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Abstract
Objectives: Focus of the Research experiment is to evaluate the uncertainty in Ethephon determination. Validation of
analytical method and identify the factors effecting the uncertainty in measurement. Methods/Statistical Analysis: A
Titrimetric Method was used for determination of Ethephon content. A certified commercially formulated solution of
Ethephon 39.00 % (w/w) S.L has been taken as a sample for analysis. An estimation of uncertainty in quantification of
Ethephon was determined by identifying the following parameters, uncertainty influencing factors and its contribution
to measurement, Type A Uncertainty (UA), Type B Uncertainty (UB), Combined Uncertainty (UC), Expanded Uncertainty
(UE) and uncertainty budget. An Experimentally calculated value of combined uncertainty in preparation of 0.1 N NaOH
solutions is 0.132%. A value of relative standard uncertainty in repeatability test of Ethephon is 0.084%. Determined
% bias value of test method is 0.06%. An estimated value of combined uncertainty in Ethephon determination is 0.373
%. Obtained value of expanded uncertainty with coverage factor of 2.26 with 95% confidence is 0.843%. Obtained %
RSD of Ethephon test result is 0.26 %. LOQ value of analytical test method is 0.36%. A Measured uncertainty value in
Ethephon determination is 39.06 ± 0.33%. Findings: This paper produces Technique for analytical method validation
and uncertainty measurements in quantitative analysis of Ethephon. Application/Improvements: As per regulatory for
laboratory accreditation bodies, it is mandatory to evaluate the uncertainty in measurement. Presented method provides
extensive details regarding uncertainty measurements.
was purchased from sigma-aldrich, Phenolphthalein 0.2 g of Ethephon (39 % S.L. sol) sample was taken
indicator was purchased from Rankem India, Thymol in 250 ml Erlenmeyer flask, added about 80 ml of freshly
blue 0.1 % w/v in alcohol indicator was purchased from distilled water and stirred gently to dissolve the contents.
fisher scientific. Ethephon 39% S.L. (Soluble concen- Added 2 drops of thymol blue indicator and titrate against
trate Liquid) solution was purchased from Hindustan 0.1 N NaOH solutions till blue color appears1,3. Repeat the
Agrotech Industries India. All the chemicals and reagents analysis process ten times and calculate the uncertainty.
were stored at 25oC ± 2oC and 40% relative humidity con- Calculation: % Ethephon by (w/w) =V×N×7.225
trolled room temperature. M
Where, V= Vol. of in ml of NaOH consumed, N =
2.2 Apparatus Normality of NaOH sol., M = Mass in g of sample taken.
Erlenmeyer flask 250 ml, Burette 50 ml ± 0.05 ml, Pipette
25 ml ± 0.03 ml and measuring cylinder 100 ml ± 0.5 ml 3. Result and Discussion
was used for the experiment. Calibrated Class ‘A’ grade
glassware of borosil used for the analysis. An Analytical
weight balance was calibrated using 2 g ± 0.01 g standard 3.1 Fish Bone Diagram of Uncertainty
weight. Influencing Factors in Analysis
The objective of this step is to understand and identify
2.3 Analysis Procedure the major uncertainty sources and its contribution to the
uncertainty2-4. Description was given in Figure 1.
2.3.1 Preparation of 0.1 N Potassium Hydrogen
Phthalate Solutions (KHP)
Dry about 25 g of Potassium hydrogen phthalate at 105oC
± 5oC for 2 hrs and allow cooling at room temperature.
Weigh 20.4223 g of dried KHP and dissolve in freshly dis-
tilled water and dilute to 1000 ml2.
2 Vol 9 (45) | December 2016 | www.indjst.org Indian Journal of Science and Technology
Samarth I. Zarad, Nitin R. Nimkar, Kishor R. Desai, Maheshwari S. Solanki, Devang M. Gandhi, Harshal M. Gandhi, Aparna A.
Khimani, Monali S. Desai and Macky N. Suraliwala
pipette1,5-8. Calculated value of standard uncertainty As this expression is a sum of independent values, the
of burette was 0.02041 ml and for pipette the obtained standard uncertainty of Molar mass of KHP is a simple
value was 0.01225 ml. As described in Table 1, % relative square root of the sum of the squares of the contributions:
standard uncertainty of burette and pipette was 0.041 % Combined standard uncertainty in Molar mass of
and 0.049% respectively. Calculated value of Combined KHP=
Uncertainty of glassware calibration (UC2) was 0.064%. = 0.0038 g/mol
UC2 =
3.2.4 Uncertainty in NaOH Solution Preparation
(UA1
% UC2 =
= 0.064 % Three readings were taken for standardization of NaOH
solution. Obtained normality of NaOH solution was
3.2.3 Uncertainty in Purity (UB4) and Molar Mass 0.1007 N calculated % relative standard uncertainty was
(UB5) of KHP 0.129 % as seen in Table 4 and 5.
