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AS/OCT 2007/CHM561

UNIVERSITI TEKNOLOGI MARA FINAL EXAMINATION

COURSE COURSE CODE EXAMINATION TIME

: : : :

QUALITY IN ANALYTICAL MEASUREMENT CHM561 OCTOBER 2007 3 HOURS

INSTRUCTIONS TO CANDIDATES 1. This question paper consists of two (2) parts : PART A (6 Questions) PART B (5 Questions) Answer ALL questions from PART A and four (4) questions from PART B in the Answer Booklet. Start each answer on a new page. Do not bring any material into the examination room unless permission is given by the invigilator. Please check to make sure that this examination pack consists of: i) ii) the Question Paper an Answer Booklet - provided by the Faculty

2.

3.

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DO NOT TURN THIS PAGE UNTIL YOU ARE TOLD TO DO SO

This examination paper consists of 4 printed pages
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AS/OCT 2007/CHM561

PART A

QUESTION 1

Sampling is important in analytical procedure in order to obtain a meaningful and valid result. Describe the sampling plan procedure one must follow to ensure he will collect the proper sample for analysis. (3 marks) QUESTION 2 Suggest three sample pretreatments for sediment sample. (3 marks) QUESTION 3 Explain four factors involved in selecting a method for analysis. (4 marks) QUESTION 4 Chemical standards and standard reference materials are important in chemical analysis to obtain quality results. Differentiate between chemical standard and standard reference material. (3 marks) QUESTION 5 What important information is included in a "chain-of-custody" procedure? (4 marks) QUESTION 6 a) Name one type of air/water/soil sampler. (1 mark) b) State two important features of the specified sampler. (2 marks)

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PARTB

QUESTION 1 Measurement uncertainty characterizes the range of values within which the true value is asserted to lie, with a specified level of confidence. Every measurement has an uncertainty associated with it, resulting from errors arising in the various stages of sampling and analysis and from imperfect knowledge of factors affecting the result. For measurements to be of practical value it is necessary to have some knowledge of their reliability or uncertainty. A statement of the uncertainty associated with a result conveys to the customers to 'quality' of the result. Discuss a good practice in the evaluation of measurement uncertainty in relation tolSO/lEC 17025:1999. (10 marks)

QUESTION 2 Method validation is carried out to ensure the performance characteristics of a method and to demonstrate that the method is scientifically sound under the conditions in which it is to be applied. Choose five important performance characteristics and explain why they are important. (10 marks) QUESTION 3 Mr Mamat is a senior chemist and a manager of an established Analytical Laboratory in this country. He practices the quality systems and quality systems documentation. a) Write a short note on quality systems documentation. (4 marks) b) Explain the GLP requirement on quality systems documentation. (6 marks) QUESTION 4 a) In the determination of cadmium in Sungai Selangor, a student used a primary standard for analysis using flame atomic absorption spectrometry. Give your comment on the validation of analytical method and suggest how it can be improved. (6 marks) Discuss the inter-laboratory comparison exercise in relation to the method validation. (4 marks)

b)

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AS/OCT 2007/CHM561

QUESTION 5 Sediment samples were taken from 8 ponds from a total of 25 sampling locations. Pond A3 was chosen for sampling due to its position (adjacent to a pond with elevated mercury) and changing water levels (may be managed as a seasonal pond). Pond A2E was chosen due to the elevated Hg levels in tissues detected. Pond A5, A6 and A7 were chosen for sampling due to their positions (adjacent to ponds with elevated mercury levels). Sediment samples will be collected from the bottom of ponds with a 2-1/4" diameter AMS sediment sludge sampler near the shore water interface. Six samples will be submitted for analysis from each pond, three from the surface (0-2 inches) and the other three at depth (6-8 inches). Upon completion of each sample collection, the sediment sample will be directly placed in an ice chest and cooled to 4 C. a) Discuss the sampling approaches involved in the above study. (6 marks)

b)

Suggest the labeling and storage procedures for the samples. (4 marks)

END OF QUESTION PAPER

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