STANDARD OPERATING PROCEDURE:
GC/MS ANALYSIS OF HSH, SEDIMENT AND WATER
FOR VOLATILE ORGANIC COMPOUNDS
Tammy Jones and Michael Hiatt
USEPA Region 9
August 19, 1983
ENVIRONMENTAL MONITORING SYSTEMS LABORATORY
LAS VEGAS, NEVADA 89114
-------
Introduction
The purpose of this standard operating procedure is to provide operator(s)
of the Finnigan OWA (Organics in Water Analyzer) Model 1020 Automated GC/MS,
with a detailed plan for operation, maintenance, quality control and collection
of verified data. Before this SOP is used, it is assumed the operator has read
Finnigan manuals 10000-90080 (OWA Operators Manual, June 1979) and 10000-90140
Rev A (OWA Service Manual, February 1981).
The operator must also read this document in its entirety before analyzing
unknown samples. All procedures for standard operation of this instrument must
be followed; at no time, without prior notification from operator's supervisor
f
or project director, should an operator disregard procedure given, or referred
to, in this document.
n
-------
CONTENTS
"Sections
I. Tuning GC/MS (OWA) for Volatile Analysis
II. Points for Documentation
III. Standard Calibration and Quantitation
IV. Standard Preparation
V. Sample Storage- Water-Fish-Sediment
VI. Sample Pre-Preparation for Fish
VII. Sample Analysis and Quantitation
VIII. Tekmar/Autosampler Operation
IX. Assembly of Data Packages
X. System Software
XI. Construction of Reverse Libraries
XII. Quality Assurance
XIII. Maintenance
Tables
1-1. Multiple Ion Parameters
1-2. GC Parameters
1-3. BFB Ion Abundance Criteria
III-l. MDL for Volatile and Semi-Volatile Priority Pollutants
111-2. Quantitation Errors and Corrective Steps
XI-1. Table of Libraries
XIII-1. Maintenance Checklist
XIII-2. Electronic Troubleshooting Chart
XIII-3. Chromatography Troubleshooting Chart
XII1-4. Troubleshooting Chart for Analyzer Module
Figures
XIII-1. Mass Spectrometer with Cover Removed
XIII-2. Removing the Analyzer
XIII-3. Mass Analyzer :
XIII-4. Exploded View of Ion Source
XIII-5. Alignment Fixture Base
XIII-6. Ion Source with Filament Assembly Installed
(continued)
iii
-------
Figures (Continued)
XIII-7. Ion Source Prior to Installation of Collector
XI11-8. Ion Source with Collector Installed
XIII-9. Electron Multiplier
XI11-10. Closeup of Multiplier Housing
XIII-11. Rear View of Vacuum Manifold
XI11-12. Ion Source Circuit Board "
XIII-13. Alcatel Pump
XII1-14. Turbomolecular Pump
XIII-15. Disk Drive
XI11-16. Air Filter Removal
Appendices
A Safe Handling of Compressed Gases in the Laboratory
B Emergency Spill Procedures
iv
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Section No. I__
Revision No.
Date: 08/19/83
Page 1 of 10~
I. TUNING GC/MS (OWA) FOR VOLATILE ANALYSIS
A. Electrometer Zero:
1. Enter Program MT (>MJ_CR*)
2. Call Scan N (See Table I) (MT N CR)
3. Enable Scan N (MT: SE CR)
4. Vary Electrometer Zero value to give average Noise intensity of 3-6 in
window 122 and in window 452. (MT: 13, value between -6 and +6)
Note: If Electrometer Zero cannot be lowered to these values Preamp
must be ajusted. This is described in OWA Service Manual VI pp. 1-3
*
5. Store correct Electrometer Zero value (MT: Kl^ CR)
B. Sensitivity:
1. (> MT CR)
2. Call Scan P (See Table I for parameter) (MT: P CR)
3. Enable Scan P (MT: SE CR)
4. Adjust ion energy value to give an approximate intensity of 32,000 for
69 m/e (MT:5, value of 1 to 10)
*CR = Carriage Return.
-------
Section No. I__
Revision No.
Date: 08/19/8T
Page z of 10"
TABLE 1-1. MULTIPLE ION PARAMETERS
=============================================================================
Scan List
Multiple Ion (MI) Scan Parameters - N P B
Total Scan Time (sec.) 0.10 0.15 0.16
Threshold 111
No. of Mass Intervals 2 44
Interval 1-
Low Mass
High Mass
Time (sec.)
Interval 2-
Low Mass
Hi,gh Mass
Time (sec.)
Interval 3-
Low Mass
High Mass
Time (sec.)
Interval 4-
Low Mass
High Mass
Time (sec.)
119.50
125.50
0.03
449.50
455.50
0.03
• •
67.50
70.50
0.03
217.50
220.50
0.03
412.50
415.50
0.03
500.50
503.50
0.03
47.50
50.50
0.03
73.80
76.80
0.03
94.50
96.50
0.03
172.50
175.50
0.03
===============================================================================
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Section No. _ I_
Revision No. _
Date: 08/19/83"
Page 3 of 10"
Note: If Ion energy cannot be Increased within the 1 to 10 value it may
be necessary to increase electron multiplier voltage. This should be done
with the awareness of the lead mass spectrometrist and recorded In the
it
injection log book. . . •>
i
5. Store correct ion energy value (MT: K0 CR)
C. BFB Calibration:
Note: 2ul of pure BFB is added to the FC43 calibration bulb. This gives
an approximate intensity for 95 m/e of 6,000 to 10,000 in Scan B or 174
m/e is < 2/3 176 m/e. Then 95 m/e <2000 an. additional 2ul BFB should be
added to the FC43.
1. Enter Program MT (>MT CR)
2. Call Scan B (See Table I for parameters) (MT: SB CR)
3. Enable Scan B (MT: SE CR)
4. Adjust scan numbers to 5-way (MT: J5 CR)
5. Adjust lense voltage to maximize intensity of 219 m/e on scope (MT: 8, 1
to 15)
6. Adjust ion program to make 174 m/e 50 to 70% of 95 m/e. (MT: 7, 0 to
20)
-------
Section No. I_
Revision No.
Date: 08/19/83
Page 4 of 10~
7. Adjust ion energy to make 75 m/e 40 to 60% of 95 m/e (MT: 5, 1 to 10)
Note: Ion energy should not be increased appreciably as the sensitivity
adjustments maximized ion energy value in Section I.B.
Resolution should be adjust (pots only or rod drive board)
res. cal. pot adjusts resolution for 174/175 m/e
MI mass. res. pot adjusts resolution for 219/220 m/e
TP14 GND (A) pot adjusts resolution for 69/70 m/e
8. Adjust resolution of 219/220 m/e to give a 30-50% valley.
9. Adjust resolution of 174/175 m/e to give a 5-10% valley.
10. Adjust resolution of 69/70 to over resolve.
11. Repeat steps 7-9 until all resolutions are within their respective limits.
12. Repeat steps 4-6 until all values are within their respective limits.
Note: Repeat steps 7-9 and 4-6 until all criteria are met.
13. Store correct ion energy ion programing and lense voltage (MT: KO/ CR)
14. Hardcopy present values (MT: to)
15. Exit program (MT: £2.
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Section No. l__
Revision No.
Date: 08/19/83
Page 5 of 10"
0. Mass Calibration:
1. Enter calibration program (> CAH;>.)
Note: This will automatically mass-calibrate system and hardcopy calibra-
tion limits. After calibration program is complete computer will request
scan parameter data. Enter previous scan list parameter used for BFB
performance evaluation as recorded in injection log book.
2. Hardcopy FC43 spectrum (>LH FC43#1;LHI2 CR)
E. Acquisition rate setting. Normally the following procedure will adequately
adjust the aquisition rate such that BFB and sample analysis can be
accomplished with the same threshold and minimum area settings. Adjust-
ments to this procedure may be necessary in the instance of new or decaying
eletron multiplier.
F. BFB Performance Confirmation:
BFB is injected and chromatographed using GC-3 (See Table 1-2). Final
relative abundance and isotope resolution is to fulfill criteria in Table
III, list B.
1. Set injector system to Auto
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Section No. I_
Revision No.
Date: 08/19/35"
Page 6 of iff"
2. Call GC parameters 3 (> GC; 3 CR x 12)
3. Set scan rate to 3 sec.
t.
•i
4. Scan parameters threshold land minimum area are adjusted In Section 1C so
.1
that BFB performance file should be < 100 sectors. This is adjusted on a
"day after" basis if BFB criteria are fulfilled (i.e., if BFB criteria is
fulfilled and file sector usage is >100, the minimum area will be
increased for the next BFB file aquisition. This can be checked as
threshold, minimum area and sector usage are recorded in the injection log
book. \
f «
Set up Aquisition file for BFB.
Note: Files are named by year, BFB, then the Sequence Number of BFB
injection. Only one BFB file will be recorded for any one 10 hour day;
e.g., 82BFB001 first BFB performance file in 1982.
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Section No. I_
Revision No.
Date: 08/19/83
Page 7 of 10~
TABLE 1-2. GC PARAMETERS
GC Parameter
Zone Temperature
Initial Temperature
Final Temperature
Initial Time
Ramp Rate
Final Time
Separator Oven
Temperature
Manifold Temperature
Current -Injection Mode
Splitless Injection
File 1
225°C
60°C
175°C
3 min.
8°C/min.
24 min.
225°C
80°C
<'P
___
File 3
225°C
70°C
165°C
3 min.
30°C/min.
10 min.
225 °C
80°C
C
40 sec.
==============
File 4
225°C
-90 °C
60°C
0 min.
30°C/min.
10 min.
225°C
80 °C
4
60 sec.
:================
File 5
225°C
160°C
200°C
0 min.
6°C/min.
10 min.
225°C
80°C
C
0 sec.
Time '
Turn Fil/Mult Off
for sec. After
Injection 0 sec. 200 sec. 90 sec. 0 sec.
Current Fil/Mult Mode MM M M
-------
Section No. I_
Revision No.
Date: 08/19/ST"
Page 8 of 10
5. Type Acquisition of file (>AC XBFBY#60)
where x = last two digits of year and
Y = Sequence Number for BFB
6. Type amount BFB Injected (sample: 20ng BFB CR)
7. Type initials of operator (> operator: >J
8. Hit return key until file information prompts are completed.
9. When screen indicates GC is ready inject 20ng BFB - (See Preparation of
Standards) and press GC start button.
10. At completion of file acquisition compare BFB spectra with that of Table
1-3, column B.
11.. Hardcopy spectra of BFB using (Ltfspectra No.) single and/or average
spectra (LAH CR)
12. Ensure that injection log book is completed for file entry.
13. Store correct ion energy ion programing and lense voltage
(MT: Kl CR)
-------
TABLE 1-3. BFB ION ABUNDANCE CRITERIA
23:133333333333333333333 3333333333333 = 3333:53333.33.2 3 33 333s = 33333333333333333S33BS33333333333a3:s333;3S3338
Ion Abundance Criteria
Mass
B
15 to 40% of base peak
30 to 60% of the base peak
Base peak, 100% relative
abundance
5 to 9% of the base peak
Less than 2% of mass 174
50 20 to 40 pet of mass 95
75 50 to 70 pet of mass 95
95 Base peak, 100 pet relative
abundance
96 5 to 9 pet of mass 95
173 Less than 1 pet of mass 95
174 70 to 90 pet of mass 95
175 5 to 9 pet of mass 95
176 70 to 90 pet of mass 95
177 5 to 9 pet of mass 95 5 to 9% of mass 176 5 to, 9% of mass 176
32133S23333333333333383333333333=33333333333338333333333SS3S3333833333S333333333333«3S33333333333«»3Z
A Fed. Regist. 1979, 44 (No.233), 69532-69539.
B Olynyk, P., W. L. Budde, and J. U. Eichelberger, 1981. Simultaneous Qualitative and Quantitative
Analyses. I. Precision Study of Compounds Amenable to the Inert Gas-Purge-and-Trap Method.
Journal of Chromatographic Science. Vol. 19. July, 1981. /IFB's WA 83-A093 and WA 83-A094
C Spies, David N. "Determination of Purgeables Organics in Sediment Using a Modified Purge and
Trap Technique"; U.S. Environmental Protection Agency Region II: Edison, NJ, October 10, 1980.
Greater than 50% of the base
peak
5 to 9% of mass 174
15 to 40% of the base peak
30 to 60% of the base peak
Base peak, 100% relative
abundance
5 to 9% of the base peak
less than 1%- of the base
peak
greater than 50% of the
base peak
5 to 9% of mass 174
Greater than 95%, but less than greater than 50% of the
101% of mass 174 base peak
•O O 30 «/>
ot ot (9 n
«o r* < o
<£>
o§3
oo z
. z o
H- O "
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Section No. I_
Revision No.
Date: 08/19/85"
Page 10 of 10
14. Hardcopy present values (MT: H CR)
15. Exit program (MT: E CR)
-------
Section No. II
Revision No. 0
Dat^: 08/19/83"
Page 1 of 4~
II. POINTS FOR DOCUMENTATION
(or Writing the Daily Log)
A. Introduction:
1. Each day a new page(s) in a sequentialy numbered log book (the Daily Log)
is to be used for the recording of the day's events.
2. The page is to be titled with the appropriate data such as title book
number, project and date.
3. The first entry is to be numbered one, with every new entry therafter
labeled sequentially. After the number of entry, the time of entry, and
then the initials of the entry maker are to be written, ex: 1) 8:10.
4. Next the entry is then to be written.
B. Writing the Entry:
1. When a different procedure is done a statement(s) defining the objective
should be included.
i
i
/
a. /What is the objective.
-------
Section No. II
Revision No. 0
Date: 06/01/SF
Page 2 of 4~
b. How Is the objective to be obtained.
c. What we do expected results.
2. The performance standard should be noted In the dally log.
ex: Time obtained and BFB Federal Register criteria were all met.
3. Standard preparation will be documented In Dally Log by SOP.
ex: 1. Internal standard prepared by SOP XX.
' 2. VOA Standard prepared by SOP YY.
3. (or) Standards prepared by SOP XX;YY.
4. Standard runs will be described (by concentration) In the dally log and
referenced to the Injection log. A chart should be made to establish the
cone, to the sample, also included in the chart should be the time of
acquisition, integration and response list.
-------
Section No. II
Revision No. 0
Date: 06/qi/^T"
Page 3 of 4~
Table of Daily Runs (Example)
'Standards
Sample Number ABC A A Acq. Int. Resp. List*
XXVOA000 150 1000 10:00 10:20 10:45
(create)
*It should be noted whether or not the stdls were created or appended to
that day response list or the previous day's. Or if the std. run was
not acceptable for either creation or appendation why it was not. An
example could be due to the response factor and why this point wasn't
acceptable for the list.
5. The preparation of the blank water should also be noted in the log - not
daily but whenever new water is boiled to be used.
*
6. Reagent blanks, samples, duplicates spikes of samples will all be noted
in the daily log and referenced to the injection log. They can be added
to the table of daily runs, as noted above, with the standard runs.
7. A statement about the quantitation method will be entered after the
response lists are completed.
\
Example: A three point linear quantitation report will be used to
report todays analysis.
8. Any abnormalities concerned with the sample analysis will be noted in the
-------
Section No. II
Revision No.~"TT
Date: 06/01 /{%""
Page 4 of f~
injection by and the daily log. One entry can be referenced to the other
log.
9. Any instrument abnormalities should also be noted.
10. After an investigation has been done, a statement(s) should be Included to
summarize findings; also, perhaps a speculatory statement could be
included if unexpected results are found.
C. Finishing the Log Book
1. Portions of the daily log not used will be filled with X and signed.
Example
XXXXXXXXXXXXXXXX
Signature
2. Each page should be signed and dated at the bottom of the page each day.
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Section No. Ill
Revision No. 0
Date: 08/19/35"
Page 1 of 12"
IV. STANDARD COMPOUND CALIBRATION AND QUANTITATION
• i
A. Prepare calibration standards at a minimum of three concentration levels
for. each parameter. One of the calibration standards should be at a
concentration near, but above, the MDL (See Table 1) and the other concen-
trations should correspond to the expected range of concentrations found in
real samples or should define the working range of the GC/MS system. IFB
requires 40 ng/ml , 20 ng/ml, and 4 ng/ml calibration curve.
