Conductivity Uncertainty

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Science Journal of Chemistry

2022; 10(6): 211-218


http://www.sciencepublishinggroup.com/j/sjc
doi: 10.11648/j.sjc.20221006.13
ISSN: 2330-0981 (Print); ISSN: 2330-099X (Online)

Calibration and ISO GUM Based Uncertainty of


Conductivity and TDS Meters for Better Water Quality
Monitoring
Adel Bassuoni Shehata*, Abdulrahman Rashed AlAskar, Rashed Abdallah Al Dosari,
Fahd Refaei Al Mutairi
Chemistry Department, National Measurement and Calibration Center (NMCC), Saudi Standards, Metrology and Quality Organization
(SASO), Riyadh, Kingdom of Saudi Arabia

Email address:

*
Corresponding author

To cite this article:


Adel Bassuoni Shehata, Abdulrahman Rashed AlAskar, Rashed Abdallah Al Dosari, Fahd Refaei Al Mutairi. Calibration and ISO GUM
Based Uncertainty of Conductivity and TDS Meters for Better Water Quality Monitoring. Science Journal of Chemistry.
Vol. 10, No. 6, 2022, pp. 211-218. doi: 10.11648/j.sjc.20221006.13

Received: November 9, 2022; Accepted: November 24, 2022; Published: November 30, 2022

Abstract: Water quality monitoring is of fundamental importance for health and environmental protection. Conductivity and
the total dissolved substance (TDS) are two important water quality parameters. Their monitoring requires good calibration of
the measuring equipment and correct assessment of the measurement uncertainty so that the water quality limits can be well
judged. Though many published research articles include conductivity and TDS measurement results, there is no published ISO
GUM approach for estimation of the uncertainty in the calibration measurement results. In this work, the linearity of a
conductivity meter was established using three certified reference materials (CRMs) of 100, 500 and 1410.7µS/cm and then a
one-point calibration using CRM of 1410.7µS/cm was carried out. The calibration method was validated by studying its
accuracy, precision and bias. The method was found fit-for-the purpose and the uncertainty sources of calibration were
identified and estimated based on ISO GUM. Then a standard solution of concentration 0.01M was prepared from high purity
KCl to provide conductivity of 1411µS/cm. The corresponding TDS value of this solution was found 745 mg/L and its
traceability to the SI units was achieved by weighing the mass of KCl using a calibrated balance and by measuring the volume
of water using a calibrated measuring flak. This solution was used to perform a one-point calibration of a TDS meter then the
meter was allowed to read the TDS 10 times and the uncertainty of the measurement results was estimated based on ISO GUM.
The results obtained proved a very good calibration of both meters. An overall approach for estimation of the calibration
uncertainty was developed, which will be very useful in water quality monitoring measurements.
Keywords: Conductivity, TDS, Calibration, Method Validation, ISO GUM Uncertainty

1. Introduction
The increase in population, industrialization and use of of rocks, leaching of soils and mining [3]. As a result, the
fertilizers in agriculture in addition to the man-made activity conductivity of water is affected specially it is related to ten
has resulted in an increasing pollution of water with various factors such as temperature, pH value, alkalinity, total
harmful substances. Because of this, the quality of drinking hardness, calcium, total solids, total dissolved solids,
water has to be checked in order to protect the population chemical oxygen demand, and the concentration of chloride
from many water-borne diseases [1, 2]. The different types of and iron in water. Conductivity is defined as the ability of a
pollutants are introduced into the natural water by weathering material to conduct an electric current [4]. It is widely
Science Journal of Chemistry 2022; 10(6): 211-218 212

