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Royal Society of Chemistry Mastership in Chemical Analysis (MChemA) Examiners’ report 2019 Jane White (Chief Examiner) Liz Moran Alastair Low Megan McLean Introduction This is the annual report of the Examiners for the Mastership in Chemical Analysis for the year ending 31 December 2019. These general comments are intended for candidates and their counsellors, to help them understand the expectations of the examiners and to aid their preparations for the MChemA. The MChemA Regulations, Syllabus and Guidance Notes can be found on the RSC website at http://rsc.li/mchema. Part A One candidate sat this paper achieving a pass mark. The candidate demonstrated an acceptable range and depth of knowledge answering questions 2, 4-7 on topics of gas chromatography, atomic spectroscopy, solid phase extraction, ELISA, Kjeldahl and Karl Fisher titrations and data analysis. The questions were designed to probe basic understanding of the underpinning theory of the techniques together with their applications and results interpretation. Part B Two candidates sat the examination in October 2019; both candidates sat both papers. One candidate had sat both Part B papers in 2018. Paper B1 Of the eight questions set, two questions were not attempted by either of the candidates. One question asked the candidates to detail the legislation relating to fruit juice and nectars. The Fruit Juices and Fruit Nectars (England) Regulations 2013 define juices and nectar and set specific standards that they should meet. However, reference should be made to other relevant legislations such as the Contaminates in Foods (England) Regulations 2013 and EC 1881/2006 which sets limits for patulin in apple juice and ochratoxin A in grape juice.

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Royal Society of Chemistry

Mastership in Chemical Analysis (MChemA)

Examiners’ report 2019

Jane White (Chief Examiner)

Liz Moran

Alastair Low

Megan McLean

Introduction

This is the annual report of the Examiners for the Mastership in Chemical Analysis for the

year ending 31 December 2019. These general comments are intended for candidates and

their counsellors, to help them understand the expectations of the examiners and to aid their

preparations for the MChemA.

The MChemA Regulations, Syllabus and Guidance Notes can be found on the RSC website

at http://rsc.li/mchema.

Part A

One candidate sat this paper achieving a pass mark. The candidate demonstrated an

acceptable range and depth of knowledge answering questions 2, 4-7 on topics of gas

chromatography, atomic spectroscopy, solid phase extraction, ELISA, Kjeldahl and Karl

Fisher titrations and data analysis. The questions were designed to probe basic

understanding of the underpinning theory of the techniques together with their applications

and results interpretation.

Part B

Two candidates sat the examination in October 2019; both candidates sat both papers. One

candidate had sat both Part B papers in 2018.

Paper B1

Of the eight questions set, two questions were not attempted by either of the candidates.

One question asked the candidates to detail the legislation relating to fruit juice and nectars.

The Fruit Juices and Fruit Nectars (England) Regulations 2013 define juices and nectar and

set specific standards that they should meet. However, reference should be made to other

relevant legislations such as the Contaminates in Foods (England) Regulations 2013 and EC

1881/2006 which sets limits for patulin in apple juice and ochratoxin A in grape juice.

The second part asking the candidates to explain how fruit juice drinks should be analysed.

The question is for a juice drink and as such is not covered by the juice and nectar

regulations. The candidates should discuss the issues associated with this type of product.

The second question related to how novel foods are authorised. The candidate should

reference The Novel Foods (England) Regulations 2018 (The Novel Foods (Scotland)

Regulations 2017) and (EU) 2015/2283 discussing the approve system in general and the

requirement for a food to be on the EU approved list prior to the food being placed on

the market.

The second part of the question asked what the status and requirements are for Chia seeds,

CBD oil, Geranium and Raspberry ketones.

Below is an example of the entry for Chia seeds from EU Novel food catalogue

The Commission Decision 2009/827/EC authorised the placing on the market of Chia (Salvia

hispanica) seeds as a novel food ingredient, to be used in bread products with a maximum

content of 5 % Chia (Salvia hispanica) seeds. The Commission Implementing Decision

2013/50/EU has authorised an extension of the use of Chia seed -no more than 10% -in

baked products, breakfast cereals, fruit nut and seed mixes, and the marketing of pre-

packed chia seeds. Additional labelling of pre-packaged Chia seeds is required to inform the

consumer that the daily intake is no more than 15 g/day. Chia seed as such may be sold to

the final consumer in a pre-packaged form only. The authorisation letter from Ireland (18

September 2015) has authorised an extension of the use of Chia seeds in fruit juices and

fruit juice blends. Chia (Salvia hispanica) is a summer annual herbaceous plant belonging to

the Labiatae Family. The species originated in mountainous areas extending from West

Central Mexico to Northern Guatemala. Chia seeds require sub-tropical conditions for their

growth.