B. Quantisation of Standards
If the file is a standard run the individual libraries are quantitated:
WQ_ File name, Lib entry #'s, unknown (CR)
After the Quantitation list has been written check to see that all the compounds
have been found. If some are missing, reset the corresponding library entry to
reflect updated relative retention time and retention time. Then enter IDOS
(>Diag
Rename Quantitation list:
ex: (+ Re 8100A542.Q1, \U81VOA642.QL CR)
-------
Section No. Ill
Revision No. ~TT
Date: 08/19/83"
TABLE III-l. MINIMUM C
SEMI-VOLATIi
Parameter
- (yg/D
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
Acenaphthene
Acrolein
Acrylonitrile
Benzene
Benzidine
Carbon tetrachloride
Chlorobenzene
1,2,4-trichlorobenzene
Hexachlorobenzene
1,2-Dichloroethane
1 ,1 ,1-trichloroethane
Hexachloroethane
1,1 -di chloroethane
1,1,2-trichloroethane
1,1,2,2-tetrachloroethane
chloroethane
bis (2-chloroethyl )ether
2-chloroethyl vinyl ether
2-chloronaphthalene
Page Z of 12
JETECTABLE LIMITS FOR VOLATILE AND
.E PRIORITY POLLUTANTS
======= ======================================
IFB Our
Value Value
10
100
100
5
40
5
5
10
10
1
5
10
5
5
10
10
10
10
18
3
20
11
1
30
2
1
3 '
3
1
1
3
1
2
1
1
2
4
3
(continued)
-------
Section No. Ill
Revision No. 0
Date: 08/19/8?"
TABLE III-l. Continued.
Parameter
. (ug/D
20. 2,4,6-trichlorophenol
21. 4-chloro-3-methy1 phenol
(para-chloro-meta-cresol )
22. chloroform
23. 2-chlorophenol
24. 1,2-dichlorobenzene
25. 1,3-dichlorobenzene
26. 1,4-dichlorobenzene
27. 3,3'.-dichlorobenzidine
28. 1,1-dichloroethane
29. trans-l,2-dichloroethene
30. 2,4-dichlorophenol
31. 1,2-dichloropropane
32. trans-l,3-dichloropropene
33. cis-l,3-dichloropropene
34. 2,4-dimethlphenol
35. 2,4-dinitrotoluene
36. 2,6-dinitrotoluene
37. 1,2-diphenylhydrazine
38. Ethyl benzene
39. Fluoranthene
IFB
Value
10
10
5
10
10
10
10
20
5
5
10
10
5
5
10
20
20
20
5
10
Page 3 of 12
5SSSSSSSSSSSSSSSSSS
Our
Value
9
5
1
3
6
8
7
5
1
2
6
1
3
4
4
9
7
NA
1
2
(continued)
-------
Section No. Ill
Revision No. 0
Date: 08/19/85"
TABLE I I 1-1. Continued.
========================================
Parameter
.(ug/D
40. 4-chlorophenyl phenyl
ether •
41. 4-bromophenyl phenyl
ether
42. bis(2-chloroisopropyl)ether
43. bis(2-chloroethoxy)-methane
44. methylene chloride
45. chloromethane
46. bromome thane
47. brdmoform
48. bromodi chloromethane
49. chlorodibromomethane
50. hexachlorobutadiene
51. hexachlorocyclopentadiene
52. isophorone
53. naphthalene
54. nitrobenzene
55. 2-nitrophenol
56. 4-nitrophenol
57. 2,4-dinitrophenol
58. 4, 6-dinitro-2-methyl phenol
59. N-Nitrosodimethylamine
==================
IFB
Value
10
10
20
20
5
10
10
10
5
5
10
10
10
10
10
20
50
50
20
NA
Page 4 of 12
=====================
Our
Value
1
1
7
7
2
2
1
2
1
2
7
4
6
2
7
6
9
10
9
10
(continued)
-------
Section No. Ill
Revision No. 0
Date: C3/19/8T"
TABLE III-l. Continued.
====================================:
Parameter
(yg/D
60.
61.
62.
63.
64.
65.
66.
67.
68.
69.
70.
71.
72.
73.
74.
75.
76.
77.
78.
79.
80.
N-nitrosodiphenylanrine
N-nl trosodi propyl ami ne
Pentachlorophenol
Phenol
81 s(2-ethylhexyl) phthalate
Benzyl butyl phthalate
Di-n-butyl phthalate
Di-n-octyl phthalate
Oi ethyl phthalate
Dimethyl phthalate
Benzo(a)anthracene
Benzo(a)pyrene
Benzo(b)fluoranthene
Benzo(k)fluoranthene
Chrysene
Acenaphthylene
Anthracene
Benzo(gh1)perylene
Fluorene
Phenanthrene
Dibenzo(ah)anthracene
IFB
Value
10
10
10
10
10
10
10
10
10
10
10
20
20
20
20
10
10
20
10
10
20
Page 5 of 12
:=s========c==r ===============
Our
Value
7
9
9
4
2
2
2
3
3
2
2
2
6
(6)
2
2
2
5
4
3
6
(continued)
-------
Section No. Ill
Revision No. 0
Date: 08/19/8?"
TABLE III-l. Continued.
==================== ====s===================z=zss==ss
Parameter IFB
. (ug/D . Value
81.
82.
83.
84.
85.
86.
87.
88.
89.
90.
91.
92.
93.
94.
95.
96.
97.
98.
99.
100.
101.
Indene(l,2,3-cd)pyrene
Pyrene
Tetrachloroethene
Toluene
Trichloroethene
Vinyl chloride
Oieldrln
Chlordane
4 ,'4 '-DDT
4, 4 '-DDE
4,4'-DDD
Endosulfan I
Endosulfan II
Endosulfan sulfate
Endrin
Endrln aldehyde
Heptachlor
Heptachlor epoxide
a-BHG (llndane)
b-BHC
d-BHC
20
10
5
5
5
10
0.005
0.050
0.010
0.005
0.010
0.005
O.OOg
0.010
0.005
0.010
0.005
0.005
0.005
0.005
0.005
Page 6 of 12
============C==M=CS=C=3=;
Our
Value
NO
2
1
1
2
1
2
1
2
2
3
8
8
3
1
3
4
1
(continued)
-------
Section No. Ill
Revision No. (L
Date: 08/19/55"
Page 7 of 12
TABLE III-l. Continued.
======================================================== ====ss:======s=cs===s=zs
Parameter IFB Our
(yg/1) Value Value
102.
103.
104.
105.
106.
107.
108.
109.
110.
111.
112.
113.
114.
115.
116.
117.
118.
119.
120.
121.
122.
====
g-BHC (lindane)
Acetone
Aniline
Benzole Acid
Benzyl alcohol
2-Butanone
Carbondisulfide
4-Chloroanillne
Dibenzofuran
2-Hexanone
2-Methyl naphthalene
4-methyl -2-pentanone
2-methyl phenol
4-methyl phenol
2-nitroanillne
3-nitroanillne
4-nltroanillne
Styrene
2,4,5-trlchlorophenol
Vinyl acetate
o-Xylene
0.005
5
5
100
20
5
1
50
10
5
20
5
5
5
100
100
100
5
100
5
5
3
8
4
6
2
4
2
4
2
2
3
2
9
2
2
8
4
4
6
NA
2
============================
-------
Section No. Ill
Revision No. 0
Date: 08/19/35"
Page 8 of 12
TABLE II1-2.
QUANTITATION ERRORS AND CORRECTIVE STEPS FOR
COMPOUNDS KNOWN TO BE PRESENT
===========================================================scco==c===e=========
Error
Observation
Correction
1.
2.
Wrong peak
integrated.
No peak
integrated,
1.
Multiple "hits" in
reverse library status
report.
Compound not in reverse
library window.
Compound in "window" and
peak shape is normal (no
attempt to integrate).
Compound in "window",
peak shape normal,
(attempt is made to
integrate).
Compound in "window"
peak shape not normal,
1. Narrow window width.
2. Raise fit threshold.
3. Make-reverse library mass
spectra more resistive
(i.e. add masses).1
1. Widen window width.
2. Change r.r.t to place
compound in window center.
1. Lower fit threshold.
2. View compound reverse
library mass spectra (VI
command) and identify any
"obscured mass-ion peak.
Remove obscured mass
fragment.1
1. Narrow window width.
1. Compound must be inte-
grated using WQ file,
reverse Lib.OWAIN1.
2. Compound can be manually
quantitated by QH of mass
peak and RP program (all
steps to be hardcopied).
1 These steps to be done with assist of lead mass spectrometrist.
-------
Section No. Ill
Revision No. 0
Date: 08/19/85"
Page 9 of 12
Return to executive (+ M CR ):
Requantitate the standard using the library with the updated entry(les).
If a standard compound can not be found in the reverse library search with the
corrections, then the error Is identified and it will be noted In the comment
column of the injection log (See Table III-2 for quantitation errors).
C. Reverse library quantitation lists are merged by adding V2. to Vl_ then V^
to \a, V4 to Vl_ and finally V5 to VI:
(? EQL V282VOA642,V182VOA642 CR)
EQL: A;E CR
> EQL V382VOA642.V182VOA642 CR
EQL: A;E CR
> EQL V482VOA642.V182VOA642 CR
EQL: A;E CR
> EQL V582VOA642.V182VOA642 CR
EQL:A;E CR
0. Rename Quantitation list to file name:
> Oiag CR
+ Co V182VOA642.QL.81VOA642.QL
+ M CR
-------
Section No. Ill
Revision No.0~
Date: 08/19/35"
Page 10 of 12"
E. Creating and Updating Response Lists/Calibration Curve
'Adjust library quantisation amount to reflect the amount of compound added,
make sure the correct amounts of the compounds and ISTOS are updated:
ex: > MQ 82VOA642 CR
MQ: :D;; (amount added), Quantisation report entry number(S);0;;
Note: Consecutive compounds of the same concentration can be strung
together as described by:
MQ: ?.
f - •
F. Update response lists: (MQ:;0;;;R;;;S;;;T;;;>or<(append or create,
dependent upon calibration checks);;E
G. After the 3-point (or more) calibration curve has been created and updated
then hardcopy updated Quantitation list;
>MQ 82VOA642 CR
MQ: H CR
H. Calibration Curve Check
Check of the calibration curve should be performed once each 8 Jiour shift.
-------
Section No. Ill
Revision No.5~
Date: 08/19/8T"
Page ll of 12"
These criteria are described in detail In the instructions for IFB Form £,
Calibration Check. The minimum response factor for the system performance
check compounds must be 0.300. If this criteria Is met, the response factor of
all compounds is calculated. A percent difference of the daily response factor
(each 8 hr. shift) compared to the average response factor from the Initial
curve is calculated. The average response factor (RF~) should be calculated for
all compounds. A system performance check must be made before this calibration
curve is used. Six compounds (the system performance check compounds) are
checked for a minimum average response factor of 0.300. These compounds (the
SPCC) are chloromethane, 1,1-dichloroethane, 2-chloroethylvinyl ether, bromo-
form, 1,1,2,2-tertrachloroethane, and chlorobenzene. The maximum percent
difference allowed for each compound flagged as 'CCC' in IFB Form X is 20%.
Only after both these criteria are met can sample analysis begin.
I. Internal standard responses and retention times in all samples must be
evaluated immediately after or during data acquisition. If the retention time
for any internal standard changes by more than 30 seconds from the latest daily
(8 hr. shift) calibration standard, the chromatographic system must be
inspected for malfunctions and corrections made as required. Ifrthe extracted
ion current profile (EICP) area for any internal standard changes by more than
a factor of two (-50% to +100%), the mass spectrometric system mus be inspected
for malfunction and corrections made as appropriate. When corrections are.made,
re-analysis of samples analyzed while the system was malfuncioning is necessary.
-------
Section No. Ill
Revision No. 0
Date: 08/19/85"
Page 12 of 12
J. Retention time and EICP area records shall be maintained in the form of
control charts (Exhibit E. Figure 3, IFB WA-83-A094) by the laboratory as a
part of its internal quality control. Internal standard response data shall
be reported on the I.S. Response Verification Data Sheet (see Exhibit B, IFB
WA-83-A094). .
-------
Section No. IV
Revision No. 0
Date: 08/19/85"
Page l of 7"
IV. STANDARD PREPARATION
t
A. The standard stock solution has two aliquots:
I
, i
The first 1s made from standard mixtures sold by Supelco (Supelco, Inc.,
Bellefonte, Pennsylvania) under the name Purge A and Purge B. Each of these
comes in 1 ml vials with a concentration of 0.2 mg/ml for each of the compounds
present in Purge A and Purge B. In addition 2-cholorethyl vinyl ether and
trichlorofluoromethane is added to the first aliquot. The final concentration
of the first aliquot is 50 ng/ul except for 2-chloro ethylvinyl ether which is
100 ng/,wl.
-f
The second aliquot contains four compounds. These are obtained in
separate ampules.
Methyl Bromide (Concentration 1510 pg/ml)
Vinyl Chloride (Concentration 7300 yg/ml)
Chloromethane (Concentration 5350 pg/ml)
Chloroethane (Concentration 1080
These compounds are stored in lab freezer, Rm. 49, and the contents of each
ampule are transferred to a separate gas-tight syringes. Measured amounts of
each are added to make a 1 ml solution with a final concentration of 50 ng/yl.
-------
Section No. IV
Revision No. 0
Date: 08/19/85"
Page 2 of T
The solvents used in the preparation of Purge A & B, Purge C are methanol and
ethylene glycol. In the preparation of Acrolein and Acrylonytrile, and
internal standards for daily use, b.oiled-distilled-purged H20 is the solvent.
Procedure for making daily solution of Purge C* for vacuum distallation and
purge and trap.
1) Pipette 904.4 yl of ethylene glycol to gas-tight syringe used for the
daily preparation of Purge C.
2) Add 33.1 yl of methyl bromide (concentration 1510 yg/ml).
f
3) Add 46.3 yl of chloroethane (concentration 1080 yg/ml).
4) Add 9.3 yl of chloromethane (concentration 5350 yg/ml).
5) Add 6.9 yl of vinyl chloride (concentration 7300 yg/ml).
Internal Standards for vacuum distillation and purge and trap.
A) The internal standard solution is made of five compounds. Three of them
are sold by Supelco (Supelco, Inc., Bellefonte, Pennsylvania) in 1 ml.
aliquots with a concentration of 20 mg/ml. The three compounds present
'Calculations for the amounts added are found in the standards log book
(1982) for Region 9, Pages 1-10.
-------
Section No. IV
Revision No. 0
Date: 08/19/IT
Page 3 of 7"
are the following:
Bromochloromethane
1,4-Dichlorobutane
l,2-Chloro-2-bromopropane
The two remaining internal standards are obtained in the pure form, they
are:
Ds-Benzene density 0.851 g/ml*
Ds-Toluene density 0.945 g/ml*
A 1 ml stock solution with a concentration of 2 mg/ml is made in the
following manner:
1) Pipette 895.6 pi of methanol into a clean 1 ml reaction vessel.
2) Pipette 100 pi of Supelco internal standard solution into the same
vessel, or
3) Add 2.1 yl D5-Benzene with a 10 pi syringe into vessel.
4) Add 2.1 ul Ds-Toluene with a 10 pi syringe into vessel.
*Refer to density measurement in the 1982 Standards Log Book for Region 9,
page 2.
-------
Section No. IV
Revision No. 0
Date: 08/19/35"
Page 4 of 7~
B) The stock internal standard solution Is used to prepare an 80 ng/5 yl
aliquot for use in sample analysis. The following procedure 1s used:
tt
1) Pipette 992 yl of boiled-distilled-purged t^O into a 1 ml crimp
top vial. ,
2) Add 8 pi of the stock internal standard solution (2 mg/ml) to the
crimp top vial.
3) Crimp a top to the vial, forming a good seal.
Ethylene Glycol
1) Pour approximately 50 ml of pure ethylene glycol into the sample holding
bulb on the volatile organic extraction rig.