applied as an essential tool for water quality assessment and 3. Results and Discussion
is measured by conductivity meters [5]. These meters can be
calibrated at specified conductivity values provided by 3.1. The Standard Solution of KCl
standard KCl solutions [6]. Conductivity and the total Potassium chloride is one of the important chemicals used
dissolved substance are correlated by the formula TDS = f x in the preparation of standard solutions for the calibration of
EC where the constant f is in the range of 0.55 to 0.9 in most the TDS and conductivity measuring instruments because it
conductivity meters and varies according to the chemical is highly soluble in water producing much ions. The TDS
composition of the ions dissolved in water [7-10]. These two meters measure the electrical conductivity, k of aqueous
water quality parameters are indicators of salinity level which solutions which is multiplied by a factor f to give the
make them very useful as one way of studying seawater corresponding TDS [19]. In this work, a mass of KCl was
intrusion [11-15]. The liquid capacity to conduct an electric heated in an oven at 400°C for two hours then left to cool to
charge depends on the dissolved ions concentrations, ionic room temperature in a desiccator. After that, a standard
strength, and temperature of measurements [16]. For accurate solution of 0.01M KCl that has conductivity of 1411 µS/cm,
and traceable measurement results of conductivity and TDS, was prepared in a measuring flask by dissolving 186.37750
the meters used for measurements are to be calibrated using mg in 250 mL ultra-pure water. The preparation was made
certified reference materials (CRMs). Calibration is defined using equation 1.
as: operation that, under specified conditions, in a first step,
establishes a relation between the quantity values with m x p
measurement uncertainties provided by measurement C= (1)
V
standards and corresponding indications with associated
measurement uncertainties and, in a second step, uses this where,
information to establish a relation for obtaining a C - concentration of KCl in mg/L;
measurement result from an indication [17]. The calibration m - mass of KCl (mg);
results can be claimed traceable to the SI units if the p - purity of KCl/100;
uncertainty of the measurement results is estimated in V - volume of KCl solution (L).
accordance with requirements of ISO GUM [18]. On the
other hand, traceability is defined as: property of a 3.2. Establishing Linearity of the Conductivity Meter
measurement result whereby the result can be related to a To measure conductivity of the KCl standard solution,
reference through a documented unbroken chain of linearity of the conductivity-meter was established using three
calibrations, each contributing to the measurement CRMs of conductivities, 99.91±0.3, 500.8±1.5 and 1410.7±2.8
uncertainty [18]. In this paper, conductivity and TDS meters µS/cm produced by the Slovak National Metrology Institute,
have been one-point calibrated and an approach to study and SMU. The meter was calibrated by each CRM then was
estimate the uncertainty sources of the calibration process has allowed to read it five times. The calibration line was plotted
been developed based on ISO GUM. The developed between conductivity values of the CRMs and the
approach will be very useful for water analytical laboratories corresponding average response values as shown in Figure 1.
in estimating their uncertainties in conductivity and TDS From this figure it can be seen that R2 equals 1 indicating that
measurement results. the meter can give very good linear results in this range.

2. Materials and Methods


2.1. Chemicals

Potassium chloride (99.5-100.5%) was supplied by


PanReac, Spain and ultrapure water was obtained by
Millipore Milli-Q RG, USA. The certified reference materials
(CRMs) of conductivity, 100, 500 and 1410.7 µS/cm were
obtained from the Slovak metrology institute, SMU.
2.2. Equipment Figure 1. Calibration line of conductivity-meter using 3 CRMs.

The conductivity and TDS meter used for measurements 3.3. The One-Point Calibration of the Conductivity-Meter
was a product of Mittler Toledo, model S230. The
The one-point calibration was performed at 25°C using a
temperature controlled water bath used in calibration was
laboratory procedure then conductivity of the CRM solution
supplied by IKA, Germany. Weighing the mass of KCl was
was measured 10 times in order to verify if the calibration
carried out by an analytical balance with resolution 0.01 mg
results lie within the uncertainty limits of the CRM. The
supplied by Mittler Toledo. The glass measuring flask used
results obtained, average, standard deviation and RSD% are
for preparation of the KCl standard solution was of class A.
shown in Table 1.
213 Adel Bassuoni Shehata et al.: Calibration and ISO GUM Based Uncertainty of Conductivity and TDS Meters for
Better Water Quality Monitoring

