WO1994001753A1 - Dispositif d'echantillonnage pour emissions de matieres particulaires ou de vapeurs en suspension dans l'air - Google Patents

Dispositif d'echantillonnage pour emissions de matieres particulaires ou de vapeurs en suspension dans l'air Download PDF

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Publication number
WO1994001753A1
WO1994001753A1 PCT/AU1993/000346 AU9300346W WO9401753A1 WO 1994001753 A1 WO1994001753 A1 WO 1994001753A1 AU 9300346 W AU9300346 W AU 9300346W WO 9401753 A1 WO9401753 A1 WO 9401753A1
Authority
WO
WIPO (PCT)
Prior art keywords
filter
emissions
adsorbent
passage
primary
Prior art date
Application number
PCT/AU1993/000346
Other languages
English (en)
Inventor
Peter J. Kirton
Original Assignee
The Broken Hill Proprietary Company Limited
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by The Broken Hill Proprietary Company Limited filed Critical The Broken Hill Proprietary Company Limited
Priority to AU45478/93A priority Critical patent/AU675959B2/en
Priority to GB9500705A priority patent/GB2283816B/en
Publication of WO1994001753A1 publication Critical patent/WO1994001753A1/fr

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2273—Atmospheric sampling
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2205—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling with filters
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
    • G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/02—Devices for withdrawing samples
    • G01N1/22—Devices for withdrawing samples in the gaseous state
    • G01N1/2273—Atmospheric sampling
    • G01N2001/2276—Personal monitors