2) Extraction of any remaining contaminants is carried out by following:
the first 20 minutes of the volatile organics extraction procedure (see
Section III).
4) The sample bulb is then removed and capped using a Buna-n-ring and glass
stopper. The bulb is labeled, dated, and kept at room temperature for
future use in preparation of standards.
-------
Section No. IV
Revision No.~"TT
Date: 08/19/SF
Page 5 of T~
Pure P-Bromofluorobenzene is diluted with methanol (spectro grade) to
make a solution with a final concentration of 40 ng/yl.
Procedure:*
1) Take 50 ul of concentrated/pure BFB density and dilute to 5 ml with
methanol.
2) Add 13.4 yl of solution made in step 1 to a clean 5 ml volumetric
flask.
3) Add methanol to solution in step 2 to fill volumetric to the 5 ml
*
mark.
Boiled-Distilled-Purged H20
1) Distilled tap water is re-distilled (Corning mega-pure distiller).
Re-distilled water is collected in a 1-liter erlermeyer flask.
2) Water is then boiled for 1/2 to 1 hour on a hot plate.
3) The re-distilled boiled water is transferred into a 1-liter round-
bottomed flask that has an o-ring neck adapter.
^Calculations for the amounts added are to be found in the 1982 Region 9
Standards Log Book pages 1-10.
-------
Section No. IV
Revision No. 0
Date: 08/19/33T
Page 6 of 7
4) The round-bottom flask is connected to the volatile extraction rig.
5) Extraction of the remaining contaminants Is carried out by following
the first 20 minutes of the volatile organlcs extraction procedure
(see Section III).
6} The water Is removed and capped with a Buna-n-ring. A source clamp
Is used to tighten the seal, then It Is labeled, dated and kept at
room temperature for daily use.
Preparation of Purge A and B; Daily STD Soln. for purge and trap analysis
*
Method A:
1) Pipette 154 yl MeOH into a std. vial (labeled STD soln. A and B).
2) Pipette 100 yl Purge A (Supelco) into same vial.
3) Pipette 100 yl Purge B (Supelco) into same vial.
4) Pipette 40 yl Purge H (Radian) into same vial.
5) Place lock type cap (green in-open or red in-closed).
-------
Section No. IV
Revision No. 0
Date: 08/19/8F
Page 7 of 7'
6) 4 yl 2-chloroethylvinyl ether (10,000 ng/yl) into small vial, using a
syringe.
7) 2 yl-Trichlorofluoromethene (10,000 ng/yl) into small vial, using a
syringe.
Method B (use when supply of Purge A and B are low)
1) 40 yl MeOH
2) 25 yl Purge A
31 25 yl Purge B
4) lOyl Purge H
5) Cap vial
*
6) 1 yl 2-chloroethylvinyl ether (10,000 ng/yl)
7) 0.5 yl Trichlrorfluoromethene (10,000 ng/yl)
-------
Section No. V
Revision No. 0
Date: 08/19/83
Page 1 of 1~
V. SAMPLE STORAGE - WATER - FISH - SEDIMENT
•A. Duplicate water samples are received In 40 ml septum vial containers and
are stored in a refrigerator placed in a volatile organic-free room.
Samples are to be analyzed within 14 days of_cojj£ctloju.
B. Upon receipt of a solid fish sample a 10 g aliquot is added to a 100 ml
sample chamber.
1. The aliquot should represent homogeneous materials and omitting
rocks and obvious organic material.
2. The sample chamber is sealed using a Buna-N o-ring, o-ring cap, and
pinch clamp. Care is taken to ensure an air-tight seal.
3. The sample chamber and sample is stored in a freezer (»-17C) placed
in a volatile organic-free room.
C. Sediment samples are received in sealed mason jars and are stored in
volatile free walk in refridgerator. Samples are jo be_analyzed within 14 days
of collection.
-------
Section No. VI
Revision No. 0
Date: 08/19/8T"
Page 1 of 3"
VI. SAMPLE PRE-PREPARATION FOR FISH
A. Homogenization:
This is ideally accomplished the day of, or the day after, receipt. If
the fish tissue amounts to less than 1/4 pound, then an industrial grade
stainless steel Hobart meat grinder is used to homogenize the sample.
Manual, homogenization involves chopping the sample as finely as possible
with the meat cleaver on the chopping board.
To use the Hobart meat grinder, the Biology Bldg. room must be set up
first. At the back of the room, .the main power, hot and cold water are
turned on. The thermostat is set to maintain the room at 10-16C. Cover
the counter tops beneath the Hobart with garbage bags. Place the Hobart
in a garbage bag also. You will need to stock the supplies listed;
paper towels ceramic or stainless spatulae
lined garbage can permanent marker
scrub pads tank of liquid nitrogen
sponges Dewar flask
alcohol/squeeze bottle 100 ml VOA bulb
deionized water/squeeze rubber gloves
bottle 250-400 ml beaker
amber grab sample bottles meat cleaver
adhesive dot labels stainless bone saw
knives cloth gloves
chop board lab soap
-------
Section No. VI
Revision No. 0
Date: 08/19/53"
Page 2 of 3~
After thorough soap and water washing, the grinder, its pieces and all
knives and cleavers are then thoroughly rinsed with deionized water and
f-
dried with paper towels. (The Hobart is placed within a large garbage
bag for the ease of room clean-up). Turn on the Hobart by pressing the
large button at the front and pour about 300-500 ml of liquid nitrogen
into the Hobart feed. To this slowly add egg-sized chunks of tissue
which have been chopped or cut using a stainless cleaver or bonesaw on a
chopping board. Cloth gloves should be worn under the rubber gloves
because everything is frozen and cold to the touch.
After adding tissue to the nitrogen-filled grinder, the plastic bag
opening is pulled down over the top so that the tissue doesn't contamin-
ate the roonu After the noise level lowers slightly and the chunk has
become powdered, more nitrogen and fish chunks are added and the process
is repeated until the whole fish has been ground into a fine frozen
powder. At no time is the tissue allowed to thaw. Weighing out of a 10
g sample of the frozen fish powder is accomplished at this time on a
calibrated top-loading balance and is clamped in a 100 ml volatile
organic analysis (VOA) bulb as is blank air from the room. Note that VOA
bulb must have its opening cleaned of sample bits before it can be
effectively sealed with its cap using the Buna-N o-ring and the clamp.
The remainder of the fish powder is stored in an amber grab bottle for
the other analyses. These three containers are placed back in the ice
-------
Section No. VI
Revision No.~TT
Date: 08/19/8F
Page 3 of 3~
chest or greenhouse freezer until they are transported to the freezer in
Chemistry Lab room 26 for processing. They are transported as before in
an ice chest with dry ice. The freezer in Room 49 of Chemistry is kept
at -20 to -IOC.
-------
Section No. VII
Revision No. 1
Date: 06/01/32"
Page 1 of 5"
VII. SAMPLE (FISH, SEDIMENT, WATER) ANALYSIS & QUANTITATION
This section contains the various procedures used for analyzing and
quantltatlng the various environmental samples. There is a 14 day turn around
time on analysis of water and sediment.
I. Water Preparation -
1. 40 ml -septum vial containers are removed from storage and allowed to
equilibrate to room temperature just before analysis.
*
2. Open one of the sample vials and carefully pour the sample into a 5ml
syringe barrel to just short of overflowing* Replace the syringe
plunger arid compress sample till the barrel's Teflon tip is adjusted to the
5 ml volume mark.
3. Add 5 ul of the ISTD solution and 80 ng of each surragate to the sample
barrel. This is done by placing the lOul-syringe needle into the larger
syringe barrel and depressing the plunger of the smaller syringe.
4. Attach 5ml-syringe to leuver-lock on Autosampler purging trap (See sec.
on Auto Sampler operation and setup)* Open valve and depress syringe
plunger, emptying 5 ml sample into purge trap.
-------
Section No. VII
Revision No.~T~~
Date: 06/01/8T"
Page 2 of 5"
5. Start purging sequence. When finished Initiate Acquire program 1f
operating manually or ASRUN If operating on automatic (see section _ J.
/,
II. Sediment Preparation
,f
1. Remove mason jar containing sediment sample from storage. Allow to
equilibrate to room temperature.
2. Weigh our lOg of sediment into a 100 ml -sample chamber.
3. Seal sample chamber to vacuum distillation apparatus using a Buna-o-ring
and> vacuum pinch clamp. Seal at porehole marked "sample."
4. Add 2 ml of blank H20 thru attaching 5 mi-syringe with 2 ml of t^O to hole
above valve 7. Open valve 7 allowing the 2 ml to flow into chamber. Shut
valve. Remove syringe.
5. Place sonicator under sample chamber and raise high enough so water level
comes to shoulder of sample chamber.
6. Place special fitted purging (glass) trap to porthole Cj, on vacuum
distillation apparatus. Immerse in liquid nitrogen.
-------
Section No. VII
Revision No. 1
Date: 06/01/82
Page 3 of 5~
7. Evacuate glass trap by opening valve at V£ until purging trap Is emptied.
Shut valve off.
8. Start sonication of sample and open valve ¥5 so that the sample chamber and
glass trap are open only to each other. Allow to equilibrate for 5 min.
9..• After equilibration open valve v"2. Now system is open to vacuum. Continue
adding liquid nitrogen to dewar at Cj as needed. Allow sample to come over
into trap for 15 min.
10. After 15 (min), trapping is completed. Shut all valves, turn off sonicator
and, lower dewar from purging trap. Remove purging trap and attach to
special marked place on autosampler.
11. Once purging trap is attached and sealed add 3 ml of blank HgO. This H20
is to contain the amounts of internal standards and surrogates as mentioned
in 1.3, this section.
12. Allow ice in trap to melt. This can be done by gently warming using a heat
gun or allowing sample to melt at own pace.
13. After sample has melted proceed as in 1.5.
-------
Section No. VII
Revision No.~T~
Date: 06/01/52"
Page 4 of 5~
III. Fish Preparation
1. Remove 100 ml sample chamber (as prepared In section > . part B) from
freezer and attach to vacuum distillation apparatus as,noted in II.3.
2. Continue as in II.3 thru 11.13.
IV. Sample Quantitation
1. After 3-pt calibration curve has been established then sample acquisitions
can be quantitated.
2. Type: WQ_ file name, Reverse library name(s), unknown (CR). This will )
start the computer quantitating the sample acquisition.
3. After quantitation is completed, observe the quantitation report. If the
amount of compound is greater than the reportable levels, and a search of
the NBS library confirms the presence of the compound(s) (i.e. the fit and
purity are high), then the level of contamination is reported to the lead
spectrometrist. He/she willthen determine, on the basis of his/her
experience, if the sample needs to be re-run for further confirmation of
the presence of such compound(s). If the lead spectrometrist decides the
amounts present warrant further confirmation the sample is re-run, possibly
at a greater dilution; the amount of dilution is determined by the lead
-------
Section No. VII
Revision No. 1
Date: 06/01/5T"
Page 5 of 5~
spectrometrist - or else, on the basis of his/her experience. If the
amount of pollutant Is sufficiently high, then at the discretion of the
lead spectrometrist, the values are reported immediately to his/her
/ ~
superior. If it is determined that there is no apparent reason to re-run
the sample, then the proper calculations are made to convert to the units
,(
reported on the STORET system.
4. See section on "Assembly of Data Packages."
-------
Section No. VIII
Revision No. 0
Date: 08/19/31"
Page 1 of 4""
VIII. Tekmar/Autosampler Operation
This section contains the various procedures that are .used for operating
the Tekmar and Autosampler.
I. Attach to the Tekmar the number of purge traps needed for the analyses.
The traps are to be slipped onto the sampling needle and Into the "screw"
nut. The nut should be gently turned until tight and so that the trap
won't slip out. The carrier gas flow tube should then gently be Inserted
Into the traps arm. The traps are to be cleaned and dried after each day's
f
use.
II. The Tekmar and autosampler switches are set Into their proper positions
depending upon which mode (Auto or Manual) Is to be used. Table 1 contains
the information to be used in setting the switches on the Tekmar and/or
Autosampler.
III. The required standard runs are injected into traps 1 thru 3 (depending upon
the number of standards to be used). The next trap is to contain the
purged t^O blank (plus internal standards and surrogates). The remaining
traps are to coircain e sample aliquots plus internal standards and .
surrogates. Pu» jmy '*y then be initiated on the first trap.
-------
Section No. VIII
Revision No. 0
Date: 08/19/35"
Page 2 of f~
TABLE 1.
-------
Section No. VIII
Revision No.~~TT
Date: 08/19/3T"
Page 3 of 4
IV. Before GC/MS operation.
A) The ASSET program Is called to screen. In asset only files 3, 4,
and 5 are used. File 5 Is for the first sample, fl.le 4 for the
middle samples and file 3 for the last sample (a dummy run). See
Table 2 for parameters. The computer will prompt the user.
...B) ADFILE is called to screen, the computer will prompt the user.
Placed Into ADFILE are the files used In the autosampler analyses.
After the last real sample number Is entered a dummy file Is added
to the ADFILE list.
*
C) XFILE is called to screen, computer will prompt the user. The asset
files used are placed into XFILE in proper order. Use AUTOS5 for
entry number 1, AUTOS4 for all other entries except the last entry
(dummy file) where AUTOS3 is used.
D) The autosampler routine is ready for initiation. ASRUN is typed
into the terminal, computer will prompt the user. Page through the
questions (unless changes are necessary). The computer will take
over analyses and quantitations.
E) If the computer is interrupted ASRUN will be terminated. In order
for the Autosampler acquisitions to automatically continue the
ADFILE and XFILE editors need to be properly reset.
-------
Section No. VIII
Revision No. 0
Date: 08/19/35"
Page 4 of 4~
TABLE 2
-------
Section No. IX
Revision No. 0
Date: 08/19/51"
Page 1 of 2
Assembly of Data Packages
I. Batch Reports
For each day's analyses there should be a batch report containing that
day's various parameters, i.e., BFB tune package and sample report package.
A. BFB tune package is to contain a copy of manual tune parameters,
calibration file (CA), copy of scan list of FC43 scan number 1 and
number 2, and a copy of the scan list of the BFB analysis.
B. Sample report package should contain:
1) A RIC with identified peaks labeled and internal standard peaks
labeled.
*
2) An updated quantitation report with a library status report.
3) A line that is 25% of the internal standards will be drawn and
any peak over or to that line will be searched.
a) Both enhanced and raw spectra will be hardcopied.
-------
Section No. IX
Revision No. 0
Date: 08/19/35""
Page 2 of 2"
b) Forward library searches of NBS library will also be
included.
c) The program ESFLS should be used as it will satisfy the
required data la and Ib.
C. A xerox copy of that day's injection log will be included.
II. Completion of Report Packages
A. A completed data package will contain all the items listed as A, B,
and C in Section I, standard analyses reports, blank water report,
and a copy of that day's updated response list.
B. Final report sheets will accompany each data package.
1) This report sheet will reflect the % of surrogates recovered,
proper report amounts of compounds found (using proper units)
and other data as prescribed by the updated IFB.
-------
Section No. JC
Revision No. 0
Date: 08/19/55"
Page 1 of l"
X. System Software
Files from older and newer Finnigan Software disc packs have been integrated
into the Region 9 systems software. The current sotware that is used as of
8/15/83 is titled 2.06.82. The files extracted from other master discs are
PREVI.PR (subroueine in ASRUN), WQ.PR, XFILE.PR, ASRUN.PR, ASRUN1.PR, ASSET.MS,
ASSET.PR AND KWQ.PR from disc 1.3.80 and 45EXEC.MS are from the Finnigan 4510
software, 182.
-------
Section No. XI
Revision No. 0
Date: 08/19/55"
Page 1 of 11
XI. CONSTRUCTION OF REVERSE LIBRARIES
A. Choice of Internal Standards. Of the four following steps one or more
of them may be used, It Is up to the discretion of the operator.
1. Internal standards are nearest compound of Interest.
2. Internal standard behaves chromatographically similar to compound of
interest.
3. Internal standard produces best precision data.
4. Internal standard quantitation mass is similar to compound of
interest.
