NIOSH Manual of Analytical Methods (NMAM), Fifth Edition

NIOSH Manual of Analytical Methods (NMAM) 5th Edition 

BACKUP DATA REPORT 

NIOSH Method No. 7302

Title: Elements by ICP using microwave digestion

Analyte: 33 elements

Author/developer: Lee C. Stone, James B. Perkins, David M. 

Rogers

Date: April 17, 2003

NOTE: Report written under contract CDC-200-2001-08000

Disclaimer: Mention of any company or product does not constitute endorsement by the National 

Institute for Occupational Safety and Health, Centers for Disease Control and Prevention. In addition, 

citations to websites external to NIOSH do not constitute NIOSH endorsement of the sponsoring 

organizations or their programs or products. Furthermore, NIOSH is not responsible for the content of 

these websites. All web addresses referenced in this document were accessible as of the publication 

date. 
ELEMENTS BY ICP USING 

MICROWAVE DIGESTION

NMAM 7302, ISSUE 1 

BACKUP DATA REPORT

LEE C. STONE

JAMES B. PERKINS

DAVID M. ROGERS

FINAL

APRIL 17, 2003

CONTRACTS CDC-200-2001-08000

Submitted To:

National Institute for Occupational

Safety and Health

Robert A. Taft Laboratories

4676 Columbia Parkway

Cincinnati, Ohio 45226

Submitted By:

DataChem Laboratories, Inc.

960 West LeVoy Drive

Salt Lake City, Utah 84123-2547
TABLE OF CONTENTS

ELEMENTS by ICP using MICROWAVE DIGESTION

INTRODUCTION ...........................................................................................................................1 

REAGENTS AND STANDARDS ..................................................................................................1 

SAMPLE PREPARATION AND INSTRUMENT CONDITIONS ...............................................3 

Sample Preparation ..............................................................................................................3 

Instrument Conditions and Calibration ................................................................................7 

LIMITS OF DETECTION ...............................................................................................................9 

PRECISION ACCURACY AND QUANTITATION STUDY ....................................................11 

Media Background .............................................................................................................14 

SUMMARY ...................................................................................................................................16 

REFERENCES ..............................................................................................................................16
ELEMENTS by ICP using MICROWAVE DIGESTION: 

Backup Data Report

INTRODUCTION

This procedure is applicable to industrial hygiene air monitoring both in the work place 

and in the environment in general. This method incorporates the speed of Inductively Coupled 

Plasma Atomic Emission Spectroscopy (ICP-AES) multi-element analysis along with the 

simplicity of microwave single acid digestion. For all of the elements studied the method is 

viable for these elements as metals, nitrates, and most of their oxides. 

REAGENTS AND STANDARDS

Presented in Tables 1 and 2 are the lists of reagents and standards used for this method 

and its evaluation. All of the standards were prepared in 20% nitric acid by the vendors. 

TABLE 1. LIST OF CHEMICALS

Chemical Vendor CAS# Purity Lot#

Nitric Acid J. T. Baker 7697-37-2 70% 9598-34

Water DataChem Laboratories 7732-18-5 ASTM Type II [1] --
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TABLE 2. LIST OF STANDARDS

