NIOSH Manual of Analytical Methods (NMAM), Fifth Edition

NIOSH Manual of Analytical Methods (NMAM) 5th Edition 

BACKUP DATA REPORT

NIOSH Method No. 6012

Title: Sulfuryl fluoride

Analyte: Sulfuryl fluoride

Author/developer: George Williamson

Date: May 12, 1993

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were accessible as of the publication date
NIOSH Manual of Analytical Methods (NMAM), Fifth Edition

Substance: Sulfuryl Fluoride

OSHA/NIOSH/ACGIH Standard: 20 mg/m3

Compound used for validation: Vikane, tradename of the Dow Chemical Co. for sulfuryl fluoride, 99%; also calibrated

standards of sulfuryl fluoride-in-air prepared by Scott-Marrin, Inc. , Riverside, CA 92507.

Storage Stability 

Gas samples (0.275-L each) from a Tedlar® gas bag containing 417 mg/m3sulfuryl fluoride were collected on tubes of 

coconut shell charcoal, stored for various lengths of time at 0-5 °C, and analyzed by ion chromatography to check for 

storage stability.

Table 6012.1 Storage stability

Day Recovered (mg/m3) Recovery (compared 

to day 1 mean)

Mean Std dev CV

1 409

1 349

1 377 378 30.02 0.0794

4 395

4 383

4 403 1.04 394 10.07 0.0257

12 382

12 368

12 372 1.01 382 17.52 0.0458

There were no significant differences in recovery due to storage time up to 12 days, compared to one-day old samples, F

(2,7)=0.47 at p=0.05.

Breakthrough 

Gas samples from Tedlar® gas bags containing 417 mg/m3SO2F2 in both 30°C “dry” air and 90% relative humidity 

(RH)/30 °C air were collected on charcoal at a flow rate of 0.1 L/min. 

Two charcoal tubes, each containing only one section of charcoal (the front tube containing 800 mg, the rear tube 200 

mg) were placed in series for sample collection. The rear charcoal tube was replaced, at timed intervals, until 10 liters

total were collected (100 minutes time).

The charcoal tubes were analyzed for SO2F2 by ion chromatography. The calculated amount of sulfuryl fluoride

collected on the front section was 3400μg for the 90% RH/30 °C air samples. Data for 90% RH/30 °C air samples is

presented below. 

Table 6012.2 Breakthrough (90% RH/30 °C air samples)

Volume (L) Cumulative Volume (L) μg SO2F2 found on Cumulative total on Cumulative % on 

rear section rear sections μg SO2F2 rear sections

1 1 0 0 0

1 2 1.8 1.8 0.26

2 4 5.8 7.6 0.56

2 6 46 54 2.6

2 8 86 140 4.9

2 10 94 234 6.40

After collecting 10 liters of 417 mg/m3SO2F2, 6.4% of the total SO2F2 collected was found on the rear charcoal sections. 
NIOSH Manual of Analytical Methods (NMAM), Fifth Edition

Data for “Dry" 30 °C air samples 

After 10 liters total collection of dry 30 °C air, NO SO2F2 WAS FOUND ON ANY REAR SECTION. The calculated 

amount found on the front section was 3500 μg. 

Desorption efficiency of Fluoride spikes on charcoal

Sulfuryl fluoride is converted to fluoride and sulfate on the charcoal sorbent by NaOH as shown by the equation: 

SO2F2 + 4NaOH --> 2NaF + Na2SO4 + 2H2O. 

To measure the desorption efficiency, fluoride was spiked on charcoal and desorbed/extracted with NaOH. 

These samples represent 8.95 to 143 mg/m3SO2F2 for a 3-L sample. 

Table 6012.3 Desorption Efficiency data

μg F spiked μg F found Desorption 

Efficiency (DE)

Mean DE Std dev CV

10 10.9 1.09

10 9.45 0.945

10 9.04 0.904

10 9.13 0.913

10 11.3 1.13 0.996 0.1058 0.106

20 20.8 1.04

20 20.5 1.03

20 19.0 0.950

20 18.3 0.915

20 21.2 1.06 0.999 0.06289 0.063

40 38.6 0.965

40 37.9 0.948

40 37.8 0.945

40 38.8 0.970

40 39.2 0.980 0.962 0.01484 0.0154

80 76.7 0.959

80 76.5 0.956

80 76.7 0.959

80 77.7 0.971

80 76.0 0.950 0.959 0.007648 0.00798

120 117 0.975

120 116 0.967

120 114 0.950

120 113 0.942

120 114 0.942 0.955 0.01506 0.0158

160 156 0.975

160 157 0.981

160 157 0.981

160 151 0.944

160 159 0.994 0.975 0.01867 0.0192

Pooled CV1=0.0518
NIOSH Manual of Analytical Methods (NMAM), Fifth Edition

Sampling and Analysis 

Calibrated gas standards were prepared in five-layer aluminized gas bags by injecting known amounts of pure Vikane 

into bags containing appropriate amounts of nitrogen gas. Two-liter samples were collected (0.1 L/min for 20 min.) on

coconut shell charcoal, extracted, and analyzed for sulfuryl fluoride.

