ENFLURANE
HALOTHANE
ISOFLURANE
Method number: |
103 |
|
Matrix: |
Air |
|
Target concentration, TC: |
|
|
enflurane |
halothane |
isoflurane |
TC |
low |
high |
low |
high |
low |
high |
|
ppm |
1 |
75 |
1 |
50 |
1 |
75 |
mg/m3 |
7.5 |
566 |
8 |
403 |
7.5 |
566 |
|
|
|
OSHA PEL: ACGIH TLV: |
None 75 ppm (566 mg/m3) for enflurane 50 ppm (403 mg/m3) for halothane |
|
Procedure: |
Samples are collected by drawing a known volume of air through standard size (6-mm
o.d., 150/75 mg) Anasorb CMS or (6-mm o.d., 140/70 mg) Anasorb 747 tubes. Samples are
desorbed with CS2 and analyzed by GC using a
flame-ionization detector (FID). |
|
Air volume and sampling rate: |
12 L at 0.05 L/min |
|
Reliable quantitation limit: |
|
|
enflurane |
halothane |
isoflurane |
Anasorb |
CMS |
747 |
CMS |
747 |
CMS |
747 |
|
ppb |
25.0 |
40.7 |
24.4 |
21.3 |
23.0 |
23.5 |
µg/m3 |
189 |
307 |
197 |
172 |
174 |
177 |
|
|
|
Standard error of estimate at the target concentration: |
|
|
enflurane |
halothane |
isoflurane |
Anasorb |
CMS |
747 |
CMS |
747 |
CMS |
747 |
|
low TC |
0.072 |
0.058 |
0.076 |
0.054 |
0.078 |
0.059 |
high TC |
0.083 |
0.077 |
0.070 |
0.058 |
0.085 |
0.061 |
|
|
| | |
Special requirements: |
Samples collected on Anasorb CMS for halothane should be stored at reduced temperature following receipt at the laboratory until analysis. |
|
Status of method: |
Evaluated method. This method has been subjected to the established evaluation procedures of the Organic Methods Evaluation Branch. |
| | |
Date: May 1994 |
Chemist: Donald Burright |
Organic Methods Evaluation Branch
OSHA Salt Lake Technical Center
Salt Lake City, UT 84165-0200
1. General Discussion
1.1 Background
1.1.1 History
The objective of this method is to eliminate the need to use two adsorbent tubes connected in
series as specified for enflurane and halothane in OSHA Method 29 (Ref. 5.1), and to expand the
methodology to include the newer anesthetic gases, isoflurane and desflurane. (Desflurane will
appear as a separate method because it requires different analytical conditions.) Enflurane,
halothane and isoflurane were each evaluated at two target concentrations because NIOSH
recommended exposure limits (Refs. 5.2 and 5.3) are considerably lower than the current ACGIH
TLVs (Ref. 5.4). For this reason, the method was evaluated at a lower target concentration of 1
ppm for all three analyses. Currently there are no OSHA PELs for these substances. Preliminary
studies were performed with the following adsorbents: Anasorb CMS, Anasorb 747, Carbosieve
S-III and activated coconut charcoal. Anasorb CMS and Anasorb 747 were both good candidates
for an improved sampler as neither adsorbent required two tube in series. Evaluation tests were
begun with both adsorbents in the anticipation that one would dearly surpass the other in
performance. Since this did not occur, both were evaluated and are presented as sampling options.
ACGIH has recommended a TLV-TWA of 75 ppm for enflurane and 50 ppm for halothane
(Ref. 5.4). The TLV for enflurane is based on the assumption enflurane is a safer anesthetic
gas than halothane. The TLV for halothane is based on a comparison of toxicity and TLVs of
trichloroethylene and chloroform. (Ref. 5.4) The ACGIH recommendations are the basis for
setting the higher target concentrations of enflurane and halothane for the evaluation of this
method. A higher target concentration of 75 ppm was set for isoflurane because it is a geometric
isomer of enflurane. NIOSH has recommended that exposure to these halogenated anesthetic
gases should be controlled with a 60-min ceiling value of 2 ppm (Ref. 5.2). The anesthetic gases
are usually administered in conjunction with nitrous oxide.
1.1.2 Toxic effects (This section is for information only and should not be taken as the basis of OSHA policy.)
Current scientific evidence obtained from human and animal studies suggest that chronic
exposure to anesthetic gases increase the risk of both spontaneous abortion and congenital
abnormalities in offspring among female workers and wives of male workers. Risks of hepatic
and renal diseases are also increased among exposed workers. (Ref 5.2) IARC states there is
inadequate evidence for the carcinogenicity of enflurane, halothane and isoflurane in both
animals and humans (Ref. 5.5).
Enflurane and isoflurane have similar health effects for acute exposure. An exposure may cause
irritation and redness in eyes, dryness and irritation of skin, and irritation of the mouth and
throat. If inhaled, headaches, dizziness, drowsiness, unconsciousness, and death can occur. (Refs.
5.6 and 5.7)
Acute exposures of halothane can cause severe irritation to the eyes, irritation of the skin,
reduction of the blood pressure, dizziness, drowsiness, and unconsciousness. Chronic exposures
can possibly cause cancer. (Ref. 5.8)
1.1.3 Workplace exposure
Enflurane, halothane and isoflurane are the most commonly used organic anesthetic gases.
Occupational exposure may occur whenever anesthetics are used in operating rooms, dental
offices and veterinary hospitals. The number of people potentially exposed was estimated to be
215,000 in 1977 (Ref. 5.2). This number is probably much higher today if the increase in the
health care industry since 1977 is considered.
1.1.4 Physical properties and other descriptive information (Refs. 5.6 - 5.9)
|
enflurane |
halothane |
isoflurane |
|
CAS number: |
13838-16-9 |
151-67-7 |
26675-46-7 |
molecular weight: |
184.49 |
197.39 |
184.49 |
boiling point, °: |
56.5 |
50.2 |
48.5 |
color: |
colorless |
colorless |
colorless |
specific gravity: |
1.52 |
1.872 |
1.50 |
molecular formula: |
C3H2OClF5 |
C2HBrClF3 |
C3H2OClF5 |
vapor pressure, kPa (mmHg): |
25.1(188.6) @22°C |
32.4(243.3) @20°C |
34.9(261.8) @22°C |
odor: |
odorless |
|
mild ethereal |
flash point, °: |
>200 |
none |
>200 |
solubility: |
miscible with organic solvents |
miscible with pet ether and other fat solvents |
miscible with organic liquids |
synonyms: |
Ethrane; 2-chloro- 1,1,2-trifluoroethyl difluoromethyl ether; methyl flurether; Efrane; Alyrane |
Fluothrane; 2-bromo-2-chloro- 1,1,1-trifluoro- ethane; Rhodialothan |
Forane; 1-chloro- 2,2,2-trigluoroethyl difluoromethyl ether; Aerrane; Forene |
structural formulas: |
![structural formulas](/dts/sltc/methods/organic/org103/org103_1str114.gif) |
The analyte air concentrations throughout this method are based on the recommended sampling
and analytical parameters. Air concentrations listed in ppm are referenced to 25° and 101.3
kPa (760 mmHg).
1.2 Limit defining parameters
1.2.1 Detection limit of the analytical procedure
The detection limits of the analytical procedure are 92.8, 87.3 and 44.7 pg for enflurane,
halothane and isoflurane respectively. These are the amounts of each analyte that will give a
response that is significantly different from the background response of a reagent blank.
(Sections 4.1 and 4.2)
1.2.2 Detection limit of the overall procedure
The detection limits of the overall procedure (mass per sample) are listed below. These are the
amounts of each analyte spiked on the sampler that will give a response that is signfticantly
different from the background response of a sampler blank. (Sections 4.1 and 4.3)
Table 1.2.2 |
Detection Limits of the Overall Procedure |
|
adsorbent enflurane halothane isoflurane |
|
Anasorb CMS |
0.679 µg |
0.709 µg |
0.625 µg |
|
7.50 ppb |
7.32 ppb |
6.91 ppb |
|
56.6 µg/m3 |
59.1 µg/m3 |
52.1 µg/m3 |
Anasorb 747 |
1.105 µg |
0.620 µg |
0.639 µg |
|
12.2 ppb |
6.40 ppb |
7.06 ppb |
|
92.1 µg/m3 |
51.7 µg/m3 |
53.3 µg/m3 |
|
1.2.3 Reliable quantitation limit
The reliable quantitation limits (mass per sample) are listed below. These are the amounts of
analyses spiked on a sampler that will give a signal that is considered the lower limit for precise
quantitative measurements. (Section 4.4)
Table 1.2.3 |
Reliable Quantitation Limits |
|
adsorbent |
enflurane |
halothane |
isonurane |
|
Anasorb CMS |
2.26 µg |
2.36 µg |
2.08 µg |
|
25.0 ppb |
24.4 ppb |
23.0 ppb |
|
188 µg/m3 |
197 µg/m3 |
173 µg/m3 |
Anasorb 747 |
3.68 µg |
2.07 µg |
2.13 µg |
|
40.7 ppb |
21.4 ppb |
23.5 ppb |
|
307 µg/m3 |
172 µg/m3 |
178 µg/m3 |
|
1.2.4 Precision (analytical Procedure)
The precisions of the analytical procedure are measured as the pooled relative standard deviation
over a concentration range equivalent to the range of 0.5 to 2 times the target concentration. (Section 4.5)
Table 1.2.4 |
Precisions of the Analytical Procedure, % |
|
target concn |
enflurane |
halothane |
isoflurane |
1 ppm |
2.77 |
1.39 |
3.50 |
50 ppm |
|
1.37 |
|
75 ppm |
2.27 |
|
2.83 |
|
1.2.5 Precision (overall procedure)
The precisions of the overall procedure at the 95% confidence level for the ambient temperature
15-18 day storage tests (at the target concentration) are listed below. This includes an additional
5% for sampling error. (Section 4.6)
Table 1.2.5.1 |
Precision of the Overall Procedure on Anasorb CMS, % |
|
target concn |
enflurane |
halothane |
isoflurane |
|
1 ppm |
14.1 |
14.9 |
15.3 |
50 ppm |
|
13.7 |
|
75 ppm |
16.3 |
|
16.6 |
|
- refrigerated storage test at 4° |
Table 1.2.5.2 |
Precision of the Overall Procedure on Anasorb 747, % |
|
target concn |
enflurane |
halothane |
isoflurane |
|
1 ppm |
11.3 |
10.6 |
11.5 |
50 ppm |
|
11.4 |
|
75 ppm |
15.1 |
|
12.0 |
|
1.2.6 Recovery
The recoveries of enflurane, halothane and isoflurane from samples used in the 15-18 day storage
tests remained above the values listed below when the samples were stored at 22°. (Section
4.7)
Table 1.2.6.1 |
Recovery from Anasorb CMS, % |
|
target concn |
enflurane |
halothane |
isoflurane |
|
1 ppm |
94.6 |
97.1 |
93.7 |
50 ppm |
|
94.5 |
|
75 ppm |
96.2 |
| 97.2 |
|
- refrigerated storage test at 4° |
Table 1.2.6.2 |
Recovery from Anasorb 747, % |
|
target concn |
enflurane |
halothane |
isoflurane |
|
1ppm |
99.6 |
99.8 |
98.7 |
50 ppm |
|
99.3 |
|
75 ppm |
98.0 |
|
97.9 |
|
1.2.7 Reproducibility
Forty-eight samples collected from controlled test atmospheres, along with a draft copy of this
procedure, were submitted for analysis by one of the OSHA Salt Lake Technical Center's service
branch laboratories. The samples were analyzed after 17-23 days of storage at 4°. No
indiividual sample result deviated from its theoretical value by more than the precision reported
in Section 1.2.5. (Section 4.8)
2. Sampling Procedure
2.1 Apparatus
2.1.1
Samples are collected using a personal sampling pump calibrated, with the sampling device
attached, within ±5% at the recommended flow rate.
2.1.2 Samples are collected with 7-cm × 4-mm i.d. × 6-mm o.d. glass sampling tubes packed with
two sections of (150/75 mg) Anasorb CMS or (140/70 mg) Anasorb 747. The sections are held in
place with a glass wool plug and two urethane foam plugs. For this evaluation, commercially
prepared sampling tubes were purchased from SKC, Inc. (catalog nos. 226-121 and 226-81).
2.2 Reagents
None required.
2.3 Technique
2.3.1 Only properly trained personnel can sample in an operating room or dental office, this is
necessary to be in compliance with OSHA's Exposure Control Plan for bloodborne pathogens. (Ref. 5.10)
2.3.2 Immediately before sampling, break off the ends of the sampling tube. All tubes should be from the same lot.
2.3.3 Attach the sampling tube to the sampling pump with flexible, non-crimping tubing. It is
desirable to utilize sampling tube holders which have a protective cover to shield the employee
from the sharp, jagged end of the sampling tube. Position the tube so that the sampled air first
passes through the larger section.
2.3.4 Air being sampled should not pass through any hose or tubing before entering the sampling tube.
2.3.5 To avoid channeling, attach the sampler vertically with the larger section pointing
downward, in the worker's breathing zone. Position the sampler so it does not impede work
performance or safety.
2.3.6 After sampling for the appropriate time, immediately remove the sampling tube and seal it
with plastic end caps.
