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Analytical instruments

Instrumentation and Control Engineering (B.E./B.Tech) · Sensors and measurement · free study notes for exams, placements and interviews

In short

Analytical instruments measure the composition of a sample - which species are present and how much - instead of a physical quantity like temperature or pressure. They work by exciting the sample with light, heat, an electric field or a carrier gas and measuring a response that depends on concentration: absorbance, electrode potential, conductivity, thermal conductivity or ion mass. In Indian industry they run refinery and fertiliser process control, continuous emission monitoring for CPCB/SPCB consent conditions, drinking-water testing to IS 10500, pharmaceutical QC under Schedule M, and food testing under FSSAI. The topic carries steady marks in Instrumentation and Measurement papers and in GATE IN (analytical instrumentation, spectroscopy, chromatography, pH and conductivity), and is asked at interviews for Thermax, Forbes Marshall, ABB, Emerson, Yokogawa, Siemens, Agilent, Shimadzu, Thermo Fisher, Chemtrols and the public-sector refineries.

Explained

Classification and the general measurement chain

Electrochemical analysers - pH, ORP, conductivity, ISE, oxygen

Optical and spectroscopic analysers

Chromatography and mass spectrometry

Other process analysers and physical-property instruments

Indian standards, statutes and practice

Key points

Formulas and examples

A = log₁₀(I₀/I) = ε c l - A absorbance (dimensionless), I₀ incident and I transmitted intensity, ε molar absorptivity (L·mol⁻¹·cm⁻¹), c concentration (mol/L), l path length (cm). Transmittance T = I/I₀; A = −log₁₀T; %T = 100T.
pH = −log₁₀ aH⁺; E = E₀ + (2.303RT/nF)·log₁₀ aH⁺ = E₀ − S·pH, with slope S = 2.303RT/F = 0.1984 × T(K) mV/pH (= 59.16 mV/pH at 298 K); R = 8.314 J/mol·K, F = 96,485 C/mol.
Conductivity κ = G·K = (1/R)(L/A) S/cm; cell constant K = L/A (cm⁻¹); resistivity ρ = 1/κ (Ω·cm); TDS (mg/L) ≈ f × κ(µS/cm), f ≈ 0.5-0.7.
Zirconia cell: E = (RT/4F)·ln(p_ref/p_meas) V ≈ 0.0496 × T(K) × log₁₀(p_ref/p_meas) mV.
Plates N = 16(tR/W)² = 5.54(tR/W½)²; HETP = L/N; Resolution R = 2(tR2 − tR1)/(W1 + W2); van Deemter HETP = A + B/u + Cu.
Magnetic-sector MS: qV = ½mv², Bqv = mv²/r → m/q = B²r²/(2V); r = (1/B)√(2Vm/q).
Detection limit CL = 3σ_blank / S, where S is the calibration slope (signal per unit concentration).
Emissions: C(mg/Nm³ at reference O₂) = C_measured × (21 − O₂_ref)/(21 − O₂_measured).

Example 1 - Beer-Lambert law and transmittance. A solution in a 1 cm cell transmits 25% of the incident light at 540 nm; ε = 6,000 L·mol⁻¹·cm⁻¹. Find the concentration, and the absorbance if the path is increased to 4 cm.

Example 2 - pH electrode slope and temperature error. A pH meter calibrated at 25 °C (59.16 mV/pH, isopotential pH 7) is used without ATC on a sample at 80 °C whose true pH is 10.00.

Example 3 - Conductivity cell and cell constant. A cell has electrodes of area 0.80 cm² spaced 1.60 cm apart; immersed in a sample it reads 4.50 kΩ.

Example 4 - GC column efficiency and resolution. On a 25 m capillary column, peak 1 has tR = 4.00 min with base width 0.20 min and peak 2 has tR = 4.50 min with base width 0.25 min.

Example 5 - Stack SO₂ corrected to reference oxygen. A CEMS reads SO₂ = 420 mg/Nm³ (dry) at a measured 9.0% O₂; the consent condition is in mg/Nm³ at 6% O₂ reference.

AnalyserPrincipleMeasuresStrengthLimitation
NDIRIR band absorptionCO, CO₂, CH₄, SO₂, NOSelective, no consumablesBlind to O₂/N₂/H₂; H₂O interference
ZirconiaNernst potential across hot ZrO₂O₂ in flue gasIn-situ, fast, cheapDamaged by unburnt fuel; heated cell
ParamagneticO₂ magnetic susceptibilityO₂ (any gas stream)No consumables, robustVibration-sensitive, costlier
pH glass electrodeMembrane potentialH⁺ activityWide range, directFragile, high impedance, alkaline error
ConductivityIonic conductionTotal ionic contentSimple, ruggedNon-specific; needs T compensation
GC-TCD/FIDPartition then detectionFull gas compositionMulti-component, high accuracyDiscontinuous, minutes per cycle
GC-MSSeparation + m/zTrace identificationUnambiguous ID, ppbCostly, lab-based, high vacuum
UV-Vis spectrophotometerBeer-Lambert absorptionColoured/UV-active solutesCheap, fast, quantitativeNeeds reagents; interference, A < 2
AASAtomic line absorptionHeavy metalsppb sensitivityOne element per lamp; flame gases

Where it is used

Interview questions

Common mistakes

Related topics

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