B. Library Order
1. Internal standard is listed first.
2. All other compounds are listed in order of elution time.
-------
Section No. XI
Revision No. 0
Date: 08/19/31"
Page z of 11"
C. Reverse library entries.
1. Quantitation mass selection is chosen on a basis of "ruggedness"
(i.e. minimum of quantisation errors, and/or best-experimental
precision).
2. Mass fragment used in reverse searches begins with all ions over 5%
of base peaks. Ions are deleted as "mass problems" are identified
in actual analysis, see Table IV.
, Note: Reverse libraries are constructed to be what "works" best and
are updated to reflect maximum precision: i.e., libraries are
improved to minimize false "hits" but maintain maximum
identification of compounds at their reported detection limits.
-------
Section No. XI
Revision No. 0
Date: 08/19/83
Page 3 of ll
Tables of Libraries: XI-1.
LIBRARY EDITOR
C. H2. CL. BR
NAME: BROMOCHLOROMETHANE
F. T. : 900 SWW :
R. R. T: 1. 00 MASS :
DATA: LIBRARYU1:
M. WT.: 128
70
128.
QUAN
AMNT
MASS INTENSITY
49 1000
91/ 100
MASS INTENSITY
93 322
95 214
LIBRARY EDITOR
Co. D6
NAME: D6 BENZENE
F. T. : -~800 SWW :
R. R. T: 1. 00 MASS :
MASS INTENSITY
128 705
130 958
DATA: LIBRARYU1:
M. WT.: 84
60
84.
QUAN
AMNT
MASS INTENSITY
54 89
MASS INTENSITY MASS INTENSITY
82 142 83 45
LIBRARY EDITOR
C7. oa
NAME: D8 TOLUENE
F. T. : 850 SWW :
R. R. T: 1. 00 MASS :
DATA: LIBRARYU1
M. WT.: 100
60
100.
QUAN
AMNT
MASS INTENSITY
98 1000
MASS INTENSITY
99 95
MASS INTENSITY
100 729
LIBRARY EDITOR DATA: LIBRARYU1:
C3. H6. CL. BR M. WT.: 156
NAME: 2-BROMO-1-CHLOROPROPANE
F. T. : 850 SWW : 60 QUAN :
R. R. T: 1. 00 MASS : 77. AMNT :
MASS INTENSITY
76 37
LIBRARY EDITOR
C4. H8. CL2
NAME: 1.4-DICHLOROBUTANE
F. T. : 850 SWW :
R. R. T: 1. 00 MASS :
MASS INTENSITY MASS INTENSITY
77 1000 78 39
DATA: LIBRARYU1:
M. WT.: 126
60
90.
QUAN
AMNT
MASS INTENSITY
49 92
55 1000
MASS INTENSITY
62 136
64 46
MASS INTENSITY
75 55
90 144
BASE M/E: 49
RET. T: 10:49
A
80.00
NG
MASS INTENSITY
132 188
BASE M/E: 84
RET. T: 10:55
80.0/0 NG
MASS INTENSITY
84 1000
BASE M/E: 98
RET. T: 12:18
80.00 NG
MASS INTENSITY
BASE M/E: 77
RET. T: 12:45
80.00 NG
MASS INTENSITY
79 369
BASE M/E: 55
RET. T: 14:02
A
80.00 NG
MASS INTENSITY
92 45
-------
Section No. XI
Revision No.0~~
Date: 08/19/8F
Page 4
of 11
Tables of Libraries XI-1. (Continued).
LIBRARY EDITOR
C. H3. CL
NAME: CHLOROMETHANE
F. T. : 850 SWW :
R. R. T: 0. 73 MASS :
MASS INTENSITY MASS INTENSITY
47 102 49 116
48 40 50 1000
LIBRARY EDITOR
C2. H3. CL
NAME: VINYL CHLORIDE
F. T. : 850 SWW :
R. R. T: 0. 76 MASS :
MASS INTENSITY MASS INTENSITY
61 86 62 1000
LIBRARY EDITOR
C. H3. BR
NAME: BROMOCHLOROMETHANE
F. T. : 950 SWW :
R. R. T: 0. 81 MASS :
MASS INTENSITY MASS INTENSITY
79 190 91 92
81 189 93 231
LIBRARY EDITOR
C2. H5. CL
NAME: CHLOROETHANE
F. T. : 950 SWW :
R. R. T: 0. 83 MASS :
DATA: LIBRARYU1:
M. WT.: 50
200 QUAN :
50. AMNT :
MASS INTENSITY
51 35
52 311
DATA: LIBRARYU1:
M. WT.: 62
200 QUAN :
62. AMNT :
MASS INTENSITY
63 41
DATA: LIBRARYU1:
M. WT.: 94
180 QUAN :
94. AMNT :
MASS INTENSITY
94 1000
95 143
DATA: LIBRARYU1:
M. WT.: 64
160 QUAN :
66. AMNT :
6 BASE
RET.
A
100.00 NG
MASS INTENSITY
7 BASE
RET.
A
100.00 NG
MASS INTENSITY
64 313
8 BASE
RET.
A
100.00 NG
MASS INTENSITY
96 941
9 BASE
RET.
A
100.00 NG
M/E: 50
T: 7:42
M/E: 62
T: 8:07
M/E: 94
T: 8:39
'
M/E: 64
T: 8:50
MASS INTENSITY
49 334
51 103
MASS INTENSITY
63 64
64 1000
MASS INTENSITY
66 309
MASS INTENSITY
-------
Section No. XI
Revision No, 0
Date: 08/19/83"
Page 5 of 11"
Tables of Libraries XI-1. (Continued).
LIBRARY EDITOR DATA: LIBRARYU1:
C. CL3. F M. WT.:
NAME: TRICHLOROFLUOROMETHANE
10
BASE M/E: 101
RET. T: 9:15
F. T. : 800 SWW : 100 QUAN :
R. R. T: 0. 87 MASS : 101. AMNT :
MASS INTENSITY MASS INTENSITY MASS INTENSITY
47 111 101 1000 103 573
LIBRARY EDITOR DATA: LIBRARYU1:
C3. H4. 0 M. WT.: 56
NAME: ACROLEIN
F. T. : . 925 SWW : 120 QUAN :
R. R. T: 0. 88 MASS : 56. AMNT :
MASS INTENSITY MASS INTENSITY MASS INTENSITY
52 21 54 31 56 1000
53 115 55 807
LIBRARY EDITOR DATA: LIBRARYU1:
C2. H2, CL2 M. WT.: 96
NAME: 1,1-DICHLOROETHENE
F. T. : 800 SWW : 100 QUAN :
R. R. T: 0. 91 MASS : 61. AMNT :
MASS INTENSITY MASS INTENSITY MASS INTENSITY
59 25 62 70 96 655
60 188 63 319 98 411
61 1000 70 11 100 50
LIBRARY EDITOR DATA: LIBRARYU1:
C3. H3. N M. WT.: 53
NAME: ACRYLONITRILE
F. T. : 950 SWW : 120 QUAN :
R. R. T: 0. 92 MASS : 53. AMNT :
A
100.00 • NG
MASS INTENSITY
105 66
11 BASE M/E:
RET. T:
A
500.00 NG
MASS INTENSITY
12 BASE M/E:
RET. T:
A
100.00 NG
MASS INTENSITY
13 BASE M/E:
RET. T:
A
500.00 NG
56
9:23
61
9:35
53
9:44
MASS INTENSITY
52 684
MASS INTENSITY
53 1000
MASS INTENSITY MASS INTENSITY
-------
Section No. XI
Revision No. 0
Date: 08/19/SI"
Page 6 of 11"
Tables of Libraries XI-1. (Continued).
LIBRARY EDITOR
C H2 CL2
NAME: METHYLENE CHLORIDE
F. T. : 950 SWW :
R. R. T: 0. 92 MASS :
DATA: LIBRARYU1:
M. WT.: 84
200
86.
QUAN
AMNT
MASS INTENSITY
82 11
84 1000
MASS INTENSITY
85 32
86 638
MASS INTENSITY
87 10
88 99
LIBRARY EDITOR DATA: LIBRARYU1:
C2. H2. CL2 M. WT.: 96
NAME: TRANS-1.2-DICHLOROETHENE
F. T. : 850 SWW : 80 QUAN :
R. R. T: 0. 95 MASS : 96. AMNT :
MASS INTENSITY
62 80
63 349
96 1000
MASS INTENSITY
59 53
60 282
61 930
>
LIBRARY EDITOR
C2. H4. CL2
NAME: 1.1-DICHLOROETHANE
F. T. : 950 SWW :
R. R. T: 0. 96 MASS :
MASS INTENSITY
97 57
98 579
99 17
DATA: LIBRARYU1:
M. WT.: 98
60
63.
QUAN
AMNT
MASS INTENSITY
61 55
63 1000
MASS INTENSITY
65 284
83 134
LIBRARY EDITOR
C. H. CL3
NAME: CHLOROFORM
F. T. : 900 SWW :
R. R. T: 1. 00 MASS :
MASS INTENSITY
85 80
98 70
DATA: LIBRARYU1:
M. WT.: 118
35
85.
QUAN
AMNT
MASS INTENSITY
47 240
48 146
51 176
MASS INTENSITY
83 1000
84 55
85 631
MASS INTENSITY
87 96
117 14
118 23
14
A
100.00 NG
MASS INTENSITY
15
BASE M/E:
RET. T:
84
9:45
BASE M/E: 96
RET. T: 10:00
A
100.00
NG
MASS INTENSITY
100 70
16
A
100.00
BASE M/E: 63
RET. T: 10:08
NG
MASS INTENSITY
100 40
17
A
100.00
BASE M/E: 83
RET. T: 10:27
NG
MASS INTENSITY
120 22
-------
Section No. XI
Revision No. 0
Date: 08/19/83
Page 7 of 11
Tables of Libraries XI-.1. (Continued).
LIBRARY EDITOR DATA: LIBRARYU1:
C2. H3. CL3 ' M. WT.: 132
NAME: 1,1,1-TRICHLOROETHANE
F. T. : 950 SWW : .'• 60 QUAN :
R. R. T: 1. 03 MASS : i 101; AMNT :
MASS INTENSITY
MASS INTENSITY
97 1000
LIBRARY EDITOR
C2. H4. CL2
NAME: 1,2-DICHLOROETHANE
F. T. : 875 SWW :
R. R. T: 1. 03 MASS :
MASS INTENSITY
101 83
117 146
DATA: LIBRARYU1:
M. WT.: 98
50
98.
QUAN
AMNT
MASS INTENSITY
49 210
51 70
61 ' 276
LIBRARY EDITOR
C. CL4
MASS INTENSITY
62 1000
63 268
64 313
MASS INTENSITY
65 46
98 185
100 95
DATA: LIBRARYU1:
M. WT.: 152
NAME: CARBON TETRACHLORIDE
F. T. : 850 SWW :
R. R. T: 1. 00 MASS :
60
117.
QUAN
AMNT
MASS INTENSITY
47 120
49 132
MASS INTENSITY
117 1000
119 952
MASS INTENSITY
121 296
LIBRARY EDITOK
C6. H6
NAME: BENZENE
F. T. : 850 SWW :
R. R. T: 1. 00 MASS :
DATA: LIBRARYU1:
M. WT.: 78
60
78.
QUAN
AMNT
MASS INTENSITY
49 37
50 150
51 166
MASS INTENSITY
52 213
74 49
76 65
MASS INTENSITY
77 268
78 1000
79 72
18
A
100.40
BASE M/E: 97
RET. T: 10:44
NG
MASS INTENSITY
119 130
121 36
19
BASE M/E: 62
RET. T: 10:47
A
100.00
NG
MASS INTENSITY
102 16
20
A
100.00 NG
MASS INTENSITY
21
A
100.00 NG
MASS INTENSITY
207 0
219 0
264 0
BASE M/E: 117
RET. T: 10:57
BASE M/E: 78
RET. T: 10:57
-------
Section No. XI
Revision No/HF
Date: 08/19/85"
Page 8 of 11'
Tables of Libraries XI-1. (Continued).
LIBRARY EDITOR
C3. H6. CL2
DATA: LIBRARYU1:
M. WT.: 112
NAME: 1,2-DICHLOROPROPANE
F. T. : 875 SWW : 69 QUAN
R. R. T: 0. 39 MASS : 63. AMNT
MASS INTENSITY MASS INTENSITY
61 276 63 969
62 1000 64 252
LIBRARY EDITOR
C2* H. CL3
NAME:* TRICHLOROEHENE
F. T. : 850 SWW :
R. R. T: 1. 00 MASS :
MASS INTENSITY
65 366
76 548
DATA: LIBRARYU1:
M. WT.: 130
60
130.
QUAN
AMNT
MASS INTENSITY
60 456
62 775
LIBRARY EDITOR
C. H. CL2. BR
MASS INTENSITY MASS INTENSITY
95 982 130 1000
97 676 132 977
NAME: BROMODICHLOROMETHANE
F. T. : 875 SWW :
R. R. T: 1. 05 MASS :
DATA: LIBRARYU1:
M. WT.: 162
70
83.
QUAN
AMNT
MASS INTENSITY
47 145
48 102
79 81
MASS INTENSITY
81 39
83 1000
85 577
MASS INTENSITY
87 127
91 32
93 33
LIBRARY EDITOR DATA: LIBRARYU1:
C4. H7. 0. CL M. WT.: 106
NAME: 2-CHLOROETHYLVINYL ETHER
F. T. : 850 SWW : 70 QUAN :
R. R. T: 1. 00 MASS : 63. AMNT :
MASS INTENSITY
57 173
62 214
63 1000
MASS INTENSITY
64 94
65 305
71 108
MASS INTENSITY
105 13
106 344
108 105
22
BASE M/E: 62
RET. T: 11:26
100.00 NG
MASS INTENSITY
112 49
23
A
100.00
BASE M/E: 130
RET. T: 11:26
NG
MASS INTENSITY
134 305
24
A
100.00
BASE M/E: 83
RET. T: 11:34
NG
MASS INTENSITY
127 81
129 113
131
25
23
BASE M/E: 63
RET. T: 11:50
A
200.00 NG
MASS INTENSITY
-------
Section No. XI
Revision No.~TT
Date: 08/19/55"
Page 9 of 11
Tables of Libraries XI-1. (Continued).
LIBRARY EDITOR DATA: LIBRARYU1:
C3. H4. CL2 M. VT.: 110
NAME: CIS-1.3-DICHLOROPROPENE
F. T. : 900 SWW : 70 QUAN :
R. R. T: 0. 98 MASS : 110. AMNT :
MASS INTENSITY
49/ 170
51 71
MASS INTENSITY
75 1000
77 293
MASS INTENSITY
110 202
112 127
LIBRARY EDITOR DATA: LIBRARYU1:
C3. H4. CL2 M. WT.: 110
NAME: TRANS-1.3-DICHLOROPROPENE
F. T. : 950 SWW : 55 QUAN :
R. R. T: 1. 00 MASS : 110. AMNT :
MASS INTENSITY
49 182
75 1000
MASS INTENSITY
77 289
110 226
MASS INTENSITY
112 151
LIBRARY EDITOR
C7. H8
NAME: TOLUENE
F. T. : 950 SWW :
R. R. T: 1. 00 MASS :
DATA: LIBRARYU1:
M. WT.: 92
40
65.
QUAN
AMNT
MASS INTENSITY
50 34
51 48
62 28
63 58
MASS INTENSITY
64 15
65 100
73 2
74 8 .
MASS INTENSITY
77 10
89 41
91 1000
92 602
LIBRARY EDITOR DATA: LIBRARYU1:
C2. H3. CL3 M. WT.: 132
NAME: 1,1.2-TRICHLOROETHANE
F. T. : 900 SWW : 40 QUAN :
R. R. T: 1. 00 MASS : 97. AMNT :
MASS INTENSITY
61 579
83 901
MASS INTENSITY
96 345
97 1000
MASS INTENSITY
101 45
132 115
134 102
26
A
100.00. NG
MASS INTENSITY
27
* A
100.00 NG
MASS INTENSITY
28
BASE M/E: 75
RET. T: 11:57
BASE M/E: 75
RET. T: 12:18
BASE M/E: 91
RET. T: 12:21
A
100.00
NG
MASS INTENSITY
93 44
29
A
100.00
BASE M/E: 97
RET. T: 12:27
NG
MASS INTENSITY
136 21
-------
Section No. XI
Revision No.~HCT
Date: 08/19/85"
Page ID of ll~
Tables of Libraries XI-1. (Continued).