2.3.7 In order to prevent occupational exposure to SLTC personnel, sampling tubes that may
become contaminated with blood or other potentially infectious materials are to be examined
prior to shipping and decontaminated (e.g., wiped off with bleach or other disinfectant) as
necessary. Contaminated items are not to be placed or stored in areas where food is kept,
and decontamination should be accomplished as soon as possible following the inspection where
contamination occurred. Decontamination is not to take place in any area where food or drink is
consumed. (Ref. 5.10)
2.3.8 Wrap each sample end-to-end with a Form OSHA-21 seal.
2.3.9 Submit at least one blank sample with each set of samples. Handle the blank sampling tube in the same manner as the other samples, except draw no air through it.
2.3.10 Record sample air volumes (in liters) for each sample, along with any potential interferences.
2.3.11 Ship any bulk sample(s) in a container separate from the air samples.
2.3.12 Submit the samples to the laboratory for analysis as soon as possible after sampling. If delay is unavoidable, store the samples at reduced temperature.
2.4 Sampler capacity
Sampler capacity is determined by measuring how much air can be sampled before the analyte
breaks through the sampler, i.e., the sampler capacity is exceeded. Breakthrough is considered to occur when the effluent from the sampler contains a concentration of analyte that is 5% of the
upstream concentration (5% breakthrough). Testing for breakthrough was performed by using an
FID to monitor the effluent from sampling tubes containing only either the 150-mg section of
Anasorb CMS or 140-mg section of Anasorb 747. Dynamically generated test atmospheres,
which were about two times the higher target concentration of each analyte, were used for the
capacity tests. The samples were collected at 0.05 L/min and the relative humidity was about
80% at 25°. The 5% breakthrough air volumes were calculated from the data of duplicate
determinations and are listed below. (Section 4.9)
Table 2.4 |
Sampler Capacity |
|
analyte |
atmospheric |
Anasorb |
Anasorb |
|
concentration |
CMS |
747 |
|
enflurane |
165 ppm |
28.8 L |
14.2 L |
|
(1247 mg/m3) |
halothane |
93 ppm |
15.8 L |
19.9 L |
|
(753 mg/m3) |
isoflurane |
165 ppm |
24.0 L |
17.5 L |
|
(1246 mg/m3) |
|
2.5 Desorption efficiency
2.5.1 The average desorption efficiencies for the analyses from the sampling media over the
range of 0.5 to 2.0 times the target concentrations (TC) are listed below. (Section 4.10)
Table 2.5.1 |
Desorption Efficiencies, % |
|
analyte |
Anasorb CMS |
Anasorb 747 |
|
low TC |
high TC |
low TC |
high TC |
|
enflurane |
100.3 |
99.8 |
103.7 |
100.5 |
halothane |
99.7 |
99.5 |
99.6 |
99.3 |
isoflurane |
99.4 |
99.2 |
100.8 |
100.2 |
|
2.5.2 The desorption efficiencies at 0.05, 0.1 and 0.2 times the target concentrations (TC) were
found to be very high and are listed below. (Section 4.10)
Table 2.5.2.1 |
Desorption Efficiencies at 0.05 to 0.2 times Low TC, % |
|
analyte |
Anasorb CMS |
Anasorb 747 |
|
0.05×Tc |
0.1×TC |
0.2×TC |
0.05×TC |
0.1×TC |
0.2×TC |
|
enflurane |
100.2 |
100.4 |
99.5 |
101.3 |
99.0 |
99.0 |
halothane |
99.6 |
100.5 |
99.8 |
84.3 |
92.6 |
94.7 |
isoflurane |
99.3 |
98.4 |
99.9 |
96.8 |
100.0 |
101.1 |
|
Table 2.5.2.2 |
Desorption Efficiencies at 0.05 to 0.2 times High TC, % |
|
analyte |
Anasorb CMS |
Anasorb 747 |
|
0.05×TC |
0.1×TC |
0.2×TC |
0.05×TC |
0.1×TC |
0.2×TC |
|
enflurane |
100.1 |
99.8 |
99.8 |
100.2 |
100.0 |
100.3 |
halothane |
99.3 |
98.9 |
98.5 |
99.6 |
98.6 |
100.4 |
isoflurane |
100.0 |
99.3 |
99.2 |
98.0 |
97.2 |
99.0 |
|
2.5.3 Desorbed samples remain stable for at least 22.5 h.
2.6 Recommended air volume and sampling rate
2.6.1 For long-term samples, collect 12 L at 0.05 L/min.
2.6.2 For short-term samples, collect 0.75 L at 0.05 L/min.
2.6.3 When short-term samples are collected, the air concentration equivalent to the reliable
quantitation limit becomes larger.
Table 2.6.3 |
Reliable Quantitabon Limits at 0.75 L |
|
adsorbent |
enflurane |
halothane |
isoflurane |
|
Anasorb CMS |
2.26 µg |
2.36µg |
2.08 µg |
|
399 ppb |
390 ppb |
368 ppb |
|
3013 µg/m3 |
3147 µg/m3 |
2773 µg/m3 |
Anasorb 747 |
3.68 µg |
2.07 µg |
2.13 µg |
|
651 ppb |
342 ppb |
377 ppb |
|
4707 µg/m3 |
2760 µg/m3 |
2840 µg/m3 |
|
2.7 Interferences (sampling)
2.7.1 It is not known if any compounds will severely interfere with the collection of enflurane,
halothane and isoflurane on Anasorb CMS or Anasorb 747. In general, the presence of other
contaminant vapors in the air will reduce the capacity of Anasorb CMS or Anasorb 747 to collect
the three analyses.
2.7.2 Nitrous oxide was tested as an interferant to the collection of halothane and it does not
interfere. (Section 4.12)
2.7.3 Suspected interferences should be reported to the laboratory with submitted samples.
2.8 Safety precautions (sampling)
2.8.1 The sampling equipment should be attached to the worker in such a manner
that it will not interfere with work performance or safety.
2.8.2 All safety practices that apply to the work area being sampled should be followed.
2.8.3 Protective eyewear should be worn when breaking the ends of the glass sampling tubes.
3. Analybcal Procedure
3.1 Apparatus
3.1.1 Gas chromatograph equipped with an FID. For this evaluation, a Hewlett-Packard 5890A
Gas Chromatograph equipped with a 7673A Automatic Sampler was used. A Forma Scientific
Model 2006 refrigerated circulator was used to cool the sample tray of the HP 7673A to 10°
to minimize evaporation.
3.1.2 A GC column capable of separating the analyte of interest from the desorption solvent,
internal standard and any interferences. A 60-m × 0.32-mm i.d. fused silica Stabilwax-D8419
column with a 1-µm df (Restek Corp., Bellefonte, PA) was used in the evaluation.
3.1.3 An electronic integrator or some other suitable means of measuring peak areas. A Waters
860 Networking Computer System was used in this evaluation.
3.1.4 Two-milliliter vials with polytetrafluoroethylene-lined caps.
3.1.5 A dispenser capable of delivering 1.0 mL of desorbing solvent to prepare standards and
samples. If a dispenser is not available, a 1.0-mL volumetric pipes may be used.
3.2 Reagents
Enflurane, USP. The enflurane used in this evaluation was manufactured by Anequest (Madison,
WI), and purchased from a local hospital.
3.2.2 Halothane, reagent grade or better. The halothane used in this evaluation was purchased
from Aldrich Chemical (Milwaukee, WI).
3.2.3 Isoflurane, USP. The isoflurane used in this evaluation was manufactured by Anequest
(Madison, WI), and purchased from a local hospital.
3.2.4 Carbon disulfide (CS2), reagent grade or better.
The CS2 used in this evaluation was
purchased from JT Baker Chemical (Phillipsburg, NJ).
3.2.5 A suitable internal standard, reagent grade. The n-decane used in this evaluation was
purchased from ICN Pharmaceuticals, Inc. (Plainview, NY).
3.2.6 Desorption solvent. The desorption solvent contains 500 µL of n-decane per 1 L
of CS2.
3.2.7 GC grade nitrogen, air, and hydrogen.
3.2.8 Toluene, chromatographic grade or better. The toluene used in this evaluation was Optima
Grade and was purchased from Fisher Scientific (Fair Lawn, NJ).
3.3 Standard preparation
3.3.1 Prepare concentrated stock standard of enflurane, halothane and isoflurane in toluene.
Prepare working analytical standards by injecting microliter amounts of concentrated stock
standards into 2-mL vials containing 1.0 mL of desorption solvent delivered from the same
dispenser used to desorb samples. For example, to prepare a target level standard of isoflurane,
inject 10 µL of a stock solution containing 672 mg/mL of isoflurane in toluene into 1 mL of
desorption solvent.
3.3.2 Bracket sample concentrations with working standard concentrations. If samples fall
outside the concentration range of prepared standards, prepare and analyze additional standards
or dilute the sample.
3.4 Sample preparation
3.4.1 Remove the plastic end caps from the sample tube and carefully transfer each section of the
adsorbent to separate 2-mL vials. Discard the glass tube, urethane foam plugs and glass wool
plug.
3.4.2 Add 1.0 mL of desorption solvent to each vial using the same dispenser as used for
preparation of standards.
3.4.3 Immediately seal the vials with polytetrafluoroethylene-lined caps.
3.4.4 Shake the vials vigorously several times during the next 30 min.
3.5 Analysis
3.5.1 Analytical conditions
GC conditions |
zone temperatures: |
60° (column) 250° (injector) 300° (detector) |
run time: |
15 min |
column gas flow: |
1.2 mL/min (hydrogen) |
septum purge: |
1.5 mL/min (hydrogen) |
injector size: |
1.0 µL (11.3:1 split) |
column: |
60-m × 0.32-mm i.d. capillary Stabilwax-DB (1.0-µm df) |
retention times: |
5.50 min (isoflurane) 5.97 min (halothane) 6.51 min (enflurane) 8.34 min (n-decane) |
FID conditions |
hydrogen flow: |
34 mL/min |
air flow: |
450 mL/min |
makeup flow: |
33 mL/min (nitrogen) |
Figure 3.5.1.1. Chromatogram obtained at the high TC with the recommended condibons. Peak
identification: (1) carbon disutfide, (2) isoflurane, (3) halothane, (4) enflurane, (5) benzene -
contaminant in CS2, (6) n-decane,
(7) toluene - from spiking solution.
Figure 3.5.1.2. Chromatogram obtained at the low TC with the recommended conditions. Peak
identification: (1) carbon disulfide, (2) isoflurane, (3) halothane, (4) enflurane, (5) benzene -
contaminant in CS2, (6) n-decane,
(7) toluene - from spiking solution.
3.5.2 An internal standard (ISTD) calibration method is used. A calibration curve can be
constructed by plotting micrograms of analyte per sample versus ISTD-corrected response of
standard injections. Bracket the samples with freshly prepared analytical standards over a range
of concentrations.
Figure 3.5.2.1. Calibrabon curve of enflurane at low TC made from data of Table 4.5.1.
Figure 3.5.2.2. Calibrabon curve of enflurane at high TC made from data of Table 4.5.2.
Figure 3.5.2.3. Calibrabon curve of halothane at low TC made from data of Table 4.5.3.
Figure 3.5.2.4. Calibration curve of halothane at high TC made from data of Table 4.5.4.
Figure 3.5.2.5. Calibration curve of isoflurane at low TC made from data of Table 4.5.5.
Figure 3.5.2.6. Calibration curve of isoflurane at high TC made from data of Table 4.5.6.
3.6 Interferences (analytical)
3.6.1 Any compound that produces an FID response and has a similar retention time as the
analyses or internal standard is a potential interference. If any potential interferences were
reported, they should be considered before the samples are desorbed.
3.6.2 Generally, chromatographic conditions can be altered to separate an interference from the analyte.
3.6.3 When necessary, the identity or purity of an analyte peak may be confirmed with additional analytical data. (Section 4.11)
3.7 Calculations
The amount of analyte per sampler is obtained from the appropriate calibration curve in terms
of micrograms per sample, uncorrected for desorption efficiency. The back (70-75 mg) section is
analyzed primarily to determine if there was any breakthrough from the front (140-150 mg)
section during sampling. If a significant amount of analyte is found on the back section (e.g.,
greater than 25% of the amount found on the front section), this fact should be reported with the
sample results. If any analyte is found on the back section, it is added to the amount on the front
section. This amount is then corrected by subtracting the total amount (if any) found on the
blank. The air concentration is calculated using the following formulae.
mg/m3 =
|
micrograms of analyte per sample liters of air sampled × desorption efficiency
|
ppm =
|
24.46 × mg/m3 molecular weight of analyte
|
where |
24.46 is the molar volume at 25° and 101.3 kPa (760 mmHg) |
|
184.49 = molecular weight of enflurane and isoflurane |
|
197.39 = molecular weight of halothane |
3.8 Safety precautions (analytical)
3.8.1 Adhere to the rules set down in your Chemical Hygiene Plan.
3.8.2 Avoid skin contact and inhalation of all chemicals.
3.8.3 Wear safety glasses, gloves and a lab coat at all ffmes while in the laboratory areas.
4. Backup Data
4.1 Determination of detection limits
Detection limits, in general, are defined as the amount (or concentration) of analyte that gives a
response (YDL) that is significantly different
[three standard deviations (SDBR)] from the
background response (YBR).
