement
method for monitoring its environmental release is of great importance. In this study, an analytical
method for the measurement of N2O in a nitrogen (N2) matrix using gas chromatography and
microelectron capture detection (GC‐μECD) has been validated. The analytical method was
validated in terms of some performance parameters such as system suitability, precision
(repeatability and reproducibility), linearity, limit of detection (LoD) and limit of quantitation (LoQ),
accuracy and method robustness. The results show that the GC system was found to be suitable for
the measurement of N2O in the N2 matrix. The repeatability and reproducibility of the method were
found to have %RSD of 1.42 and 0.71, respectively, indicating that the method is repeatable and
reproducible for N2O measurement. The linearity of the method was excellent, having the R2 value of
0.9998. The LoD and LoQ of the method were found to be 0.10 and 0.34 µmol mol-1, respectively.
Evaluation of method accuracy showed that the method is also accurate for the measurement of N2O
in the N2 matrix. The method’s roughness indicated that the method was quite stable and unaffected
by slight changes in the experimental conditions. From this study, it can be concluded that the
validated method can be used in testing laboratory for internal quality assurance programs purposes
related to the measurement of N2O in N2 matrix.

KEYWORDS: Nitrous oxide; Method validation; Gas chromatography; Electronic capture

detector.

1. INTRODUCTION
The concentration of nitrous oxide (N2O) in atmosphere has reached to about 398.55
nmolmol-1 (equivalent to part per billion) in 2014 and tend to increase, where 40% of that
amount was originated from anthropogenic activities such as agriculture, transportation, and
industries (Anderson et al., 2010). TheN2O is one of the most potent greenhouse gases and its
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

atmospheric lifetime is about 150 years (de Miranda et al., 2015). The N2O has very high
global warming potentials (GWPs) at about 298 times relative to CO2 and significantly
contribute to the earth’s climate (Ermolaev, 2015; Komiya et al., 2010). In this regards,
accurate data obtained by a valid measurement method for monitoring the environmental
release of the N2O to decrease its forcing on global warming effect is of great importance.

For the measurement of N2O, a number of analytical technique having reliable

procedure have been reported such as those based on chromatographic (with electron capture,
thermal conductivity, atomic emission, and mass selective detections) and spectroscopic
(infra-red, laser absorption, and cavity ring-down) (Akdeniz et al., 2009; Teodoru et al., 2015;
Vardag et al., 2014; Wang, 2012; Zhang et al., 2013). Among others, gas chromatography
equipped with micro-electron capture detector (GC-µECD) is an obvious method and widely
used, employing a range of detectability. Besides, the GC-µECD has low operational cost
compared to other methods.

Regardless its tremendous capacity over other methods, a practical application of the
GC-µECD to provide accurate and reliable results for the N2O measurement has created a
need to re-assess the measurement practice of testing laboratories. Owing to the fact that a
good laboratory practice for the testing laboratories as the basis for accreditation assessment
complying with ISO/IEC 17025 is important. According to ISO/IEC 17025, a reliable and
accurate result can only be obtained by using a validated method (BSN, 2008). Method
validation is a part of quality assurances to declare that a high quality of analytical result is
provided (Budiman and Zuas, 2015). In general, method validation refers to a documented
procedure used by a laboratory to ensure that the method performance for the determination
of particular analyte meets the required criteria (EURACHEM, 2014).

In this paper, the study results from validation of analytical method of GC-µECD for
the measurement of N2O in N2 matrix were evaluated.The evaluation was emphasized based
on the following validation parameters such as method suitability, precision (repeatability
and reproducibility), linearity, limit of detection (LoD) and quantification (LoQ), accuracy,
and roughness. Specifically, the study is designed to provide a practical example to personals
in testing laboratories in implementation of validation method for their existing internal
quality assurance programs in the field of gas measurement.