Analyte Primary ID# Primary Conc. Vendor Lot#

Al IP-PS-02-012 1000 μg/mL CPI 2AF233

As IP-PS-02-012 500 μg/mL CPI 2AF233

Ba IP-PS-02-012 200 μg/mL CPI 2AF233

Be IP-PS-02-012 200 μg/mL CPI 2AF233

Ca IP-PS-02-012 1000 μg/mL CPI 2AF233

Co IP-PS-02-012 200 μg/mL CPI 2AF233

Cr IP-PS-02-012 200 μg/mL CPI 2AF233

Cu IP-PS-02-012 200 μg/mL CPI 2AF233

Fe IP-PS-02-012 500 μg/mL CPI 2AF233

Li IP-PS-02-012 200 μg/mL CPI 2AF233

Mg IP-PS-02-012 500 μg/mL CPI 2AF233

Mn IP-PS-02-012 200 μg/mL CPI 2AF233

Mo IP-PS-02-012 200 μg/mL CPI 2AF233

Na IP-PS-02-012 500 μg/mL CPI 2AF233

Ni IP-PS-02-012 500 μg/mL CPI 2AF233

Pb IP-PS-02-012 500 μg/mL CPI 2AF233

Se IP-PS-02-012 1000 μg/mL CPI 2AF233

Sr IP-PS-02-012 200 μg/mL CPI 2AF233

Ti IP-PS-02-012 200 μg/mL CPI 2AF233

V IP-PS-02-012 200 μg/mL CPI 2AF233

Zn IP-PS-02-012 200 μg/mL CPI 2AF233

Zr IP-PS-02-012 200 μg/mL CPI 2AF233

B IP-PS-02-026 10000 μg/mL EM Science B1065147

K IP-PS-02-068 10000 μg/mL EM Science B2025030

P IP-PS-02-035 10000 μg/mL EM Science B2025035

Si IP-PS-02-026 10000 μg/mL EM Science B1125060

Sn IP-PS-02-038 10000 μg/mL EM Science B0065078

Te IP-PS-02-040 1000 μg/mL EM Science B1125041

Tl IP-PS-02-046 10000 μg/mL EM Science A8075015

Ag IP-PS-02-058 10000 μg/mL EM Science B2015115

Cd IP-PS-02-028 10000 μg/mL EM Science B1025044

Sb IP-PS-02-084 1000 μg/mL EM Science B1045121

Pt IP-PS-02-123 10000 μg/mL EM Science B0125146
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SAMPLE PREPARATION AND INSTRUMENT CONDITIONS

Sample Preparation

Calibrated personal sampling pumps equipped with MCE filters are used to monitor work 

place exposure conditions for airborne inorganic contaminants. The pumps are set at a flow rate

of between 1 and 4 L/min. For a total sample volume see Table 3. Sample loading limits can be 

estimated from TWA values (see Table 4), instrument sensitivity, and sampling flow rate [2]. A 

filter loading of approximately 2 mg of dust should not be exceeded. Once collected the sample 

cassette filter holders are removed from the personal sampling pumps and submitted for ICPAES analysis.

For this backup study, blank MCE filters were spiked with the elements of interest and 

transferred to clean PTFE digestion vessels. To each vessel was added 10 mL of 1:1 nitric acid 

and ASTM type II water. The vessels and their contents were then weighed and the weights 

recorded. The associated method blanks and spiked QC filters were also prepared in this same 

manner. The digestion vessels were then placed into a programmable microwave oven (CEM 

MDS-2100) and digested using the following conditions:

Stage 1 2 3 4 5

POWER 80% 80% 0% 0% 0%

PRESSURE 50 75 0 0 0

RUN TIME 10:00 20:00 5:00 0 0

TIME 5:00 15:00 0 0 0

TEMPERATURE 150 °C 150 °C 0 °C 0 °C 0 °C

FAN SPEED 100% 100% 100% 100% 100%

NUMBER OF VESSELS: 12

After digestion was complete the vessels were allowed to cool and then they were reweighed and the weights recorded. The lids were then removed and the contents of the vessels 
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were rinsed into 25 mL volumetric flasks with ASTM type II water and diluted to the mark. The 

samples were then submitted for ICP-AES analysis.

NOTE: The purpose for weighing the vessels before and after digestion was to determine 

if there had been any sample loss. If there had been significant loss the sample in question was 

discarded and a new sample prepared and digested. In the case of real world samples if the loss 

was greater than one half gram but less than three grams a note would be made in the lab records. 