YDL - YBR = 3(SDBR)
The measurement of YBR and SDBR in chromatographic
methods is typically inconvenient and difficult because YBR is usually
extremely low. Estimates of these parameters can be made with data obtained from the analysis
of a series of analytical standards or samples whose responses are
in the vicinity of the background response. The regression curve obtained for a plot of instrument
response versus concentration of analyte will usually be linear. Assuming SDBR and
the precision of the data about curve are similar, the standard error of estimate (SEE) for the regression curve
can be substituted for SDBR in the above equation. The following
calculations derive a formula for DL:
Yobs = |
observed response |
Yest = |
estimated response from regression curve |
n = |
total number of data points |
k = |
2 for linear regression curve |
At point YDL on the regression curve
YDL - A(DL) + YBR |
A = analytical sensitivity (slope) |
therefore
Substituting 3(SEE) + YBR for YDL gives
4.2 Detection limit of the analytical procedure (DW)
The DW is measured as the mass of analyte actually introduced into the chromatographic
columns. Ten analytical standards were prepared in equal descending increments with the highest
standard containing 10.02, 10.68 and 9.89 µg/mL of enflurane, halothane and isoflurane
respecffvely. This is the concentration that would produce a peak approximately 10 times the
baseline noise of a reagent blank near the elution time of the analyte. These standards, and the
reagent blank, were analyzed with the recommended analytical parameters (1-µL injection
with a 11.3:1 split), and the data obtained were used to determine the required parameters (A and
SEE) for the calculation of the DLAP.
Table 4.2.1 |
DLAP Data for Enflurane |
A = 3.81 SEE = 117.9 |
|
concentration |
mass on column |
area counts |
(µg/mL) |
(pg) |
(µV-s) |
|
0 |
0 |
0 |
0.956 |
84.4 |
455 |
1.90 |
168 |
840 |
2.84 |
251 |
1002 |
3.77 |
333 |
1145 |
5.60 |
494 |
2090 |
6.50 |
574 |
2105 |
7.39 |
653 |
2610 |
8.28 |
731 |
2869 |
9.15 |
808 |
3041 |
10.02 |
884 |
3519 |
|
Figure 4.2.1 Plot of the data from Table 4.2.1 to determine the DLAP of enflurane, DLAP = 92.8 pg.
Table 4.2.2 |
DLAP Data for Halothane |
A = 4.08 SEE = 118.7 |
|
concentration |
mass on column |
area counts |
(µg/mL) |
(pg) |
(µV-s) |
|
0 |
0 |
0 |
1.02 |
90 |
413 |
2.03 |
179 |
916 |
3.03 |
267 |
1219 |
5.97 |
527 |
2366 |
6.93 |
612 |
2501 |
7.88 |
696 |
2907 |
8.82 |
779 |
3219 |
9.76 |
861 |
3416 |
10.68 |
943 |
4035 |
|
Figure 4.2.2. Plot of the data from Table 4.2.2 to determine the DW of halothane, DLAP = 87.3 pg.
Table 4.2.3 |
DLAP Data for Isoflurane |
A = 2.34 SEE = 34.90 |
|
concentration |
mass on column |
area counts |
(µg/mL) |
(pg) |
(µV-s) |
|
0 |
0 |
0 |
0.944 |
83 |
288 |
1.88 |
166 |
421 |
2.80 |
247 |
627 |
3.72 |
328 |
794 |
5.53 |
488 |
1230 |
6.41 |
566 |
1307 |
7.30 |
644 |
1537 |
8.17 |
721 |
1711 |
9.03 |
797 |
1921 |
9.89 |
873 |
2090 |
|
Figure 4.2.3 Plot of the data from Table 4.2.3 to determine the DLAP of isoflurane, DLAP = 44.7 pg.
4.3 Detection limit of the overall procedure (DLOP)
The DLOP is measured as mass per sample and expressed as equivalent air concentration, based
on the recommended sampling parameters. Ten samplers were spiked with equal descending
increments of analyte, such that the highest sampler loading was 9.15, 9.76 and 9.03
µg/sample of enflurane, halothane and isoflurane respectively. This is the amount, when
spiked on a sampler, that would produce a peak approximately 10 times the baseline noise for a
sample blank. These spiked samplers, plus a sample blank, were analyzed with the recommended
analytical parameters, and the data obtained used to calculate the required parameters (A and
SEE) for the calculation of the DLOP.
Table 4.3.1 |
DLOP Data for Enflurane |
|
mass per |
area counts on |
area counts on |
sample |
Anasorb CMS |
Anasorb 747 |
(µg) |
(µV-s) |
(µV-s) |
|
0.956 |
441 |
292 |
1.90 |
651 |
735 |
2.84 |
1042 |
1109 |
3.77 |
1423 |
1449 |
4.69 |
1618 |
1690 |
5.60 |
1858 |
1786 |
6.50 |
2084 |
2430 |
7.39 |
2378 |
2393 |
8.28 |
2635 |
2749 |
9.15 |
3035 |
3238 |
|
Figure 4.3.1.1. Plot of the data to determine the DLOP of enflurane on Anasorb CMS, (SEE = 71.55).
Figure 4.3.1.2. Plot of the data to determine the DLOP of enflurane on Anasorb 747, (SEE = 124.5).
Table 4.3.2 |
DLOP Data for Halothane |
|
mass per |
area counts on |
area counts on |
sample |
Anasorb CMS |
Anasorb 747 |
(µg) |
(µV-s) |
(µV-s) |
|
0 |
0 |
0 |
1.02 |
512 |
382 |
2.03 |
761 |
812 |
3.03 |
1224 |
1263 |
4.02 |
1554 |
1670 |
5.00 |
1870 |
1999 |
5.97 |
2192 |
2481 |
6.93 |
2526 |
2795 |
7.88 |
2721 |
3059 |
8.82 |
3288 |
3319 |
9.76 |
3677 |
3761 |
|
Figure 4.3.2.1. Plot of the data to determine the DLOP of halothane on Anasorb CMS, (SEE = 85.02).
Figure 4.3.2.2 Plot of the data to determine the DLOP of halothane on Anasorb 747, (SEE = 79.37).
Table 4.3.3 |
DLOP Data for Isodurane |
|
mass per |
area counts on |
area counts on |
sample |
Anasorb CMS |
Anasorb 747 |
(µg) |
(µV-s) |
(µV-s) |
|
0 |
0 |
0 |
0.944 |
274 |
245 |
1.88 |
444 |
442 |
2.80 |
654 |
630 |
3.72 |
845 |
813 |
4.63 |
963 |
1041 |
5.53 |
1195 |
1088 |
6.41 |
1349 |
1326 |
7.30 |
1564 |
1488 |
8.17 |
1622 |
1615 |
9.03 |
1877 |
1825 |
|
Figure 4.3.3.1. Plot of the data to determine the DLOP of isoflurane on Anasorb CMS, (SEE = 41.65).
Figure 4.3.3.2. Plot of the data to determine the DLOP of isoflurane on Anasorb 747, (SEE = 41.51).
4.4 Reliable quantitation limit (RQL)
The RQL is considered the lower limit for precise quantitative measurements. It is determined
from the regression line parameters obtained for the calculations of the DLOP (Section 4.3),
providing at least 75% of the analyte is recovered. The RQL is defined as the amount of analyte
that gives a response (YRQL) such that
YRQL - YBR = 10(SDBR)
therefore
Figure 4.4.1. Chromatogram of the RQL for all three analyses on Anasorb CMS.
Figure 4.4.2. Chromatogram of the RQL for halothane and isoflurane on Anasorb 747.
Figure 4.4.3. Chromatogram of the RQL for enflurane on Anasorb 747.
Table 4.4 |
Reliable Quantitation Limits |
|
adsorbent |
enflurane |
halothane |
isoflurane |
|
Anasorb CMS |
2.26 µg |
2.36 µg |
9 2.08 µg |
|
225 ppb |
219 ppb |
207 ppb |
|
1695 µg/m3 |
1770 µg/m3 |
1560µg/m3 |
|
91.7% |
95.9% |
104.1% |
Anasorb 747 |
3.68 µg |
2.07 µg |
2.13 µg |
|
366 ppb |
192 ppb |
212 ppb |
|
2760 µg/m3 |
1553 µg/m3 |
1598 µg/m3 |
|
109.2% |
102.9% |
103.6% |
|
The RQL for each analyte was calculated and listed above along with the recovery of the analyte
peak near the RQL.
4.5 Precision (analytical method)
The precision of the analytical procedure is measured as the pooled relative standard deviation
(RSDP). Relative standard deviations are determined from six replicate
injections of analyte standards at 0.5, 0.75, 1, 1.5 and 2 times the target concentration.
After assuring that the RSDs satisfy the Cochran test for homogeneity at the 95% confidence
level, RSDP was calculated.
Table 4.5.1 |
Instrument Response to Enflurane at Low TC |
|
× target concn |
0.5× |
0.75× |
1× |
1.5× |
2× |
(µg/mL) |
45.6 |
68.4 |
91.2 |
136.8 |
182.4 |
|
area counts |
5802 |
8044 |
11502 |
15685 |
21003 |
(µV-s) |
5762 |
7971 |
11748 |
15514 |
20685 |
|
5592 |
8178 |
11513 |
15995 |
19527 |
|
5604 |
8024 |
10887 |
16911 |
20585 |
|
5898 |
8173 |
11441 |
15579 |
19114 |
|
5902 |
8146 |
11336 |
15502 |
19871 |
![mean](/dts/sltc/methods/images/mean.gif) |
5760 |
8089 |
11405 |
15864 |
20131 |
SD |
136.8 |
87.6 |
287.4 |
544.1 |
740.3 |
RSD (%) |
2.37 |
1.08 |
2.52 |
3.42 |
3.67 |
|
Table 4.5.2 |
Instrument Response to Enflurane at High TC |
|
× target concn |
0.5× |
0.75× |
1× |
1.5× |
2× |
(µg/mL) |
3405 |
5108 |
6810 |
10215 |
13620 |
|
area counts |
313768 |
442725 |
588885 |
909618 |
1266303 |
(µV-s) |
295385 |
449118 |
614061 |
884040 |
1231585 |
|
306119 |
444388 |
600184 |
888369 |
1239847 |
|
302927 |
452003 |
605174 |
873998 |
1195472 |
|
302101 |
463954 |
583097 |
872158 |
1232590 |
|
315239 |
450679 |
623083 |
934700 |
1220325 |
![mean](/dts/sltc/methods/images/mean.gif) |
305923 |
450478 |
602414 |
893814 |
1231020 |
SD |
7523.3 |
7523.5 |
15044.1 |
24117.5 |
23253.5 |
RSD (%) |
2.45 |
1.67 |
2.48 |
2.69 |
1.88 |
|
Table 4.5.3 |
Instrument Response to Halothane at Low TC |
|
× target concn |
0.5× |
0.75× |
1× |
1.5× |
2× |
(µg/mL) |
48.62 |
72.93 |
97.24 |
145.9 |
194.5 |
|
area counts |
4652 |
6892 |
9563 |
14067 |
19459 |
(µV-s) |
4572 |
6936 |
9438 |
14324 |
18888 |
|
4781 |
6802 |
9773 |
14181 |
18732 |
|
4625 |
6931 |
9501 |
14180 |
19216 |
|
4630 |
6802 |
9694 |
14534 |
18964 |
|
4609 |
6960 |
9404 |
14271 |
19499 |
![mean](/dts/sltc/methods/images/mean.gif) |
4645 |
6887 |
9562 |
14260 |
19126 |
SD |
71.8 |
69.5 |
145.6 |
160.7 |
315.0 |
RSD (%) |
1.54 |
1.00 |
1.52 |
1.12 |
1.64 |
|
Table 4.5.4 |
Instrument Response to Halothane at High TC |
|
× target concn |
0.5× |
0.75× |
1× |
1.5× |
2× |
(µg/mL) |
2431 |
3646 |
4862 |
7293 |
9724 |
|
area counts |
214963 |
31920 |
427008 |
631533 |
876733 |
(µV-s) |
211987 |
326882 |
426550 |
625176 |
856581 |
|
218236 |
322866 |
430225 |
620733 |
870877 |
|
215433 |
325338 |
429946 |
632545 |
849740 |
|
214585 |
329467 |
436427 |
647793 |
860103 |
|
207597 |
319337 |
433215 |
623791 |
847012 |
![mean](/dts/sltc/methods/images/mean.gif) |
213800 |
323849 |
430562 |
630262 |
860174 |
SD |
3635.3 |
4144.4 |
3759.2 |
9723.2 |
11694.2 |
RSD (%) |
1.70 |
1.27 |
0.87 |
1.54 |
1.35 |
|
Table 4.5.5 |
Instrument Response to Isoflurane at Low TC |
|
× target concn |
0.5× |
0.75× |
1× |
1.5× |
2× |
(µg/mL) |
45.0 |
67.5 |
90.0 |
135.0 |
180.0 |
|
area counts |
3164 |
4584 |
6793 |
9544 |
14068 |
(µV-s) |
3083 |
4690 |
6928 |
9750 |
13672 |
|
3239 |
4700 |
6791 |
10564 |
13408 |
|
2983 |
4510 |
6209 |
10076 |
12670 |
|
3120 |
4546 |
6809 |
9707 |
13257 |
|
3147 |
4757 |
6621 |
9820 |
12437 |
![mean](/dts/sltc/methods/images/mean.gif) |
3123 |
4631 |
6692 |
9910 |
13252 |
SD |
85.9 |
98.2 |
256.0 |
364.5 |
611.5 |
RSD (%) |
2.75 |
2.11 |
3.82 |
3.67 |
4.61 |
|
Table 4.5.6 |
Instrument Response to Isoflurane at High TC |
|
× target concn |
0.5× |
0.75× |
1× |
1.5× |
2× |
(µg/mL) |
3360 |
5040 |
6720 |
10080 |
13440 |
|
area counts |
192010 |
285648 |
377707 |
560192 |
831803 |
(µV-s) |
198666 |
302263 |
389365 |
536323 |
808032 |
|
196337 |
286004 |
390013 |
576197 |
832183 |
|
197101 |
283263 |
392882 |
581411 |
807540 |
|
184540 |
294184 |
416447 |
572522 |
811381 |
|
202374 |
287224 |
410104 |
564809 |
803188 |
![mean](/dts/sltc/methods/images/mean.gif) |
95171 |
289764 |
396086 |
565242 |
815688 |
SD |
6199.9 |
7149.2 |
14430.4 |
16102.5 |
12896.4 |
RSD (%) |
3.17 |
2.46 |
3.64 |
2.84 |
1.58 |
|
The Cochran test for homogeneity:
The critical value of the g-statistic, at the 95% confidence level, for five variances, each
associated with six observations is 0.5065. Because the g-statistic does not exceed this value, the
RSDs can be considered equal and they can be pooled (RSDP) to
give an estimated RSD for the concentration range studied.
