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ICAR AICE-JRF/SRF Food Analysis: Proximate, Chemical & Instrumental Methods: practice questions

ICAR AICE-JRF/SRF (PhD) — Food Processing Technology, Food Safety & Quality, Processing and Food Engineering · India · ICAR through the National Testing Agency

Original practice questions written to the published syllabus · not past papers
10worked here, free
69written to this exam in this subject
15syllabus units

What this subject covers

How a food laboratory measures what is in a food: sampling, proximate analysis, official methods, and the instruments — spectroscopy, chromatography, mass spectrometry and electrophoresis — that a food analyst runs. It is the core of the food analyst qualification in countries that license analysts.

In the exams: ICAR AIEEA-PG Code 18 Unit I (modern analytical techniques in food analysis); ICAR AICE 35.b Unit 6 (research techniques); core of food analyst examinations

What ICAR AICE-JRF/SRF asks from it

ICAR AICE-JRF/SRF (PhD) — Food Processing Technology, Food Safety & Quality, Processing and Food Engineering

35.b Unit 6 names spectroscopy (visible, IR, UV), chromatography (TLC, GLC, HPLC, gel filtration, ion exchange, affinity), electrophoresis (PAGE, SDS-PAGE), isoelectric focusing, ultracentrifugation and potentiometry; 35.b Unit 1 names ISO/IEC 17025 and NABL accreditation. Expect deeper questions on MS/MS, matrix effects, validation statistics and quality control.

Where the 69 questions fall

How our questions for ICAR AICE-JRF/SRF spread across the units of Food Analysis: Proximate, Chemical & Instrumental Methods. Difficulty: 5 easy, 49 medium, 15 hard.

Method validation and quality control in the analytical laboratory11
UV-visible, fluorescence and infrared spectroscopy7
Mass spectrometry and hyphenated techniques7
Vitamin analysis6
Chromatography: TLC, GC and HPLC6
Electrophoresis and immunoassays: SDS-PAGE and ELISA6
Carbohydrates, sugars and dietary fibre5
Atomic absorption and ICP spectroscopy5
Moisture and total solids3
Protein: Kjeldahl and Dumas methods3
Sampling and sample preparation2
Official methods and method compendia: AOAC, ISO and national manuals2
Ash and mineral analysis2
Fat: Soxhlet, Mojonnier and Gerber methods2
Physical tests: pH, titratable acidity, refractometry and colour2

10 practice questions, worked

Choose an answer, then open the working. Each explanation says why the right answer is right and why the others are not.

1 · Official methods and method compendia: AOAC, ISO and national manuals · medium

In the Codex classification of methods, a Type I (defining) method is one that

  1. is a tentative method that has not yet been fully validated
  2. is any method that meets performance criteria
  3. is used only in disputes as a reference
  4. defines a value obtainable only by that method
Answer and working

D. defines a value obtainable only by that method

Type I defines the value (e.g. some empirical methods); Type II is reference; Type III alternative approved; Type IV tentative.

Further reading: Codex CXS 234, General Standard for Methods of Analysis and Sampling

2 · Moisture and total solids · medium

Karl Fischer titration is preferred for low-moisture products because it

  1. measures all volatile compounds as water
  2. needs no reagents at all
  3. measures water specifically
  4. works only above 50 % moisture
Answer and working

C. measures water specifically

The iodine–sulphur dioxide reaction is specific to water; oven methods count all volatiles.

Further reading: Nielsen (ed.), Food Analysis

3 · Vitamin analysis · medium

Before HPLC of vitamins A and E in fatty foods, samples are usually

  1. saponified
  2. ashed at 550 °C
  3. digested with sulphuric acid
  4. fermented with yeast
Answer and working

A. saponified

Alkaline saponification removes triglycerides and releases the vitamins for extraction.

Further reading: Nielsen (ed.), Food Analysis

4 · UV-visible, fluorescence and infrared spectroscopy · medium

Near-infrared analysers for grain protein rely on

  1. a single absorption band unique to protein in every grain sample
  2. direct measurement of nitrogen atoms
  3. multivariate calibration against reference methods
  4. the Beer–Lambert law with no calibration
Answer and working

C. multivariate calibration against reference methods

NIR bands overlap, so chemometric models (e.g. PLS) are built from samples analysed by Kjeldahl or Dumas.

Further reading: Nielsen (ed.), Food Analysis

5 · UV-visible, fluorescence and infrared spectroscopy · medium

In UV-visible spectrophotometers, the lamp used for the ultraviolet region is usually a

  1. tungsten lamp
  2. sodium lamp
  3. hollow-cathode lamp
  4. deuterium lamp
Answer and working

D. deuterium lamp

Deuterium for UV, tungsten-halogen for visible; hollow-cathode lamps are for AAS.

Further reading: Skoog, Holler and Crouch, Principles of Instrumental Analysis

6 · Atomic absorption and ICP spectroscopy · medium

Mercury is commonly determined by

  1. flame emission photometry
  2. Soxhlet extraction
  3. biuret colorimetry
  4. cold-vapour atomic absorption
Answer and working

D. cold-vapour atomic absorption

Mercury is reduced to elemental vapour and measured without a flame; hydride generation is used for arsenic and selenium.

Further reading: Skoog, Holler and Crouch, Principles of Instrumental Analysis

7 · Chromatography: TLC, GC and HPLC · medium

In reversed-phase HPLC on a C18 column with water–methanol, the compounds that elute first are

  1. the most polar
  2. the most non-polar
  3. the largest
  4. the most volatile
Answer and working

A. the most polar

Polar compounds interact weakly with the non-polar stationary phase and elute early.

Further reading: Skoog, Holler and Crouch, Principles of Instrumental Analysis

8 · Electrophoresis and immunoassays: SDS-PAGE and ELISA · medium

Sandwich ELISA is suited to food allergens because allergenic proteins

  1. are too small to bind any antibody
  2. have at least two antibody-binding sites
  3. are volatile and leave the sample
  4. fluoresce strongly
Answer and working

B. have at least two antibody-binding sites

Capture and detection antibodies bind different epitopes of the large protein.

Further reading: Nielsen (ed.), Food Analysis

9 · Method validation and quality control in the analytical laboratory · hard

A blank's standard deviation is 0.02 absorbance units and the calibration slope 0.5 absorbance per mg/L. Using LOQ ≈ 10σ/S, the limit of quantification is

  1. 0.132 mg/L
  2. 0.01 mg/L
  3. 0.40 mg/L
  4. 2.50 mg/L
Answer and working

C. 0.40 mg/L

LOQ = 10 × 0.02/0.5 = 0.40 mg/L. 0.132 is the LOD (3.3σ/S); 0.01 multiplies σ by S; 2.50 inverts.

Further reading: Eurachem, The Fitness for Purpose of Analytical Methods

10 · Method validation and quality control in the analytical laboratory · medium

In India, laboratories testing food for regulatory purposes are commonly required to be accredited by

  1. UKAS to ISO 9001
  2. BIS to ISO 22000
  3. FSSAI to Codex Type I methods
  4. NABL to ISO/IEC 17025
Answer and working

D. NABL to ISO/IEC 17025

NABL is India's accreditation body for testing and calibration laboratories under ISO/IEC 17025.

Further reading: Eurachem, The Fitness for Purpose of Analytical Methods

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Read the subject

Food Analysis: Proximate, Chemical & Instrumental MethodsThe full study manual, free ICAR AICE-JRF/SRFFormat, sections and how it has changed

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Food Analysis: Proximate, Chemical & Instrumental Methods for other exams

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