If greater than three grams a note would be made in the analytical report. If a loss occurs there is 

the possibility that one or more of the analytes may experience some loss. Where the digestion 

ovens are working perfectly weighing of the samples is not necessary.
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TABLE 3. PROPERTIES AND SAMPLING VOLUMES

Properties [3] Air Volume, L @ OSHA PEL [4]

Element (Symbol) Atomic Weight MP, °C MIN MAX

Silver (Ag) 107.87 961 250 2000

Aluminum (Al) 26.98 660 5 100

Arsenic (As) 74.92 817 5 2000

Barium (Ba) 137.3 727 5(2) 200(2)

Boron (B)(1) 10.81 2300 5 2000

Beryllium (Be) 9.01 1278 1250 2000

Calcium (Ca)(1) 40.08 842 5 200

Cadmium (Cd) 112.40 321 13 2000

Cobalt (Co) 58.93 1495 25 2000

Chromium (Cr) 52.00 1890 5 1000

Copper (Cu) 63.54 1083 5 1000

Iron (Fe) 55.85 1535 5 100

Potassium (K) (1) 39.10 63 5 2000

Lithium (Li)(1) 6.94 179 100 2000

Magnesium (Mg) 24.31 651 5 67

Manganese (Mn) 54.94 1244 5 200

Molybdenum (Mo) 95.94 651 5 67

Sodium (Na)(1) 22.99 98 13 2000

Nickel (Ni) 58.71 1453 5 1000

Phosphorus (P) 30.97 44 25 2000

Lead (Pb) 207.19 328 50 2000

Platinum (Pt) 195.09 1769 1250 2000

Antimony (Sb) 121.76 630 10(2) 2000(2)

Selenium (Se) 78.96 217 13 2000

Strontium (Sr)(1) 87.62 769 5 2000

Tin (Sn) 118.69 232 20(2) 2000(2)

Tellurium (Te) 127.60 450 25 2000

Titanium (Ti) 47.90 1675 5 100

Thallium (Tl) 204.37 304 25 2000

Vanadium (V) 50.94 1890 5 2000

Yttrium (Y) 88.91 1495 5 1000

Zinc (Zn) 65.37 419 5 200

Zirconium (Zr) 91.22 1852 5 200

(1) No PEL, REL, STEL data found [5][6].

(2) Air Volumes Estimated from TWA and LOQs (see Tables 4 and 7) [2].
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TABLE 4. EXPOSURE LIMITS, CAS #, RTECS [5][6]

Exposure Limits, mg/m3 (Ca=carcinogen; C=ceiling limit; *not adopted due to adverse effects at this level

Element (Symbol) CAS # RTECS OSHA NIOSH ACGIH

Silver (Ag) 7440-22-4 VW3500000 0.01 (soluble, metal) 0.01 (soluble, metal) 0.1 (metal)

0.01 (soluble)

Aluminum (Al) 7429-90-5 BD0330000 15 (total dust)

5 (respirable)

10 (total dust)

5 (respirable, fume)

2 (salt, alkyls)

10 (dust)

5 (powder, fume)

2 (salt, alkyls)

Arsenic (As) 7440-38-2 CG0525000 0.010 (inorganic) C 0.002, Ca 0.01, Ca

Barium (Ba) 7440-39-3 0.5 [6]

Boron (B) 7440-42-8

Beryllium (Be) 7440-41-7 DS1750000 0.002, C 0.005 Not to exceed 0.0005, 

Ca

0.002, Ca

Calcium (Ca) 7440-70-2 Varies Varies varies

Cadmium (Cd) 7440-43-9 EU9800000 0.2, C 0.6 (dust)

0.1, C 0.3 (fume)

lowest feasible conc., 

Ca

0.01 (total), Ca

0.002 (respirable), Ca

Cobalt (Co) 7440-48-4 GF8750000 0.1 0.05 (dust, fume) 0.05 (dust, fume)

Chromium (II) (Cr) 22541-79-3 GB6260000 0.5 0.5 Not given

Chromium (III) (Cr) 16065-83-1 GB6261000 0.5 0.5 0.5

Chromium (VI) (Cr) 18540-29-9 GB6262000 C 0.1 0.001 (dust) 0.05 (soluble)

0.05 (insoluble), Ca

Copper (Cu) 7440-50-8 GL5325000 1 (dust, mists)

0.1 (fume)

1 (dust, mists)

0.1 (fume)

1 (dust, mists)

0.2 (fume)

Iron (Fe) 1309-37-1 NO7400000 10 (fume) as oxide 5 (dust, fume) as oxide 5 (fume) as oxide