2. MATERIALS AND METHODS

2.1. Materials

Two standard gas mixtures of N2O in N2 matrix were used in this study. The two
standard gas mixtures were in-house prepared gravimetrically at our laboratory in accordance
with ISO Guide 6142: Gas analysis - Preparation of calibration gas mixtures - Part 1:
Gravimetric method for Class I mixtures (ISO Guide, 2015). The final concentrations of the
two N2O standard are 3.25 µmol mol-1 (labeled as NN-A standard) and 0.37 µmol mol-1
(labeled as NN-B standard). The µmol mol-1 is equal to part per million. The NN-A standard
was used in all experiment runs, while the NN-B standard was only used as a reference
standard on the evaluation of method accuracy.
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

2.2. Instrumentation

An Agilent 7890B GC system equipped with a micro electron capture detector

(µECD, Agilent Technologies, Santa Clara, CA) was used. In a typical work, separation of
N2O was achieved using Hayesep Q packed columns (HQ 1.2 m, 1/8 inch OD, UM, Agilent
Technology G3591-82519, precolumn) and a Hayesep R packed column (HR 1.8 m, 1/8 inch
OD, Agilent Technology, G3591-82102, main column). The carrier gas was purified before
entering the column using hydrocarbon filter (activated charcoal, Agilent Technology, USA).

2.3. Procedure

Measurement of N2O

A certain volume of gas sample from standard cylinder was injected to the GC system
through a mass flow controller (MFC, Brooks Instrument, USA). The MFC was used to
maintain the consistency of gas flow rate. The MFC was installed between sample cylinder
and a 1 mL sample loop (Agilent Technologies, USA) on the GC system. The detection of
the N2O was conducted by using a µECD under optimized analytical conditions as listed in
Table 1. The output signal was monitored using installed software (OpenLAB CDS
Chemstation Edition Rev. C.01.07, Agilent Technology, USA), on a HP personal computer
(HP ProDesk 490 G2 MT, Hawlett-Packard Company). The measurement data was estimated
by automated integration of the area under the resolved chromatographic profile.

Validation of Analytical Methods

The analytical method was firstly developed by investigating the suitability of the
GC-µECD system. System suitability was conducted by injecting the NN-A standard into the
GC-µECD under the same operating condition (Table 1) and the profile of generated
chromatogram of the N2O was then evaluated in term of its retention time, peak area, and
peak height. The acceptance criterion of each parameter is set to maximum 2.5% of relative
standard deviation (%RSD). After that, the developed method was validated. In the practical
experiment, the validation process was carried out by assessing the measured data for each
following validation parameters such precision (repeatability and reproducibility), linearity,
limit of detection (LoD) and quantification (LoQ), accuracy, and roughness. The assessment
procedure used for the calculation of the validation parameters were adopted from literatures
(EURACHEM, 2014;Zuas and Budiman, 2016). Repeatability of the method was established
by examining the response of the NN-A standard and expressed as percentage relative
standard deviation (%RSD) from seven replications injections under the same operating
condition and over a short time interval. The method reproducibility was determined by a
similar procedure to that of repeatability except the time of 2 days interval was used instead
of the same day. In addition, the method reproducibility was also assessed by using graphical
technique so called control limit chart (Hovind et al., 2001; Masson, 2007). The linearity of
the method was carried out by the evaluation of N2O calibration curve. The calibration curve
was constructed by plotting peak area of some N2O standard as a function of their
concentration. The N2O standards used in constructing the calibration curve were obtained by
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

diluting the NN-A standard (3.25 µmol mol-1) using dynamic dilution method. The LoD and
LoQ of the method was determined at a signal-to-noise ratio (S/N) of 3 and 10, respectively,
of the N2O chromatogram at the lowest concentration used. The accuracy of the method was
evaluated by comparing the concentration of NN-A standard against another independent gas
standard (NN-B standard). Robustness of the method was determined by investigating the
effect of small changes of the GC-µECD operating parameters (oven temperature, flow rate
of carrier gas, and detector temperature) on the N2O measurement results.