Definitions

  • the present invention relates to a device for sampling particulate and vapour emissions in occupational hygiene applications and to a method of analysing such emissions.
  • pill and vapour emissions is understood herein to cover any emissions of potential interest, for example, from a personal occupational health view point including but not limited to compounds ranging between very volatile low molecular weight organics to high boiling point particulates and dusts.
  • the present invention is particularly suited although not limited to monitoring personal exposure to aromatic compounds including polycyclic aromatic hydrocarbon (PAH) emissions.
  • PAH polycyclic aromatic hydrocarbon
  • the OSHA procedure produces a result which is variously termed coal tar pitch volatiles (CTPV) , benzene soluble matter (BSM) , or benzene soluble fraction of total particulate matter (BSFTPM) .
  • CTPV coal tar pitch volatiles
  • BSM benzene soluble matter
  • BSFTPM benzene soluble fraction of total particulate matter
  • the last expression is usually reduced to benzene soluble fraction (BSF) .
  • BSF benzene soluble fraction
  • This value expresses the portion of particulate matter, sampled from the air by filtration, which is soluble in benzene.
  • the sampling device for the OSHA procedure consists of a 37mm diameter glass fibre filter held in a polystyrene cassette.
  • the sampling flow rate is nominally 2 L/min, which is achieved by the use of a small battery operated pump.
  • the OSHA procedure is designed for measurement of personal exposure to the above substances.
  • evaporative loss may account for 70- 80% of the total mass of these PAH emissions. It is well known that the OSHA procedure suffers from evaporative loss but existing standards of exposure to PAH emissions are based on OSHA results (expressed as CTPV or BSF) and OSHA is reluctant to change the sampling procedure.
  • NIOSH set out to improve the collection efficiency of the OSHA procedure by including an adsorbent-filled glass tube as a back-up behind the filter.
  • the adsorbent prescribed is XAD-2, a styrene-divinylbenzene co-polymer.
  • the procedure makes use of a Teflon (Registered Trade Mark) filter because of reported improvements in sampling efficiency compared to glass fibre filters.
  • the filter is contained in a polystyrene cassette as in the OSHA procedure.
  • the sampling flow rate is nominally 2 L/min.
  • the filter is extracted with benzene - producing a BSF result - and the XAD-2 is extracted with a suitable solvent followed by chromatographic analysis of the compounds extracted.
  • pyrene is distributed in equal proportions between the filter and the back-up adsorbent.
  • Pyrene is an important chemical because its analysis, in conjunction with that of 1-hydroxypyrene in urine, is used as an indicator of exposure to PAH emissions.
  • the volatility of pyrene is low enough to cause it to condense on the inner walls of the sampling apparatus.
  • NIOSH device there is a relatively large surface area for condensation between the filter and the XAD-2 adsorbent and thus the potential for pyrene loss is appreciable.
  • the materials of construction polystyrene cassette and plastic connecting tubing) will not allow recovery of condensed pyrene by solvent washing.
  • NIOSH procedure A further weakness of the NIOSH procedure is its inability to allow measurement of very volatile compounds, such as benzene.
  • the use of the NIOSH procedure necessitates a separate sampling exercise for these compounds.
  • An object of the present invention is to provide a device for sampling airborne emissions in the environment and a method of quantifying such emissions which alleviates the disadvantages of the OSHA and NIOSH sampling procedures described above in relation to polycyclic aromatic hydrocarbons.
  • a device for sampling airborne particulate or vapour emissions comprising: a passage having an inlet and an outlet, a filter means located in the passage for adsorbing emissions, and a primary adsorbent in the passage for emissions not adsorbed by the filter.
  • the device further comprises a pump means for pumping air through the passage.
  • the primary adsorbent be located immediately downstream of the filter so that there are no voids between the filter and the primary adsorbent.
  • the filter comprises glass fibre or Teflon.
  • the primary adsorbent comprises graphitised carbon.
  • the device be formed from a solvent resistant plastic material.
  • the device further comprises a secondary adsorbent in the passage downstream of the filter and the primary adsorbent for adsorbing emissions not adsorbed by the filter and the primary adsorbent. It is preferred particularly that the secondary adsorbent be charcoal.
  • the device comprises, a main sampler body, and a sampling head detachably coupled to the main sampler body, the sampling head defining the inlet of the passage.
  • the main sampler body be adapted to receive the filter and that the filter be accessible when the sampling head is detached from the main sampler body.
  • the main sampler body be adapted to receive the primary adsorbent.
  • the device further comprises a sleeve detachably coupled to the main sampler body, the sleeve defining the outlet of the passage and being adapted to receive the secondary adsorbent.
  • sampling head, the sampling body, and the sleeve be detachably coupled together by "quick-connect” or “twist-lock” fittings.
  • the small volume of the solvent is 200-400 ⁇ L.
  • the solvent be carbon disulphide.
  • the method further comprises mass spectrometric analysis of samples.
  • Figure 1 is a schematic view of a preferred embodiment of a device for sampling particulate or vapour emissions in accordance with the present invention.
  • Figure 2 is a schematic view of the device shown in Figure 1 in a disassembled form to illustrate the main components of the device.
  • the device 3 shown in the figures is adapted to be attached to a mounting plate 5 of a lapel clip so that it can be carried conveniently by persons exposed to an environment containing airborne emissions of interest.
  • the device 3 comprises a passage, generally identified by the numeral 7, having an inlet 9 and an outlet 11.
  • the outlet 11 is adapted to be coupled by means of a hose connector 13 and hose (not shown) to a pump (not shown) which is operable to draw air at a prescribed flow rate, typically 2 L/min, through the passage 7 from the inlet 9 to the outlet 11.
  • the device 3 further comprises, a filter 15 located in the passage 7 near the inlet 9 for adsorbing emissions of interest, a back-up primary adsorbent 17 in the passage 7 immediately downstream of the filter 15 for adsorbing emissions of interest that are not adsorbed by the filter 15, and a further back-up secondary adsorbent 19 in the passage 7 immediately downstream of the primary adsorbent 17 for adsorbing emissions of interest that are not adsorbed by the filter 15 and the primary adsorbent 17.
  • the filter 15 prevents the primary adsorbent 17 escaping from the inlet 9 of the passage 7.
  • the device 3 further comprises, a retaining screen 31 which separates the primary adsorbent 17 and the secondary adsorbent 19, and a retaining screen 33 which prevents the secondary adsorbent 19 escaping from the outlet 11 of the passage 7.
  • the filter 15, the primary adsorbent 17, and the secondary adsorbent 19 may be formed from any suitable materials depending on the emissions of interest.
  • the filter 15 be formed from glass fibre or Teflon supported on a fine stainless steel support grid 37 ( Figure 2) and that the primary and secondary adsorbents 17, 19 comprise graphitised carbon and charcoal, respectively.
  • charcoal be coconut charcoal.