Potassium (K) 7440-09-7

Lithium (Li) 7439-93-2

Magnesium (Mg) 1309-48-4 OM3850000 15 (dust) as oxide 10 (fume) as oxide* 10 (fume) as oxide

Manganese (Mn) 7439-96-5 OO9275000 C 5 1; STEL 3 0.2

Molybdenum (Mo) 7439-98-7 QA4680000 5 (soluble)

15 (total insoluble)

5 (soluble)*

10 (insoluble)*

5 (soluble)

10 (insoluble)

Sodium (Na) 7440-23-5

Nickel (Ni) 7440-02-0 QR5950000 1 0.015, Ca 1.5 (metal)

(soluble)

0.2 (insoluble), Ca

Phosphorus (P) 7723-14-0 TH3500000 0.1 0.1

Lead (Pb) 7439-92-1 OF7525000 0.05 <0.1 0.15

Platinum (Pt) 7440-06-4 TP2160000 0.002 1 (metal) 1 (metal)

Antimony (Sb) 7440-36-0 CC4025000 0.5 0.5

Selenium (Se) 7782-49-2 VS7700000 0.2 0.2 0.2

Strontium (Sr) 7440-24-6

Tin (Sn) 7440-31-5 XP7320000 2 2

Tellurium (Te) 13494-80-9 WY2625000 0.1 0.1 0.1

Titanium (Ti)

 TiO2

7440-32-6

13463-67-7

XR1700000

XR2275000

As TiO2, 15

as TiO2, 5 (respirable)

lowest feasible, Ca 10

Thallium (Tl) 7440-28-0 XG3425000 0.1 (skin) (soluble) 0.1 (skin) (soluble) 0.1 (skin)

Vanadium (V)

 V2O5

7440-62-2

1314-62-1

YW240000

YW1355000

C 0.5 (respirable) as 

V2O5

C 0.1 (fume) as V2O5

C 0.05 0.05 (respir.) as V2O5

Yttrium (Y) 7440-65-5 ZG2980000 1 1 1

Zinc (Zn) 1314-13-2 ZH4810000 5 (ZnO fume)

15 (ZnO dust)

5 (ZnO respirable)

5; STEL 10 (ZnO fume)

5; C 15 (ZnO dust)

5; STEL 10 (ZnO fume)

10 (ZnO dust)

Zirconium (Zr) 7440-67-7 ZH7070000 5 5, STEL 10 5, STEL 10
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Instrument Conditions and Calibration

The ICP spectrometer should be setup and calibrated according to the manufacturers 

recommendations. Typically acid blank and multi-element working standards are used for 

calibration. These two point curves cover the linear working range of the analytes of interest. 

Listed in Table 5 are the concentrations of the standards that make up the top end of the curves 

set up for this work.

The following multi-element combinations are chemically compatible in 20% HNO3.

a. Al, As, Ba, Be, Ca, Co, Cr, Cu, Fe, Li, Mg, Mn, Mo, Na, Ni, Pb, Se, Sr, Ti, V, Y, 

Zn, Zr;

b. B, K, P, Si, Sn, Te, Tl;

c. Ag, Cd, Sb;

d. Pt.

Continuing Calibration Verification Standard (CCV) or standards that contain analytes of 

interest are analyzed after every ten analyses (minimum frequency), and recoveries are checked 

with media blanks and spikes, every twenty samples.
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TABLE 5. Calibration Standard Concentrations

Analyte Primary ID# Primary Conc.