Table 4.5.7 |
Cochran Test Results and Pooled Relative Standard Deviations |
|
|
enflurane |
halothane |
isoflurane |
|
TC |
low |
high |
low |
high |
low |
high |
g |
0.3515 |
0.2808 |
0.2785 |
0.3058 |
0.3465 |
0.3317 |
RSDP % |
2.77 |
2.27 |
1.39 |
1.37 |
3.50 |
2.83 |
|
4.6 Precision (overall procedure)
The precision of the overall procedure is determined from the storage data in Section 4.7. The
determination of the standard error of estmate (SEER) for a
regression line ptotted through the graphed storage data allows the inclusion of
storage time as one of the factors affecting overall precision. The SEER is
similar to the standard deviation, except it is a measure of the dispersion
of data about a regression line instead of about a mean. It is determined with the following
equation:
Yobs |
= |
observed % recovery at a given time |
Yest |
= |
estimated % recovery from the regression line at the same given time |
n |
= |
total number of data points |
k |
= |
2 for linear regression |
k |
= |
3 for quadratic regression |
An additional 5% for pump error (SP) is added to the SEER by
the addition of variances to obtain the total standard error of the estimate.
The precision at the 95% confidence level is obtained by multiplying the standard error of
estimate (with pump error included) by 1.96 (the z-statistic from the standard normal distribution
at the 95% confidence level). The 95% confidence intervals are drawn about their respective
regression lines in the storage graphs, as shown in figures 4.7.1.1.1 through 4.7.2.6.2. The
precisions of the overall procedure and the assodated figures are listed below.
Table 4.6.1 |
Precision of the Overall Procedure on Anasorb CMS, % |
|
target concn |
enflurane |
halothane |
isoflurane |
|
1 ppm |
14.1 |
14.9 |
15.3 |
|
Fig. 4.7.2.1.1 |
Fig. 4.7.2.3.2 |
Fig. 4.7.2.5.1 |
50 ppm |
|
13.7 |
|
|
|
Fig 4.7.1.3.1 |
|
75 ppm |
16.3 |
|
16.6 |
|
Fig. 4.7.1.1.1 |
|
Fig. 4.7.1.5.1 |
|
Table 4.6.2 |
Precision of the Overall Procedure on Anasorb 747, % |
|
target concn |
enflurane |
halothane |
isoflurane |
|
1 ppm |
11.3 |
10.6 |
11.5 |
|
Fig. 4.7.2.2.1 |
Fig. 4.7.2.4.1 |
Fig. 4.7.2.6.1 |
50 ppm |
|
11.4 |
|
|
|
Fig. 4.7.1.4.1 |
|
75 ppm |
15.1 |
|
12.0 |
|
Fig. 4.7.1.2.1 |
|
Fig. 4.7.1.6.1 |
|
4.7 Storage test
4.7.1 Analyte storage at high target concentration
4.7.1.1 Storage samples were generated by sampling from a controlled test atmosphere
containing 2120 mg/m3 of enflurane,
about 3.7 times the 75-ppm target concentration. Anasorb
CMS tubes were used to sample for 60 min at 0.05 L/min, the relative humidity was about 80%
at 22°. Thirty-six storage samples were prepared. Six samples were analyzed immediately
after generation, fifteen tubes were stored at reduced temperature (4°) and the other fifteen
were stored in a closed drawer at ambient temperature (about 22°). At 2-4 day intervals,
three samples were selected from each of the two sets and analyzed.
Table 4.7.1.1 |
Storage Test for Enflurane on Anasorb CMS |
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery (%) |
|
0 |
90.0 |
101.5 |
98.0 |
90.0 |
101.5 |
98.0 |
|
101.9 |
103.4 |
95.3 |
101.9 |
103.5 |
95.3 |
3 |
101.0 |
101.6 |
94.6 |
90.9 |
88.3 |
95.6 |
6 |
102.1 |
105.1 |
107.3 |
111.1 |
103.6 |
98.7 |
9 |
101.8 |
104.1 |
95.4 |
90.7 |
97.0 |
100.5 |
13 |
97.8 |
88.4 |
91.9 |
98.3 |
112.7 |
103.3 |
15 |
91.1 |
102.7 |
90.7 |
92.0 |
100.2 |
102.3 |
|
Figure 4.7.1.1.1. Ambient storage test for enflurane on Anasorb CMS.
Figure 4.7.1.1.2. Refrigerated storage test for enflurane on Anasorb CMS.
4.7.1.2 Storage samples were generated by sampling from a controlled test atmosphere
containing 2118 mg/m3 of enflurane, about 3.7 times the 75-ppm target concentration. Anasorb
747 tubes were used to sample for 60 min at 0.05 L/min, the relative humidity was about 80% at
22°. Thirty-six storage samples were prepared. Six samples were analyzed immediately after
generation, fifteen tubes were stored at reduced temperature (4°) and the other fifteen were
stored in a closed drawer at ambient temperature (about 22°). At 2-4 day intervals, three
samples were selected from each of the two sets and analyzed.
Table 4.7.1.2 |
Storage Test for Enflurane on Anasorb 747 |
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery (%) |
|
0 |
96.3 |
97.4 |
106.9 |
96.3 |
97.4 |
106.9 |
|
102.1 |
101.7 |
102.5 |
102.1 |
101.7 |
102.5 |
2 |
92.4 |
84.7 |
100.8 |
96.9 |
101.4 |
98.2 |
6 |
92.0 |
104.1 |
97.6 |
95.1 |
96.9 |
99.6 |
9 |
102.2 |
96.7 |
106.3 |
93.1 |
104.2 |
99.0 |
12 |
97.2 |
112.2 |
105.2 |
102.1 |
103.0 |
105.6 |
16 |
102.0 |
102.6 |
105.7 |
99.1 |
112.2 |
106.9 |
|
Figure 4.7.1.2.1 Ambient storage test for enflurane on Anasorb 747.
Figure 4.7.1.2.2. Refrigerated storage test for enflurane on Anasorb 747.
4.7.1.3 Storage samples were generated by sampling from a controlled test atmosphere
containing 2146 mg/m3 of halothane, about 5.3 times the 50-ppm target concentration. Anasorb
CMS tubes were used to sample for 60 min at 0.05 L/min, the relative humidity was about 80%
at 22°. Thirty-six storage samples were prepared. Six samples were analyzed immediately
after generation, fifteen tubes were stared at reduced temperature (4°) and the other fifteen
were stored in a closed drawer at ambient temperature (about 22°). At 24 day intervals, three samples were selected from each of the two sets and analyzed.
Table 4.7.1.3 |
Storage Test for Halothane on Anasorb CMS |
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery (%) |
|
0 |
103.3 |
104.3 |
90.8 |
103.3 |
104.3 |
90.8 |
|
98.3 |
95.5 |
98.7 |
98.3 |
95.5 |
98.7 |
4 |
101.5 |
95.4 |
96.9 |
106.6 |
91.4 |
99.6 |
6 |
103.2 |
88.7 |
96.0 |
99.1 |
95.8 |
98.8 |
8 |
103.5 |
101.1 |
97.7 |
108.3 |
92.9 |
100.4 |
12 |
106.0 |
91.0 |
94.5 |
108.7 |
102.0 |
102.3 |
15 |
96.06 |
91.1 |
93.6 |
103.6 |
90.6 |
101.1 |
|
Figure 4.7.1.3.1. Ambient storage test for halothane on Anasorb CMS.
Figure 4.7.1.3.2. Refrigerated storage test for halothane on Anasorb CMS
4.7.1.4 Storage samples were generated by sampling from a controlled test atmosphere
containing 2305 mg/m3 of halothane, about 5.7 times the 50-ppm target concentration. Anasorb
747 tubes were used to sample for 60 min at 0.05 L/min, the relative humidity was about 80% at
22°. Thirty-six storage samples were prepared. Six samples were analyzed immediately after
generation, fifteen tubes were stored at reduced temperature (4°) and the other fifteen were
stored in a closed drawer at ambient temperature (about 22°). At 3-4 day intervals, three
samples were selected from each of the two sets and analyzed.
Table 4.7.1.4 |
Storage Test for Halothane on Anasorb 747 |
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery(%) |
|
0 |
99.1 |
100.0 |
103.9 |
99.1 |
100.0 |
103.9 |
|
100.5 |
99.7 |
96.9 |
100.5 |
99.7 |
96.9 |
3 |
99.4 |
99.2 |
96.2 |
98.6 |
104.2 |
98.9 |
6 |
98.8 |
104.2 |
98.8 |
101.5 |
100.1 |
97.3 |
10 |
99.1 |
103.5 |
94.9 |
100.9 |
105.0 |
101.3 |
13 |
95.8 |
104.5 |
98.7 |
101.3 |
95.7 |
95.5 |
17 |
103.8 |
104.8 |
99.6 |
102.7 |
105.9 |
99.2 |
|
Figure 4.7.1.4.1. Ambient storage test for halothane on Anasorb 747.
Figure 4.7.1.4.2. Refrigerated storage test for halothane on Anasorb 747.
4.7.1.5 Storage samples were generated by sampling from a controlled test atmosphere
containing 3050 mg/m3 of isoflurane, about 5.4 times the 75-ppm target concentration. Anasorb
CMS tubes were used to sample for 60 min at 0.05 L/min the relative humidity was about 80% at
22°. Thirty-six storage samples were prepared. Six samples were analyzed immediately after
generation, fifteen tubes were stored at reduced temperature (4°) and the other fifteen were
stored in a closed drawer at ambient temperature (about 22°). At 2-4 day intervals, three
samples were selected from each of the two sets and analyzed.
Table 4.7.1.5 |
Storage Test for Isoflurane on Anasorb CMS |
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery (%) |
|
0 |
99.7 |
103.6 |
93.9 |
99.7 |
103.6 |
93.6 |
|
99.0 |
85.4 |
97.8 |
99.0 |
85.4 |
97.8 |
4 |
111.9 |
104.8 |
97.5 |
106.7 |
91.7 |
92.1 |
7 |
99.2 |
94.2 |
90.2 |
108.8 |
103.0 |
100.6 |
11 |
113.1 |
102.9 |
102.3 |
106.5 |
99.1 |
91.4 |
13 |
103.9 |
96.4 |
92.0 |
108.0 |
105.3 |
103.6 |
15 |
108.0 |
105.1 |
106.1 |
105.0 |
100.3 |
96.8 |
|
Figure 4.7.1.5.1. Ambient storage test for isoflurane on Anasorb CMS.
Figure 4.7.1.5.2. Refrigerated storage test for isoflurane on Anasorb CMS.
4.7.1.6 Storage samples were generated by sampling from a controlled test atmosphere
containing 2992 mg/m3 of isoflurane, about 5.3 times
the 75-ppm target concentration. Anasorb 747 tubes were used to sample for 60 min
at 0.05 L/min, the relative humidity was about 80% at 22°. Thirty-six storage
samples were prepared. Six samples were analyzed immediately after
generation, fifteen tubes were stored at reduced temperature (4°) and the other fifteen were
stored in a dosed drawer at ambient temperature (about 22°). At 3-4 day intervals, three
samples were selected from each of the two sets and analyzed.
Table 4.7.1.6 |
Storage Test for Isoflurane on Anasorb 747 |
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery (%) |
|
0 |
92.3 |
99.3 |
99.1 |
92.3 |
99.3 |
99.1 |
|
99.6 |
100.6 |
101.5 |
99.6 |
100.6 |
101.5 |
4 |
99.6 |
97.4 |
102.6 |
97.0 |
92.1 |
98.2 |
7 |
92.5 |
94.9 |
101.0 |
103.2 |
102.8 |
103.5 |
10 |
100.5 |
103.2 |
102.5 |
98.0 |
97.0 |
100.7 |
14 |
103.1 |
100.6 |
108.3 |
106.8 |
102.4 |
105.9 |
18 |
107.7 |
100.1 |
105.1 |
103.1 |
100.5 |
104.1 |
|
Figure 4.7.1.6.1. Ambient storage test for isoflurane on Anasorb 747.
Figure 4.7.1.6.2. Refrigerated storage test for isoflurane on Anasorb 747.
4.7.2 Analyte storage at low target concentration
4.7.2.1 Storage samples were generated by sampling from a controlled test atmosphere
containing 58.2 mg/m3 of enflurane, about 7.7 times the 1-ppm target concentration. Anasorb
CMS tubes were used to sample for 30 min at 0.05 L/min, the relative humidity was about 80%
at 22°. Thirty-six storage samples were prepared. Six samples were analyzed immediately
after generation, fifteen tubes were stored at reduced temperature (4°) and the other fifteen
were stored in a closed drawer at ambient temperature (about 22°). At 2-4 day intervals,
three samples were selected from each of the two sets and analyzed.
