Page:NIOSH Manual of Analytical Methods - 5043.pdf/1

 p-TOLUENESULFONIC ACID

C7H8O3S

MW: 172.20

METHOD: 5043, Issue 1

5043

CAS: 104-15-4

RTECS: XT6300000

EVALUATION: PARTIAL

OSHA : no PELs NIOSH: no RELs ACGIH: no TLVs (1 ppm = 7.03 mg/m3 @ NTP)

PROPERTIES:

Issue 1: 15 January 1998

solid; MP 106 to 107 C when anhydrous; d 1.20 g/mL @ 20 C; BP 140 C @ 20 mm Hg; VP not significant @ 25 C

NAMES & SYNONYMS: 4-methylbenzenesulfonic acid; p-methylphenylsulfonic acid; tosic acid

SAMPLING

MEASUREMENT

SAMPLER:

FILTER (13-mm glass fiber)

FLOW RATE:

1 to 3 L/min

VOL-MIN: -MAX:

10 L @ 1000 L

SHIPMENT:

routine

SAMPLE STABILITY:

at least 29 days @ 25 C [1]

BLANKS:

2 to 10 field blanks per set

EXTRACTION:

2 mL 2% isopropanol in water v/v; ultrasonic bath, 10 min

100 µL

COLUMN:

3.9-mm ID x 15 cm stainless steel packed with 10-µm µ-Bondapak C18

DETECTOR:

UV @ 222 nm

CALIBRATION:

standard solutions of ptoluenesulfonic acid in isopropanol: water

RANGE:

0.27 to 120 µg/sample [1]

not determined

ESTIMATED LOD:

0.08 µg/sample [1]

not determined

PRECISION ( r):

0.046 @ 3 to 15 µg/sample [1]

BIAS:

not determined

ACCURACY:

p-toluenesulfonic acid

21% acetonitrile/79% water containing 0.005 M Pic® A v/v; 1 mL/min

not studied

):

ANALYTE:

MOBILE PHASE:

RANGE STUDIED:

rT

HPLC, UV DETECTOR

INJECTION VOLUME:

ACCURACY

OVERALL PRECISION (

TECHNIQUE:

APPLICABILITY:p-Toluenesulfonic acid at 0.0027 to 1.2 mg/m3 can be determined in a 100-L air sample by this method. This method has been used to analyze samples collected at a foundry & machining company where p-toluenesulfonic acid was a catalyst in a process to produce a resin from resorcinol and furfuryl alcohol [2].

INTERFERENCES: None identified.

OTHER METHODS: Chromatographic methods for determination of p-toluenesulfonic acid in solution have been published [3-7]. None has been published for air analysis. An alternative air sampler for the present method is a midget impinger containing isopropanol [1,2].

NIOSH Manual of Analytical Methods (NMAM), Fourth Edition