A synopsis of the requirements for use should be given.

Question 1 asked candidates to discuss unregulated mycotoxins. In particular the methods

of analysis and how the results would be interpreted. EC 1881/2006 sets limits for certain

commodities and mycotoxins. The question was looking for candidates to discuss the

analysis for a range of mycotoxins and how the analyst would interpret results where no

limits are set. The candidate should have made reference to using EFSA recommendation,

WHO, Codex or other sources information sources. They may have discussed toxicity data

and conversion to daily acceptable levels. The second part of the question asked how you

would analyse for marine biotoxins and how the results would be interpreted. Although not

many labs are accredited for biotoxins, a Public Analyst should have an understanding of the

subject as they may subcontract samples for this analysis. An understanding of the different

types of biotoxins would be expected with a basic understanding of the methods of analysis.

Question 2a asked the candidates to identify the compositional standards for dairy product and explain the analysis required for official controls. The answers should address the compositional standards for all dairy products and should include reference to EC No

1234/2007, EC 835/2004, Code of practice on the compositional standards for cream

designation in the UK, Code of practice on the compositional standards for cheese designation in the UK and Code of practice on edible ices,

Question 2b asked how you would analysis for fat in different types of dairy products ie milk,

yogurt and cheese. The candidate should discuss the use of Gerber fat, Rose Gottlieb, Acid

hydrolysis method and the determination of milk fat from butyric acid content.

Question 4 asked the candidates to discuss the legislation, standards and analysis for 4

products:- Fresh tuna, whisky based liqueur, Steak and kidney pie and Cereal based snacks.

The candidates were expected to think passed the obvious and ideally be aware of ongoing

issues particularly with fresh tuna. OPSON has looked at the use of unpermitted additives in

tuna as well as histamine, freshness and speciation. The candidates were also require to

understand the definitions of a liqueur from the Spirit Drink Regulations 2008 (110/2008) and

definitions in The Products Containing Meat etc Regulations 2014. The cereal based snacks

required discussion around testing for GMO, nutritional analysis, health and nutritional

claims if were declared.

Question 5a asked the candidates to identify three foods which are not required to bear a

list of ingredients. The candidates should state that EU 1169/2011 Article 19 lists foods that

do not require an ingredients list. The foods that are exempt should be listed along with any

criteria that must be met to qualify for the exemption.

Question 5b asked candidates to state the specific provisions concerning the indication of

ingredients by descending order of weight for four categories of ingredient:

i. Added water and volatile products

ii. Mixtures of spices or herbs, where none significantly predominates

iii. Ingredients constituting less than 2% of the finished product

iv. Refined oils

The candidates should be aware of the requirements of Annex VII of 1169/2011 and how

they would affect the ingredients list

Question 5c asked the candidate to summarise the presentation requirements for the

mandatory particulars as prescribed by these Regulations. The candidate should make

reference to the requirements within 1169/2011 and any appropriate guidance documents.

Question 6a asked the candidate to outline the relevant legislation and guidance that covers the microbiological safety of food. The Microbiological Criteria Regulation 2073/2005 establishes microbiological criteria for certain micro-organisms and provides rules to be complied with by food business operators. The candidates should also reference HPA Guidance for Food Examiners and The safety and shelf-life

of vacuum and modified atmosphere packed chilled foods with respect to non-proteolytic Clostridium botulinum.

Question 6b

The candidate was asked what examinations would applied to Raw milk cheese, Rice based

food, vacuum packed food and a cooked sliced meat

Consideration should have been given to

EC2073/2005 end of manufacture

EC2073/2005 during shelf-life

HPA guidelines

Vacuum packed guidance.