3. RESULTS AND DISCUSSION

3.1. System suitability

In a GC experiment, a system suitability test is an essential part with the purpose to

verify that the GC system is adequate enough for an intended measurement. The suitability
test of the GC system has been accepted in wide application because reliable measurement
results obtained are based on a specific suitability parameters. In this regards, the suitability
test was conducted by injecting seven replicates of N2O (0.99 µmol mol-1) under the same
operating conditions (Table 1). The obtained chromatograms was carried out by observing its
suitability criteria including retention time, peak area, and peak height. Figure 1 displays a
representative of the GC-µECD chromatogram of N2O in N2 matrix. The suitability properties
of the chromatogram are listed in Table 2. From Table 2, it can be seen that the GC-µECD
used in this study is extremely suitable for measurement of N2O in N2 matrix because all
evaluated parameters have %RSD values less than 2.5, indicating that the measurements of
N2O in N2 matrix under the suitable condition were very consistence from run to run.

Table 1. Optimized operating condition of the GC-µECD for the measurement of N2O in N2
matrix

Parameter Operating condition

Sample
Flow rate (via MFC) 150 mL/min
Volume loop 1 mL, stainless steel
Valve Box heater 100oC, On
Oven temperature 90oC (isothermal)
Carrier gas N2,60 psi
Make-up gas P5 (5% CH4 in Ar), 2 mL/min
Detector
Detection system µECD
Temperature 350oC
Electrometer On
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

Figure 1-Representative chromatogram of N2O (0.99 µmol mol-1) in N2 Matrix.

Table 2. Suitability data of the GC-µECD system for the measurement of N2O in N2 matrix.

Parameter Average value (n = 7) %RSD

Retention time 1.05 0.39
Peak area 71.08 1.85
Peak height 14.00 1.29

3.2. Precision

Repeatability (intra-day precision) was conducted to assess the closeness between

measured values form a number of measurements over a short period (EURACHEM,
2014;Zuas et al., 2016). Seven-injection replications of N2O standard (2.87 µmol mol-1) were
performed and the repeatability of the method was predicted by comparing the relative
standard deviation (%RSD) of the measurements against the calculated value obtained by
means of Horwitz function (Eq. 1) (Jichem et al., 2001).

(1)

where is the concentration of target analyte in decimal fraction. The results of the method
repeatability evaluation are depicted in Table 3. As it can be seen in Table 3, the %RSD of
the method repeatability was found to be 1.42, which is lower than 8.93 (0.67 x CV-Horwitz).
This finding implies that the analytical method is categorized as an repeatable for the
measurement of N2O in N2 matrix (Jichem et al., 2001).
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

The reproducibility (inter-day precision) is an analytical parameter indicating a variability of

repeated measurement results that are obtained by using the same test method under different
measurement day (Budiman and Zuas, 2015; EURACHEM, 2014). Seven repeated
injection measurements at different days (day 1 and day 2) for the evaluation of method
reproducibility were conducted and the results are listed in Table 3. It can be found that the
%RSD value obtained (0.71 in Table 3) from the N2O measurement are less than its
corresponding CV Horwitz, implying that the analytical method is reproducible.

Table 3. Evaluation results for the precision of analytical method.

Parameters Precision

Repeatability Reproducibility

Average 2.99a 2.87b

SD 3.04 1.40
%RSD 1.42 0.71
CV-Horwitz 13.40 13.40
0.67 x CV-Horwitz 8.93 8.93

Number of injection (n) = 7 replications; b Average value from day

a

1 (n = 7) and day 2 (n = 7).

