NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

PARTICULATES NOT OTHERWISE REGULATED, RESPIRABLE 0600

DEFINITION: aerosol collected by sampler

with 4-µm median cut point

CAS: None RTECS: None

METHOD: 0600, Issue 3 EVALUATION: FULL Issue 1: 15 February 1984

Issue 3: 15 January 1998

OSHA: 5 mg/m³

NIOSH: no REL

ACGIH: 3 mg/m³

PROPERTIES: contains no asbestos and quartz less than 1%;

FLOW RATE: nylon cyclone: 1.7 L/min

VOL-MIN: 20 L @ 5 mg/m³

SHIPMENT: routine

SAMPLE

STABILITY: stable

BLANKS: 2 to 10 eld blanks per set

ACCURACY: dependent on size distribution [1]

ANALYTE: mass of respirable dust fraction

BALANCE: 0.001 mg sensitivity; use same balance

CALIBRATION: National Institute of Standards and

RANGE: 0.1 to 2 mg per sample

ESTIMATED LOD: 0.03 mg per sample

PRECISION: <10 µg with 0.001 mg sensitivity balance;

loadings, bers, and water-saturated dusts also interfere with the cyclone’s size-selective properties. The use of conductive

samplers is recommended to minimize particle charge eects.

OTHER METHODS: This method is based on and replaces Sampling Data Sheet #29.02 [6].

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

PARTICULATES NOT OTHERWISE REGULATED, RESPIRABLE: METHOD 0600, Issue 3, dated 15 January 1998 - Page 2 of 6

1. Sampler:

a. Filter: 5.0-µm pore size, polyvinyl chloride lter or equivalent hydrophobic membrane lter

supported by a cassette lter holder (preferably conductive).

b. Cyclone: 10-mm nylon (Mine Safety Appliance Co., Instrument Division, P. O. Box 427, Pittsburgh,

4. Weights, NIST Class S-1.1, or ASTM Class 1.

5. Static neutralizer, e.g., Po-210; replace nine months after the production date.

6. Forceps (preferably nylon).

7. Environmental chamber or room for balance, e.g., 20 °C ± 1 °C and 50% ± 5% RH.

SPECIAL PRECAUTIONS: None.

1. Equilibrate the lters in an environmentally controlled weighing area or chamber for at least 2 h.

2. Weigh the lters in an environmentally controlled area or chamber. Record the lter tare weight,

(mg).

a. Zero the balance before each weighing.

4. Remove the cyclone’s grit cap before use and inspect the cyclone interior. If the inside is visibly

scored, discard this cyclone since the dust separation characteristics of the cyclone may be altered.

Clean the interior of the cyclone to prevent reentrainment of large particles.

5. Assemble the sampler head. Check alignment of lter holder and cyclone in the sampling head to

prevent leakage.

6. Calibrate each personal sampling pump to the appropriate ow rate with a representative sampler

in line.

NOTE 1: Because of their inlet designs, nylon and aluminum cyclones are calibrated within a large

vessel with inlet and outlet ports. The inlet is connected to a calibrator (e.g., a bubble meter).

7. Sample 45 min to 8 h. Do not exceed 2 mg dust loading on the lter. Take 2 to 4 replicate samples for

each batch of eld samples for quality assurance on the sampling procedure (see Step 10).

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

PARTICULATES NOT OTHERWISE REGULATED, RESPIRABLE: METHOD 0600, Issue 3, dated 15 January 1998 - Page 3 of 6

NOTE : Do not allow the sampler assembly to be inverted at any time. Turning the cyclone to

anything more than a horizontal orientation may deposit oversized material from the cyclone

body onto the lter.

SAMPLE PREPARATION:

8. Remove the top and bottom plugs from the lter cassette. Equilibrate for at least 2 h in an

environmentally controlled area or chamber.