Volume of 

Primary

Final 

Volume

Final 

Concentration

Al IP-PS-02-012 1000 μg/mL 20 mL 2000 mL 10 μg/mL

As IP-PS-02-012 500 μg/mL 20 mL 2000 mL 5 μg/mL

Ba IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Be IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Ca IP-PS-02-012 1000 μg/mL 20 mL 2000 mL 10 μg/mL

Co IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Cr IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Cu IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Fe IP-PS-02-012 500 μg/mL 20 mL 2000 mL 5 μg/mL

Li IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Mg IP-PS-02-012 500 μg/mL 20 mL 2000 mL 5 μg/mL

Mn IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Mo IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Na IP-PS-02-012 500 μg/mL 20 mL 2000 mL 5 μg/mL

Ni IP-PS-02-012 500 μg/mL 20 mL 2000 mL 5 μg/mL

Pb IP-PS-02-012 500 μg/mL 20 mL 2000 mL 5 μg/mL

Se IP-PS-02-012 1000 μg/mL 20 mL 2000 mL 10 μg/mL

Sr IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Ti IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

V IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Zn IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

Zr IP-PS-02-012 200 μg/mL 20 mL 2000 mL 2 μg/mL

B IP-PS-02-026 10000 μg/mL 1 mL 1000 mL 10 μg/mL

K IP-PS-02-068 10000 μg/mL 5 mL 1000 mL 50 μg/mL

P IP-PS-02-035 10000 μg/mL 2 mL 1000 mL 20 μg/mL

Si IP-PS-02-026 10000 μg/mL 5 mL 1000 mL 50 μg/mL

Sn IP-PS-02-038 10000 μg/mL 1 mL 1000 mL 10 μg/mL

Te IP-PS-02-040 1000 μg/mL 10 mL 1000 mL 10 μg/mL

Tl IP-PS-02-046 10000 μg/mL 2 mL 1000 mL 20 μg/mL

Ag IP-PS-02-058 10000 μg/mL 0.2 mL 1000 mL 2 μg/mL

Cd IP-PS-02-028 10000 μg/mL 0.2 mL 1000 mL 2 μg/mL

Sb IP-PS-02-084 1000 μg/mL 10 mL 1000 mL 10 μg/mL

Pt IP-PS-02-123 10000 μg/mL 2 mL 2000 mL 10 μg/mL
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LIMITS OF DETECTION

The limits of detection (LOD) and quantitation (LOQ) are determined according to the

protocol given in the Environmental Protection Agency’s 40 CFR [7] in the which seven or more 

duplicates within the range of 1#TC/MDL#5 are analyzed and calculated (see Table 6).

Where:

TC = test concentration

MDL = the method detection limit or LOD

The wavelength at which an analyte is measured is generally the most sensitive available. 

Where there are spectral interferences from other elements in a sample, it may be necessary to 

use an alternate wavelength. With a fixed wavelength instrument this is not always possible. In 

this study two different ICP’S were used. Most of the data for this study was generated using a 

fixed channel Fisons ARL Accuris ICP-AES. For those analytes were there were possible 

interference problems on the Fisons, a Perkin Elmer Optima 3000 DV ICP-AES was employed 

(see Table 6).

The duplicates for this study were prepared following the procedure in the sample 

preparation section. They were processed through the sample digestion procedure along with 

filter blanks and quality control (QC) samples. 

From the LODs the LOQs for each of the analyts are calculated using the formula:

LOQ= 3.3X LOD.
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TABLE 6. WAVELENGTHS AND DETECTON LIMITS

Element(a) Wavelength 

(nm)[8]

LOD

(μg/sample)

Ag 328.1 0.1

Al 308.2 1

As 193.8 1

Ba 493.4 0.06

B 249.7 0.5

Be 313.0 0.009

Ca 315.9 2

Cd 228.8 0.1

Co 228.6 0.3

Cr(b) 267.7 0.4

Cu 324.8 0.07

Fe 259.9 2

K 766.5 2

Li 670.8 0.03

Mg 279.1 0.5

Mn 257.6 0.02

Mo 202.0 0.2

Na 589.0 4

Ni 231.6 0.2

P 214.9 2

Pb 220.4 0.6

Pt(b) 265.9 8

Sb 206.8 0.4

Se 196.1 3

Sn(b) 189.9 0.8 

Sr 421.6 0.02

Te(b) 214.3 2

Ti 337.3 0.2

Tl 190.9 0.9

V 292.4 0.1

Y(b) 371.0 0.02

Zn(b) 213.9 0.1

Zr 339.2 0.06

(a) Unless otherwise specified all reported values were obtained with a Fisons ARL Accuris ICP-AES; 

performance may vary with instrument and should be independently verified.