  • the device 3 is formed from a number of components having "quick-connect” and “twist- lock” fittings for ease of assembly and disassembly of the device 3.
  • the components include a main sampler body 21 which is adapted to receive the filter 15 and the primary adsorbent 17, a sampling head 23 having a plurality of openings 25, typically 7, which define the inlet 9 of the device 3 and satisfy the SAA design criteria for inhalable dusts as specified in As 3640/1989, a sleeve 27 which is adapted to receive the secondary adsorbent 19, and the hose connector 13.
  • the retaining screen 31 is connected to the sleeve 27 and the retaining screen 33 is connected to the hose connector 13.
  • the sampler body 21, the sleeve 27, and the hose connector 13 comprise "quick-connect" couplings, and the sampling head 23 comprises a "twist-lock” coupling.
  • the components of the device 3 may be formed from any suitable materials. It is preferred that the components be formed from Teflon or polypropylene for chemical inertness.
  • the filtered PAH emissions are extracted ultrasonically in a small (typically 1.0 mL) capped vial using a very small volume (typically 200-400 ⁇ D of carbon disulphide as a solvent.
  • the adsorbed PAH emissions are extracted separately from the primary and secondary adsorbents 17, 19 in 1 mL vials using small amounts of CS 2 .
  • the extracted solutions are analysed by capillary gas chromatography (capillary GC) using flame ionisation detection.
  • Instrument settings will vary depending on the type of GC used.
  • a mass spectrometric analysis of samples could be used to characterise material being sampled, but this is desirable, not essential.
  • a detection limit of 20-50ng/m 3 should be routinely achievable, depending on the sophistication of analytical equipment. This limit may be lowered significantly by careful operation of both GC and data system.
  • the device 3 and foregoing method of analysis are suitable for measuring PAH emissions from aluminium smelters and oil refineries, and preliminary results indicate it should be suitable for use in sampling environmental tobacco smoke.
  • the device 3 should be applicable to a wide variety of workplace environments. It is noted that in some cases it may be necessary to use a different solvent or even a displacing compound to ensure that compounds of interest are fully eluted from the adsorbent(s) .
  • the device 3 will also make it possible to seek a correlation between urinary metabolites of specific PAH emissions and occupational exposure to PAH emissions. Previous attempts to link urinary 1-hydroxypyrene with pyrene, when samples were collected by filter without any back-up, yielded poor correlation.
  • the device 3 can generate BSF results which agree with those from standard procedures (eg. OSHA) .
  • the device 3 can replace the NIOSH sampling apparatus, being more rugged and compact and having the advantage of greater potential accuracy because the intimate contact (ie. no voids) between the filter 15 and the primary adsorbent allows no room for condensation. In particular, in the case of sampling PAH emissions this means that all the pyrene is recovered.
  • the device 3 is ideally suited to the monitoring of personal exposure to a wide range of particulate or vapour emissions including but not limited to, PAH emissions discussed previously, diesel exhaust emissions, vapours from paint-line operations, decomposition products from the heating of powdered paints, organic vapours evolved in road surfacing and in the production of aluminium, and vapour generated in the electrolytic production of manganese.
  • PAH emissions discussed previously, diesel exhaust emissions, vapours from paint-line operations, decomposition products from the heating of powdered paints, organic vapours evolved in road surfacing and in the production of aluminium, and vapour generated in the electrolytic production of manganese.
  • the overall size, shape and mass is similar to current OSHA and NIOSH devices and so should be accepted readily be workers.
  • the device 3 meets standard requirements of flow rate for inhalable dust sampling.
  • the float and sink bath contained perchlorethylene, tetrabromoethane (TBE) and a light hydrocarbon distillate called "Ampol 143".
  • TBE tetrabromoethane
  • Ampol 143 The standard procedure for sampling tetrabromoethane (NIOSH 2003) recommends using silica gel tubes while charcoal is specified for perchlorethylene and the hydrocarbons.
  • Charcoal cannot be used for sampling TBE because of a surface catalysed dehydrohalogenation of TBE to give tribromoethylene, a reaction which does not occur with either silica gel or graphitised carbon.
  • Two separate sampling exercises are required to measure airborne concentrations of all the bath components when using standard procedures. It was found that a device 3 packed with graphitised carbon and charcoal successfully enabled analysis of all components from the one sample.
  • the device 3 containing a PVC (GLA 5000) filter and silica gel adsorbent was used to collect mist generated from the electrolytic production of manganese.
  • the aim was to measure sulphuric acid and manganese sulphate together.
  • manganese sulphate and sulphuric acid both collect on the filter and some sulphuric acid passes through to the adsorbent.
  • dry air was drawn through the sampler to cause all the sulphuric acid (as S0 3 ) to evaporate from the filter and be collected on the adsorbent.
  • the results obtained showed that all of the sulphate extracted from the filter was due to manganese sulphate and only sulphuric acid was found on the silica gel adsorbent. This was the first time that these two species had been successfully determined in combination in a single sample.
  • the device 3 was used to sample fumes evolved during bake-out of the smelting cupola for aluminium production.
  • the samples were analysed for the 16 U.S. EPA priority PAH compounds.
  • the samples were collected alongside conventional NIOSH samplers which were set up according to NIOSH standard method 5516.
  • the samples obtained by the NIOSH procedure were subject to component loss by breakthrough from the absorbent during high temperature sampling conditions. Specifically, there was component loss of 6 of the 16 compounds being measured (naphthalene, acenaphthylene, acenaphthene, fluorene, phenanthrene and anthracene) in a significant number of samples from the NIOSH sampler. There was no breakthrough of these components in the device 3.
  • the device 3 was used to characterise fumes and vapours evolved during heating of paints. Two typical examples of this application are heating of powdered paint and welding of painted steel.
  • the design of the device 3, incorporating a filter 15 and primary and secondary absorbents 17, 19 ensured successful sample collection, especially in the case of the welding operation were solids as well as vapours were evolved. There is no conventional or standard procedure which uses a single sampler for evolved components in these applications. It has been found possible to analyse both organic and inorganic material collected on the filter during sampling.
  • the preferred embodiment of the device 3 as shown in Figure 2 comprises a single sleeve 27 and retaining screen 31 which, when assembled, define a section for an adsorbent
  • the present invention is not so limited.
  • the device 3 may comprise two or more such sleeves which, when assembled, define a series of passages which may be filled as required by suitable adsorbents.
  • the primary adsorbent 17 is graphitised carbon and the secondary adsorbent 19 is charcoal
  • the first charcoal section (the secondary adsorbent 19) retains all the water and some of the organics and the second charcoal section retains the remainder of the organics.