CALIBRATION AND QUALITY CONTROL:

before and after sample collection. Calibrate the balance with National Institute of Standards and

10. The set of replicate eld samples should be exposed to the same dust environment, either in a

) on control charts. Take corrective

11. Weigh each lter, including eld blanks. Record this post-sampling weight, (mg), beside its

corresponding tare weight. Record anything remarkable about a lter (e.g., visible particles,

overloading, leakage, wet, torn, etc.).

CALCULATIONS:

12. Calculate the concentration of respirable particulate, (mg/m³), in the air volume sampled, (L):

, mg/m³,

where: = tare weight of lter before sampling (mg),

EVALUATION OF METHOD:

1. Bias: In respirable dust measurements, the bias in a sample is calculated relative to the appropriate

expected for some workplace aerosols. However, bias within ± 0.20 would be expected for dusts

with geometric standard deviations greater than 2.0, which is the case in most workplaces.

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

PARTICULATES NOT OTHERWISE REGULATED, RESPIRABLE: METHOD 0600, Issue 3, dated 15 January 1998 - Page 4 of 6

Bias can also be caused in a cyclone by the pulsation of the personal sampling pump. Bartley, et

al. [12] showed that cyclone samples with pulsating ow can have negative bias as large as −0.22

relative to samples with steady ow. The magnitude of the bias depends on the amplitude of the

pulsation at the cyclone aperture and the dust size distribution. For pumps with instantaneous

ow rates within 20% of the mean, the pulsation bias magnitude is less than 0.02 for most dust size

distributions encountered in the workplace.

Electric charges on the dust and the cyclone will also cause bias. Briant and Moss [13] have found

electrostatic biases as large as −50%, and show that cyclones made with graphite-lled nylon

2. Precision: The gure 0.068 mg quoted above for the precision is based on a study [3] of weighing

Imprecision equal to 0.010 mg was used for estimating the LOD and is based on specic suggestions

[8] regarding lter weighing using a single 0.001 mg balance. This value is consistent with another

study [15] of repeat lter weighings, although the actual attainable precision may depend strongly

on the specic environment to which the lters are exposed between the two weighings.

[2] Bowman JD, Bartley DL, Breuer GM, Shulman SA [1985]. The precision of coal mine dust sampling.

[3] Parobeck P, Tomb TF, Ku H, Cameron J [1981]. Measurement assurance program for the weighings

[4] ACGIH [1996]. 1996 Threshold limit values (TLVs™) for chemical substances and physical agents

[5] American Conference of Governmental Industrial Hygienists [1991]. Notice of intended change—

[6] NIOSH [1977]. NIOSH Manual of sampling data sheets. Cincinnati, OH: National Institute for

[7] Higgins RI, Dewell P [1967]. A gravimetric size selecting personal dust sampler. In: Davies CN, Ed.

[8] Bowman JD, Bartley DL, Breuer GM, Doemeny LJ, Murdock DJ [1984]. Accuracy criteria

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

PARTICULATES NOT OTHERWISE REGULATED, RESPIRABLE: METHOD 0600, Issue 3, dated 15 January 1998 - Page 5 of 6

[12] Bartley DL, Breuer GM, Baron PA, Bowman JD [1984]. Pump uctuations and their eect on cyclone

[13] Briant JK, Moss OR [1983]. The inuence of electrostatic charge on the performance of 10-mm

[14] Koqut J [1994]. Private Communication from MSHA, May 12, 1994.

[15] Vaughn NP, Chalmers CP, Botham [1990]. Field comparison of personal samplers for inhalable dust.

METHOD REVISED BY:

APPENDIX: Jarless Method for Calibration of Cyclone Assemblies

O with a “TEE” connector and exible tubing. Connect other end of

NOTE: A light load can be a 5-µm lter and/or an adjustable valve. A heavy load can be several 0.8-

µm lters and/or adjustable valve.

2. Adjust the pump to 1.7 L/min, as indicated on the bubble meter/tube, under the light load

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition

PARTICULATES NOT OTHERWISE REGULATED, RESPIRABLE: METHOD 0600, Issue 3, dated 15 January 1998 - Page 6 of 6

Figure 2.2. Block diagram with cyclone as the test load.