Table 1. Conductivity indications of the 1410.7 µS/cm. where


Conductivity 1410 – 1409 – 1411 – 1409 – 1412- 1410 – 1409 – RSD % - percentage relative standard deviation;
(µS/cm) 1411 – 1409 - 1412 SD - standard deviation;
Ave 1410.2 - average of conductivity indications.
SD 1.23 The obtained bias value, 0.035% was much smaller than
RSD% 0.09
the precision threshold (5%), indicating a very good
These conductivity values were tested for outliers using precision of the one-point conductivity calibration method.
Grubbs test and no outlier result was found. The normal 3.5. Accuracy of the Method
distribution of the results was tested by the Kernel density
function which showed a clear Gaussian distribution as it can Accuracy is defined as: “closeness of agreement between a
be seen in Figure 2. measured quantity value and a true quantity value of a
measurand” [17]. Accuracy was calculated for each value
using equation 3 and the results were reported in Table 2.

xi
Accuracy % = x 100 (3)
xCRM

Table 2. Accuracy results in case of the calibration by CRM 1410.7 uS/cm.

xCRM Indication (xi) Accuracy %


1410.7 1410 99.95
1410.7 1409 99.88
Figure 2. The normal distribution of the calibration results. 1410.7 1411 100.02
1410.7 1409 99.88
The conductivity values in Table 1 were plotted within the 1410.7 1412 100.09
1410.7 1410 99.95
expanded uncertainty limits of the CRM (±2.8 µS/cm) as
1410.7 1409 99.88
shown in Figure 3. In this Figure, the solid central line 1410.7 1411 100.02
represents the conductivity value of the CRM (1410.7µS/cm) 1410.7 1409 99.88
and the dashed lines represent the upper and the lower 1410.7 1412 100.09
uncertainty limits. It is clear that the 10 conductivity
measured values lie within the uncertainty limits of the CRM From these results, it is clear that the calculated accuracy
confirming a strong traceability of the measurement results to ranges from 99.88 to100.09%, which means that the method
the SI units. produces a small measurement error giving rise to a very
good accuracy of the calibration results.
3.6. The Method Bias

Bias is defined as: “average of replicate indications minus


a reference quantity value”. Based on this definition, bias
was calculated in percentage relative (b%) by equation 4
using the average value of the conductivity indications and
the value of the CRM [17]. The average of indications was
found 1410.2 µS/cm and the bias was found 0.04% which is
smaller than the pre-defined value, 0.5% assuring a good
trueness of the calibration results produced by this method.
Figure 3. CRM 1410.7 µS/cm indications within the uncertainty limits.
x − xref
b (%) = (4)
3.4. Precision of the Method xref
Precision is defined as “closeness of agreement between
where
indications or measured quantity values obtained by replicate
- average of conductivity indication;
measurements on the same or similar objects under specified
xref - conductivity of the CRM indicated in the certificate.
conditions” [17]. In the ICH, it is mentioned that the RSD at
95% confidence limit is an indication on the precision of the 3.7. Uncertainty of the Conductivity Measurements
method [20, 21]. Using data in Table 1, the RSD% was
calculated by equation 2. The estimation of uncertainty in measurements based on
ISO GUM starts by writing the measurement model and
RSD % =
SD
x 100 (2) identifying the uncertainty sources then quantifying
x uncertainty of each source [18]. Hence, the measurement
Science Journal of Chemistry 2022; 10(6): 211-218 214

model of conductivity is defined by equation 5 [19]. was calculated from equation 9 and was found 1409.9 µS/cm
[19]. Then uncertainty due to the effect of temperature on the
kT electrode was estimated as ±0.3 µS/cm resulting from the
k25 = (5)
1 + α (T − 25 °C ) difference between conductivity at 25°C and conductivity at
the solution temperature (kT) using equation 10.
where,
k25 - conductivity at 25°C; kT = k 25 x (1 + α (T − 25 ) ) (9)
kT - CRM conductivity measured at temperature T °C;
α25 - temperature coefficient. uT elect = k 25 − kT (10)
The temperature coefficient, α can be calculated by
equation 6 and was taken as 2%/k [19]. The combined effect of the two temperature uncertainty
contributions was calculated as ±0.309 µS/cm using equation
1  kT − k25  11 in which c1 and c2 are the sensitivity coefficients
α 25 =   x 100 (6) calculated as 20.6 µS.cm-1/°C and 1 respectively.
k25  T − 25 °C 