LIBRARY EDITOR
C. H. CL. BR2
DATA: LIBRARYU1:
N. WT.: 296
NAME: DIBROMOCHLOROMETHANE
F. T. : 850 SWW : ,
R. R. T: 1. 03 MASS :
MASS INTENSITY
79 305
91 808
93 170
MASS INTENSITY
94 102
127 1000 '
129 901
LIBRARY EDITOR
C2. CL4
NAME: TETRACHLOROETHENE -
F. T. : 900 SWW :
R. R. T: 1. 04 MASS :
MASS INTENSITY
82 108
94 579
96 383
MASS INTENSITY
129 761
131 725
133 228
LIBRARY EDITOR
C6. H5. CL
NAME: CHLOROBENZENE
F. T. : 900 SWW :
R. R. T: 1. 08 MASS :
70
127.
MASS
131
208
210
DATA:
M. WT.:
70
166.
MASS
164
166
168
DATA:
M. WT.:
60
114.
QUAN :
AMNT :
INTENSITY
171
198
64
LIBRARYU1:
164
QUAN :
AMNT :
INTENSITY
767
1000
465
LIBRARYU1:
112
QUAN :
AMNT :
MASS INTENSITY
50 488
51 527
MASS INTENSITY
56 68
76 93
LIBRARY EDITOR
C8. H10
NAME: ETHYLBENZENE
F. T. : 900 SWW :
R. R. T: 1. 09 MASS :
MASS INTENSITY
77 986
78 67
DATA: UBRARYU1:
M. WT.: 106
160
79.
QUAN
AMNT
MASS INTENSITY
50 73
51 171
63 65
65 141
MASS INTENSITY
74 19
77 97
78 98
79 48
MASS INTENSITY
89 28
91 1000
92 77
105 39
30
A
100.00 NG
MASS INTENSITY
31
BASE M/E: 127
RET. T: 12:57
BASE M/E: 166
RET. T: 13:05
A
100.00
NG
MASS INTENSITY
170 91
32
BASE M/E: 112
RET. T: 13:49
100.00 NG
MASS INTENSITY
112 1000
114 322
33
BASE M/E: 91
RET. T: 14:03
100.00 NG
MASS INTENSITY
106 251
-------
Section No. XI
Revision No. D"~
Date: 08/19/55"
Page 11 of 11
Tables of Libraries XI-1. (Continued).
LIBRARY EDITOR
C. H. BR3
NAME: BROMOFORM
F. T. : 850 SWW :
R. R. T: 1. 12 MASS :
DATA: LIBRARYU1:
M. HT.: 250
100
173.
QUAN
AMNT
MASS INTENSITY
79 98
81 103
91 105
MASS INTENSITY
93 140
94 80
171 510
MASS INTENSITY
173 1000
175 493
250 37
LIBRARY EDITOR DATA: LIBRARYU1:
C2. H2. CL4 M. WT.: 166
NAME: 1,1,2,2-TETRACHLOROETHANE
F. T. : 925 SWW : 120 QUAN :
R. R. T: 1. 16 MASS : 96. AMNT :
MASS INTENSITY
60 157
61 ,170
83 1000
85 637
MASS INTENSITY
87 99
95 151
96 108
97 100
MASS INTENSITY
98 64
131 70
132 25
133 66
34
A
100.00
BASE M/E: 173
RET. T: 14:40
NG
MASS INTENSITY
252 126
254 115
256 31
35
BASE M/E: 83
RET. T: 15:08
100.00 NG
MASS INTENSITY
166 43.
168 55
170 25
-------
Section No. XII
Revision No.5~"
Date: 08/19/55"
Page 1 of 2
IX. Quality Assurance
A. Spikes - A minimum of 1/10 of all samples prepared (1/10 which 1/10 fish,
1/10 waters) will be prepared and stored (see Section V). Sample spikes
will be obtained from the OWA operator and injected onto the solid sample
as in Section _ . Water samples will be spiked by the operator with the
addition of internal standards.
B. Duplicate Spikes - A minimum of 1/10 of all samples prepared (1/10 solids,
1/10 fish, 1/10 waters) will be replicates and will be prepared as in the
spike preparation.
*
C. Travel blanks (water) will be supplied when practical from random sampling
sites and continue to be recorded as a function of sample site, transpor-
tation source, and travel time.
D. Spiked travel blanks (water) will be sent to sample sources to be returned
with the collected samples.
Note: Trave1 blanks should be sent pretuned by different means to identify
best approach and the travel blanks, spikes sent to collection source
accordingly, :
E. Cross :noc .. ,,'ill be supplied and completed.
-------
Section No. XII
Revision No. 0
Date: 08/19/55"
Page 2 of 2"
F. Limits of detection will be confirmed periodically by quantitation of
detection limits by decreasing concentration of spikes until compound is
not found or cannot be confirmed by forward library searches. The limits
of detection should be calculated for each media type.
All detection limits found will be recorded in a QA/QC log as well as
blanks, travel blanks, spike recoveries, and travel blank recoveries.
These values will be addressed when reporting data are media types.
-------
\
Section No. XIII
Revision No.*~TT
Date: 08/19/51"
Page I of 37 "
XIII. MAINTENANCE
A. To assure continuous proper functioning of the Finnlgan OWA, maintenance
of the system should be performed as per Table XIII-1. (from Finnlgan OWA
1000 Series GC/MS Service Manual pp. 2.4-2.6).
B. The following procedure should be utilized to clean the source and rods
when so indicated in Table XIII-1.
The following procedure covers cleaning the ion source and changing the
electron multiplier. Routine replacement of the filament assembly 1s
recommended with each cleaning of the ion source, as it is not practical
to clean the filament assembly. You will need the following tools and
equipment.
1/2-in. (13 mm) end wrench
100-mm section of 5-in. (130 mm) 00 plastic pipe
disposable nylon gloves
lint-free industrial tissues
long-nose pliers
small screwdriver (l/8-in./3-mm blade)
number 600 aluminum oxide abrasive
cotton swabs
ultrasonic cleaner
methanol
aqua regia
stainless steel wire
Bunsen burner or propane torch
alignment fixture for ionizer assembly (base P/N 01504-20170; pin
P/N 01504-20180) •
replacement filament assembly (P/N 30004-60020)
plastic bag
volt-ohm-mi11iammeter
dental inspection mirror
-------
Section No. XIII
Revision No. 0
Date: 08/19/18"
Page 2 of 37 "
You must have a clean and clutter-free place to work.
f
Removing the analyzer. You will need a l/2-1n. (13-mm) end wrench or an
adjustable wrench and something to set the analyzer on when it 1s removed.
A short (100-mm) length of 5-1n. (130-mm) OD plastic "pipe works well.
1. Remove the cover from the mass spectrometer and set It aside.
Note: Do not touch the inner surfaces of the vacuum manifold and
magnet well, flor the analyzer, with your bare hands. Natural body
oils will contaminate and necessitate cleaning of any part that has
been touched. These oils will cause long-term background problems
in the spectra if present. Wear clean disposable vinyl gloves1
when handling such parts.
2. Remove the magnet from the magnet well and set it aside, then remove
the magnet well. See Figure XIII-1.
3. Make sure that the cables connected to the analyzer are properly
identifed (n.b. RF1 and RF2), the disconnect the cables.
)
Caution: The transfer line from the glass jet separator extends into
the ion source (see Figure XIII-2). It is necessary to swing the far
1P/N 00301-03600 small; 00301-09700 medium.
-------
Section No. XIII
Revision No.~lT~
Date: 08/19/|f"
Page 3 of 37~
Figure XIII-1. Mass spectrometer with cover removed.
end of the analyzer to the left (away from the GC) to clear the ion
»
source before withdrawing the analyzer from the vacuum manifold. It
helps to have somebody watching from the front.
4. Remove the right, left, and top capscrews that secure the analyzer
the manifold, and loosen the bottom one a little. Hold the analyzer
in place as you remove the fourth screw to prevent the analyzer from
slipping and being damaged.
5. Swing the analyzer to the left to clear the ion source, and carefully
withdraw it from the vacuum manifold.
6. Place the analyzer on a suitable support (Figure XIII-3). Place wads
-------
Section No. XIII
Revision No. 0
Date: 08/19/83
Page 4 of 37 "
TRANSFER
LINE
Figure XIII-2. Removing the analyzer from the vacuum manifold (plain view).
Analyzer must be swung to the right to clear the interface transfer line.
of clean, lint-free tissues in the ends of the vacuum manifold to
keep dust out.
Note: Sterile technique must be used in the following steps. Do not
touch with bare hands any part that you do not intend to clean. Wear
disposable nylon gloves when handling clean parts. Tools must be
clean and free from oils.
General considerations. It is necessary to hold binding posts with
pliers to keep them from rotating when you are loosening or tightening
screws. This is especially important with the connections to the
quadrupole rods, where rotation of the binding posts could throw;the
rods out of alignment; and also with the filament connections, where
rotation of the posts could break the filament.
-------
Section No. XIII
Revision No.~^T~
Date: 08/19/55"
Page 5 of 37~
Figure XII1-3. Mass analyzer.
Ion source: Note the orientation of the ion source assembly with
respect to the quadrupole housing before you remove it. The odds are
against you if you don't. Disconnect the leads from the ion source,
then remove the three screws that secure the ion source assembly to
the quadruple housing and lift the ion source assembly from the
housing. See Figure XIII-4 for identification of parts.
-------
Section No. XIII
Revision No. 0
Date: 08/19/83"
Page 6 of 3f"
.. • t , J /— ION VOLUME
COLLECTOR
LENS
APERTURE
FILAMENT
ASSEMBLY
Figure XIII-4. Exploded view of ion source.
1. Remove and discard the filament assembly.
2. Remove the collector.
3. Remove the ion volume, extractor, lens, and aperture.
-------
Section No. XIII
Revision No.~lT
Date: 08/l°/83
Page 1 of 37"
4. Using a slurry of number 600 aluminum oxide in water and a
cotton swab, remove all contamination from the ion volume.
(Contamination appears as dark or discolored areas.) Use a
wooden stick cut at an angle to clean the Inside corners. Try
not to let the slurry dry on the metal, as dried aluminum oxide
is difficult to remove. Rinse off the aluminum oxide with
running water and place the parts in a small container of
detergent and water. Clean the extractor, lens, and aperture
in the same way.
5. Place the container of parts in an ultrasonic cleaner for 60
seconds, then rinse with water. From this point on, parts must
be handled with clean tools to prevent recontami nation.
6. Using clean tools, place the parts in a container of water; and
place the container in the ultrasonic cleaner for 60 seconds.
Caution: Ultrasound may cause the small screws in the binding
posts to vibrate loose. Take care that none are lost in rinsing.
7. Rinse the parts with methanol.
8. Place the parts in a clean beaker of methanol, and place the
beaker in the ultrasonic cleaner for 60 seconds.
-------
Section No. XIII
Revision No, 0
Date: 08/19/ST
Page 8 of 37"
9. Inspect the parts, and ensure that all spots and particles have
been removed.
10. Immerse the sapphire spacers 1n aqua regia and rinse them with
distilled water. -
11. If the ceramic parts have metal deposits (dark streaks) on them,
immerse them in aqua regia and rinse them with distilled water.
Remove organic contaminants by stringing the parts on a stainless
steel wire and heating them in a Bunsen or propane flame until
they are red hot.
12. Check to ensure that each of the threaded rods extends 13 mm
(1/2 in.) above the ionizer adapter, then set the adapter on the
alignment fixture base (Figure XIII-5).
13. Stack the aperture, lens, extractor, and ion volume assembly on
the studs, using the appropriate bushings and spacers (see
Figure XIII-4). Install the four nuts, but do not tighten them.
14. Insert the three screws into the mounting holes for the filament
assembly and collector. Leave the screws loose for later removal
15. Insert the alignment-fixture pin through the ion volume, lens,
-------
PIN
01504-20180
ION
VOLUME
EXTRACTOR
LENS
APERTURE
ADAPTER
BASE
01504-20170
STORE PIN HERE
WHEN NOT IN USE
Section No. XIII
Revision No. iQT
Date: 08/19/8T"
Page 9 of 37 "
Figure XIII-5. Alignment fixture base and
pin, with assembled ion source.
extractor, and aperture and into the alignment-fixture base.
16. Tighten the four nuts. (DO NOT OVERTIGHTEN; finger-tight is
enough) and remove the alignment-fixture pin.
17. Remove the three loose screws and install the new filament :
assembly. See Figure XIII-6. Position tf? f r-..nent assembly
-------
Section No. XIII
Revision No. 0
Date: 08/19/83
Page 10 of 37"
parallel and as close as possible to the Ion volume without
touching.
Figure XI11-6. Ion source with filament assembly
installed. Note arrangement of spacers.
18. Look through the ion volume from the collector side and be sure
that the filament is visible in the center of the slit (Figure
XI11-7). Tighten the screws.
Figure XIII-7. Ion source assemb.y pr,-.
installation o. collector. Loc thr-'
the ion volume from the col lee or $v
and make S1."-? that the filar '
visible in the center of the slit.
-------
Section No. XIII
Revision No. 0
Date: 08/19/83T
Page 11 of 37'
19. Install the collector, making sure that the bushing and spacers
are 1n the proper sequence (Figure XI11-8).
Figure XIII-8. Ion source assembly
with collector installed. Note
arrangement of spacers.
20. Position the collector so that it is parallel to and 0.5 to 1.0
mm from the ion volume, then tighten the screw.
Quadrupole: Normally, contamination occurs only at the ends of
the rods nearest the ion source. If the rods are dirty, discon-
nect the rf leads and unscrew the four binding posts. Note: if
the ends of the rods are marked with a punch mark (characters or
center punch). It will be necessary to reinstall the rods with
the punch-marked ends facing in the same direction after they
are cleaned. Remove the single screw holding the quadrupole
-------
Section No. XIII
Revision No. 0
Date: 08/19/85"
Page 12 of 37
assembly to the housing and, grasping one rod, draw the assembly
from the housing. Handle the quadrupole assembly by the ceramic
Insulators to avoid misalignment. Place a clean plastic bag
over the remainder of the analyzer to keep dust out of the
multiplier. Using number 600 aluminum oxide/water slurry as
before, clean the quadrupole rods. Do not disassemble the rods
from the ceramic spacers.
Caution. To avoid stressing the assembly and possible misalign-
ment, rest each rod against a stable support while cleaning.
Rinse the ends of the rods with methanol. Do not allow methano'l
to come into contact with the ceramic insulators. The ceramic
will absorb methanol and generate a strong methanol background
when the filter is put back into service. Slide the filter
assembly into the housing, making sure that the marked ends of
the rods are facing the same wasy as before. Replace and tighten
the screw that secures the filter assembly to the housing.
Replace the four binding posts.
Caution. Tighten the binding post finger tight only. Over-
tightening may turn the rod-retaining screws, necessitating.
realignment of the rod assembly.
-------
Section No. XIII
Revision No. 0
Date: 08/19/53"
Page 13 of 37
If the electron multiplier Is not to be changed, proceed to
Reassembly.
Electron multiplier. The normal life of an electron multiplier
———— ^
is 6 to 18 months. We recommend that you budget for a new
multiplier once per year. To change the electron multiplier,
proceed as follows.
1. Disconnect the leads from the ion source and quadrupole filter.
2. Remove the three screws at the base of the multiplier housing
and lift off the entire assembly, exposing the multiplier.
3. Loosen the upper screws (Figure XIII-9) in the high-voltage and
anode couplings and remove the two screws that secure the
multiplier to the flange plate. Remove the multiplier.
4. Install the new multiplier on the flange, making sure that the
leads are connected to the proper terminals (bottom) lead to
ANODE, upper lead to HV).
5. Replace the housing, aligning the punch mark on the housing.
with the punch mark on the flange (Figure XIII-10).
-------
Section No. XIII
Revision No. 0
Date: 08/19/5T"
Page 14 of 37
Figure XIII-9. Electron multiplier.