Vol 9 (45) | December 2016 | www.indjst.org Indian Journal of Science and Technology 3
Measurement of Uncertainty Associated with Quantification of Ethephon
Table 3. Standard uncertainty of KHP elements Table 4. Standard uncertainty in g/mol of KHP
Element Atomic Quoted Standard Elements of Calculation Result Standard
weight Uncertainty Uncertainty KHP uncertainty
(a) (a/√3) C8 8×12.0107 96.0856 0.0037
C 12.0107 ±0.0008 0.00046
H5 5×1.00794 5.0397 0.00020
H 1.00794 ±0.00007 0.000040
O4 4×15.9994 63.9976 0.00068
O 15.9994 ±0.0003 0.00017
K 39.0983 ±0.0001 0.000058 K 1×39.0983 39.0983 0.000058
4 Vol 9 (45) | December 2016 | www.indjst.org Indian Journal of Science and Technology
Samarth I. Zarad, Nitin R. Nimkar, Kishor R. Desai, Maheshwari S. Solanki, Devang M. Gandhi, Harshal M. Gandhi, Aparna A.
Khimani, Monali S. Desai and Macky N. Suraliwala
Vol 9 (45) | December 2016 | www.indjst.org Indian Journal of Science and Technology 5
Measurement of Uncertainty Associated with Quantification of Ethephon
3.3 Uncertainty Budget ments by virtue of Precision, LOQ and Uncertainty value
Budget represent the summary of all uncertainty compo- for determination of Ethephon.
nents in tabular form3,6. Uncertainty budget gives quick
view at the totality of information associated with uncer- 5. Acknowledgement
tainty measurements. An Estimated value of uncertainty
in Ethephon determination was 39.06 ± 0.33% as seen in We are Thankful to Pollucon Laboratories Pvt. Ltd, Surat,
Table 7. India for Funding this project and supporting us during
the experiment of Uncertainty Measurements.
6. References
1. Kanagasabapathy K. NABL 141, Guidelines for estima-
tion and expression of uncertainty in measurement. India:
NABL; 2016. p. 38-42.
2. Rice EW, Baird RB, Eaton AD, Clesceri LS. APHA, Standard
Methods for the Examination of Water and Waste Water.
22nd ed. APHA, USA. 2012. p. 2-31.
1. % Uncertainty in Repeatability of Ethephon determination (UA2) 3. Taylor BN, Kuyatt CE. NIST Technical Note 1297. Guideline
was 0.084. for evaluating and expressing the uncertainty of NIST mea-
2. % combined Uncertainty of NaOH Solution preparation (UC1) surement results. NIST, USA. 1993. p. 11.
was0.132. 4. Sangathan MKS. IS: 14408: 1996. Ethephon Technical
3. % Bias was (UBias) 0.166. Specifications. India: BIS; 2012. p. 2.
4. % Combined Glassware Uncertainty (UC2) was 0.064. 5. Chowdhury S, Datta AK, Saha AD, Sengupta S, Paul
5. % Weigh Balance Uncertainty (UB1) was 0.289. R, Maity S, Das A. Traits influencing yield in Sesame
Figure 2. Calculated values of uncertainty influencing (Sesamum indicum L.) and multilocational trials of yield
factors in determination of Ethephon. parameters in some desirable plant types. Indian Journal of
Science and Technology. 2010 Feb; 3(2):163-6.
6. Ellison SLR, Williams A. EURACHEM/CITAC guide CG
4. Conclusion 4. Quantifying Uncertainty in Analytical Measurement. 3rd
ed. UK: Eurachem; 2012. p. 41-50.
An estimation of uncertainty in analytical method was 7. Krishnan V, Gopi M, Amerjothy M. Morphological diver-
calculated with the parameters such as uncertainty in sity and some newly recorded plant Galls in Tamil Nadu,
glassware calibration, Uncertainty in Analytical method India. Indian Journal of Science and Technology. 2011 Sep;
and uncertainty in reagent preparation. Uncertainty bud- 4(9):1067-73.
get was prepared to summarize the measured uncertainty 8. Runsheng Y, Zuyu L, Zhizhong W. In vitro estrogenic
value and its contribution towards uncertainty measure- potency of phytoestrogen-glycosides and some plant flava-
ments description was show in Figure 1 and Figure 2. noids. Indian Journal of Science and Technology. 2010 Dec;
Current Method is found suitable for Analytical measure- 3(12):1142-7.
6 Vol 9 (45) | December 2016 | www.indjst.org Indian Journal of Science and Technology