Table 4.7.2.1 |
|
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery (%) |
|
0 |
82.6 |
88.7 |
94.1 |
82.6 |
88.7 |
94.1 |
|
98.8 |
98.3 |
102.9 |
98.8 |
98.3 |
102.9 |
4 |
90.1 |
92.9 |
97.0 |
90.4 |
101.0 |
101.7 |
7 |
91.6 |
99.9 |
102.2 |
96.6 |
103.9 |
99.0 |
11 |
99.1 |
96.6 |
100.9 |
90.0 |
100.8 |
96.9 |
13 |
88.3 |
95.9 |
97.3 |
104.9 |
97.7 |
98.1 |
15 |
96.3 |
92.1 |
95.6 |
86.6 |
93.0 |
102.0 |
|
Figure 4.7.2.1.1. Ambient storage test for enflurane on Anasorb CMS.
Figure 4.7.2.1.2. Refrigerated storage test for enflurane on Anasorb CMS.
4.7.2.2 Storage samples were generated by sampling from a controlled test atmosphere
containing 59.4 mg/m3 of enflurane, about 7.9 times the 1-ppm target concentration. Anasorb 747
tubes were used to sample for 30 min at 0.05 L/min, the relative humidity was about 80% at
22°. Thirty-six storage samples were prepared. Six samples were analyzed immediately after
generation, fifteen tubes were stored at reduced temperature (4°) and the other fifteen were
stored in a closed drawer at ambient temperature (about 22°). At 2-6 day intervals, three
samples were selected from each of the two sets and analyzed.
Table 4.7.2.2 |
Storage Test for Enflurane on Anasorb 747 |
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery (%) |
|
0 |
101.8 |
93.4 |
96.5 |
101.8 |
93.4 |
96.5 |
|
100.0 |
103.4 |
98.3 |
100.0 |
103.4 |
98.3 |
3 |
102.3 |
98.9 |
97.3 |
99.0 |
96.3 |
101.1 |
6 |
101.7 |
104.0 |
102.9 |
98.8 |
101.8 |
100.3 |
12 |
98.3 |
100.2 |
96.4 |
98.0 |
98.2 |
101.3 |
14 |
101.1 |
101.3 |
102.7 |
102.2 |
104.2 |
96.7 |
18 |
98.6 |
99.0 |
95.8 |
106.9 |
100.7 |
103.0 |
|
![graph](/dts/sltc/methods/organic/org103/org103_44fig47221.gif)
Figure 4.7.2.2.1. Ambient storage test for enflurane on Anasorb 747.
![graph](/dts/sltc/methods/organic/org103/org103_45fig47222.gif)
Figure 4.7.2.2.2. Refrigerated storage test for enflurane on Anasorb 747.
4.7.2.3 Storage samples were generated by sampling from a controlled test atmosphere
containing 70.1 mg/m3 of halothane, about 8.7 times the
1-ppm target concentration. Anasorb CMS tubes were used to sample for 30 min
at 0.05 L/min, the relative humidity was about 80% at 22°. Thirty-six
storage samples were prepared. Six samples were analyzed immediately
after generation, fifteen tubes were stored at reduced
temperature (4°) and the other fifteen were stored in a closed drawer
at ambient temperature (about 22°). At 2-5 day intervals,
three samples were selected from each of the two sets and analyzed.
Table 4.7.2.3 |
Storage Test for Halothane on Anasorb CMS |
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery (%) |
|
0 |
91.7 |
93.8 |
98.7 |
91.7 |
93.8 |
98.7 |
|
101.1 |
103.6 |
106.9 |
101.1 |
103.6 |
106.9 |
3 |
80.6 |
88.4 |
95.5 |
89.3 |
95.4 |
105.5 |
8 |
78.8 |
85.6 |
90.1 |
92.6 |
99.3 |
100.5 |
12 |
79.2 |
85.3 |
92.4 |
86.5 |
107.4 |
100.0 |
14 |
77.2 |
86.9 |
98.0 |
97.0 |
98.6 |
101.2 |
16 |
73.4 |
80.0 |
92.0 |
92.5 |
94.4 |
100.2 |
|
![graph](/dts/sltc/methods/organic/org103/org103_46fig47231.gif)
Figure 4.7.2.3.1. Ambient storage test for halothane on Anasorb CMS.
![graph](/dts/sltc/methods/organic/org103/org103_47fig47232.gif)
Figure 4.7.2.3.2. Refrigerated storage test for halothane on Anasorb CMS.
4.7.2.4 Storage samples were generated by sampling from a controlled test atmosphere
containing 71.2 mg/m3 of halothane, about 8.8 times the 1-ppm target concentration. Anasorb
747 tubes were used to sample for 30 min at 0.05 L/min, the relative humidity was about 80% at
22°. Thirty-six storage samples were prepared. Six samples were analyzed immediately after
generation, fifteen tubes were stored at reduced temperature (4°) and the other fifteen were
stored in a closed drawer at ambient temperature (about 22°). At 2-4 day intervals, three
samples were selected from each of the two sets and analyzed.
Table 4.7.2.4 |
Storage Test for Halothane on Anasorb 747 |
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery (%) |
|
0 |
97.8 |
104.5 |
97.5 |
97.8 |
104.5 |
97.5 |
|
99.4 |
101.0 |
99.8 |
99.4 |
101.0 |
99.8 |
3 |
99.2 |
102.0 |
98.0 |
97.3 |
99.0 |
103.4 |
6 |
- |
100.2 |
100.8 |
98.4 |
105.3 |
97.1 |
9 |
104.5 |
103.7 |
101.0 |
98.9 |
111.2 |
102.6 |
13 |
101.0 |
102.7 |
100.6 |
106.0 |
102.3 |
99.7 |
15 |
105.7 |
103.0 |
101.4 |
113.3 |
101.0 |
101.1 |
|
![graph](/dts/sltc/methods/organic/org103/org103_48fig47241.gif)
Figure 4.7.2.4.1. Ambient storage test for halothane on Anasorb 747.
![graph](/dts/sltc/methods/organic/org103/org103_49fig47242.gif)
Figure 4.7.2.4.2. Refrigerated storage test for halothane on Anasorb 747.
4.7.2.5 Storage samples were generated by sampling from a controlled test atmosphere
containing 50.4 mg/m3 of isoflurane, about 6.7 times the 1-ppm target concentration. Anasorb
CMS tubes were used to sample for 30 min at 0.05 L/min, the relative humidity was about 80%
at 22°. Thirty-six storage samples were prepared. Six samples were analyzed immediately
after generation, fifteen tubes were stored at reduced temperature (4°) and the other fifteen
were stored in a closed drawer at ambient temperature (about 22°). At 24 day intervals, three
samples were selected from each of the two sets and analyzed.
Table 4.7.2.5 |
Storage Test for Isoflurane on Anasorb CMS
|
|
time
| ambient storage
| refrigerated storage
|
(days)
| recovery (%)
| recovery (%)
|
|
0
| 79.1
| 88.1
| 91.8
| 79.1
| 88.1
| 91.8
|
| 98.9
| 98.0
| 103.2
| 98.9
| 98.0
| 103.2
|
4
| 97.8
| 96.5
| 101.7
| 90.7
| 101.8
| 105.7
|
7
| 91.5
| 97.4
| 102.2
| 94.5
| 103.7
| 100.8
|
11
| 97.6
| 94.0
| 98.7
| 89.3
| 102.3
| 100.0
|
13
| 85.4
| 95.1
| 98.0
| 105.3
| 98.9
| 96.1
|
15
| 92.1
| 87.4
| 92.7
| 85.0
| 89.4
| 99.4
|
|
![graph](/dts/sltc/methods/organic/org103/org103_50fig47251.gif)
Figure 4.7.2.5.1. Ambient storage test for isonurane on Anasorb CMS.
![graph](/dts/sltc/methods/organic/org103/org103_51fig47252.gif)
Figure 4.7.2.5.2. Refrigerated storage test for isoflurane on Anasorb CMS.
4.7.2.6 Storage samples were generated by sampling from a controlled test atmosphere
containing 52.7 mg/m3 of isoflurane, about 7 times the 1-ppm target concentration. Anasorb 747
tubes were used to sample for 30 min at 0.05 L/min, the relative humidity was about 80% at
22°. Thirty-six storage samples were prepared. Six samples were analyzed immediately after
generation, fifteen tubes were stored at reduced temperature (4°) and the other fifteen were
stored in a closed drawer at ambient temperature (about 22°). At 2-6 day intervals, three
samples were selected from each of the two sets and analyzed.
Table 4.7.2.6 |
Storage Test for Isoflurane on Anasorb 747 |
|
time |
ambient storage |
refrigerated storage |
(days) |
recovery (%) |
recovery (%) |
|
0 |
102.3 |
90.5 |
96.7 |
102.3 |
90.5 |
96.7 |
|
100.0 |
104.2 |
96.8 |
100.0 |
104.2 |
96.8 |
3 |
101.8 |
98.0 |
98.4 |
100.7 |
97.4 |
102.0 |
6 |
102.5 |
102.6 |
101.2 |
98.4 |
102.3 |
100.6 |
12 |
97.7 |
98.5 |
96.7 |
99.9 |
100.5 |
102.3 |
14 |
99.5 |
99.5 |
100.9 |
102.8 |
101.6 |
96.0 |
16 |
98.4 |
96.9 |
97.0 |
107.6 |
101.8 |
103.2 |
|
![graph](/dts/sltc/methods/organic/org103/org103_52fig47261.gif)
Figure 4.7.2.6.1. Ambient storage test for isoflurane on Anasorb 747.
![graph](/dts/sltc/methods/organic/org103/org103_53fig47262.gif)
Figure 4.7.2.6.2. Refrigerated storage test for isoflurane on Anasorb 747.
4.8 Reproducibility
4.8.1 Analyte reproducibility at high target concentration
4.8.1.1 Six samples for each adsorbent were prepared by collecting them from a 75-ppm
controlled test atmosphere containing enflurane and isoflurane for 4 h at 0.05 L/min. The
samples were submitted to an OSHA Salt Lake Technical Center service branch. The samples
were analyzed after being stored for 21 days at 4°. Sample results were corrected for
desorption efficiency. No sample result for enflurane or isoflurane had a deviation greater than
the precision of the overall procedure determined in Section 4.6.
Table 4.8.1.1.1 |
Reproducibility Data for Enflurane |
|
|
Anasorb CMS |
Anasorb 747 |
sample |
expected |
reported |
recovery |
deviation |
reported |
recovery |
deviation |
|
(mg/m3) |
(mg/m3) |
(%) |
(%) |
(mg/m3) |
(%) |
(%) |
|
1 |
570 |
546.3 |
95.9 |
-4.1 |
517.6 |
90.8 |
-9.2 |
2 |
570 |
517.3 |
90.9 |
-9.1 |
533.1 |
93.5 |
-6.5 |
3 |
570 |
544.1 |
95.5 |
-4.5 |
520.3 |
91.3 |
-8.7 |
4 |
570 |
556.9 |
97.7 |
-2.3 |
532.1 |
93.4 |
-6.6 |
5 |
570 |
518.7 |
91.0 |
-9.0 |
499.6 |
87.7 |
-12.3 |
6 |
570 |
536.9 |
94.2 |
-5.8 |
524.0 |
91.9 |
-8.1 |
|
Table 4.8.1.1.2 |
Reproducibility Data for Isoflurane |
|
|
Anasorb CMS |
Anasorb 747 |
sample |
expected |
reported |
recovery |
deviabon |
reported |
recovery |
deviation |
|
(mg/m3) |
(mg/m3) |
(%) |
(%) |
(mg/m3) |
(%) |
(%) |
|
1 |
562.5 |
596.6 |
106.1 |
+6.1 |
562.3 |
100.0 |
0 |
2 |
562.5 |
550.2 |
97.8 |
-2.2 |
576.6 |
102.5 |
+2.5 |
3 |
562.5 |
591.1 |
105.1 |
+5.1 |
564.0 |
100.3 |
+0.3 |
4 |
562.5 |
609.0 |
108.3 |
+8.3 |
578.1 |
102.8 |
+2.8 |
5 |
562.5 |
564.8 |
100.3 |
+0.3 |
540.3 |
96.1 |
-3.9 |
6 |
562.5 |
587.4 |
104.4 |
+4.4 |
569.2 |
101.2 |
1.2 |
|
4.8.1.2 Six samples for each adsorbent were prepared by collecting them from a 50-ppm
controlled test atmosphere containing halothane for 4 h at 0.05 L/min. The samples were
submilted to an OSHA Salt Lake Technical Center service branch. The samples were analyzed
after being stored for 17 days at 4°. Sample results were corrected for desorption efficiency.
No sample result for halothane had a deviation greater than the precision of the overall procedure
determined in Section 4.6.
Table 4.8.1.2 |
Reproducibility Data for Halothane |
|
|
Anasorb CMS |
Anasorb 747 |
sample |
expected |
reported |
recovery |
deviation |
reported |
recovery |
deviation |
|
(mg/m3) |
(mg/m3) |
(%) |
(%) |
(mg/m3) |
(%) |
(%) |
|
1 |
408 |
411.0 |
100.7 |
+0.7 |
406.2 |
99.6 |
-0.4 |
2 |
408 |
406.6 |
99.7 |
-0.3 |
411.1 |
100.8 |
+0.8 |
3 |
408 |
402.8 |
98.7 |
-1.3 |
411.5 |
100.8 |
+0.8 |
4 |
408 |
409.8 |
100.4 |
+0.4 |
410.6 |
100.6 |
+0.6 |
5 |
408 |
399.7 |
98.0 |
-2.0 |
401.7 |
98.5 |
-1.5 |
6 |
408 |
406.4 |
99.6 |
-0.4 |
408.1 |
100.0 |
0 |
|
4.8.2 Analyte reproducibility at low target concentration
4.8.2.1 Six samples for each adsorbent were prepared by collecting them from a 1-ppm
controlled test atmosphere containing enflurane and isoflurane for 4 h at 0.05 L/min. The
samples were submitted to an OSHA Salt Lake Technical Center service branch. The samples
were analyzed after being stored for 22 days at 4°. Sample results were corrected for
desorption efficiency. No sample result for enflurane and isoflurane had a deviation greater than
the precision of the overall procedure determined in Section 4.6.