(b) Values reported were obtained with a Perkin Elmer (PE) Optima 3000 DV ICP-AES. Sample concentration 

was based on Fisons ICP-AES LOD data. 
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PRECISION ACCURACY AND QUANTITATION STUDY

To determine the precision and accuracy of this method, six concentrations ranging from 

1X LOQ to 300X LOQ for each element were studied. For each level, six blank filters were 

spiked with certified standards and digested following the procedure outlined in the section on 

sample preparation. After digestion the samples were analyzed, the raw data collected, and 

precision and accuracy calculated (see Tables 7 and 8).

The acceptable NIOSH recovery range is from 75% to 125%. The percent recoveries at 

the 1X LOQ level, range from 65.6% to 127% compared to 92.4% to 112% for the 3X LOQ 

level. Thus the range of quantitation is in general 3X LOD and above.
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TABLE 7. PRECISION AND ACCURACY

Element(a) 1X LOQ

(μg/sample)

%

Recovery

(N=6)

%

RSD

3X LOQ

(μg/sample)

%

Recovery

(N=6)

%

RSD

10X LOQ

(μg/sample)

%

Recovery

(N=6)

%

RSD

Ag 0.495 84.6 10.3 1.50 95.5 1.01 4.95 101 1.07

Al 2.48 74.5 40.5 7.50 92.7 0.981 24.8 82.9 3.87

As 2.48 100 10.7 7.50 101 2.22 24.8 104 2.12

Ba 0.248 111 8.59 0.752 104 3.09 2.48 102 0.664

B 1.24 127 6.19 3.75 112 2.96 12.4 100 0.618

Be 0.025 89.2 7.15 0.076 95.8 2.36 0.251 99.6 0.995

Ca 7.43 134 2.94 22.5 107 2.87 74.3 110 0.701

Cd 0.495 94.6 7.30 1.50 98.8 3.46 4.95 105 0.746

Co 1.24 94.9 8.71 3.75 99.7 1.72 12.4 103 0.403

Cr(b) 1.24 109 7.97 3.75 103 7.87 12.4 82.4 1.13

Cu 0.248 85.8 12.9 0.752 98.8 3.47 2.48 102 2.10

Fe 4.95 123 10.4 15.0 112 2.43 49.5 90.1 2.97

K 4.95 86.8 23.0 15.0 98.3 5.70 49.5 98.6 2.86

Li 0.248 80.4 4.78 0.752 92.4 2.98 2.48 93.7 1.05

Mg 2.48 81.9 12.9 7.50 89.3 3.52 24.8 101 1.65

Mn 0.248 72.1 4.78 0.752 86.2 2.38 2.48 104 0.555

Mo 0.743 99.8 7.59 2.25 96.8 5.41 7.43 111 0.874

Na 12.4 110 5.72 37.5 100 0.823 124 98.7 1.94

Ni 0.743 72.6 16.8 2.25 98.3 5.21 7.43 87.9 5.93

P 4.95 96.8 6.62 15.0 100 5.67 49.5 100 0.974

Pb 2.48 112 7.66 7.50 98.9 3.94 24.8 98.7 1.00

Pt(b) 25.0 99.2 1.43 75.0 98.3 0.282 250 99.1 2.63

Sb 2.48 105 5.08 7.50 94.4 3.21 24.8 103 1.01

Se 12.4 98.9 4.80 37.5 104 3.21 124 88.1 3.83

Sn(b) 12.4 110 4.62 37.5 105 5.04 124 103 2.51

Sr 1.24 101 1.48 3.75 92.6 2.36 12.4 101 0.393

Te(b) 4.95 114 4.83 15.0 90.1 21.8 49.5 106 1.87

Ti 0.495 101 8.18 1.50 101 1.70 4.95 99.1 0.625

Tl 2.48 93.6 7.52 7.5 103 4.14 24.8 104 1.85

V 0.248 65.6 22.0 0.752 93.7 4.74 2.48 100 1.92

Y(b) 0.124 111 5.28 0.376 107 4.44 1.24 88.3 2.23

Zn(b) 0.495 105 17.5 1.50 106 13.1 4.95 86.0 1.41

Zr 0.248 74.1 19.3 0.750 93.1 5.35 2.48 98.6 1.95

(a) Unless otherwise specified all reported values were obtained with a Fisons ARL Accuris ICP-AES; performance may vary with 

instrument and should be independently verified.