Table 6012.4 Recovery data

Level Amount taken (mg/m3) Amount found (mg/m3) Recovery

1X 21 21.3 1.013

1X 21 21.3 1.015

1X 21 20.9 0.9948

4X 83 78.8 0.950

4X 83 78.8 0.950

4X 83 77.6 0.934

8X 167 174 1.041

8X 167 170 1.018

8X 167 173 1.034

1X mean=1.01; std dev=0.01113; CV=0.0110

4X mean=0.944; std dev=0.008718; CV=0.00923

8X mean=0.994; std dev=0.03984; CV=0.04007

Samples (0.2-L and 0.28-L) were collected on charcoal tubes from Tedlar® gas bags containing 417 mg/m3

sulfuryl fluoride in dry air at room temperature. 

Table 6012.5 Recovery data

Level Amount taken (mg/m3) Amount found (mg/m3) Recovery

20X (0.2L) 417 412 0.9890

20X (0.2L) 417 370 0.8880

20X (0.2L) 417 340 0.8161

20X (0.2L) 417 212* 0.5088*

20X (0.2L) 417 726* 1.740*

20X (0.28L) 417 324 0.7779

20X (0.28L) 417 352 0.8451

20X (0.28L) 417 315 0.7549

0.2L mean=0.898; std dev=0.08686; CV=0.0968

0.28L mean=0.793; std dev=0.04685; CV=0.0591

*results lie beyond the mean±3sd

Two- to six-liter samples were taken on charcoal tubes from Tedlar® gas bags containing 21 mg/m3 and 167 mg/

m3SO2F2 in both dry air and in 90% relative humidity air, at room temperature (RT) and 30 °C. 
NIOSH Manual of Analytical Methods (NMAM), Fifth Edition

Table 6012.6 Recovery data

Level Amount taken (mg/m3) Amount found (mg/m3) Recovery

1X (dry air, RT) 21 15.0 0.7128

1X (dry air, RT) 21 14.6 0.6928

1X (dry air, RT) 21 15.2 0.7228

1X (90% RH, RT) 21 14.8 0.7028

1X (90% RH, RT) 21 13.7 0.6514

1X (90% RH, RT) 21 13.6 0.6471

4X (dry air, 30°C) 83 60.1 0.7235

4X (dry air, 30°C) 83 59.2 0.7134

4X (dry air, 30°C) 83 59.6 0.7184

4X (dry air, 30°C) 83 59.2 0.7134

4X (90% RH, 29°C) 83 59.6 0.7184

4X (90% RH, 29°C) 83 59.2 0.7134

4X (90% RH, 29°C) 83 58.4 0.7034

4X (90% RH, 29°C) 83 56.7 0.6832

8X (dry air, RT) 167 169 1.011

8X (dry air, RT) 167 166 0.9964

8X (dry air, RT) 167 174 1.044

8X (90% RH, RT) 190 190 1.139

8X (90% RH, RT) 170 170 1.018

8X (90% RH, RT) 165 165 0.9862

8X (90% RH, RT) 184 184 1.101

8X (90% RH, RT) 169 169 1.014

Note 1: In December 1989 DPSE/MRSB was requested by DSHEFS/IWSB to evaluate the method of Bouyoucos et al.1for 

sampling at fumigation sites for low and high levels of SO2F2 under conditions of high relative humidity. 

Note 2: The 5-layer aluminized gas bags were consistently better for SO2F2 recovery in this study. Recovery from 5-layer 

bags was 0.994 ± 0.03984 sd, n=9, (21-167 mg/m3). Recovery from Tedlar® bags was 0.828 ± 0.1547 sd, n=28, (21-417 

mg/m3). 

Note 3: During the analyses of charcoal tubes for SO2F2 the Dionex AS4A anion separator column showed signs of loss of 

resolution. Fluoride was not being successfully separated from a closely eluting peak (thought to be formate or acetate).

This problem is possibly due to the binding of polyvalent anions from the charcoal sampling media to active sites on the

column. None of the clean-up procedures restored the column to a satisfactory level of performance. Another AS4A

column was used to complete the analyses. A regularly scheduled testing of the guard column (Dionex AG4A) for

contamination may allow for the timely cleaning of the separator column. Even though sulfate theoretically could be

used to measure levels of sulfuryl fluoride, fluoride results were more reliable and so were used exclusively. 

Precision and Accuracy2
NIOSH Manual of Analytical Methods (NMAM), Fifth Edition

Sampling and Analysis2

References

[1] Bouyoucos SA, Melcher RG, Vaccaro JR [1983]. Collection and determination of sulfuryl fluoride in air by ion

chromatography. Am Ind Hyg J 44:57-61.

[2] NIOSH [1977]. Documentation of NIOSH Validation Tests. Cincinnati, OH: U.S. Department of Health, Education

and Welfare, Center for Disease Control, National Institute for Occupational Safety and Health. DHEW (NIOSH)

Publication No. 77-185.