Loosen screws a and remove screws b
to replace the electron multiplier.
TAPPED HOLE
PUNCH MARK
PUNCH MARK
Figure XIII-10. Closeup of Multiplier housing,
showing punch marks.
-------
Section No. XIII
Revision No. 0
Date: 08/19/33"
Page 15 of 37 '
Reassembly:
1. Reconnect the rf leads to the quadrupole mass filter.
2. Reinstall the ion source and connect the leads.
3. Using an ohmmeter, check that no element is shorted to any other
or to ground.
RF1 to RF2
Ground to RF1
Ground to RF2
Ground to lens
Ground to extractor
Ground to ion volume
Ground to collector
Ground to filament 1
Ground to filament 2
Lens to extractor
Lens to ion volume
Lens to collector
Lens to filament 2
Lens to filament 2
Extractor to ion volume
Extractor to collector
Extractor to filament 1
Extractor to filament 2
Ion volume to collector
Ion volume to filament 1
Ion volume to filament 2
Collector to filament 1
Collector to filament 2
Filament 1 to filament 2
\-~/
(-0)
(-0)
(-0)
131
open circuit (»n)
open circuit («n)
open circuit (-0)
open circuit
open circuit
open circuit
open circuit
open circuit , „,
open circuit («8)
open circuit («8)
open circuit («n)
open circuit («n)
open circuit (-Q)
open circuit («n)
open circuit (•£})
open circuit (•«)
open circuit
open circuit
open circuit
open circuit
open circuit *fi
open circuit (•«)
open circuit («8)
0.2 ohms
(»n)
(•«)
(»n)
Installation:
-------
Section No. XIII
Revision No. 0
Date: 08/19/55"
Page 16 of 37
Caution. The transfer line from the glass jet separator projects
Into the 1on source when the analyzer 1s Installed. Angle the
analyzer well to the left (as viewed from the rear) and maintain
this attitude while Inserting It into the vacuum manifold, until
the flanges meet. Have someone watch from the front to make
sure that the transfer line enters the ion source without damage.
1. Install the analyzer, securing 1t with the four screws. Tighten
the screws. Tighten the screws uniformly.
Note: It is good practice to tighten the screws a little at a
time in diametrically opposite pairs. See Figure XIII-11.
0
$
*
*
> •
Figure XIII-11. Rear view of vacuum manifold.
Tighten screws in this order:
1, 3, 2, 4, 1, 3, 2. 4, etc.
-------
Section No. XIII
Revision No. 0
Date: 08/19/31"
Page 17 of 37"
2. Using a dental Inspection mirror, check that the transfer line
Is 1.5 to 3 mm from the 1on volume. Reposition the source, if
necessary, then check-that the transfer line 1s still properly
aligned with the Ion-source opening.
Note: If the Instrument Is equipped with a solid-probe Inlet,
the opening In the Ion volume must be accurately centered with
respect to the Inlet barrel. If 1t Is not, loosen the three
screws that secure the Inlet assembly to the vacuum manifold and
shift the Inlet assembly.
3. Use the VOM to check that none of the ion-source components is
shorted to any other, then attach the cables to the rear
connectors.
4. Install the magnet well and tighten the.four capscrews.
«
5. Move the PUMP switch on the power controller to PUMP and the
ANALYZER VOLTAGES switch to ENABLED. Wait 10 minutes. Press
the yellow RESET button. The RESET light should go out; if not,
check the SYSTEM STATUS lights.
60 vmall the magnet in the magnet well in a vertical orientation
aiM connect the VOM to test points 6 (+) and 7 (-} on the
-------
Section No. XIII
Revision No."~TT
Date: 08/19/1F
Page 18 of 37
Ion-source board (Figure XIII-12). (Test points are numbered
from top to bottom of the board.)
/. "
7. Start the data'system and run the manual tune program (MT).
Turn on the filament. The VOM should indicate between 0 and 250
.t
mV DC. Rotate the magnet back and forth and move It in and out
while watching the VOM, the object being to obtain maximal
collector current. (The measurement is across 100 ohms, so 100
mV represents 1 mA of collector current.) If the maximal
reading is less than 60 mV, turn the magnet end for end and try
again. Low collector current may indicate that the filament is
not properly aligned.
Note: Collector current should be 80% of the total emission
current, which can be read at test points 6 (-) and 8 (+).
Emission current"is factory set at 750 pA (read 75 mV) and
should require no attention.
8. Turn the ANALYZER VOLTAGES switch to STANDBY (or run the system).
Vacuum System:
Purging the Alcatel pumps: The Alcatel vacuum pumps can be purged without
interrupting the system operation. Unscrew the knob shown in Figure XIH-13
-------
Section No. XIII
Revision Itoo 0 ,
Date: 08/19/%3"~
Page _19 of 37
Figure Xiil=12. Ion-source circuit boardo Connect VOM to TP 4(+)
and TP5 (-). Test points are numbered from top.
-------
Section No. XIII
Revision No. 0
Date: 08/19/55"
Page 20 of 37
GAS
BALLAST
SIGHT
GLASS
GAS
BALLAST
VALVE
DRAIN
PLUGS
Figure XI11-13. Alcatel pump, showing gas
ballast valve, drain plug, fill
plug, and sight glass.
a few turns to open the gas ballast valve. Let the pump run with the gas
ballast valve open for about 5 minutes, then close the valve.
Changing the oil in the Alcatel pumps. Oil changes should be performed
while the pump is warm. Shut down and vent the system. Disconnect the
pump hose and power cord. Place the pump on a bench. Remove the drain
plug Figure XIII-13) and allow the oil to drain, the replace the plug and
fill the pump with fresh oil to the middle of the sight glass. Alcatel
oil VP1 is recommended. Start up the system.
Changing the oil in the turbomolecular pump. To change the oil in the
turbomolecular pump, stop the pumps and vent the vacuum system as
described under Mass Spectrometer maintenance, above. Then follow tilt-
instructions in the legend to Figure XIII-14o
-------
Section No. XIII
Revision No. 0
Date: 08/19/5T"
Page 21 of 37
OIL RESERVOIR
Figure XIII-14. Turbomolecular pump. Before removing the oil reservoirs,
vent the vacuum system to the atmosphere, then unscrew the reservoirs,
taking care not to damage the 0-rings. Wipe out the reservoirs with
e clean rag. Wipe the 0-ring and oil it lightly with T12 oil. Fill
the reservoirs with 10 ml of T12 oil and reattach them to the pump.
(Tighten lightly.)
Regenerating the filter/drier: The filter/drier (Figure XIII-1) is filled
with indicating DRIERITE (anhydrous calcium sulfate). Indicating DRIERITE
is a distinct blue. When exhausted, it turns to a rose red or pink.
Regeneration will restore the blue color. DRIERITE granules should be
removed from the col urn and spread evenly, one granule deep, on a tray.
Heat for 1 h at about 200C. The dessicant should then be cooled in a
tightly-closed container before you refill the column. Felt filters
should be dried at 100°C for about 30 minutes before reassembly.
DISK DRIVE:
-------
Section No. XIII
Revision No.T"
Date: 08/19/51"
Page 22 of 37
Caution. There is no warranty on the read/write heads nor the disks;
preventive maintenance of these items is the customer's responsibility.
It is therefore extremely important that the preventive maintenance
procedures suggested in this manual be performed at suitable intervals.
We suggest inspection of the air filter and the read/write heads three
months after the installation of the system and at regular intervals
thereafter, based on the condition of these items at the first inspection.
Read/Write Heads: .
Because of the very small clearance between the head and disk surfaces, it
is,imperative that the heads as well as the disks be kept clean. When in
the flying attitude, the heads are separated from disk surface by only a
few micrometers; and because of the high disk speed, even small particles
adhering to the heads may cause damage to the head or to the surface of
the disk. To inspect the heads for accumulation of dust or oxide parti-
cles, remove the disk pack and illuminate the head area. The upper heads
can be seen with the aid of a dental-type mirror.
Caution. Do not touch the head surfaces or bring them into contact with
any object other than the cleaning applicator.
To clean the heads, use 91% isopropyl alcohol in solution with 9% distilled
-------
Section No. XIII
Revision No. 0
Date: 08/19/31"
Page 23 of 37
water. Do not use any other kind of liquid. Apply with a lint-free
cotton swab1.
Spindle Chuck and Cone:
Clean the surfaces of the spindle chuck and cone (Figure XIII-15) using
alcohol-moistened disposable wipes (Kimwipes). Ferrous particles adhering
to the magnet ring can be removed with masking tape.
Figure XIII-15. Disk drive showing spindle chuck and cone.
Air Filter:
To inspect the air filter, pull the disk drive out on its rails and remove
IPerkin-Elmer recommends Foam Floss-tipped swabs, which leave no residue.
-------
Section No. XIII
Revision No. 0
Date: 08/19/83
Page 24 of 37
the sheet metal cover under the left front corner (seven screws, see
Figure XII1-16). Loosen the two wedge-shaped clamps on the filter and
remove the filter element. Peel off the styrofoam prefliter and Inspect
the filter. A clean filter is pure white. A dirty filter will be white
around the edges where the adhesive for the prefliter blocks the flow of
air and gray or black 1n the center. If the filter is dirty, 1t must be
replaced.
FILTER
Figure X-16. Air filter removal.
-------
Section No. XIII
Revision No.""TT~
Date: 08/19/55"
Page 25 Of 37"
Parts Order Requests:
To order parts, call the Finnlgan Parts Center (408) 732-0940.
C. The following troubleshooting charts (Tables XIII-1 thru XIII-4) should be
utilized if difficulties are encountered in OWA operation. These charts
should be used before contacting Finnigan Service Representative.
Note: Maintenance and troubleshooting guide (Tables XIII-1 thru XIII-4)
from Finnigan manuals 10000-90080 and 10000-90140.
-------
Section Wo0 am
Revision Mo0 0
Oitet 08/19/33
26 of 37
TABLE XIII-lo MAINTENANCE CHECKLIST (PREVENTATIVE MAINTENANCE):
1 ©tesa jc/j
2. ©laso jc3
3. fctoss onctyxcr ^^
assy
o aotcr Rgc; scnssr swi
moso
g»
6. Atesd vcs^atm giS5^3 (§8
y.
Q.
SJ/SJCTfl
e3
°cga saseo BJcRtofa assy
D. Ai7 sate? as feciferai e3 eago
afco • •
3. S^rcJ eafeto ea
' fl. Yapo
Topo
; fl. PoKi
f&eocisago
loohs.
oco.
fcyi?y goes sftapo.
©3 as?
& ea
CT
B5C3C1
o
&
EOTSQVAL
eioa«.
oo
ore &?
li
-------
Section NOc ___
Revision Wo<> 0
Date: 08/19/15"
27 of 37
TABLE-XIII-1. MAINTENANCE CHECKLIST (PREVENTATIVE MAINTENANCE) (Continued),
fl. Para
S. Afijustasio Sg
•3. P>e£)aenc? garage
ratio
S.
0. Aff fifsc?
?. UTO fusoa to jfto ©g
tef packed
IL
soptura in 610 ©6
i. Conic? gas
Wtc?
7.
0.
0. Pceted coluffm (glass
?@. Fceticd eehjma ((nets!
m. OcHcae? pe^ i© Cg-ftfl
. ©6 e@o3 esc/a fcra
goa
to
tho
-------
Section No. XIII
Revision No. 0
Date: 08/19/83
Page 28 of 37
Item
TABLE XI11-2: ELECTRONIC TROUBLESHOOTING CHART
s=css=s==Bssssssssasssss===ssssss=sss=sass=ssss=as8ssa8ssssssc=BS
Symptom Probable Cause Corrective Action
NOTE: Unless otherwise specified, all paragraph
and page references pertain to the Sigma 3
Service Manual from Perkin-Elmer (part no.
00920-05902, August 1978 issue).
1. GC will not enable.
2.
Oven fan will not
rotate.
3.
4.
No display on front
panel.
Oven, injector and
detector will not
heat.
Fl blown
F2 blown
SI (power switch) open
Replace Fl
Replace F2
Check SI with ohm
meter.
Lower fan tangled in cables Reposition cables.
Oven lid micro switch
defective
Kl oven relay defective.
B2 fan motor defective.
F4 blown +5VDC
Fl in power supply blown
F2 in power supply blown
F3 in power supply blown
F4 in power supply blown
+15VDC power supply failure
-15VDC power supply failure
+5VDC power supply failure
+12VDC power supply failure
MPU PCB defective
Check for continuity
with ohm meter; if
required, replace the
faulty switch.
Check for continuity
with ohm meter; if
required, replace the
faulty relay.
Check for proper fan
rotation and check
that windings are not
open. If defective,
replace faulty motor.
Replace F4.
Check with ohm meter
and replace defective
fuse.
Check power supply
with volt meter and
replace. If defec-
tive, refer to section
3.4.3.
Check TP14 (DAC vol-
tage); if incorrect,
replace MPU PCB card.
-------
Section No. XIII
Revision No. 6
Date: 08/19/8?"
Page 29 of 37 '
Item
Symptom
TABLE XIII-2. (Continued).
Probable Cause
Corrective Action
5. Oven will not heat Oven max temp set too low
but Injector and
detector will heat.
Oven heater open
Defective control circuit
on temp control PC8 card
No set point from MPU
Oven Triac defective
Oven lid micro switch open
6. Injector will not Defective control circuit
heat oven and on the temp PCB card
detector will heat.
Check oven max 1s set
correctly, power-down
and power-up. Reset
oven temp.
Check heater with ohm
meter; if open,
replace hester.
Check TP7 (oven Triac
pulse); 1f incorrect,
check TP3, if correct,
replace temp
corrective action PCB
card; 1f Incorrect,
check oven sensor with
ohm meter.
Check TP8 (oven set
point); if incorrect,
replace MPU PCB card.
Check oven Triac wave-
form with a suitable
scope.
Check switch for con-
tinuity with ohm
meter; if defective,
replace the switch.
Check TP9 injector
Triac pulses; if
correct, check
injector Triac
waveform; if
incorrect, check TP5.
If TP5 is correct,
replace temp PCB card;
if incorrect, check
injeccor sensor with
ohm meter.
-------
Section No. XIII
Revision No. 0
Date: 08/19/1?"
Page 30 of 37~
Item
TABLE XIII-2. .(Continued).
: = === ===== === ==== = = = = ======= ==3=:== ==== ==== =
Symptom Probable Cause
Corrective Action
6. Injector heater cartridge
open
Injector Triac defective
7. Detector will not Defective control circuit
heat oven and on temp PCB card
injector will heat.
Injector and No set point from MPU PCB
detector will not card
heat.
Unable to read any GC/IO PCB card defective
actual temps or set
points.
MPU PCB card defective
Check for continuity
with ohm meter and
replace, if defective.
Check injector Triac
waveform; 1f
incorrect, replace
Triac.
Check TP8 detector
Triac pulses; 1f
correct, check
detector Triac
circuit; if incorrect,
check TP12, and if
TP12 is correct,
replace temp PCB card.
If TP12 is incorrect,
check injector sensor
with meter.
Check TP9 zone set
point; if incorrect,
replace MPU PCB; if
correct, check for
loose or open cable
from MPU to temp
control.
Connect test box in
place of GC/IO; if GC
works, replace GC/IO;
if GC does not work,
check MPU.
Check MPU TP14 (DAC
voltage); if
incorrect, replace MPU
PCB card; if correct,
check cable from
keyboard to MPU.
-------
Section No. XIII
Revision No.~"TT~
Date: 08/19/53"
Page 31 of 37~
Item
TABLE XIII-2. (Continued).
== = ==== = = = ======== = = === = =====================:======:r=:5== ==c======== ==r:r
Symptom Probable Cause Corrective Action
9.
10.
11.
12.
13.
Actual temps are
Incorrect.
Trip, Ready, and Display
PCB card defective
Temp control PCB card needs
alignment
MPU needs alignment
READY indicator Trip, Ready, and Display
light will not come PCB card defective or
on. misaligned.
MPU PCB card defective
Oven will not pro- MPU PCB card defective
gram temperature.
Oven door solenoid +24VDC missing
will not operate.