Moreover, based on the concept of fit for purpose for establishing the reproducibility
of a GC measurement, controlling the quality of the measurement results is required. To
achieve the purpose of such quality control, the process is carried out by constructing a
common control program so called a control limit chart (warning and action limit) (Hovind et
al., 2001). The control limit chart consists of five lines including one average line (AL), two
warning limit (WL) lines, and two control limit (CL) lines. The AL represents the mean of
the control values. The values of the two WL lines are the AL line + two times standard
deviation (AL ± 2SD), while the two CL lines are the AL line ± three times standard
deviation (AL ± 3SD) (Masson, 2007). Figure 2 represents the control limit chart for the
measurement of the N2O in N2 matrix. The results indicate that all control data values lie
within or inside the warning limit, meaning that no occurrence error can be found for the
measurement reproducibility. In a word, the analytical method for the measurement of N2O
in N2 matrix is reproducible, which is in agreement with the above finding related to the
%RSD and CV-Horwitz evaluation. However, if the control data values fall outside the limit,
therefore, a remedial action is required to identify and remove the source of error (Zuas and
Budiman, 2016).
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

Figure 2-The chart of control limit for the measurement of N2O in N2 matrix.

3.3. Linearity

In every method validation process, evaluation of the method linearity is extremely

crucial to be performed because the linearity shows the method ability (within the given
range) to obtain test result that are directly proportional to the concentration of the target
analyte in the sample (EURACHEM, 2014). The linearity of the method was determined by
analysing seven replicate injections of N2O standard at nine concentration levels ranging
from 0.19 to 3.25 µmol mol-1. These concentration levels were obtained by diluting the NN-
A standard (3.25 µmol mol-1) by using dynamic dilution method. The obtained peak area of
each N2O standards were plotted against their concentration to obtain a calibration curve and
the result is shown in Figure 3a. The linearity of the method was statistically evaluated and
the results are tabulated in Table 4. From the Table 4, it can be seen that the correlation
coefficient (R2) of the method linearity for nine concentration point was found to be 0.9998,
indicating that the analytical method for N2O measurement in N2 matrix is fitted to the linear
model.

Moreover, the calibration curve was graphically evaluated by using a response factor
model. This graphical model is used to evaluate the linearity data obtained from a calibration
curve model, where the graph was obtained by plotting the response factor (peak area divided
by their respective concentration) against corresponding concentration. The response factor
against analyte concentration in a linear range should be relatively constant, with a minimum
limit of 95% and a maximum of 105 % of the constant response. Figure 4 displays a
graphical evaluation of the linearity of the analytical method for N2O measurement. From
Figure 4, it can be seen that response factor from three concentration points (0.19, 0.29 and
0.39 µmol mol-1) exceeds the maximum limit (105% constant response). Thus, these three
outlier points were excluded and the six remains points (0.59, 0.79, 0.99, 2.28, 2.86, and 3.25
µmol mol-1) were used in constructing a new calibration curve and the result is displayed in
Figure 3b. It can be seen from Figure 3b, the new calibration curve has R2 = 0.9998, which is
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

very similar to the R2 of the previous calibration curve (Figure 3a), implying that they have
same level in linearity. However, from linearity data as shown in Table 4, it can be observed
that new calibration curve (six concentration points as in Figure 3b) has greater slope (65.15)
than previous one (nine concentration points as shown in Figure 3a). The greater slope of the
new calibration curve indicates that its sensitivity is better than previous calibration curve. In
addition, the intercept of the new calibration curve (i.e., 0.057) was found to be lower than
previous calibration curve (1.275). For a linear equation, the intercept represents the constant
systematic error or constant bias and the value of the intercept should be as close to zero as
possible (Jhang et al., 2004). This implies that the constant systematic errors/constant bias of
the new calibration curve (six concentration points) much smaller than the previous
calibration curve (nine concentration points). In conclusion, the linearity of the analytical
method from the new calibration curve for the measurement of the N2O in N2 matrix is more
favorable than previous one.

Figure 3-Calibration curve of: (a) nine concentration points, and (b) six concentration points.