( c1 . uT CRM ) + ( c2 . uT elect )
2 2
From the model in equation 5, explicit sources of the uc (T ) = (11)
uncertainty can be identified as: conductivity of the CRM and
the effect of temperature on the CRM and on the measuring 3.7.2. Uncertainty from the Implicit Sources
electrode. There are also implicit sources of uncertainty that The implicit sources of uncertainty were combined and
come from accuracy and resolution of the conductivity-meter in added as an uncertainty term (∆k) so that its conductivity
addition to the repeatability of measurements. All the sources equals zero but it has an effect on the uncertainty [23, 24].
are illustrated in the fishbone structure shown in Figure 4. Thus the measurement model in equation 5 was modified to
equation 12.

kT
k25 = + ∆k (12)
1 + α (T − 25 °C )

(i). Uncertainty of Resolution of the Conductivity-Meter


Value of the resolution was taken from manual of the
conductivity meter and was divided by 2 to get the
expanded uncertainty Uexp. Then the expanded uncertainty
was divided by √3 to get the standard uncertainty of the
Figure 4. Fishbone structure showing uncertainty sources in conductivity
measurements. resolution (uResol) according to equation 13 assuming a
rectangular distribution.
3.7.1. Uncertainty from the Explicit Sources
Resolution
uR e sol = (13)
(i). Reference Material (CRM) 2 3
The standard uncertainty, uCRM can be calculated by
dividing the expanded uncertainty provided in the certificate (ii). Uncertainty of Accuracy of the Conductivity-Meter
of the CRM by 2 according to equation 7. Accuracy was taken from manual of the conductivity
meter as a percentage value and was divided by √3 to get the
U CRM
uCRM = (7) standard uncertainty (uAccu) according to equation 14. The
2 obtained result was multiplied by the value of the measured
conductivity to get the uncertainty in (µS/cm).
(ii). Effect of Temperature on the CRM
Values of conductivity of the CRM were reported in the Accuracy %
certificate at 20°C and 25°C. The differences in conductivity u Accuracy = (14)
3
(∆EC) and in temperature (∆T) were calculated and the sensitivity
coefficient (ci) was calculated by dividing (∆EC) by (∆T). The ci (iii). Uncertainty Due to the Repeatability of Measurements
was found 20.6 µS.cm-1/°C and was multiplied by the standard In the one-point calibration, conductivity of the CRM
uncertainty u(t) of the calibrated thermometer as in equation 8 to (1410.7 µS/cm) was measured 5 times at 25°C and the
calculate the uncertainty due to the effect of temperature on the uncertainty, urept was obtained by dividing the standard
CRM. The obtained uncertainty was found ±0.11 µS/cm. deviation of the mean by the square root of the number of
measurements (n) using equation 15.
u T = u (t thermometer ) x ci
CRM
(8)
SD
(iii). Effect of Temperature on The Electrode of the Meter
urept = (15)
n
The conductivity at the solution temperature, kT (24.9°C)
215 Adel Bassuoni Shehata et al.: Calibration and ISO GUM Based Uncertainty of Conductivity and TDS Meters for
Better Water Quality Monitoring