Question 7 asked the candidate to give an outline of the relevant legislation which governs

the presence of acrylamide in food and to include in the answer its formation, health effects,

methods of analysis and ways of controlling acrylamide in one chosen product type.

In 2015 the Scientific Panel on Contaminants in the Food Chain (CONTAM) of the European

Food Safety Authority (‘the Authority’) adopted an opinion on acrylamide in food (4). Based

on animal studies, the Authority confirms previous evaluations that acrylamide in food

potentially increases the risk of developing cancer for consumers in all age groups. Since

acrylamide is present in a wide range of everyday foods, this concern applies to all

consumers but children are the most exposed age group on a body weight basis.

Regulation 2017/2158 establishes best practice, mitigation measures and benchmark

levels for the reduction of the presence of acrylamide in food. The regulations also give

the performance criteria required for methods of analysis.

Paper B2

Both candidates attempted paper B2. Only one question was not attempted and this was

question asked the candidates to discuss the method validation requirements for the

analysis of anions in potable waters using ion chromatography for 20 marks. Method

validation is an essential activity within any laboratory and ensuring methods are fit for

purpose an integral role of the Public Analyst. The principles of method validation include

ascertaining the level of interest from the client or in this case from legislation - The Water

Supply (Water Quality) Regulations 2016. Carrying out a literature search to determine what

methods maybe appropriate if one is not indicated in the legislation. Establishing

performance criteria from legislation if appropriate. Carrying out appropriate analysis of

spikes, certified reference material, blanks etc. in appropriate matrixes. Evaluation of

method/s against the performance criteria identified. The Drinking Water Inspectorate

indicates minimum requirements for replicates, spikes etc. Relevant guidance documents,

such as the Drinking water inspectorate guidance document and Accreditation Requirements

for Sampling and Testing in Accordance with the Drinking Water Testing Specification

(DWTS) should be referenced.

Question 1 (Policy) asked the candidates to discuss the current policy on the interpretation

of the results of food allergen analysis in light of recent food incidents and include your

opinion(s) on how allergen management and the presentation of information should be

developed in food preparation and service environments. Due to recent high profile incidents

there has been a number of consultations on current allergen labelling. The question

prompts candidates to discuss how results are interpreted including where current legislation

stipulates limits such as those for sulphur dioxide and gluten and the issues surrounding

interpretation were no legislative limit is give. Is VITAL an acceptable approach? Should

every food require an ingredient list? The candidate is asked to discuss the topic in a logic

and informed manner expressing a coherent argument for their options regarding the future

policies for allergen labelling.

Question 2 (Policy) asked the candidates to discuss the threat to food authenticity in a

worldwide food supply chain in relation to the FSA mission statement - “Our job is to use our

expertise and influence so that people can trust the food they buy and eat is safe and what it

says it is.” Our food comes from a worldwide market where food supply chains are varied

and sometime very complex. The threat to food authenticity may come from different

sources such as deliberate adulteration, cross contamination, differing legislative standards

etc. Whatever the cause consumers maybe disadvantage or worse still have their health

compromised. The question invites discussion of the issues associated with an extended

food chain. The candidate should explore the opportunities for adulteration, why it may occur

along with how adulteration may be detected and the solutions that could be used to mitigate

the issues such as the use of blockchain, DNA tracking or other possible solutions.

Question 3a (Agriculture) asked the candidate to outline one method of analysis for each

of the different forms of nitrogen in a fertiliser. The Fertilisers (Sampling and Analysis)

Regulations 1996 Schedule 2 sets out the methods of analysis to be used for fertilisers.

Methods for different types of nitrogen stipulated in the regulations should be outline

Question 3b (Agriculture) asked the candidate to discuss the preparation of different types

of solid fertiliser for analysis. . The Fertilisers (Sampling and Analysis) Regulations 1996

Schedule 2 outline how different types of fertilisers should be prepared. This includes what

samples should not be ground.

Question 4 (Agriculture) asked candidates to outline the main provisions of Regulation EC

767/2009 regarding the placing on the market and use of animal feeding stuffs for 20 marks.

