Dumas Method

Group 10

Abigail S.

JOURNAL
Elissa O.
Tiffany B.

REVIEW
OUTLINE
▣ About Journal
▣ Introduction
▣ Material and Methods
▣ Results and Discussion
▣ Conclusion
▣ References
▣ Recommendations
2
“Cereal protein analysis
via Dumas method:
Standardization of a
micro-method using the
EuroVector Elemental
Analyser”

3
About Journal

Penulis : S. Serrano, F. Rincón, and J. García-Olmo

Tahun terbit : 2013

CITATION

Serrano, S., Rincón, F. and García-Olmo, J. (2013). Cereal

protein analysis via Dumas method: Standardization of a
micro-method using the EuroVector Elemental
Analyser. Journal of Cereal Science, 58(1), pp.31-36.

4
INTRODUCTION
combusting a
sample of known
Dumas
mass at high
Method
temperature in the
presence of oxygen

To determine
the molecular
weight of an
unknown gas based on digestion
Kjeldahl
of the sample with
Method
sulphuric acid

5
DUMAS METHOD
(by Jean Baptiste Dumas in 1831)

▣ The method consists ▣ the Dumas method

of combusting a has a great
sample of known potential for
mass in a high accuracy, speed of
temperature range of analysis and
800-900°C chamber automation.
in the presence
of oxygen.
▣ Organic compounds
are mixed with CuO
and then heated with
atmospheric CO2
6
 KJEHDAL METHOD
(by Kjeldahl in 1883)
▣ In the case of direct titration, the
▣ Based on digestion of the
sample with sulphuric
acid
▣ The organic matter is
decomposed by oxidation▣
and organic nitrogen is
reduced to
ammoniumsulphate
▣ Inorganic forms of
nitrogen such as nitrates ▣
and nitrites are not
usually measured
ammonia gas is captured by boric
acid, forming an ammonium borate
complex, which is neutralized by a
standardized mineral acid.
In the case of back titration, the
ammonia is captured by a
standardized mineral acid and the
excess acid is titrated with a
standard alkaline base solution
The time-consuming and multiple
steps of the analytical procedure,
together with the use of corrosive
and toxic chemicals
7
 Dumas Method gives a more reliable measure
of organic nitrogen than KM and offers greater
precision in the determination of protein
content in cereals and oilseeds

Advantages :

Faster
More economical
Less Polluting
Safer

8
 The aim of this study was to
analyze the effect of certain ACFs on
the DM analytical process, using a
PlacketteBurman experimental
design to identify IFs and later to
optimize the IF combination.
 MATERIAL & METHODS
▣ The Dumas method is based on combustion of
the whole sample in an oxygen-enriched
atmosphere at a high temperature in order to
ensure complete combustion.
▣ A EuroVector Elemental Analyser EA3000
equipped with Callidus software was used.
▣ Two samples obtained from the Community
Bureau of Reference (BCR).
▣ Certified reference materials (CRMs)

Analytical Instrument 10
 MATERIAL & METHODS
▣ Two cereal reference materials :
-BCR-381 rye (Secale cereale L.) flour, 1.249 0.1 %N)

-BCR-382 wheat (Triticum aestivum) flour (screening the

factors affecting the DM analytical process)

Reference Materials 11
MATERIAL & METHODS

Screening Phase 12
MATERIAL & METHODS
▣ Accuracy is the concordance between the detected
value obtained and the certified reference value, the
R1 (CRM-381) and R3 (CRM-382) responses will
measure the difference between both detected
(mean of four replicates) and certified values.

▣ Precision is the variability of results obtained by

analyzing the same sample using the same method
of analysis to validation, so R3 (CRM-381) and R4
(CRM-382) responses were used to measure the SD of
four replicates determinations.

Optimization Phase 13
 RESULTS AND DISCUSSION

▣ It must therefore be concluded

that certain factors in DM
implementation are critical for
ensuring adequate precision.
▣ This difference in nitrogen
concentration prompted a
difference in uncertainty,
uncertainty for rye and wheat
samples was 4.8 10 4 and 7.5 10 4.

▣ In other words, as oxygen volume increases, measurement

becomes less accurate, leading to a higher-than-actual result for
N content. Moreover, this loss in accuracy is accompanied by a
sharp increase in R2 and R4 ( 2.6 for rye and 8 for wheat), thus
prompting a major loss in precision. 14
The presence of an excessive volume of O2
during sample combustion leads to
i. Greater oxidation of the reactor reducing agent
(Cu) and a shortening of its useful life.
ii. The appearance of partially-overlapping peaks,
preventing their adequate integration, with the
result that the measured amount of N is higher
than the real amount.
iii. An increase in background noise and thus a loss
of precision.

15
▣ In order to validate the conditions suggested here for the use
of the DM for protein measurement in cereals, five
measurements were performed for Wheat (2.1067, 2.1253,
2.1254, 2.1365 and 2.1162, mean 2.122 e real values 2.12% and SD
0.011) and Rye (1.2534, 1.2728, 1.2655, 1.2685 and 1.2533, mean
1.262 cereal value 1.249%- and SD 0.009).
▣ Beljkas et al. (2010) concluded that since the DM procedure is
very simple and almost completely automated, there are
relatively few sources of uncertainty compared to the KM.

16
 CONCLUSION
▣ Measurement of nitrogen content using the DM
requires the prior optimization of analytical
conditions for each sample type
▣ Application of a non-geometric PlacketteBurman
experimental design enabled the identification of
two critical factors:
-RFT (rear furnace temperature)
-GCT (GC oven temperatures)

17
RECOMMENDATION

+ -
▣ This journal ▣ There’s no
increases our conclusion part in
knowledge about this journal.
Dumas Method.

18
REFERENCES

AOAC, 1990. Official Methods of Analysis, 4th Supplement (1993). 992.23 Method, 15th ed.
AOAC International, Arlington, Virginia.
Beljkas, B., Matic, J., Milovanovic, I., Jovanov, P., Misan, A., Saric, L., 2010. Rapid method for
determination of protein content in cereals and oilseeds: validation, measurement
uncertainty and comparison with the Kjeldhal method. Accreditation and Quality
Assurance 15, 555e561.
Belliardo, J.J., Wagstaffe, P.J., 1988. BCR reference materials food and agricultural analysis:
and overview. Fresenius Zeitschrift für Analytische Chemie 332, 533e538.
Chiacchierini, E., Dáscenzo, F., Restuccia, D., Vinci, G., 2003. Milk soluble whey
proteins: fast and precise determination with Dumas method. Analytical Letters
36 (11), 2473e2484.
Daun, J.K., DeClercq, D.R., 1994. Comparison of combustion and Kjeldhal Methods
for determination of nitrogen in Oilseeds. Journal of the American Oil Chemists’
Society 71 (10), 1069e1072.
Kjeldahl, J., 1883. A new method for the determination of nitrogen in organic matter. Zeitschrift
fur Analytische Chemie 22, 366e382.
Thompson, M., Owen, L., Wilkinson, K.,Wood, R., Damant, A., 2002. A comparison of the
Kjeldahl and Dumas methods for the determination of protein in foods, using data
from a proficiency testing scheme. Analyst 127, 1666e1668.
Williams, P., Sobering, D., Antoniszyn, J., 1998. Protein testing methods at the Canadian grain
Commission. In: Wheat Protein Symposium, Saskatoon, Canada, March 9e10.
THANKYOU