Health and Safety

Executive

Measurement of oil mist from mineral

oil-based metalworking fluids
Laboratory method using inhalable sampler and gravimetric
analysis
Scope
MDHS84/2
1 This method describes a gravimetric procedure for the measurement of time-
weighted average concentrations of oil mist. Oil mist may be formed from mineral
oil used as a coolant or lubricant during the machining of metal components. It is
applicable to aerosol formed by mineral oils with viscosities greater than 18 mm2 s-1
(or centi-Stokes, cSt) at 40 °C. Lower viscosity oils contain a greater proportion of
volatile components. The aerosol of a low viscosity oil may be unstable and lose
volatile constituents while trapped on a filter during air monitoring, consequently the
gravimetric analysis may underestimate the original airborne aerosol concentration
in these samples.

Summary
2 A measured volume of air is drawn through a pre-weighed filter mounted in an
inhalable dust sampler. The filter is reweighed to determine the mass of inhalable
aerosol deposited on the filter.

3 If the inhalable particulate concentration is greater than half of any specified

target value, it is recommended that the filter should be further extracted in
cyclohexane to remove any contribution from any potential interferences deposited
on it, by reweighing the filter after extraction.

4 The use of alternative methods not included in the MDHS series is acceptable
provided they can demonstrate the accuracy and reliability appropriate to the
application.

Recommended sampling
5 Sampling should be carried out as described in MDHS141 for inhalable dusts
for 2 to 8 hours with a recommended minimum sample volume of 240 litres at 2
litres per minute.

Prerequisites
6 Users of this method will need to be familiar with the content of MDHS14.1

Methods for the

Safety
Determination of 7 Users of this method should be familiar with standard laboratory practice and
Hazardous Substances carry out a suitable risk assessment. It is the user’s responsibility to establish
Health and Safety appropriate health and safety practices and to ensure compliance with regulatory
Laboratory requirements.
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Executive

Equipment
8 An inhalable dust sampler, pre-cleaned as specified by the manufacturer: An
IOM sampler operated as described in MDHS141 has been found suitable.

9 Binder-free glass fibre or mixed cellulose ester membrane filters (0.8 μm mean
pore diameter). A 25 mm glass fibre GF/A filter has been found to be suitable for
use with the IOM sampler.

10 Personal sampling pumps that meet the requirements of BS EN 13137.2

11 A portable flow meter calibrated against a primary standard, with a

measurement uncertainty typically less than ±2%.

12 Flexible plastic tubing for making a leak-proof connection from the sampling
train to the pump; belts or harnesses to facilitate attachment of sampling apparatus
to subjects; flat-tipped tweezers for loading and unloading the filters into sampler
cassettes.

Laboratory apparatus and reagents

13 During the analysis, use only reagents of a recognised analytical grade.

14 Cyclohexane (>99.5% purity).

15 A microbalance calibrated against a primary standard, capable of weighing to

a precision of 10 μg or better.

16 A selection of laboratory glassware including beakers, measuring cylinders

and covered Petri dishes cleaned with acetone and dried.

Preparation and sampling

17 Load the filters in a clean dust-free environment into clean filter cassettes with
the flat tipped tweezers and allow equilibration with laboratory air overnight before
weighing. Wear disposable gloves to assemble the filter cassettes to avoid
contamination from the hands.

18 Weigh the filter cassettes and place in their transport clips or load into the
inhalable dust sampler and cap with the protective covers.

19 Set aside a minimum of six pre-weighed filter cassettes to be used as blanks.

Where more than forty samples are taken, a minimum of three blank filters should
be used for every twenty samples. Ensure that the blanks are treated in the same
way as the samples but without drawing air through them.

20 Sampling should be carried out in accordance with the procedures described

in MDHS141 for inhalable dust.

21 Select a suitable sampling time, such that the filter does not become
overloaded with aerosol (An 8-hour time-weighted average concentration may be
derived from the results for two or more consecutive samples).

22 Connect each sampler, excluding the blanks, to a sampling pump using

plastic tubing, ensuring that no leaks can occur and set the flow rate using the
calibrated flow meter.
Measurement of oil mist from mineral oil-based metalworking fuids Page 2 of 5
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23 Attach the sampler in the breathing zone of the subject within 200 mm of the
mouth and nose.

24 When ready to begin sampling, remove the protective cover from the sampler,
switch on the pump and check and adjust the flow rate if necessary.

25 Record the time and sample details at the start of the sampling period.

26 At the end of the sampling period, measure the flow rate using the calibrated
flow meter, switch off the sampling pump, and record the flow rate and the time.
Also note the reading on the elapsed time indicator, if fitted.

27 Reseal the sampler with its protective cover and disconnect it from the
sampling pump.

28 In a clean area, where oil mist is absent, and wearing clean disposable gloves,
remove the filter cassette from each sampler, place in their transport clips and
transport back to the laboratory in a suitable container. Alternatively, transport the
samples in the capped sampling heads.

29 Store the samples in a refrigerator if they are not to be analysed immediately.

Sample analysis
30 Allow the filters cassettes to equilibrate with laboratory air overnight before
weighing.