The combined standard uncertainty contributions of ∂k25 1


= (17)
accuracy, resolution and repeatability was obtained by ∂kT α (T − 25 °C ) + 1
equation 16 in which c1, c2 and c3 are the sensitivity
coefficients. Each of them equals 1 since they are expressed kT α
∂k25
in the conductivity unit, µS/cm. =− (18)
∂T (α (T − 25) + 1)2
( c3 .uRept )
2
u∆ k = ( c1. u Acc )2 + ( c2 . u Resol )2 + (16)
∂k25
=1 (19)
The results obtained of the three implicit sources of ∂∆k
uncertainty were reported in Table 3. Using these sensitivity coefficients, the combined standard
3.7.3. The Combined Standard Uncertainty of the uncertainty, uc was calculated using equation 20 and the
Conductivity Meter Calibration obtained result was reported in Table 3.
In order to calculate the combined standard uncertainty, 2 2 2
the model equation 12 was differentiated to derive the  ∂k25   ∂k   ∂k 
uc =  . uCRM  +  25 . uT  +  25 . u∆k  (20)
sensitivity coefficients shown in equations 17-19.  ∂kT   ∂T   ∂∆k 
 

Table 3. Uncertainty budget of the calibration of a conductivity-meter.

Standard Probability Sensitivity Contribution to the


Quantity Xi Estimate xi Unit
uncertainty u(xi) distribution coefficient ci ui(y)
CRM 1410.7 1.4 µS/cm Normal 1.0002 1.40028
Effect of temperature 1410.7 0.304 µS/cm Normal -28.21 -8.57422
Resolution 0.29 µS/cm
∆k Accuracy 0 4.07 4.12 µS/cm Normal 1 4.122564
Repeatability 0.58 µS/cm
Combined standard uncertainty, uc 9.62
Expanded uncertainty, Uexp (µS/cm) 19.23 (1.36%)

In the meanwhile, the implicit sources of uncertainty are:


3.7.4. The Expanded Uncertainty (UExp) the repeatability of measurements in addition to the inputs of
The expanded uncertainty was calculated by multiplying the concentration of the KCl solution (mass, purity and volume)
combined standard uncertainty, uc by a coverage factor k=2 to as in equation 1. All these sources are shown in the fishbone
provide a confidence level of about 95% according to equation 21. structure given in Figure 5.
U exp = uc x k (21)

3.7.5. Calibration of the TDS Meter Using the Prepared


KCl Standard Solution
After the one-point calibration of the conductivity meter
using a CRM of conductivity 1410.7 µS/cm, the meter was
reset to the TDS mode and was one-point calibrated by the
standard solution of KCl. The calibrated meter was allowed
to read TDS of the solution 10 times at 25°C and the results
obtained were reported in Table 4.

Table 4. TDS of the KCl standard solution.

TDS (mg/L) 747 – 743 – 742 -746 – 748- 741 – 747 – 745 – 743 - 747 Figure 5. Fishbone structure showing uncertainty sources in TDS
measurements.
Ave 745
SD 2.47
RSD% 0.33 The standard uncertainty of conductivity has been
explained above and was found ±5.86 µS/cm. Uncertainty of
3.7.6. The TDS Calibration Uncertainty the factor f (TDS/k) was estimated as the standard deviation
The mathematical model used for calculation of the TDS is of the average of 5 determinations divided by ˅5 and was
expressed in equation 22 [19]. From this model, the explicit found ±0.00082 mg.L-1/µS.cm-1. The concentration of the
sources of uncertainty can be identified as the conductivity (k) prepared solution was calculated using the mathematical
and the factor f. model in equation 1. From this model, the sources of
uncertainty of the KCl solution concentration can be
TDS = f x k (22) identified as: mass, purity and volume of the solution. The
Science Journal of Chemistry 2022; 10(6): 211-218 216