Table 4.8.2.1.1 |
Reproducibility Data for Enflurane |
|
|
Anasorb CMS |
Anasorb 747 |
sample |
expected |
reported |
recovery |
deviation |
reported |
recovery |
deviation |
|
(mg/m3) |
(mg/m3) |
(%) |
(%) |
(mg/m3) |
(%) |
(%) |
|
1 |
7.62 |
8.02 |
105.2 |
+5.2 |
7.81 |
102.5 |
+2.5 |
2 |
7.62 |
7.58 |
99.5 |
-0.5 |
7.82 |
102.6 |
+2.6 |
3 |
7.62 |
7.62 |
100.0 |
0 |
7.82 |
102.6 |
+2.6 |
4 |
7.62 |
6.55 |
86.0 |
-14.0 |
6.95 |
91.2 |
-8.8 |
5 |
7.62 |
7.58 |
99.5 |
-0.5 |
7.73 |
101.4 |
+1.4 |
6 |
7.62 |
7.65 |
100.4 |
+0.4 |
8.48 |
111.3 |
+11.3 |
|
Table 4.8.2.3 |
Reproducibility Data for Isoflurane |
|
|
Anasorb CMS |
Anasorb 747 |
sample |
expected |
reported |
recovery |
deviation |
reported |
recovery |
deviation |
|
(mg/m3) |
(mg/m3) |
(%) |
(%) |
(mg/m3) |
(%) |
(%) |
|
1 |
7.52 |
7.74 |
102.9 |
+2.9 |
7.91 |
105.2 |
+5.2 |
2 |
7.52 |
7.47 |
99.3 |
-0.7 |
8.22 |
109.3 |
+9.3 |
3 |
7.52 |
7.65 |
101.7 |
+1.7 |
8.32 |
110.6 |
+10.6 |
4 |
7.52 |
6.58 |
87.5 |
-12.5 |
7.09 |
94.3 |
-5.7 |
5 |
7.52 |
7.15 |
95.1 |
-4.9 |
8.22 |
109.3 |
+9.3 |
6 |
7.52 |
7.59 |
100.9 |
+0.9 |
7.70 |
102.4 |
+2.4 |
|
4.8.2.2 Six samples for each adsorbent were prepared by collecting them from a 1-ppm
controlled test atmosphere containing halothane for 4 h at 0.05 L/min. The samples were
submitted to an OSHA Salt Lake Technical Center service branch. The samples were analyzed
after being stored for 23 days at 4°. Sample results were corrected for desorption efficiency.
No sample result for halothane had a deviation greater than the precision of the overall procedure
determined in Section 4.6.
Table 4.8.2.2 |
Reproducibility Data for Halothane |
|
|
Anasorb CMS |
Anasorb 747 |
sample |
expected |
reported |
recovery |
deviation |
reported |
recovery |
deviation |
|
(mg/m3) |
(mg/m3) |
(%) |
(%) |
(mg/m3) |
(%) |
(%) |
|
1 |
8.40 |
7.38 |
37.9 |
-12.1 |
8.79 |
104.6 |
+4.6 |
2 |
8.40 |
7.80 |
92.9 |
-7.1 |
8.53 |
101.5 |
+1.5 |
3 |
8.40 |
8.32 |
99.0 |
-1.0 |
9.03 |
107.5 |
+7.5 |
4 |
8.40 |
7.93 |
94.4 |
-5.6 |
8.81 |
104.9 |
+4.9 |
5 |
8.40 |
8.20 |
97.6 |
-2.4 |
8.70 |
103.6 |
+3.6 |
6 |
8.40 |
8.67 |
103.2 |
+3.2 |
8.93 |
106.3 |
+6.3 |
|
4.9 Sampler capacity
4.9.1 Anasorb CMS
4.9.1.1 The sampling capacity of the front section of an Anasorb CMS sampling tube was tested
by sampling from a dynamically generated test atmosphere of
enflurane (1247 mg/m3 or 165
ppm). The samples were collected at 0.05 L/min and the relative humidity was about 80% at
22°. A GC with a gas sampling valve was placed in-line behind the 150-mg front test
section. The valve was rotated to measure the amount of enflurane passing through the sampler at
the time of rotation. The 5% breakthrough air volume was determined to be 28.8 L.
Table 4.9.1.1 |
Capacity of Enflurane on Anasorb CMS |
|
first test |
second test |
air volume |
breakthrough |
air volume |
breakthrough |
(L) |
(%) |
(L) |
(%) |
|
17.54 |
0 |
16.39 |
0 |
18.24 |
0.79 |
17.11 |
0.27 |
19.62 |
1.57 |
20.76 |
0.69 |
21.93 |
2.07 |
20.97 |
1.04 |
23.18 |
2.50 |
22.18 |
1.34 |
24.19 |
2.87 |
22.90 |
1.57 |
25.06 |
3.23 |
24.20 |
1.98 |
26.12 |
3.93 |
25.55 |
2.38 |
26.99 |
4.41 |
26.46 |
2.83 |
28.48 |
5.03 |
27.57 |
3.33 |
29.23 |
5.59 |
27.72 |
3.81 |
29.99 |
6.25 |
28.44 |
4.24 |
|
Figure 4.9.1.1. Five percent breakthrough air volume for enflurane on Anasorb CMS.
4.9.1.2 The sampling capacity of the front section of an Anasorb CMS sampling tube was tested
by sampling from a dynamically generated test atmosphere of halothane (753 mg/m3 or 93.3
ppm). The samples were collected at 0.05 L/min and the relative humidity was about 80% at
22°. A GC with a gas sampling valve was placed in-line behind the 150-mg front test
section. The valve was rotated to measure the amount of halothane passing through the sampler
at the time of rotation. The 5% breakthrough air volume was determined to be 15.8 L.
Table 4.9.1.2 |
Capacity of Halothane on Anasorb CMS |
|
first test |
second test |
air volume |
breakthrough |
air volume |
breakthrough |
(L) |
(%) |
(L) |
(%) |
|
5.88 |
0 |
6.06 |
0 |
7.10 |
0 |
7.26 |
0 |
8.37 |
0 |
8.52 |
0 |
12.42 |
3.11 |
12.53 |
3.08 |
12.93 |
3.28 |
13.03 |
3.21 |
13.44 |
3.71 |
13.53 |
3.65 |
13.94 |
4.11 |
14.03 |
4.00 |
14.55 |
4.53 |
14.63 |
4.29 |
15.06 |
4.64 |
15.13 |
4.47 |
15.56 |
4.97 |
15.63 |
4.72 |
16.07 |
5.26 |
16.13 |
4.96 |
16.58 |
5.74 |
16.63 |
5.19 |
17.09 |
5.83 |
17.73 |
5.58 |
17.59 |
6.24 |
17.64 |
5.87 |
18.10 |
6.32 |
|
Figure 4.9.1.2. Five percent breakthrough air volume for haothane on Anasorb CMS.
4.9.1.3 The sampling capacity of the front section of an Anasorb CMS sampling tube was tested
by sampling from a dynamically generated test atmosphere of isoflurane (1246 mg/m3 or 165
ppm). The samples were collected at 0.05 L/min and the relative humidity was about 80% at
22°. A GC with a gas sampling valve was placed in-line behind the 150-mg front test sector.
The valve was rotated to measure the amount of isoflurane passing through the sampler at the
time of rotation. The 5% breakthrough air volume was determined to be 24.0 L.
Table 4.9.1.3 |
Capacity of Isoflurane on Anasorb CMS |
|
first test |
second test |
air volume |
breakthrough |
air volume |
breakthrough |
(L) |
(%) |
(L) |
(%) |
|
9.10 |
0 |
10.10 |
0 |
13.48 |
0.42 |
14.11 |
0.96 |
14.51 |
0.73 |
15.12 |
1.42 |
15.50 |
1.03 |
16.13 |
1.76 |
16.48 |
1.39 |
17.14 |
1.96 |
17.76 |
1.75 |
18.50 |
2.42 |
19.19 |
2.36 |
20.06 |
3.15 |
20.41 |
2.86 |
21.17 |
3.74 |
21.50 |
3.24 |
22.27 |
4.24 |
22.68 |
3.67 |
23.49 |
5.21 |
23.86 |
4.32 |
24.70 |
6.16 |
24.85 |
4.65 |
25.70 |
6.89 |
|
Figure 4.9.1.3. Five percent breakthrough air volume for isoflurane on Anasorb CMS.
4.9.2 Anasorb 747
4.9.2.1 The sampling capacity of the front section of an Anasorb 747 sampling tube was tested
by sampling from a dynamically generated test atmosphere of enflurane (1247 mg/m3 or 165
ppm). The samples were collected at 0.05 L/min and the relative humidity was about 80% at
22°. A GC with a gas sampling valve was placed in-line behind the 140-mg front test
section. The valve was rotated to measure the amount of enflurane passing through the sampler at
the time of rotation. The 5% breakthrough air volume was determined to be 14.2 L.
Table 4.9.2.1 |
Capacity of Enflurane on Anasorb 747 |
|
first test |
second test |
air volume |
breakthrough |
air volume |
breakthrough |
(L) |
(%) |
(L) |
(%) |
|
9.85 |
0 |
10.10 |
0 |
13.13 |
1.40 |
13.43 |
2.22 |
13.69 |
3.12 |
13.94 |
3.98 |
14.24 |
5.61 |
14.49 |
6.29 |
14.75 |
7.77 |
15.00 |
8.12 |
15.25 |
9.13 |
15.50 |
9.95 |
|
Figure 4.9.2.1. Five percent breakthrough air volume for enflurane on Anasorb 747.
4.9.2.2 The sampling capacity of the front section of an Anasorb 747 sampling tube was tested
by sampling from a dynamically generated test atmosphere of halothane (753 mg/m3 or 93.3
ppm). The samples were collected at 0.05 L/min and the relative humidity was about 80% at
22°. A GC with a gas sampling valve was placed in-line behind the 140-mg front test
section. The valve was rotated to measure the amount of halothane passing through the sampler
at the time of rotation. The 5% breakthrough air volume was determined to be 19.9 L.
Table 4.9.2.2 |
Capacity of Halothane on Anasorb 747 |
|
first test |
second test |
air volume |
breakthrough |
air volume |
breakthrough |
(L) |
(%) |
(L) |
(%) |
|
16.07 |
0 |
16.13 |
0 |
17.34 |
0 |
17.38 |
0 |
18.86 |
0.52 |
18.89 |
0.45 |
19.87 |
2.56 |
19.94 |
2.37 |
20.18 |
5.06 |
20.19 |
4.86 |
20.43 |
8.67 |
20.44 |
8.70 |
20.69 |
12.58 |
20.69 |
12.70 |
|
Figure 4.9.2.2. Five percent breakthrough air volume for halothane on Anasorb 747.
4.9.2.3 The sampling capacity of the front section of an Anasorb 747 sampling tube was tested
by sampling from a dynamically generated test atmosphere of isoflurane (1246 mg/m3 or 165
ppm). The samples were collected at 0.05 L/min and the relative humidity was about 80% at
22°. A GC with a gas sampling valve was placed in-line behind the 140-mg front test
section. The valve was rotated to measure the amount of isoflurane passing through the sampler
at the time of rotation. The 5% breakthrough air volume was determined to be 17.5 L.
Table 4.9.2.3 |
Capacity of Isoflurane on Anasorb 747 |
|
first test |
second test |
air volume |
breakthrough |
air volume |
breakthrough |
(L) |
(%) |
(L) |
(%) |
|
11.21 |
0 |
10.66 |
0 |
12.20 |
0 |
11.62 |
0 |
13.20 |
0.18 |
12.68 |
0.12 |
13.94 |
0.35 |
13.64 |
0.61 |
14.44 |
0.59 |
14.39 |
1.12 |
14.94 |
0.93 |
14.90 |
1.59 |
15.44 |
1.36 |
15.40 |
2.13 |
15.94 |
1.94 |
15.91 |
2.86 |
16.43 |
2.50 |
16.41 |
3.72 |
16.93 |
3.29 |
16.92 |
4.62 |
17.43 |
4.07 |
17.42 |
5.56 |
17.93 |
4.85 |
17.93 |
6.69 |
18.43 |
5.73 |
18.43 |
7.69 |
|
|
18.94 |
8.76 |
|
Figure 4.9.2.3 Five percent breakthrough air volume for isoflurane on Anasorb 747.
4.10 Desorption efficiency and stability of desorbed samples
4.10.1 Anasorb CMS at high target concentration (TC)
4.10.1.1 Enflurane
The desorption efficiencies (DE) of enflurane were determined by liquid-spiking150 mg portions
of Anasorb CMS with amounts equivalent to 0.05 to 2 times the 75-ppm target concentration.
These samples were stored overnight at ambient temperature and then desorbed and analyzed.
The average desorption emciency over the working range of 0.5 to 2 times the target
concentration is 99.8%.