MPU PCB card defective
If MPU and keyboard
are working correctly,
replace Trip, Ready,
and Display PCB card.
Align temp PCB card as
per paragraph 4.12.1
Align MPU PCB card as
per paragraph 4.12.3.
Check part number of
IC4, refer to para-
graph 3.7.2b; If in-
correct, replace dis-
play PCB card; if
correct, check PIN1 of
IC13.
Check PIA2 pin 4 for a
logic high value.
Refer to paragraph
3.7.2B. If P1A2 is
incorrect, replace MPU
PCB card.
Replace MPU PCB card.
Check +24VDC, if
faulty, replace power
supply PCB card.
Check PIA2 Pin 6 (a
high signal is an open
vent command); refer
to paragraph 3.7.3; if
incorrect, replace MPU
PCB card.
-------
Section No. XIII
Revision No. 0
Date: 08/19/83
Page 32 of 37"
Item
TABLE XIII-2. (Continued).
===========================================
Symptom Probable Cause
Corrective Action
13.
14.
Sub-ambient assem-
bly will not work.
Trip, Ready, and Display
PCB card defective
Clogged flow restrictor in
air line
Faulty mini piston
Sub-ambient switch in OFF
position
CO2 Tank empty or not dip
tube type
Trip, Ready, and Display
PCB card defective
+24VDC power supply is
faulty
Pressure too low (LN2
only)
Check collector of
Q12; refer paragraph
•3.7.3; if incorrect,
replace display PCB;
if correct, check
solenoid with ohm
meter.
If vent solenoid is
actuating, the flow
restrictor should
allow piston to open
fully in 45 t 15
seconds; if not,
replace restrictor.
Disconnect air line at
piston, and check that
piston moves freely;
if the piston does not
move freely,, then
replace it.
Position the sub-ambi-
ent switch on back of
GC to ON.
Check collecor of Q12;
refer to paragraph
3.7.3; if incorrect,
replace display PCB
card; if correct,
check S/A solenoid.
Check 24VDC power
supply, if power
supply is faulty,
replace power supply
PCB card.
Check that pressure is
20 to 30 Ibs. at tank.
-------
Section No. XIII
Revision No. 13"
Date: 08/19/55"
Page 33 of 37
Item
TABLE XII1-3. CHROMATOGRAPHY TROUBLESHOOTING CHART
S==S2=S=32S=S=SS=SSS=S===8SS8SS=S==SSS2S===SSSS8S3:SSSSSCSS8SSSSSS
Symptom Probable Cause Corrective Action
NOTE: Unless otherwise specified, all
paragraph and page references pertain to
the Sigma 3 Service Manual from Perkin-Elmer
(part no. 00920-05902, August 1978 issue).
1. Non reproducible
quantitation
Sample evaporation
Septum leaking
Faulty syringe
Detector or injector too
cool
Insufficient head pressure
on regulator or controller
Ghost peaks
Leaks
Oven temperature unstable
Defective pressure regula-
tor or flow controller
Use fresh sample.
Change septum.
Use test syringe.
Check with temp meter,
if the reading is
lower than set
temperature, refer to
the electronics
troubleshooting guide.
Increase input
pressure.
Contaminated septurns,
injector and column;
clean or replace
column. Refer to
paragraph 4.3.2B.
Section 4.4.
Check with temp meter
and if incorrect,
refer to the
electronic trouble-
shooting guide.
Bypass to test.
(continued)
-------
Section No. XIII
Revision No. 0
Date: 08/19/37"
Page 34 of 37"
Item
Symptom
TABLE XI I 1-3. (Continued).
sssaassss=as=3Ssssassssssss
Probable Cause
Corrective Action
2. Peak tailing
3. Low response
Injection too large
Dead space in column
adapters
Incorrect temp for sample
Column condition
Injector, oven detector
temp out of calibration
Incorrect column for
application
Reduce volume.
'Change fittings.
Review application.
Use a test column.
Use temp meter. If
defective, refer to
paragraph 4.12.1.
Review application.
Leaks at column connections Refer to Section 4.4.
Septum leak Replace septum.
Faulty syringe Use test syringe.
Contaminated Gases Change cylinders.
Poor injection technique
Review injection
procedures.
-------
Section No. XIII
Revision No. 0
Date: 08/19/8T
Page 35 of 37
TABLE XII1-4. TROUBLESHOOTING CHART FOR ANALYZER MODULE
a==ss==rss=========s================================================
Item Symptom Probable Cause Remedy
1. Low sensitivity
Ion source contamination.
Magnet misalignment.
Contaminated lens.
Defective or misaligned
quadrupole.
Contaminated rod.
RF failure.
Refer to operating
manual cleaning
procedure.
NOTE: With an emis-
sion current of 750
yA from the filament.
the collector current
will be at least 600
yA. The filament
alignment and magnet
adjustment will
influence this value,
and if these are
optimal then collector
currents below 600 yA
indicate a contamin-
ated source; if the
collector current is
below 400 yA the
source is grossly con-
taminated. Another
indication of source
contamination is the
need for higher than
normal extractor
voltage; greater than
5 volts.
Refer to the
Operator's Manual
quadrupole alignment
procedure.
NOTE: Quadrupole
filter contamination
is usually diagnosed
as differential loss
of high mass sensitiv-
ity, poor resolution
and poor peak shapes.
Together these factors
(continued)
-------
Section No. XIII
Revision No. 0
Date: 08/19/%T
Page 36 of 37"
s===================r
Item Symptom
TABLE XIII-4. (Continued).
:sss2ssss==s==s=ss^=s:
Probable Cause
Corrective Action
1.
2. Low output
Calibration
difficulty
No spectra
Multiplier gain decreased
due to multiplier failure
or contamination. v
Malfunction in high voltage
circuit.
Poorly tuned source or air
leak.
Contaminated quadrupole
filter.
Filament failue.
No filament voltage.
cause progressive
difficulty in tuning
•and calibration. The
rods are contaminated
and should be cleaned.
Refer to the
Operator's Manual
maintenance procedure.
Replace multiplier.
Troubleshoot High
Voltage circuit (see
Test procedures and
adjustments in Section
10 of this manual).
Adjust MT and/or AT,
check for air leak as
described in Section
13 of this manual.
Clean rods according
to operating manual
maintenance procedure.
Replace filament.
Check for filament
voltage at the fila-
ment connector.
Troubleshoot power
module as required
(see Section 9 and Ion
Source PCB Testing in
Section 10 of this
manual).
-------
Section No. XIII
Revision No. 0
Date: 08/19/5T"
Page 37 of 37~
TABLE XIII-4. (Continued).
============================================================s===s=========-====
Item Symptom Probable Cause Corrective Action
5. Manifold tempera-
ture low
Defective manifold heater
circuit.
Wrong or no temperature
data entered in system.
Check manifold heater
connections, heater
and sensor element
continuity, verify
presence of heater
voltage (220 VAC) from
power module. Repair/
replace defective
components.
Run SS program to
enter temperature
data.
6. Manifold tempera-
ture runaway
Wrong or no temperature
data in system.
Defective temperature
cutoff control.
7. No heater voltage Blown fuse.
Defective heater triac
circuit.
Enter program SS.
Replace temperature
cutoff element.
Replace heater fuse or
triac circuit compo-
nent in power module
(see Section 9 of this
manual).
-------
Section No. XIV
Revision No.~~T"
Date: 06/01/37"
Page 1 of 1 "
XI. SAFETY
Wear
,(
During any work, the analyst should wear appropriate safety equipment.
Lab coats, safety glasses "and safety shoes should be worn at all times,
including sample and standard-analysis and preparation. The operator should
also be aware of hot surfaces (manifold, transfer line, etc.) and take pre-
cautions against thermal burns.
Gases ,
The gases normally used with this instrument are compressed air, helium,
and liquid nitrogen (see Appendix A, Safe Handling of Compressed Gases in the
Laboratory). The operator and other authorized laboratory personnel should
exercise caution in handling the liquid nitrogen, as the extremely cold liquid
can cause severe burns and frostbite. The helium and air should be handled as
specified in Appendix A.
Spills
Spill control pillows should be applied immediately to all spills. Spills
of extremely toxic substances should be reported to the supervisor immediately
after cleanup (see Appendix B).
-------
Section No. XV
Revision No. 0
Date: 08/19/83"
Page l of l~
Miscellaneous
A. File Deletion In ID0S
1. Sometimes It 1s necessary to delete files In ID0S.
2. Any files which aren't protected should be protected first.
3. > DIAG (CR)
+ PRO LIBRARYNB.LX/33 (CR)
4. Still in ID0S you are ready to delete.
+ DE 0:
This command will give you a file 0.-82VOAXXX.XX
Type (Y) if you want to delete just type (CR) and it will now list
the next file for delection.
5. Skip all protected files or this will stop DE and give you a (+)•
6. To get out of IDOS:
+ M (CR)
-------
Section No. A
Revision No. 1
Date: 06/01/3F
Page 1 of 12
APPENDIX A
SAFE HANDLING OF COMPRESSED GASES
IN THE LABORATORY
-------
Section No. A
Revision No. 1
Date: 06/01/3T
Page 1 of 12
APPENDIX A
SAFE HANDLING OF COMPRESSED GASES
IN THE LABORATORY
-------
Section No. 'A'
Revision No. 1
Date: Q6/01/8T"
Page 2 of 12"
SATE HANPLTNC OF COMPRSSSIP CASES IS ?H£ LABORATORY
(Taken from AXE8JCAS LABORATORY, September. 1978)
Although tha safety record of eha coaprasaad
gas industry is excellent, the questions
raised by tha users of gaa products, and tha
accidents involving these same users, show
that cany of them havo neither learned nor
applied'tho safety measures that would earn
their "license" for handling coeprassad
gaa. When handled by personnel who ara prep-
orly trained and aware of the potential
hazards, coapressod gases ara an safe to...
work with as most of the ordinary chemical
liquids and solids normally handled on a
routine basis in any laboratory.
A compressed gas is defined by tho Dope.
of Transportation (DOT) as "any material
or mixture having in the container an ab-
solute pressure exceeding 40 pai at 70°T
or, regardless of the pressure at 70°F,
having an absolute pressure exceeding
104 pal at 130°T; or any Liquid flacaablo
material having a vapor pressure exceed-
ing 40 psi absolute at 100°T as determined
by AS7M Test D-J23." .
i
Hazards
The handling of compressed gases must bo
considered more hazardous than the hand-
ling of liquid and solid materials be-
cause of the following properties
unique to compressed gases; pressure.,
diffusivity, low flash points for flaa-
mable gases, lev boiling points, and no
visual and/or odor detection of many
hazardous gases. Hazards may arise aa
a result of equipment failure and leakage
froa systems that are not pressure-
tight. Also, improper pressure control
may cause unsafe reaction rates duo to
poor flow control. Diffusion of leak-
ing gases may cause rapid contamination
of tho atmosphere, giving riso to
toxicity, anesthetic effaces, asphyxi-
ation, and rapid formation of explosive
concentrations of flammable gases. Th<
flash point of a flammable gas under
pressure is always lower than ambient
or rooa teaperature. Leaking gas can
therefore rapidly form an explosive
mixture with air.
Lev-boiling-point materials can cause
frostbite on contact with living tissui
This is common among the cryogenic
liquids such as nitrogen and oxygen,
but it also can result froa contact
of the liquid phase of liquefied gases
such as carbon dioxide, fluorocarbons,
and propyleae. Some compressed gases
are similar to other chemicals in that
they are corrosive,'irritating, and
highly reactive.
The procedures adopted for tho safe
handling of compressed gases are main!
centered on cootaicmont of the aatoria
to prevent its escape to atmosphere,
and proper control of pressure and
flow. All rules and regulations are
directed toward these ends. Knowledge
of emargeacy procedures is iaportant
to liait property damage or injury, bu
is usually necessary only because a
basic rule of handling has been broken
It is far better to observe tho rules
and avoid the need for emergency aea-
sures. A listing of some cosaoa vio-
lations of basic rules for handling
compressed gases is given in Table 1.
-------
COKP81SSO CASES (cent.)
Section No. A
Revision No.T
Date: 06/01/1?
Page 3 of 12
Table 1
Common OSHA violations
involving comprassod gas
L una«curod crttneon
I CrfcfldersatorodoitnowtpnMoctivocaM
X Noncompatibto gaaea (»wen as ftrdrogon end oaroon)
stored tog«iner
4. CrKndvrvatosoban who* cylinder tenet in USA (en ah
tacAcd roowiaior «KtA a tioa«d ditctonjo *e««o is net
1 Rr« citine visners «o« areaon! during voiding, burning.
or brazing operations
& NO sal try sno««f« and oyowasn tounsams oAoro
earre>i*o gaa«« are uMd
T. NO ga* masks anojor t««niiy to&w ed n«ef creaa vhoto tox
«aoo or atorod
Crllndera
Tba oupplior ooako to asoura tha aafacy
of cylindars through adhara&ca to roju-
latieaa aae forth by tho Dopartaaat of
Traasportatioa, and by oopplyias cy-
liadoro with spocifie ralvoa, Labola*
o&d/er oarkinga In oeeerdoaea with
recognised standards. It la mandatory
for tha ouppllar to ohip cylinders nanu-
factured In conforaance with DOT
rogulatlooa and to follow DOT ragulatioe
In tho testing and inspection of cyLinda
tho proper filling of these cylinders,
and tho uao of safety devices that are
approved by the Bureau of Explosives.
Figure 1 ahovo cylinder parts and im-
portant cylinder aarkiags. The cylinder
cap (1) protects the cylinder valve. Tb
valve handwhoel (2) Is uaed to open and
close tho cylinder valvo. Valves are
occasionally not equipped vith hand-
wheels, and require special vrencheo
to effect operation. The valve packing
sue (3).contains a packing gland and
packing around tho otoa. It Is adjust I
only occasionally and Is usually
tightened if leakage la observed around
valve stem. It should nee be tanpered
with when used In conjunction with
diaphrag»-typo valves. A safety device
(4) peralts gas to escape if the teaper-
aturo gets high enough to endanger tho
cylinder by increased unsafe pressures.
Tho valve outlet connection (5) connect!
to pressure and/or flow-regulating
equipment. Various types of connections
are provided to prevent interchange of
equlpaenc for iscoopatiblo gases,
usually identified by CCA (Coap?ess«d
Cas Association) nuaber: for esasple,
CCA So. 330 Is us«d for hydrogen, «er-
vieo. A cylinder cellar (6) holds the
cylinder cap at all tiaes, except vhea
regulating eeuiptsent Is attached to
cylinder v&lv@. Tha valve outlet csp
(7) protects valve threads fro*-
-------
COKP&TSSED CASES (coat)
Section No. A
Revision No.T
Date: 06/01/82"
4 of 12
and keeps the outioc clean; is to nee
used universally.
Specification nuabor (8) signifies chat
the cylinder conforao eo the Department
of Transportation specification POT-3A,
governing svaterlala of construction,
capacities, and tost procedures, ,an4
that tho service pressure for which tho
cyllndar la designed la 2265 psig at ?0°F.
The eylladac serial ttusbar io Indicated
by (9), and (10) Indicates tho dato
(aonth and year: la thio case, Juno
1975) of Initial hydrostatic tenting.
Thar oaf tar, hydrostatic pressure testa
are performed, on cylinders, for moat
gases, every .5 years to deteralne their
fitness for further use. At this time
nov test dates are stamped Into tho
shoulder of the cylinder. The original
inspector* a Insignia for conducting
hydrostatic and other required testa to
approve the cylinder under DOT specif 1-
caciona la shovn by (11) •
rilling
Nonliq.uefied gaaes say bo filled to tho
service pressure marked on a cylinder.
These markings will appear on tho
shoulder of the cylinder, i.e.,
MT3A-2000, indicating that the cylia-
der has been manufactured in accordance
with DOT specification 3A, and the
cylinder filling pressure la 2000 pal
at 70°?.
Since cospressed gaa cylinders aro
handled by a number of dlf ferene
types of plant personnel, it might
be veil to consider tho precautions
to be takan in b^M^Ttg f roa tho tiao
It is delivered until tho tiao it la
asp tied and ready for return.