(b) Values reported were obtained with a Perkin Elmer Optima 3000 DV ICP-AES. Sample concentration was based on Fisons ICPAES LOD data.
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TABLE 8. PRECISION AND ACCURACY

Element(a) 30X LOQ

(μg/sample)

%

Recovery

(N=6)

%

RSD

100X LOQ

(μg/sample)

%

Recovery

(N=6)

%

RSD

300X LOQ

(μg/sample)

%

Recovery

(N=6)

%

RSD

Ag 15.0 99.9 1.01 50.0 99.1 0.593 150 99.0 0.497

Al 75.0 102 0.295 250 101 0.474 750 98.7 0.462

As 75.0 101 0.754 250 104 1.16 750 107 0.340

Ba 7.52 100 0.297 25.0 102 0.839 75.2 101 0.438

B 37.5 101 0.813 125 99.7 0.964 375 99.5 0.454

Be 0.760 96.9 0.448 2.53 101 1.24 7.60 103 0.714

Ca 225 100 0.395 749 103 1.08 2250 104 0.620

Cd 15.0 100 1.01 50.0 103 1.43 150 104 0.701

Co 37.5 99.9 0.455 125 102 1.04 375 103 0.566

Cr(b) 37.5 99.7 1.43 125 96.6 1.59 375 94.2 3.36

Cu 7.52 103 0.518 25.0 103 0.628 75.2 101 0.371

Fe 150 102 0.331 500 104 1.35 1500 103 0.263

K 150 101 0.631 500 100 0.438 1500 98.8 0.472

Li 7.52 100 0.528 25.0 99.8 0.744 75.2 95.1 0.749

Mg 75.0 99.7 0.296 250 100 0.674 750 98.2 0.309

Mn 7.52 101 0.313 25.0 104 0.974 75.2 103 0.389

Mo 22.5 105 0.461 75.0 109 1.06 225 110 0.373

Na 375 99.7 0.766 1250 101 0.561 3750 97.7 0.457

Ni 22.5 103 0.315 75.0 104 1.12 225 104 0.592

P 150 99.3 0.609 500 101 1.83 1500 104 0.315

Pb 75.0 93.7 0.283 250 95.1 1.02 750 95.7 0.570

Pt(b) 750 94.1 0.985 3330 93.6 1.22 10000 95.7 1.49

Sb 75.0 101 0.446 250 102 0.913 750 103 0.255

Se 375 102 0.483 1250 104 1.07 3750 106 0.270

Sn(b) 375 101 1.04 1250 96.6 1.81 3750 90.3 3.23

Sr 37.5 97.1 0.430 125 99.5 0.689 375 97.5 0.553

Te(b) 150 107 0.914 500 105 1.44 1500 103 0.614

Ti 15.0 96.7 0.249 50.0 99.0 0.888 150 98.8 0.575

Tl 75.0 97.6 0.395 250 99.4 1.31 750 99.3 0.352

V 7.52 101 0.700 25.0 103 0.966 75.2 103 0.341

Y(b) 3.76 105 1.23 12.5 103 1.60 37.6 102 3.33

Zn(b) 15.0 101 1.66 50.0 98.9 1.09 150 97.4 3.42

Zr 7.50 95.3 1.20 25.0 95.9 0.233 75.0 95.4 0.971

(a) Unless otherwise specified all reported values were obtained with a Fisons ARL Accuris ICP-AES; performance may vary with 

instrument and should be independently verified.