Figure 4-A graphical of control limit chart for the measurement of N2O at nine concentration
points.
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

3.4. LoD and LoQ

In every analytical measurement, the LoD and LoQ are also essential to be conducted.
The LoD is defined as the lowest concentration of an analyte in a sample that can be detected,
but not necessarily quantified as an exact value. The concentration of analyte at the LoD level
can only be determined qualitatively. In other hands, a quantitative analysis is also possible to
be performed at the LoD level; however, it may lead produce an inaccurate result since the
uncertainty contribution is larger than the measurement result itself (EURACHEM, 2014).
The LoQ is defined as the lowest concentration of an analyte in a sample that can be
quantified with appropriate precision and accuracy, meaning that the minimum concentration
of analyte in the sample can be reliably determined by conducting the LoQ evaluation). The
LoD and LoQ of the N2O were determined using a signal to noise (S/N) ratio method. Based
on this S/N method the ratio values of LoD and LoQ are 3:1 and 10:1, respectively
(EURACHEM, 2014;Zuas et al., 2016). The LoD and LoQ were determined from 0.59 µmol
mol-1(as the lowest N2O standard used in the linearity evaluation at six point concentrations
range) and the results are tabulated in Table 4. From Table 4, it was found that the LoD and
LoQ of the analytical method were 0.10 and 0.34 µmol mol-1, respectively.

Table 4. Data indicating linearity of the method for N2O in N2 matrix and their LoD and LoQ
values.

Calibration Slope Intercept Linear range R2 LoDa LoQa

curve (µmol mol-1) (µmol mol-1) (µmol mol-1)
Nine pointsb 64.67 1.28 0.19 - 3.25 0.9998 0.09 0.29
Six pointsc 65.15 0.06 0.59 - 3.25 0.9998 0.10 0.34
aAverage
value from seven injection replications.
b
N2O standards were 0.19; 0.29; 0.39;0.59; 0.79; 0.99; 2.28; 2.86; and 3.25 µmol mol-1.cN2O
standards were 0.59; 0.79; 0.99; 2.28; 2.86; and 3.25 µmol mol-1.

3.5. Accuracy

Accuracy of an analytical method is defined as the closeness or the agreement

between the measured and an accepted/true value (Taverniers et al., 2004; EURACHEM,
2014). Experimentally, the accuracy is a combination of the bias and precision of the
analytical procedure; the bias of method ( ) is the difference between the measured value
and the value from certificate of reference standard, which was calculated using an
expression below (Eq. 2) (EURACHEM, 2014).

(2)

where is the average of measured value of reference standard, and is value from
certificate of reference standard. For assessing the method accuracy, the values of
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

repeatability ( ), reproducibility ( ), and uncertainty value ( ) form certificate of

reference standard are included. A combination those three components results in value by
using the following expression (Eq. 3) (EURACHEM, 2014):

(3)

where is standard deviation from reproducibility (inter day precision). is the standard
deviation from repeatability (intra day precision), is number of replications and is the
uncertainty of NN-B standard. The ISO Guide 33:2015 “Reference materials - Good practice
in using reference materials” (ISO Guide, 2015) defines the acceptance criteria, where no
bias is found if the value falls within at confidence level 95% (Eq. 4).

(4)

From the Table 5, it can be evaluated that the measured value of the N2O falls within ,
implying that no evidence of bias can be found in the analytical method for the measurement
of N2O in N2 matrix. In a word, the analytical method for the measurement of N2O in N2
matrix is accurate.

Table 5. Accuracy data of the GC-µECD for the measurement of N2O in N2 matrix

Bias,
(µmol mol-1) (µmol mol-1) (µmol mol-1) (µmol mol-1)
- 0.258 0.173 0.346 -0.346 < - 0.258 < 0.346

3.6. Robustness

Robustness is a part of analytical method validation to evaluate the effect a number of

analytical method parameters (factors) on the results of a measurement. The method
robustness defines the capacity to generate some results, which remains unaffected by minor
changes of the experimental conditions during analysis (EURACHEM, 2014). In this study,
the robustness of the method was assessed by investigating the effect of small changes of the
GC-µECD parameters (such as oven temperature, flow rate of the carrier gas, and detector
temperature) on the measured concentration of the N2O in N2 matrix. For the robustness
study, a standard containing 2.99 µmol mol-1 N2O was used and the results of the robustness
study are tabulated in Table 6. It can be seen in Table 6, small changes of the GC-µECD
parameters have no significant effects on the measured concentration of N2O in N2 matrix
implying that the analytical method used is robust.
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