Table 4.10.1.1.1 |
Desorbtion Efficiency of Enflurane from Anasorb CMS at High TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
340.5 |
681 |
1362 |
3403 |
6810 |
13620 |
|
DE (%) |
101.4 |
98.5 |
100.2 |
100.2 |
99.8 |
99.3 |
|
98.7 |
98.3 |
97.2 |
99.6 |
98.2 |
98.9 |
|
100.5 |
100.3 |
100.1 |
99.9 |
100.6 |
98.9 |
|
98.9 |
100.7 |
101.6 |
101.2 |
100.7 |
100.1 |
|
100.8 |
100.0 |
99.6 |
100.3 |
99.7 |
97.8 |
|
100.1 |
100.7 |
100.2 |
101.0 |
101.0 |
99.2 |
![mean](/dts/sltc/methods/images/mean.gif) |
100.1 |
99.8 |
99.8 |
100.4 |
100.0 |
99.0 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after intial analysis. After the original analysis was performed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was -2.0% for samples that were
resealed with new septa, and -4.2% for those that retained their punctured septa.
Table 4.10.1.1.2 |
Stability of Desorbed Samples for Enflurane from Anasorb CMS |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
99.8 |
97.3 |
-2.5 |
100.7 |
98.7 |
-2.0 |
98.2 |
96.7 |
-1.5 |
99.7 |
95.4 |
-4.3 |
100.6 |
98.6 |
-2.0 |
101.0 |
94.8 |
-6.2 |
|
(averages) |
|
|
(averages) |
|
99.5 |
97.5 |
-2.0 |
100.5 |
96.3 |
-4.2 |
|
4.10.1.2. Halothane
The desorption efficiencies (DE) of halothane were determined by liquid-spiking 150-mg
portions of Anasorb CMS with amounts equivalent to 0.05 to 2 times the 50-ppm target
concentration. These samples were stored overnight at ambient temperature and then desorbed
and analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the
target concentration is 99.5%.
Table 4.10.1.2.1 |
Desorption Efficiency of Halothane from Anasorb CMS at High TC |
|
×target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
243.1 |
486.2 |
972.4 |
2431 |
4862 |
9724 |
|
DE (%) |
99.4 |
98.6 |
98.9 |
99.1 |
99.8 |
99.6 |
|
99.6 |
98.5 |
96.5 |
98.8 |
98.0 |
99.9 |
|
97.4 |
99.1 |
98.5 |
101.8 |
100.0 |
99.4 |
|
101.0 |
99.3 |
99.5 |
99.6 |
99.7 |
100.1 |
|
99.0 |
98.9 |
98.3 |
99.5 |
99.2 |
98.6 |
|
99.2 |
99.0 |
99.1 |
99.8 |
99.9 |
98.5 |
![mean](/dts/sltc/methods/images/mean.gif) |
99.3 |
98.9 |
98.5 |
99.8 |
99.4 |
99.4 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after initial analysis. After the original analysis was performed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was -1.5% for samples that were
resealed with new septa, and -3.4% for those that retained their punctured septa.
Table 4.10.1.2.2 |
Stability of Desorbed Samples for Halothane from Anasorb CMS |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
99.8 |
97.4 |
-2.4 |
99.7 |
97.7 |
-2.0 |
98.0 |
97.1 |
-0.9 |
99.2 |
96.1 |
-3.1 |
100.0 |
98.8 |
-1.2 |
99.9 |
94.8 |
-5.1 |
|
(averages) |
|
|
(averages) |
|
99.3 |
97.8 |
-1.5 |
99.6 |
96.2 |
-3.4 |
|
4.10.1.3 Isoflurane
The desorption efficiencies (DE) of isoflurane were determined by liquid-spiking 150-mg
portions of Anasorb CMS with amounts equivalent to 0.05 to 2 times the 75-ppm target
concentration. These samples were stored overnight at ambient temperature and then desorbed
and analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the
target concentration is 99.2%.
Table 4.10.1.3.1 |
Desorption Efficiency of Isoflurane from Anasorb CMS at High TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
336 |
672 |
1344 |
3360 |
6720 |
13440 |
|
DE (%) |
100.2 |
97.3 |
99.6 |
99.8 |
99.1 |
97.6 |
|
99.2 |
99.3 |
99.4 |
99.3 |
97.6 |
97.3 |
|
98.7 |
99.9 |
100.9 |
99.4 |
99.7 |
97.8 |
|
101.3 |
100.2 |
99.3 |
100.7 |
99.7 |
98.5 |
|
100.9 |
99.1 |
99.5 |
100.2 |
103.3 |
96.8 |
|
99.9 |
99.9 |
96.5 |
100.8 |
99.5 |
98.1 |
![mean](/dts/sltc/methods/images/mean.gif) |
100.0 |
99.3 |
99.2 |
100.0 |
99.8 |
97.7 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after initial analysis. After the original analysis was performed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was -2.3% for samples that were
resealed with new septa, and -4.1% for those that retained their punctured septa.
Table 4.10.1.3.2 Stability of Desorbed Samples for Isoflurane from Anasorb CMS |
|
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
99.1 |
96.2 |
-2.9 |
99.7 |
98.0 |
-1.7 |
97.6 |
95.5 |
-2.1 |
103.3 |
98.1 |
-5.2 |
99.7 |
97.8 |
-1.9 |
99.5 |
93.9 |
-5.4 |
|
(averages) |
|
|
(averages) |
|
98.8 |
96.5 |
-2.3 |
100.8 |
96.7 |
-4.1 |
|
4.10.2 Anasorb 747 at high target concentration (TC)
4.1 0.2.1 Enflurane
The desorption efficiencies (DE) of.enflurane were determined by liquid-spiking 140-mg
portions of Anasorb 747 with amounts equivalent to 0.05 to 2 times the75-ppm target
cocentration. These samples were stored overnight at ambient temperature and then desorbed and
analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the target
concentration is 100.5%.
Table 4.10.2.1.1 |
Desorption Effidency of Enflurane from Anasorb 747 at High TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
340.5 |
681 |
1362 |
3405 |
6810 |
13620 |
|
DE (%) |
100.9 |
100.6 |
101.4 |
98.9 |
103.9 |
99.5 |
|
99.1 |
99.1 |
98.0 |
100.0 |
100.9 |
100.3 |
|
101.1 |
99.5 |
98.4 |
98.9 |
105.3 |
102.6 |
|
101.7 |
99.6 |
102.5 |
98.3 |
99.5 |
101.0 |
|
99.9 |
101.8 |
102.0 |
100.6 |
100.2 |
102.3 |
|
98.6 |
99.6 |
99.7 |
97.6 |
100.5 |
97.5 |
![mean](/dts/sltc/methods/images/mean.gif) |
100.2 |
100.0 |
100.3 |
99.1 |
101.8 |
100.5 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after initial analysis. After the original analysis was perfommed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was -0.5% for samples that were
resealed with new septa, and -3.7% for those that retained their punctured septa.
Table 4.10.2.1.2 |
Stability of Desorbed Samples for Enflurane from Anasorb 747 |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
99.5 |
99.4 |
-0.1 |
105.3 |
99.3 |
-6.0 |
100.2 |
98.9 |
-1.3 |
103.9 |
99.8 |
-4.1 |
100.5 |
100.3 |
-0.2 |
100.9 |
99.8 |
-1.1 |
|
(averages) |
|
|
(averages) |
|
100.1 |
99.5 |
-0.5 |
103.4 |
99.6 |
-3.7 |
|
4.10.2.2 Halothane
The desorption efficiencies (DE) of halothane were determined by liquid-spiking 140-mg
portions of Anasorb 747 with amounts equivalent to 0.05 to 2 times the 5-ppm target
concentration. These samples were stored overnight at ambient temperature and then desorbed
and analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the
target concentration is 99.3%.
Table 4.10.2.2.1 |
Desorption Efficiency of Halothane from Anasorb 747 at High TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
243.5 |
486.2 |
972.4 |
2431 |
4862 |
9724 |
|
DE (%) |
98.9 |
98.9 |
100.0 |
99.9 |
99.3 |
99.1 |
|
98.7 |
98.2 |
98.1 |
-100.1 |
100.6 |
98.4 |
|
100.4 |
98.2 |
101.5 |
100.2 |
100.1 |
100.7 |
|
100.6 |
98.3 |
100.4 |
100.5 |
96.5 |
99.6 |
|
100.4 |
98.1 |
101.3 |
99.3 |
96.6 |
101.1 |
|
98.7 |
99.9 |
100.8 |
100.7 |
97.0 |
97.1 |
![mean](/dts/sltc/methods/images/mean.gif) |
99.6 |
98.6 |
100.4 |
100.1 |
98.4 |
99.3 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after infflal analysis. After the original analysis was performed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was +1.5% for samples that were
resealed with new septa, and -1.6% for those that retained their punctured septa.
Table 4.10.2.2.2 |
Stability of Desorbed Samples for Halothane from Anasorb 747 |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
96.5 |
96.6 |
+0.1 |
99.3 |
98.0 |
-1.36 |
96.6 |
98.6 |
+2.0 |
100.6 |
99.0 |
-1.6 |
97.0 |
99.3 |
+2.3 |
100.1 |
98.3 |
-1.8 |
|
(averages) |
|
|
(averages) |
|
96.7 |
98.2 |
+1.5 |
100.0 |
98.4 |
-1.6 |
|
4.10.2.3 Isoflurane
The desorption effciencies (DE) of isoflurane were determined by liquid-spiking 140-mg
portions of Anasorb 747 with amounts equivalent to 0.05 to 2 times the 75-ppm target
concentration. These samples were stored overnight at ambient temperature and then desorbed
and analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the
target concentration is 100.2%.
Table 4.10.2.3.1 |
Desorption Efficiency of Isoflurane from Anasorb 747 at High TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
336 |
672 |
1344 |
3360 |
6720 |
13440 |
|
DE (%) |
97.9 |
97.7 |
99.3 |
100.3 |
102.8 |
98.3 |
|
98.5 |
96.6 |
96.4 |
101.5 |
104.0 |
99.5 |
|
99.3 |
97.1 |
100.2 |
98.2 |
99.6 |
101.7 |
|
98.9 |
96.7 |
99.9 |
100.4 |
100.1 |
100.2 |
|
96.9 |
98.6 |
101.3 |
100.3 |
99.5 |
101.3 |
|
96.7 |
96.6 |
97.1 |
99.6 |
99.1 |
96.5 |
![mean](/dts/sltc/methods/images/mean.gif) |
98.0 |
97.2 |
99.0 |
100.1 |
100.9 |
99.6 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after initial analysis. After the original analysis was performed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was -3.4% for samples that were
resealed with new septa, and -4.8% for those that retained their punctured septa.
Table 4.10.2.3.2 |
Stability of Desorbed Samples for Isoflurane from Anasorb 747 |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
100.1 |
94.0 |
-6.1 |
102.8 |
97.2 |
-5.6 |
99.5 |
96.4 |
-3.1 |
104.0 |
97.2 |
-6.8 |
99.1 |
98.1 |
-1.0 |
99.6 |
97.6 |
-2.0 |
|
(averages) |
|
|
(averages) |
|
99.6 |
96.2 |
-3.4 |
102.1 |
97.3 |
-4.8 |
|
4.10.3 Anasorb CMS at low target concentration (TC)
4.10.3.1 Enflurane
The desorption efficiencies (DE) of enflurane were determined by liquid-spiking 150 mg
portions of Anasorb CMS with amounts equivalent to 0.05 to 2 times the 1-ppm target
concentration. These samples were stored overnight at ambient temperature and then desorbed
and analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the
target concentration is 100.3%.
Table 4.10.3.1.1 |
Desorption Efficiency of Enflurane from Anasorb CMS at Low TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
4.56 |
9.12 |
18.24 |
45.6 |
91.2 |
182.4 |
|
DE (%) |
99.4 |
100.2 |
99.5 |
101.0 |
98.7 |
99.1 |
|
99.2 |
98.7 |
99.3 |
102.2 |
98.7 |
100.2 |
|
101.4 |
101.2 |
97.7 |
101.1 |
97.7 |
101.8 |
|
101.5 |
100.0 |
99.0 |
101.3 |
98.7 |
100.4 |
|
99.4 |
101.6 |
100.0 |
99.4 |
99.4 |
102.8 |
|
99.4 |
100.5 |
101.7 |
100.9 |
100.3 |
101.8 |
![mean](/dts/sltc/methods/images/mean.gif) |
100.2 |
100.4 |
99.5 |
101.0 |
98.9 |
101.0 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after initial analysis. After the original analysis was perfommed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was +3.3% for samples that were
resealed with new septa, and +0.9% for those that retained their punctured septa.
Table 4.10.3.1.2 |
Stability of Desorbed Samples for Enflurane from Anasorb CMS |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
98.7 |
101.4 |
+2.7 |
98.7 |
98.7 |
0 |
98.7 |
101.9 |
+3.2 |
99.4 |
99.8 |
+0.4 |
97.7 |
101.7 |
+4.0 |
100.3 |
102.8 |
+2.5 |
|
(averages) |
|
|
(averages) |
|
98.4 |
101.7 |
+3.3 |
99.5 |
100.4 |
+0.9 |
|
4.10.3.2 Halothane
The desorption efficiencies (DE) of enflurane were determined by liquid-spiking 150-mg
portions of Anasorb CMS with amounts equivalent to 0.05 to 2 times the 1-ppm target
concentration. These samples were stored overnight at ambient temperature and the desorbed and
analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the target
concentration is 99.7%.