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Biomedical Technology (AREA)
  • Molecular Biology (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Sampling And Sample Adjustment (AREA)

Abstract

Un dispositif (3) conçu pour échantillonner des émissions de matières particulaires ou de vapeurs en suspension dans l'air, telles que des émissions d'hydrocarbures aromatiques polycycliques, comprend: un corps principal (21) d'échantillonnage et une tête d'échantillonnage (23) accouplée de manière amovible avec le corps d'échantillonnage (21). Le dispositif (3) comprend de plus, un passage (7) formé dans le corps d'échantillonnage (21), la tête d'échantillonnage (23) définissant un orifice d'entrée dans le passage (7). De plus, le dispositif (3) comprend un filtre (15) situé dans le passage (7) et destiné à absorber les émissions, et un absorbant primaire (17) situé dans le passage (7) immédiatement en aval du filtre (15) de sorte qu'il n'y ait pas de vides entre le filtre (15) et l'absorbant primaire (17).
PCT/AU1993/000346 1992-07-13 1993-07-13 Dispositif d'echantillonnage pour emissions de matieres particulaires ou de vapeurs en suspension dans l'air WO1994001753A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
AU45478/93A AU675959B2 (en) 1992-07-13 1993-07-13 Sampling device for airborne particulate or vapour emissions
GB9500705A GB2283816B (en) 1992-07-13 1993-07-13 Sampling device for airborne particulate and vapour emissions

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
AUPL345592 1992-07-13
AUPL3455 1992-07-13
AUPL865593 1993-05-06
AUPL8655 1993-05-06

Publications (1)

Publication Number Publication Date
WO1994001753A1 true WO1994001753A1 (fr) 1994-01-20