Table 6. Statistical analysis of three-parameter variation effect using one-way ANOVA

Parameter Mean Values p-values

Oven Temperature
- 92 oC - 3.010
- 90 oC - 2.991 0.999
- 88 oC - 3.045
Detector temperature
- 352 oC - 2.797
- 350 oC - 2.991 0.999
- 342 oC - 2.625
Carrier Gas Flow rate
- 62 psi - 3.139
- 60 psi - 2.991 0.998
- 58 psi - 2.891

4. CONCLUSION

For a routine work, validation of an analytical method used is crucial important.

Evaluation results for each validation parameter indicated that the validated method offers a
sufficient proof concerning the reliability of the GC-µECD method for the measurement of
N2O in N2 matrix with further keeping the degree of user confidence regarding their
analytical data. In addition, the developed and validated method could also be used as a good
reference for local and international in the validation of the measurement method for other
target gas components.

5. ACKNOWLEDGEMENT

The authors gratefully acknowledged the Indonesian Government for financially

supporting this study within the scope of project “Strengthening Chemical Metrology
Competency and Infrastructure” and Ministry of Research, Technology and Higher
Education of Indonesia through Supporting Program Batch II No. 1883.1/D/KPT/2016. The
authors also would like to extend our appreciation to K. D. Purnama from Diponegoro
University for helping in data collection.
 The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

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The Journal of Engineering and Exact Sciences - JCEC, Vol. 03 N. 03 (2017) 381–394

DETERMINAÇÃO DO ÓXIDO NITROSO EM UMA MATRIZ

DE NITROGÊNIO, USANDO CROMOTOGRAFIA EM FASE
GASOSOA COM DETECTOR DE CAPTURA ELETRÔNICA:
VALIDAÇÃO DO MÉTODO ANALÍTICO
O. ZUAS1, M. R. MULYANA1, N. HAMIM2, H. BUDIMAN1

Gas Analysis Laboratory, Metrology in Chemistry Research Group, Research Centre for
1

Metrology, Indonesian Institute of Sciences (RCM-LIPI)

2
Electrochemistry Laboratory, Metrology in Chemistry Research Group, Research Centre for
Metrology, Indonesian Institute of Sciences (RCM-LIPI)
E-mail: [email protected]

RESUMO: A presença de óxido nitroso (N2O), um dos gases de efeito de estufa mais potentes,
contribui significativamente para o aquecimento global. Desta forma, é muito importante
disponibilizar métodos de medição exatos e válidos para a monitorização da emissão deste gás para
o ambiente. Neste estudo, foi validado um método analítico para a medição de N2O numa matriz de
azoto (N2) usando cromatografia em fase gasosa com microdetector de captura eletrônica (GC-
µECD). O método analítico foi validado em termos de alguns parâmetros de desempenho, como a
adequação do sistema, precisão (repetibilidade e reprodutibilidade), linearidade, limite de detecção
(LoD) e limite de quantificação (LoQ), exatidão e robustez do método. Os resultados mostram que o
GC é adequado para a medição de N2O numa matriz de N2. A repetibilidade e reprodutibilidade do
método foi quantificada por desvios padrão relativos (RSD) de 1,42 % e 0,71 %, respectivamente,
indicando que o método é adequado para medições de N2O. A linearidade do método foi excelente,
tendo-se observado um R2 de 0,9998. O LoD e LoQ do método é 0,10 e 0,34 µmol mol-1,
respectivamente. A avaliação da exatidão do método demonstrou que este também é exato para
medições de N2O em matriz de N2. A robustez do método indica que o método é bastante estável e
pouco afetado por alterações nas condições experimentais. Pode-se concluir deste estudo que o
método validado pode ser usado em laboratórios de ensaio para programas internos de garantia da
qualidade relacionados com medições de N2O em matriz de N2.

PALAVRAS-CHAVE: Óxido nitroso, Validação de método, Cromatografia em fase gasosa,

Detector de captura eletrônica.