uncertainty of each of them was estimated as described 2 2 2


u  u  u 
below. uC = C  m  +  p  +  V  (26)
 m   p  V 
(i). Purity (p)
The purity of KCl provided by PanReac was 99.95-100.5% As for the implicit sources of uncertainty, a term ∆TDS
(i.e .100±0.5) and its standard uncertainty up was obtained as including the uncertainty of the concentration of KCl and the
±0.0029 by dividing the value 0.5% by V3. repeatability of measurements was added to the model
equation 22 in condition that its TDS equals zero but it has an
(ii). Mass (m)
uncertainty [23, 24]. Thus the model equation was modified
The uncertainty associated with the mass of KCl was
to equation 27 and the combined uncertainty of both implicit
estimated using equation 23 where um is the mass of sample
sources was calculated according to equation 28 in which c1
multiplied by a calibration factor quoted from the calibration
and c2 are the sensitivity coefficients. Each ci equals 1 since
certificate of the balance. The result was found ±0.0032 mg
both uncertainties are expressed in the TDS unit, mg/L.
u ( m) = 2 x (um )2 (23) TDS = k x f + ∆ TDS (27)

( )
(iii). Volume (V) 2
The uncertainty in the volume of water arises from three
u∆ TDS = ( c1 x uCRM ) + c2
2
x urept (28)
contributions: calibration, repeatability and temperature. The
calibration certificate quotes the expanded uncertainty in In order to calculate the combined standard uncertainty in
volume of the flask used in the preparations of the KCl the TDS calibration results, equation 27 was differentiated to
solution as: ±0.07 mL. The standard uncertainty was obtained obtain the sensitivity coefficients given in formulas 29-31.
as Uexp/2 (±0.035 mL). The effect of volume repeatability Using these coefficients, the combined standard uncertainty,
was estimated by ten fill and weigh experiments of the flask uc was calculated by equation 32.
which gave a standard deviation of 0.024 mL. This was used
∂TDS
directly as a standard uncertainty. Meanwhile, uncertainty of = f (29)
the temperature effect on volume of the flask was calculated ∂k
from equation 24. Since the flask was calibrated at 20°C and
∂TDS
the temperature variation in the laboratory was ±3°C, the =k (30)
volume was multiplied by 3 and by the coefficient of volume ∂f
expansion for water (2.1 x 10-4°C-1).
∂TDS
=1 (31)
uT = (V ) x (limit of T variation ) x (2.1 x 10
−4
) (24) ∂∆TDS

The uncertainty of calibration, repeatability and  ∂TDC 


2
 ∂TDC   ∂TDC
2

2

temperature was combined to give the standard uncertainty of uC =  ∂k . uk  +  ∂f . u f  +  ∂∆TDC . u∆TDC  (32)
     
volume uc (V) as ±3.46 mL according to equation 25.
The expanded uncertainty was calculated using a coverage
( )
2
( c . ucal )2 + + ( c3 . uT )
2
uC (V ) = 1 c6 . urept (25) factor k=2 to provide confidence level of approximately 95%
according to equation 33.
The combined standard uncertainty of the concentration of
U exp = uc x k (33)
the prepared KCl solution resulting from the mass, purity and
volume was estimated by equation 26 and was found ±4.08
The results obtained are shown in Table 5.
mg/L.

Table 5. Uncertainty budget of the calibration of a TDS-meter.


Estimate Standard Probability Sensitivity Contribution to the
Quantity Xi Unit
xi uncertainty u(xi) distribution coefficient ci ui(y)
conductivity 745 9.6 µS/cm Normal 0.52 4.99
Factor f 0.52 0.00084 mg.L-1/µS.cm-1 Normal 1410.2 1.185
TDS Soln 3.46 mg/L
∆TDS 0 4.80 Normal 1 4.80
Repeatability 1.16 mg/L
Combined standard uncertainty 7.05
Expanded uncertainty (µS/cm) 14.09 (1.89%)

The calculated expanded uncertainty in the concentration of plotted as shown in Figure 6. The figure shows that the 10
the KCl solution (±6.92 mg/L) was added and subtracted from measured TDS values lie within the expanded uncertainty
the average TDS (745 mg/L) shown in Table 4 to establish the limits of the TDS of the KCl solution indicating a very good
uncertainty limits within which the measured TDS values were traceability of the calibration results to the SI units.
217 Adel Bassuoni Shehata et al.: Calibration and ISO GUM Based Uncertainty of Conductivity and TDS Meters for
Better Water Quality Monitoring

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