A good working knowledge of Regulation (EC) No 767/2009 is essential for a future Agricultural Analyst. The candidate was expected to outline the main provisions of the legislation. The basic principle that feed should be safe and does not have a direct adverse effect on the environment or animal welfare is the fundamental. Furthermore it should be sound, genuine, unadulterated, fit for its purpose and of merchantable quality; and labelled, packaged and presented in accordance with the provisions laid down in this Regulation and other applicable Community legislation. The regulations outline the mandatory labelling requirements for feed material and compound feeds. These are covered in articles 15, 16, 17 and 18. Annex 1 to 6 should be outline including the technical provisions, prohibited materials, permitted tolerances required for nutritional declarations and the labelling requirements for additives.

Question 5a (Agriculture) asked the candidates to discuss the issues associated with the

onsite sampling of bulk feed, on farm mixes and mineral feeds. EC regulation No

152/2009 outlines the requirements for sampling. However the candidate would be expected

to discuss practical issues associated sampling as well as the requirements of the

regulations.

Question 5b (Agriculture) asked the candidate to discuss how you would assess the

quality of forage feed. The candidate should define a forage feed and the feed value it brings

as well as what affects it quality.

Question 6 asked candidates to outline the official methods of analysis for Phosphorus soluble in neutral ammonium citrate in a NPK fertiliser, Magnesium in a fertiliser, Starch in an animal feed,Oil in an animal feed and Claviceps purpurea in a feed material. The fertiliser methods are stipulated in The Fertilisers (Sampling and Analysis) Regulations 1996. The animal feeds methods are given in The Feed (Sampling and Analysis and Specified Undesirable Substances) (Scotland) Regulations 2010 enacting 152/2009. These regulations provide methods for a starch and oil in feeds. Claviceps purpurea The examination is performed in cereals. Quantification is performed by selecting and weighing of ergot and its fragments with a

particle size > 0,5 mm out of the test sample or an aliquot of it.

Question 8a asked the candidate what are the treatments permitted on natural mineral water. The Natural Mineral Water, Spring Water and Bottled Drinking Water (England) Regulations 2007 set out the treatments that are permitted on a natural mineral water.

Question 8b asked the candidates to discuss what indicator analytes may be used to

determine the source of water discovered in a residential basement? The candidates were

asked to include the challenges in interpreting the results. The answer should include a

discussion of the different types of water that may be present and their unique

characteristics. This would inform the analysis that is carried out to determine the source of

the water. However consideration has to be given to the material the water may have passed

through and how this would have affected the results.

.

Part C

One candidate sat the examination in 2019.

Question 1 was not completed by the candidate. The question asked the candidate to

interpret results obtained for the analysis of Melamine Bowls for Formaldehyde. The

candidate had to determine if the results of the replicates constituted a fail and report

appropriately.

Question 2 asked the candidate to write a certificate for a PK fertiliser 0-5-14 containing

magnesium. The results of analysis and declared values were given. The candidate had to

take into account the different permitted tolerance and determine if the name of the feed was

correct

Question 3 asked to candidate to write a certificate of analysis for a Pure Palm Oil. The oil

was found to contain Sudan 4 and salt.

Microscopy

Candidates are reminded that they should visually inspect the whole specimen prior to

commencing analysis. A written description of the material should be given. The object

should then be examined using a low powered microscope. Any distinctive features should

be noted. If the specimen is comprised of more than one material, the material should be

separated prior to examination under a high powered microscope. Candidates should label

the individual slides and produce labelled drawings of the distinguishing features found.

Question 4 asked the candidate to identify a material found in a jar of ‘Black bean cook-in

sauce‘. The material did not have any distinguishing features.

Question 5 asked the candidate to identify a material found in an unlabelled container within

a shop. They material was liquorice root.

Question 6 asked the candidate to identify unexplained material collecting on surfaces in a

house. The specimen was comprised of material produced from a carpet which had started

to degrade.

Interactive

Question 7 asked the candidate to examine a bagged sliced bread which had been sampled

following a complaint of an unusual taint. The candidate was asked to investigate the issue

and report their findings. The hot bread had been placed on new pine cooling boards and

the taint originated from the terpenes released from the wood.

Question 8 asked the candidates to investigate a report of an alleged illness has been

received from a member of the public after consumption of a vegetarian takeaway meal. The

meal comprised of a meat dish, dhal and rice. The dhal contained significant levels of

bacillus cereus.

J. White

Chief Examiner

8 January 2020