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GB (1) GB2283816B (fr)
NZ (1) NZ253980A (fr)
WO (1) WO1994001753A1 (fr)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1531325A1 (fr) * 2003-11-14 2005-05-18 Institut Français du Pétrole Procédé et dispositif pour prélever des composés gazeux contenus dans un courant gazeux notamment dans des gaz d'échappement dilués d'un moteur à combustion interne
WO2012100364A1 (fr) * 2011-01-26 2012-08-02 Universidad Técnica Federico Santa María Dispositif compact et portatif permettant le prélèvement d'échantillons représentatifs d'air avec du matériel à faible débit afin de déterminer de manière qualitative et quantitative la présence de composés chimiques organiques et inorganiques dans l'air, et procédé d'utilisation dudit dispositif
CN106289882A (zh) * 2016-07-19 2017-01-04 天津大学 一种实验室火焰石英探针在线取样系统及取样方法
WO2018149670A1 (fr) * 2017-02-17 2018-08-23 Stat Peel Ag Dispositif de filtration
US10739268B2 (en) 2015-03-25 2020-08-11 Steel Peel AG Device for measuring the exposure to small particles, in particular nano tubes

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3677708A (en) * 1969-12-15 1972-07-18 Beckman Instruments Inc No2 analysis and scrubber therefor
US3933431A (en) * 1974-07-23 1976-01-20 The United States Of America As Represented By The United States Energy Research And Development Administration Method and apparatus for sampling atmospheric mercury
US4080170A (en) * 1976-09-20 1978-03-21 Borkenstein Robert F Alcohol retainer cartridge and method for using same
GB2078128A (en) * 1980-06-24 1982-01-06 Nat Res Dev Monitoring gases
US4920270A (en) * 1987-09-08 1990-04-24 Lee Grodzins Radon detection
WO1991001001A1 (fr) * 1989-07-06 1991-01-24 The Secretary Of State For Defence In Her Britannic Majesty's Government Of The United Kingdom Of Great Britain And Northern Ireland Detecteur permettant de controler des composes de faible poids moleculaire
AU1262692A (en) * 1990-09-04 1992-03-30 Caterpillar Inc. Gas sampling device and dilution tunnel used therewith

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2153525B (en) * 1984-01-27 1987-09-16 Coal Ind Improvements in atmosphere monitoring

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3677708A (en) * 1969-12-15 1972-07-18 Beckman Instruments Inc No2 analysis and scrubber therefor
US3933431A (en) * 1974-07-23 1976-01-20 The United States Of America As Represented By The United States Energy Research And Development Administration Method and apparatus for sampling atmospheric mercury
US4080170A (en) * 1976-09-20 1978-03-21 Borkenstein Robert F Alcohol retainer cartridge and method for using same
GB2078128A (en) * 1980-06-24 1982-01-06 Nat Res Dev Monitoring gases
US4920270A (en) * 1987-09-08 1990-04-24 Lee Grodzins Radon detection
WO1991001001A1 (fr) * 1989-07-06 1991-01-24 The Secretary Of State For Defence In Her Britannic Majesty's Government Of The United Kingdom Of Great Britain And Northern Ireland Detecteur permettant de controler des composes de faible poids moleculaire
AU1262692A (en) * 1990-09-04 1992-03-30 Caterpillar Inc. Gas sampling device and dilution tunnel used therewith

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1531325A1 (fr) * 2003-11-14 2005-05-18 Institut Français du Pétrole Procédé et dispositif pour prélever des composés gazeux contenus dans un courant gazeux notamment dans des gaz d'échappement dilués d'un moteur à combustion interne
FR2862386A1 (fr) * 2003-11-14 2005-05-20 Inst Francais Du Petrole Procede et dispositif pour prelever des composes gazeux contenus dans un courant gazeux, notamment dans des gaz d'echappement dilues d'un moteur a combustion interne
WO2012100364A1 (fr) * 2011-01-26 2012-08-02 Universidad Técnica Federico Santa María Dispositif compact et portatif permettant le prélèvement d'échantillons représentatifs d'air avec du matériel à faible débit afin de déterminer de manière qualitative et quantitative la présence de composés chimiques organiques et inorganiques dans l'air, et procédé d'utilisation dudit dispositif
US10739268B2 (en) 2015-03-25 2020-08-11 Steel Peel AG Device for measuring the exposure to small particles, in particular nano tubes
CN106289882A (zh) * 2016-07-19 2017-01-04 天津大学 一种实验室火焰石英探针在线取样系统及取样方法
WO2018149670A1 (fr) * 2017-02-17 2018-08-23 Stat Peel Ag Dispositif de filtration

Also Published As

Publication number Publication date
NZ253980A (en) 1997-01-29
GB2283816B (en) 1996-05-29
GB9500705D0 (en) 1995-03-08
GB2283816A (en) 1995-05-17

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