Table 4.10.3.2.1 |
Desorpbon Efficiency of Halothane from Anasorb CMS at Low TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
4.862 |
9.724 |
19.45 |
48.62 |
97.24 |
194.5 |
|
DE (%) |
101.1 |
100.3 |
100.8 |
99.1 |
98.7 |
98.2 |
|
99.7 |
103.2 |
99.1 |
98.3 |
99.5 |
98.7 |
|
98.8 |
99.5 |
100.8 |
100.3 |
99.1 |
100.1 |
|
99.7 |
100.0 |
98.5 |
100.0 |
100.2 |
100.5 |
|
99.5 |
100.5 |
99.4 |
98.9 |
102.4 |
100.1 |
|
98.9 |
99.7 |
100.2 |
97.5 |
101.1 |
101.7 |
![mean](/dts/sltc/methods/images/mean.gif) |
99.6 |
100.5 |
99.8 |
99.0 |
100.2 |
99.9 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 2.5 h after initial analysis. After the original analysis was performed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
eanalyzed with fresh standards. The average percent change was +1.1% for samples that were
resealed with new septa, and -1.6% for those that retained their punctured septa.
Table 4.10.3.2.2 |
Stability of Desorbed Samples for Halothane from Anasorb CMS |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
98.7 |
100.9 |
+2.2 |
100.2 |
99.3 |
-0.9 |
99.5 |
99.5 |
0 |
102.4 |
99.2 |
-3.2 |
99.1 |
100.1 |
+1.0 |
101.1 |
100.4 |
-0.7 |
|
(averages) |
|
|
(averages) |
|
99.1 |
100.2 |
+1.1 |
101.2 |
99.6 |
-1.6 |
|
4.10.3.3 Isoflurane
The desorption efficiencies (DE) of isoflurane were determined by liquid-spiking 150-mg
portions of Anasorb CMS with amounts equivalent to 0.05 to 2 times the 1-ppm target
concentration. These samples were stored overnight at ambient temperature and then desorbed
and analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the
target concentration is 99.4%.
Table 4.10.3.3.1 |
Desorption Efficiency of Enflurane from Anasorb CMS at Low TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
4.50 |
9.00 |
18.0 |
45.0 |
90.0 |
183.0 |
|
DE% |
98.6 |
99.3 |
100.2 |
100.3 |
96.9 |
98.6 |
|
99.3 |
98.1 |
98.1 |
98.9 |
97.6 |
100.2 |
|
99.1 |
98.5 |
101.1 |
101.3 |
97.1 |
101.5 |
|
99.0 |
98.3 |
100.1 |
99.6 |
97.9 |
98.7 |
|
100.1 |
97.2 |
98.5 |
100.2 |
98.5 |
101.6 |
|
99.5 |
99.0 |
101.4 |
100.6 |
98.4 |
100.4 |
![mean](/dts/sltc/methods/images/mean.gif) |
99.3 |
98.4 |
99.9 |
100.2 |
97.7 |
100.2 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after initial analysis. After the original analysis was perfomned, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was +3.6% for samples that were
resealed with new septa, and +1.9% for those that retained their punctured septa.
Table 4.10.3.3.2 |
Stability of Desorbed Samples for Enflurane from Anasorb CMS |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
96.9 |
101.6 |
+4.7 |
97.9 |
97.1 |
-0.8 |
97.6 |
99.8 |
+2.2 |
98.5 |
101.1 |
+2.6 |
97.1 |
101.1 |
+4.0 |
98.4 |
102.5 |
+4.1 |
(averages) |
(averages) |
97.2 |
100.8 |
+3.8 |
98.3 |
100.2 |
+1.9 |
|
4.10.4 Anasorb 747 at low target concentration (TC)
4.10.4.1 Enflurane
The desorption efficiencies (DE) of enflurane were determined by liquid-spiking 140-mg
portions of Anasorb 747 with amounts equivalent to 0.05 to 2 times the 1-ppm target
concentration. These samples were stored overnight at ambient temperature and then desorbed
and analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the
target concentration is 103.7%.
Table 4.10.4.1.1 |
Desorption Efficiency of Enflurane from Anasorb 747 at Low TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
4.56 |
9.12 |
18.24 |
45.6 |
91.2 |
182.4 |
|
DE (%) |
102.0 |
100.5 |
99.1 |
103.2 |
102.3 |
101.9 |
|
102.2 |
100.2 |
98.4 |
102.3 |
104.2 |
105.3 |
|
96.9 |
97.9 |
99.6 |
102.2 |
101.6 |
103.7 |
|
102.4 |
98.2 |
98.2 |
100.9 |
104.6 |
103.8 |
|
101.2 |
97.7 |
99.7 |
107.8 |
106.3 |
103.6 |
|
102.9 |
99.4 |
99.0 |
107.4 |
100.6 |
104.6 |
![mean](/dts/sltc/methods/images/mean.gif) |
101.3 |
99.0 |
99.0 |
104.0 |
103.3 |
103.8 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after initial analysis. After the original analysis was performed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was -2.1% for samples that were
resealed with new septa, and -2.9% for those that retained their punctured septa.
Table 4.10.4.1.2 |
Stability of Desorbed Samples for Enflurane from Anasorb 747 |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
102.3 |
98.4 |
-3.9 |
104.6 |
99.4 |
-5.2 |
104.2 |
100.9 |
-3.3 |
106.3 |
101.9 |
-4.4 |
101.6 |
102.6 |
+1.0 |
100.6 |
101.4 |
+0.8 |
|
(averages) |
|
|
(averages) |
|
102.7 |
100.6 |
-2.1 |
103.8 |
100.9 |
-2.9 |
|
4.10.4.2 Halothane
The desorption efficiencies (DE) of halothane were determined by liquid-spiking 140-mg
portions of Anasorb 747 with amounts equivalent to 0.05 to 2 times the1-ppm target
concentration. These samples were stored overnight at ambient temperature and then desorbed
and analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the
target concentration is 99.6%.
Table 4.10.4.2.1 |
Desorption Efficiency of Halothane from Anasorb 747 at Low TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
4.862 |
9.724 |
19.45 |
48.62 |
97.24 |
194.5 |
|
DE(%) |
85.2 |
95.7 |
94.8 |
98.0 |
98.3 |
101.0 |
|
84.5 |
93.3 |
97.2 |
98.3 |
100.2 |
100.9 |
|
85.2 |
92.7 |
94.3 |
99.7 |
97.9 |
99.0 |
|
83.1 |
91.7 |
94.2 |
99.8 |
100.9 |
98.9 |
|
84.5 |
90.7 |
93.7 |
99.7 |
101.6 |
99.1 |
|
83.5 |
91.4 |
94.2 |
98.9 |
100.7 |
100.5 |
![mean](/dts/sltc/methods/images/mean.gif) |
84.3 |
92.6 |
94.7 |
99.1 |
99.9 |
99.9 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after initial analysis. After the original analysis was performed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was ±0% for samples that were
resealed with new septa, and -3.0% for those that retained their punctured septa.
Table 4.10.4.2.2 |
Stability of Desorbed Samplies for Halothane from Anasorb 747 |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
98.3 |
98.4 |
+0.1 |
100.9 |
97.6 |
-3.3 |
100.2 |
98.1 |
-2.1 |
101.6 |
97.8 |
-3.8 |
97.9 |
99.9 |
+2.0 |
100.7 |
98.9 |
-1.8 |
|
(averages) |
|
|
(averages) |
|
98.8 |
98.8 |
±0 |
101.1 |
98.1 |
-3.0 |
|
4.10.4.3 Isoflurane
The desorption efficiencies (DE) of isoflurane were determined by liquid-spiking 140-mg
portions of Anasorb 747 with amounts equivalent to 0.05 to 2 times the 1-ppm target
concentration. These samples were stored overnight at ambient temperature and then desorbed
and analyzed. The average desorption efficiency over the working range of 0.5 to 2 times the
target concentration is 100.8%.
Table 4.10.4.3.1 |
Desorption Efficiency of Isoflurane from Anasorb 747 at Low TC |
|
× target concn |
0.05× |
0.1× |
0.2× |
0.5× |
1.0× |
2.0× |
(µg/sample) |
4.50 |
9.00 |
18.0 |
45.0 |
90.0 |
180.0 |
|
DE (%) |
97.1 |
100.0 |
98.1 |
103.2 |
99.3 |
99.4 |
|
92.3 |
99.6 |
102.2 |
97.6 |
99.9 |
102.8 |
|
96.4 |
100.2 |
101.1 |
99.4 |
99.2 |
100.8 |
|
97.8 |
100.0 |
102.5 |
98.5 |
101.5 |
101.7 |
|
99.4 |
100.0 |
101.0 |
104.0 |
102.9 |
100.8 |
|
97.9 |
100.1 |
101.4 |
103.8 |
97.5 |
101.5 |
![mean](/dts/sltc/methods/images/mean.gif) |
96.8 |
100.0 |
101.1 |
101.1 |
100.1 |
101.2 |
|
The stability of desorbed samples was investigated by reanalyzing the target concentration
samples 22.5 h after initial analysis. After the original analysis was performed, three vials were
recapped with new septa while the remaining three retained their punctured septa. The samples
vials were stored in the refrigerated sampling tray for the GC injector. The samples were
reanalyzed with fresh standards. The average percent change was -1.3% for samples that were
resealed with new septa, and -4.4% for those that retained their punctured septa.
Table 4.10.4.3.2 |
Stability of Desorbed Samples for Isoflurane from Anasorb 747 |
|
punctured septa replaced |
punctured septa retained |
initial |
DE after |
|
initial |
DE after |
|
DE |
one day |
difference |
DE |
one day |
difference |
(%) |
(%) |
|
(%) |
(%) |
|
|
99.3 |
97.4 |
-1.9 |
101.5 |
96.8 |
-4.7 |
99.9 |
97.0 |
-2.9 |
102.9 |
95.0 |
-7.9 |
99.2 |
100.2 |
+1.0 |
97.5 |
96.8 |
-0.7 |
|
(averages) |
|
|
(averages) |
|
99.5 |
98.2 |
-1.3 |
100.6 |
96.2 |
-4.4 |
|
4.11 Qualitative analysis
The anesthetic gases can be easily separated and identified by GCA\MS. Mass spectra for
enflurane, halothane and isoflurane, which were separated using conditions similar to the
information given in Section 3.5, were obtained from a Perkin-Elmer Ion Trap Detector
interfaced to a Hewlett-Packard Series II GC.
Figure 4.11.1. Mass spectrum of enflurane.
Figure 4.11.2. Mass spectrum of halothane.
Figure 4.11.3. Mass spectrum of isoflurane.
4.12 Nitrous oxide interference
A test was developed to study the ability of nitrous oxide to interfere with the collection of
anesthetic gases on the recommended sampling tubes. A 100-L gas-sampling bag was filled with
dry air and 1.50 mL of water was added to raise the humidity to 80% at 22°. Halothane was
selected as a typical anesthetic gas and 20µL (37.4 mg) was added to the bag. Nitrous oxide
(430.5 mg) was also added. This produced an atmosphere containing 46.4 ppm of halothane and
2390 ppm of nitrous oxide. A second bag was prepared to dupiclate the first one except no
nitrous oxide was added. Air samples were drawn at 0.05 L/min for 4 h from both bags using
Anasorb CMS and Anasorb 747. No halothane was detected on any of the back-up sections. The
results show that nitrous oxide does not substantially interfere with the collection of halothane
from an atmosphere containing both gases.
Table 4.12 |
Parts-per-million recovered from Gas-Sampling Bags |
|
Anasorb |
halothane |
halothane with |
|
|
nitrous oxide |
|
CMS |
44.9 |
40.3 |
747 |
45.6 |
45.7 |
|
5. References
5.1 OSHA Analytical Methods Manual, 2nd ed., U.S. Department of Labor, Occupational Safety
and Health Administration; Salt Lake Technical Center; Salt Lake City, UT 1993; "Method 29 -
Enflurane and Halothane" (1981); American Conference of Governmental Industrial Hygienists
(ACGIH); Cincinnati, OH, Publ. No. 4542.
5.2 NIOSH Criteria for a Recommended Standard: Occupational Exposure to Waste Anesthetic
Gases and Vapors, U.S. Department of Health and Human Services, Public Health Service,
Center for Disease Control, National Institute for Health for Occupational Safety and Health,
Cincinnati, OH, 1977, DHHS (NIOSH) Publ. 77-140.
5.3 NIOSH Recommendations for Occupational Safety and Health: Compendium of Policy
Documents and Statements, U.S. Department of Health and Human Services, Public Health
Service, Center for Disease Control, National Institute for Health for Occupational Safety and
Health, Cincinnati, OH, 1992, DHHS (NIOSH) Publ. 92-100.
5.4 Documentation of the Threshold Limit Values and Biological Exposure Indices, 5th ed.,
American Conference of Governmental Industrial Hygienists (ACGIH); Cincinnati, OH, 1986.
5.5 MRC Monograph on the Evaluation of Carcinogenic Risks to Humans:
Overall Evaluation of Carcinogenicity: An Update of IARC Monographs Volumes 1 to 42, International Agency for
Research on Cancer (IARC), Lyon, France, 1987, Supplement 7, pp. 93-95.
5.6 Material Safety Data Sheet: Ethrane, Anaquest, Liberty Corner, NJ, March 1992.
5.7 Material Safety Data Sheet: Forane, Anaquest, Liberty Corner, NJ, March 1992.
5.8 Material Safety Data Sheet 2-Bromo-2-chloro-1,1,1-trifluoroethane, Aldrich Chemical Co.,
Milwaukee, WI, May 1992.
5.9 Merck Index, Budavari, S. Ed., 11th ed., Merck & Co., Rahway, NJ, 1989.
5.10 OSHA Instruction CPL 2-2.60, Exposure Control Plan for Federal OSHA Personnel with
Occupational Exposure to Bloodbome Pathogens, March 7,1994; Occupational Safety and Heath
Administration, U.S. Department of Labor, Washington, D.C.
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