(b) Values reported were obtained with a Perkin Elmer Optima 3000 DV ICP-AES. Sample concentration was based on Fisons ICPAES LOD data.
ELEMENTS by ICP using MICROWAVE DIGESTION – Backup Data Report Last Updated: April 17, 2003

Page 14 of 16

Media Background

Media blank results for MCE filters showed no background greater than the LOQ of any of the 

elements. Thus, subtraction of the media blank from the spiked filter results was not found to be 

necessary (see Table 9). The LOQs listed in Table 9 are calculated from the LODs of the Fisons ICPAES (see section on Limits of Detection and Quantitation Study) and approximate the 1X LOQs found 

in Tables 7 and 8.
ELEMENTS by ICP using MICROWAVE DIGESTION – Backup Data Report Last Updated: April 17, 2003

Page 15 of 16

TABLE 9. MEDIA BACKGROUND RESULTS

Element(a) 

Average 

(N=6) 

(μg/sample)

LOQ

(μg/sample)

Ag -0.0838 0.4

Al -0.7439 4

As -0.1216 3

Ba 0.3529 0.2

B 0.0325 2

Be -0.0025 0.03

Ca 2.4224 6

Cd -0.0505 0.4

Co -0.2234 1

Cr(b) 0.7468 0.8

Cu 0.0149 0.2

Fe 1.2912 7

K -0.8592 8

Li -0.0514 0.1

Mg -0.4986 2

Mn -0.0831 0.07

Mo -0.0912 0.7

Na 0.4418 10

Ni -0.2431 0.5

P -0.1945 7

Pb 0.3096 2

Pt(b) -0.0215 25

Sb 0.0840 1

Se -0.1967 10

Sn(b) 0.0652 3

Sr -0.0171 0.06

Te(b) 0.0228 1

Ti 0.0242 0.7

Tl -0.6471 3

V -0.0827 0.4

Y(b) -0.0019 0.007

Zn(b) 0.1618 0.4

Zr 0.0147 0.2

(a) Values and LOQs reported were obtained with a Fisons ARL Accuris ICP-AES; performance may vary with instrument 

and should be independently verified.

(b) Values and LOQs reported were obtained with a Perkin Elmer Optima 3000 DV ICP-AES.
ELEMENTS by ICP using MICROWAVE DIGESTION – Backup Data Report Last Updated: April 17, 2003

Page 16 of 16

SUMMARY

This method is for the analysis of metal and nonmetal dust collected on MCE filters in the 

work place and environment in general. This method increases the applicability of NMAM 7300 [9] 

for trace elements and the simultaneous elemental analysis. Using a microwave digestion approach 

simplifies and expedites the analysis. The elimination of perchloric acid [10] in the sample digestion 

helps to improve the safety of the method.

REFERENCES

[1] ASTM # 1193-77 (1983).

[2] “The Industrial Environment - its Evaluation & Control”, NIOSH, U.S. Department of Health 

Education and Welfare, (1973).

[3] Lide, D R “Handbook of Chemistry and Physics”, 74th Edition, ISBN: 0-8493-0474-1, 

(1993-1994).

[4] Perkins, J B Wheeler, D L Nicholson, K “ELEMENTS by ICP”, NIOSH, NMAM 7300, 

(Aug. 1994).

[5] NIOSH Pocket Guide To Chemical Hazards, DHHS (NIOSH), U.S. Department of Health and 

Human Services, Publication No. 97-140, (June 1997).

[6] 2002 TLV’s and BEI’s, ACGIH Worldwide, ISBN: 1-882417-46-1, (2002).

[7] Environment Protection Agency,40 CFR Ch. 1 (7-1-91 Edition), Part 136, Appendix B

[8] Harrison, G R “MIT Wavelength Tables”, Vol. 1, 2nd Edition, ISBN: 0-262-08002-8, 

(Aug. 1969).

[9] NIOSH Manual of Analytical Methods, 2nd ed., B. 7, P&CAM 351, U.S. Department of 

Health and Human Services, Publ. (NIOSH) 82-100 (1981).

[10] CRC Handbook of Laboratory Safety, 4th Edition, 1995, A Keith Furr, CPC Press, Boca 

Raton, Florida.

Written By: Lee C. Stone, James B. Perkins, David M. Rogers, DataChem Laboratories, Salt Lake 

City, Utah under NIOSH Contract CDC-200-2001-08000