Determination of total inhalable particulate concentration

31 Weigh the samples and blanks cassettes and calculate the total inhalable
particulate airborne concentration (oil mist and other airborne particles) using the
equation:

TIP = (M2 - M1) – B1 x 1000

FxT

where

TIP = total inhalable particulate (oil mist and other airborne particles) (mg.m-3)

M1 = weight of sample cassette before sampling (mg)

M2 = weight of sample cassette after sampling (mg)

B1 = average blank filter weight change (mg)

F = average flow rate during sampling (l.min-1)

T = sampling time (min)

32 Calculate the limit of detection by multiplying the standard deviation of the

weight changes in the blank filters by three. Where the blank-corrected weight
change of a sample filter is less than the limit of detection, record the total inhalable
particulate concentration of the sample as less than the limit of detection.

Measurement of oil mist from mineral oil-based metalworking fuids Page 3 of 5

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33 If the total inhalable particulate airborne concentration exceeds half of any

target value, the filters should be further analysed by extracting the oil from the
filters and determining the oil mist concentration.

Determination of oil mist concentration

34 Extract each filter for 1 hour in a covered glass Petri dish in 10 ml of
cyclohexane. Carefully decant the cyclohexane and perform a second extraction
with a further 10 ml of cyclohexane.

35 Remove the filter from the petri dish using clean flat-tipped tweezers and allow
to dry in a dust-free fume cupboard.

36 Reweigh the filters after equilibration overnight and calculate the oil mist
concentration using the equation:

OM = (M2 - M3) - B2 x 1000

FxT

where

OM = oil mist concentration (mg.m-3)

M2 = sample filter weight before solvent extraction (mg)

M3 = sample filter weight after solvent extraction (mg)

B2 = average blank filter weight change after extraction (mg)

37 Calculate the limit of detection by multiplying the standard deviation of the

weight changes in the blank filter by three. Where the blank-corrected weight
change of a sample filter weight changes is less than the limit of detection, record
the oil mist concentration as less than the limit of detection.

Appendix: Additional information

Detection limit
1 Under the stated sampling and analytical conditions, the limit of detection for
samples taken over an 8-hour sampling period at 2 l.min-1 is typically around
0.1 mg.m-3.

Overall uncertainty
2 Preliminary investigations indicate that the analytical method does not exhibit
significant bias. The analytical recovery from filters spiked with a variety of
metalworking fluids has been shown to be between 94 and 98%, with a relative
standard deviation of 1%. If the analytical measurements are made within the
working range of the method, the overall uncertainty of the method should meet
the specifications of BS EN 482.3

Interferences
3 As well as collecting oil from the aerosol, there is the possibility of the filter
also collecting oil droplets by impaction from spray formed in the course of
operations involving the metalworking fluid. In such circumstances the effects may
Measurement of oil mist from mineral oil-based metalworking fuids Page 4 of 5
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be reduced by choosing an inhalable sampler which minimises the occurrence of

direct impaction of metalworking fluid droplets by shielding the sample filter to a
certain extent. If this interference is perceived to be a potential problem, its
magnitude can be estimated by collecting two filter samples adjacent to each
other, but with only one connected to a sampling pump. Comparison of the
analytical results from both filters should reveal if there has been significant
interference.

4 In some workplace atmospheres there may be other aerosols present which

may contribute to the analytical result (eg water-mix metalworking fluids). Such
interference will affect this analytical method if they are present at significant
concentration and are soluble in cyclohexane.

References
1 General methods for sampling and gravimetric analysis of respirable, thoracic
and inhalable aerosols MDHS14/4 HSE 2014
www.hse.gov.uk/pubns/mdhs/index.htm

2 BS EN 13137:2013 Workplace atmospheres. Pumps for personal sampling of

chemical and biological agents. Requirements and test methods British Standards
Institution

3 BS EN 482:2012 Workplace exposure. General requirements for the

performance of procedures for the measurement of chemical agents British
Standards Institution

You should use the current edition of any standards listed.

Further information
For information about health and safety, or to report inconsistencies or inaccuracies
in this guidance, visit www.hse.gov.uk/. You can view HSE guidance online and
order priced publications from the website. HSE priced publications are also
available from bookshops.

British Standards can be obtained in PDF or hard copy formats from BSI:
http://shop.bsigroup.com or by contacting BSI Customer Services for hard copies
only Tel: 020 8996 9001 email: [email protected].

This guidance is issued by the Health and Safety Executive. Following the guidance
is not compulsory, unless specifically stated, and you are free to take other action.
But if you do follow the guidance you will normally be doing enough to comply with
the law. Health and safety inspectors seek to secure compliance with the law and
may refer to this guidance.

This MDHS is available at: www.hse.gov.uk/pubns/mdhs/index.htm.

For further information about this method or other MDHS methods, please visit
HSL’s website: www.hsl.gov.uk or email: [email protected]

© Crown copyright If you wish to reuse this information visit

www.hse.gov.uk/copyright.htm for details. First published 11/14.

Published by the Health and Safety Executive MDHS84/2 11/14 Page 5 of 5