Receipt and eontant Identification
When a cylinder la received, it
should have 1) content Identification
by stenciling or labela, 2) a DOT
label, and 3) a valvo-protoction
cap* Under-no circumstances ahould
tho moana of Identification bo reaovod
froa tho cylinder. The valve-protection
cap (Tlguro 1) should also regain in
plica until tha user has secured the
cylinder and is ready to withdraw.the
contents. DOT labels are required
for cylinders in interstate trans*
porcatioa. Some states require these
labela for intrastate shipments also.
These labels have a mini mm of pre-
cautionary handling inforaation and will
classify the cylinder contents as
flrmahlo, nouflasaablo, poison, or
corroaivo.
Unfortunately, there la aa yet no uai-
fomicy la tho identification of
cylinder contents, although a standard
for «L"*'1p<"S coapressed gases is avail*
ablo. Soae auppliera provide adequate
atenclling or labela with as such Infor-
mation on thea aa possible, warning
against possible hazards associated
with tho cylinder contents. On tho
other hand, cylinders say bo received
with no identification other than a
color code. Under no circumstances
should such cylinders be accepted.
Color codes are of value only la help-
ing the supplier to segregate large
nvsbors of cylinders into various
gas services.
Proper Stogsjto
After cylinders are received, ghsy
should be stored la a detached aad
well-ventilated or opensided building.
-------
COtCPttSSD CASES (coat)
Section No.
Revision No
Date: 06/01/82"
Page 5 of 12"
Storage buildings or arena should bo firo
resistant, veil ventilated, located away
from sources of ignition or excassivo heat,
and dry. Such areas should bo prominently
posted vith tho names of tho gases.being
seorod. Indoor atorage areas ohould not
bo located near boilers, otoaa or hoe
voter pipes, or any aoureen of ignition.
Outdoor storage araas should have tho
proper drainage and should bo protected
from the direct rays of tho sun in local-
ities where high teaperaeures prevail.
Subsurface storage areas should bo
avoided. Cylinders should bo protected
against tampering by unauthorized
personnel.
Cylinders should bo chained in place or
put in partitioned cells to prevent thea
from falling over. Where gases of diff-
erent types are stored at tho saao loca-
tion, cylinders should bo grouped by
types of gas and the groups arranged
to take into account tho gases contained—
for example, fla-aablo gases should not
bo stored near oxidizing gases. Stor-
age in a laboratory should bo confined
to only thooo cylinders in use. la all
cases, storage areas should comply vith
local, state, and municipal requirements
as vail as with tho standards of tbo
Compressed Gas Association and tho
Bational Fire. Protection Association.
Transportation
When cylinders are bains moved fros a
storage area into tbo laboratory, the
valve-protection cap should bo loft in
place. Tho cylinder should then bo trans-
ported by moans of a suitable hand truck.
Such a hand truck should bo provided
vith a chain or belt for aocuring tho
cylinder on tho truck. Do not lift
cylinders by tho cap. Avoid dragging
or sliding cylinders. Use hand trucks
even for short distances.
Securing Cylinder Prior To
Vhoa the cylinder has reached ita des-
tination in the laboratory, it should
bo secured to a vail, a bench, or son*
other fira support, or placed in a
cylinder stand. Onco tho cylinder ha;
boon secured, tho cap may bo removed,
exposing tha valve. Tho number of
cylinders 'in a laboratory should bo
liaitod, to ainlatte the firo and
toxicity bazardo.
Safety Relief Devices
Safety devices ere incorporated in
all DOT cot? r eased gas cylinders,
except thoso containing poison or
toxic gao, vhoro tho risk of exposure
to fuaea ia considered more hazardous
than that of a potential cylinder
failure.
Uhoro safety devices are required to
moot DOT regulations , they must bo
approved by the Bureau of Explosives.
Theso saf ocy devices are of four
basic typos:
1. Spring-leaded safety relief,
used mostly for lev-pressure, liquefi
flacaablo gasea.
2. Frangible disk, used mostly for
high-pressure cylinders.
3. Frangible disk backed up by a
fusiblo metal.
6. Fusible metal.
Tho spring-loaded safety relief typo
consists of a spring-loaded seat that
opens to relievo excessively high
pressures and then closes vhon tho
pressure returns to a safo value.
Tho frangible disk vill burst Jut
-------
COMPRESSES CXSCS (coat)
Section No. A
Revision No.~T
Date: gs/Ol/IT"
Page 6 of 12
considerably above the oarrico pressure
but not balov or at the hydrostatic coat
pressure of a cylinder, and will release
tho entire cylinder coat onto. Tho
frangible disk backed op by a fuatblo .
ootal will fuactioa only If tho tempera-
ture la high enough to malt tho fusible
aatali afear which excessive pceaourao
«U1 burst tha disk, resulting la
release of tha aatlro eoataato of tho
eylladar. Tha fusible ratal devices
ealt at axeaaalvo temperatures (approx-
imately 160-212°F), allowing tho oatlra
contents of tho cyliadar to escape.
Any of theao devices will prevent a
eylladar from bursting duo to exeessive-
ly high tasperaturea. Bowovar, tho
latter .two devices may not prevent a
cylinder from bursting la eaaaa whara
aa overfilled cyliadar la exposed to
a temperature that la excessive but not
high enough to malt tho fuaibla metal
aafocy.devices. Since tho proper func-
tioning of cylinder safety devices depeada
to a largo extant on tho proper f11ling
of a cyliadar, such filling should
aev«z bo attenpted by tho user, unless
express permission hao beea obtained
from the gas supplier. Safety devices
may also fall to function properly if am
intense flaae irpinging oa the side vail
of a cylinder weakens tha metal to tho
point of failure before heat or pressure
can cause the safety device to function
properly. Tlnally, it must bo empha-
sized that taspering with cylinder
safety devices la extremely hazardous.
Knowing Tho Caa To Be Handled
It is of the ucaaat isportanco that tha
uaer bo vail avaro of thoso properties
of a compressed gaa that represent
Hazards (such aa flasoability, toxicity,
choaical activity, and corrosive
effects). Every attespt should bo
made to learn these various properties
before tho gaa is put to use./ It la
sooetiaefl difficult to determine tho
major hazard of aay one gas, siaco this
factor la influenced a great deal by
how tha gaa la used. In a laboratory
la tho presence of aa opaa flame, tho
f lasaabillty of carbon monoxide might
wall bo tho major hazard, whereas in a
pilot-plant run using carboa monoxide
aa a roactaat, leakage, and therefore
toxicity, may represent tho major hazard
Figure 2 shown tho flaemability ranges
of various gases. Although the flaa-
mability ranges of the liquefied petro-
leum gases such aa butan* and propane
are relatively short, only very small
concentrations are necessary to ereato
flasaable mixtures. Tha flaaaability
ranges of acetylene, carbon monoxide,
othylene.oxide, hydrogen sulfide, and
hydrogen are extremely long. Indict-
ing that they can fora explosive
mixtures with air under a wide variety
of conditions.
l«WlT« O*
OUTAMtt
ttOOVTAMft
OUTlNtt
CAAOOM MOMOUOC
.MTOBOOCN
MTQMOCtM SXA^IBt
0 •« >• SO •• M *• »«
CAS % IW *«
H
Figure 2
-------
COKPKESSED CASES (cont)
Section No. A
Revision No. 1
Date: 06/01/8F
Page 7 of 1?"
It la important to knev what materials of
construction muat bo unad with a gas to
provoat failure of oquipmoat duo to corro-
aion, or to avoid poaaibla formation of
hazardous eoapousda (ouch ao acetylidas
formed by the reaction ef coppor with
acetylene or gases containing acetylene .
ta aa ispurity) or tho possible formation
ef fulminates when mercury la used la tho
presence of rrmrmia.. •'
'«[
Tho hararda of toxic, flairniMo, and
corrosive gaseo can bo minimized by
working la vull-ventilated areaa. Vhoro
possible, work should bo dona la a hoed,
employing cyllador siiaa that will asauro
uso of *\\ the gaa vlthla a raaooaablo
aaouat of tiao. Loako ahouLd not bo
ailovad to so oaehoekad. Advtao tho
attpplisr iasodlately of eyllador leako
that cnnnot bo atoppod by slaplo adjuat-
moat, auca aa tightoning a packlag aot.
f
•rooar Plachxrco of Cylinder Contenca
.or controllad reaoval of tho liquid phaao
of a liquofiod gaa, a mnttiial control la
uaod. Spatial liquid flow regulators
aro alao availablo. It Boat bo rtusoaborod
that withdrawal of liquid Bust aocasaarily
bo carriod out at tho vapor pressure* of
tho oatarlal. Aay attoapt to redueo tho
pruoura will result la flaahiaj ef all
or part of tbo liquid to tho gaa phaao.
Safaty rcliaf davicta should bo iaatallod
la all liquid-transfor liaoa to rollavo
auddcn, dangerous hydrostatlc-or vapor*
prvasuro buildnpo.
Tor noaliquofiad gasoa, tho aoae eooaoa
dovico used to roduco prasauzo Co a
aafo valuo for gaa rnaoval la a prosauro
ragulator. It consists of a spring-
(or gas*) loaded diaphragm that controlo
tho throttling of aa orfico. Delivery
pros aura will exactly balance tho dollvdry
pressure spring to give a relatively
constant delivery pressure.
Pressure Regulator Handling and Use
A regulator ahould be attached to a
cylinder without forcing the threada.
If tho inlet of a regulator doaa not
fit tho cylinder outlet, no effort
ahould bo made ta try to ferco
fitting. A poor fit aay indicate
that the regulator la mot intended
for uso oa tho gao choaon.
Tho following procedure ahould bo used
to obtain tho required delivery
presauro:
1. After the regulator has boon
attached to tho cylinder valvo outlet,
tarn tho delivery pressure-adjusting
acrow countorclockviao until it turna
freely.
2. Opea tho cylinder valve slowly
until tho tank gauge on tho regulator
ragiataro-tho cylinder pressure. At
thia point, tho cylinder pressuro
ahould be checked ta oeo if it la at
tho expected value. A largo error may
indicato that tho cylinder valvo la --\
3. With tho flow-control valvo at
tho regulator outlet closed, turn the
delivery pressure-adjusting acrev
clockviao until the required delivery
preasuro la reached. Control of flow
g^n be regulated by Banna of a valvo
supplied la the regulator outlet or bj
a ffuppleaentary valve put la a pipelii
downstream from the' regulator. The
regulator itself should not bo used
aa a flev control by adjusting tho
presauro to obtain different flev
ratea. Thia defeato tho purpose of
tho preasuro regulator, and la soso
caaaa whore higher flovo are obtaiaei
la thia manner, tho presauro sotting
may bo in exceso of the:dosign proa-
sura of tho STStaa.
-------
COKPS£SSn> CASES (coot)
Section No. A
JRev1s1on No.~T
Date: 06/01/oT"
Page 8 of 12
Types ef Pressure Regulators
Tbo proper choice of a regulator depends
on the delivery-pressure rao4o required,
tho. degree ef accuracy of dollvery proa-
ouro to bo maintained, and tho flow rato
-required. There ore two basic typoo of
pressure regulators, single-stage oaH
double, or tvo-stago. The single-
stage typo vill ahov a alight variation
la delivery pressure as tho cylinder
pressure dropa. It vill alao show a
greater drop in dftlivory pressure than
a two-stage regulator aa the flow rata
lo increased, la addition, it vill ahov
a higher "lock-up" pressure (pressure
increase above the delivery oet-point
necessary to atop flow) than tho eve*
stage regulator. In general, the tvo-
atage regulator vill deliver a eoro
nearly constant pressure under BOTO atria-
gent operating conditions than vill the
aingle-atage regulator.
Peterainatieo ef Cylinder Content
*
Aa the content of a cylinder of non-
liquefied gas ia" discharged, the cylinder
proaaura decreases by an asount propor-
tional to the aaount vithdravn. Tho
cylinder should be considered eapty
while poaitivo pressure (25 paig or
greater) atill roaains, in order to
prevent auck-back and contamination.
failure to close tho valvo on aa
eapty cylinder vill allow air and naia-
turo to bo dravn into tho cylinder aa
it "breathes" during teaperature
changes; an exploaive mixture may
build up if the gas is fli-nablo; and
an oxtreaely corrosive condition vill
be created in cylinders that contain
chlorine, hydrogen chloride, or other
acid-forming or corrosive, gases.
Aa the vapor phase of a liquefied gaa
is vithdravn from a cylinder, tho cyl-
inder preaauro or vapor pressure vill
reaain constant as long as any liquid
is present. This condition holds true
if tho teaperaturo does not vary. I£,
however, the material ia vithdravn
froo the cylinder at a rapid rate, the
material itself vill supply tho heat
for vaporization, end upon subsequent
cooling, the vapor proaouro vill bo
lowered. It io, therefore, iapeaaible
to determine the content of a cylinder
containing a liquefied gas, except by
weighing. Cylinders containing
liquefied gases are staaped or tagged
vith tho tare weight in order to allow
tho content to be determined.
An indication of cylinder-content
depletion for oomo high preaauro
liquefied gases ouch as carbon dioxide
ethane, and nitrous oxide can bo ob-
tained by noting the cylinder preasurt
After depletion of the liquid phaoo, '
the cylinder pressure will decrease
below the normal vapor pressure. A
cylinder containing carbon dioxide vU
have approximately 201 of ito original
content remainingafter depletion of
tho liquid phase. Aa vith cyLlndero
of nonliqnefied gases, cylinders
containing liquefied gases should
never bo completely eaptied, in order
to prevent truck-back and contaainatiot
of tho cylinder.
Handling tapty Cylinders
Whero cylinders are considered esaty,
the valves should bo closed. Valve-
protection capa, outlet dust caps, an
other accessories shipped vith the
cylinder should be attached to the
cylinder as received. Tho cylinder
should be marked or labeled "empty."
Cylinders should then bo placed in a
proper storage area, segregated fron
full cylinders, to await pickup for
return to the aupplior. :'
i
Careleaaneao in the h«**i<;«ig of an
eapty cylinder could result in ito
being mistaken for a full cylinder.
Tha connecting of an eapsy cylinder t
-------
COXPttSSO CASES (coat)
Section No.
Revision No."
Date: 06/01/IT"
Page 9 of ^12
a high-prosauro ayatea could eauoo foreign
maceriala to back up lace tbo cylinder,
rooultino la oil tha attendant hazarda of
ouek-back, and tbo pooalblo violent reaction
within the cylinder.
La ak Potaction
Chock cylinders and all eonnoctiona uador
proaaura for leaks prior to uaing cho
contents. Whoa using toxic gasea, it in
adrisablo that aoaa dovico or indicator
ba uood to warn of tha presence of toxic
coneantrations. For example, otrlpa of
lead acetate paper can bo hung in an
aroa vharo hydrogen aulfido ia being
uaod. Although tola gaa haa a disagreeable
Oodor, it ooon deadena tho aonso of small,
rendering tho uaar incapable of detecting
increasing dangarbua concentrations by
odor.
Cyliadara that develop looks ahould bo
treated aa follova: Cylinder valve—
packing leaks of acidic gasea, ouch an
chlorine, hydrogen chloride, hydrogen
aulfido, and aulfur dioxide, can uaually
bo corractod by tightening tha valvo
packing nut (turn clockviso aa vievod
froa abovo). If Talvo laaka poralat or if
loaki appoar at any portion of tho
cylinder, adyiae the aupplior isaodiatoly.
E*move tha cylinder to a hood or location
where the leakage cannot eautto daaago
until tho coneonta can aafety bo dia-
peaod of by vonting or abaorption in wntor
or caustic oolution or until information
on other maana of dispooal aa rococanoded
by the supplier ia obtained. Cylinder
valve-packing leaka of basic gaaoo
(asaonia and xainea) can bo atopped by
tightening tho packing out (turn counter*
clockviao aa viewod fron above). Laako
of those basic gasea through tha vulva
outlet that cannot bo controlled by
turning the handwhaol to tho clooed
position ahould be stopped by plugging
the outlet with 3/8-in pipe plugs. 12
laaka persist, roaavo the cylinder to a
•hood and ask cho auppliar for inform-
ation en bow to resedy tha problea.
On raro occaaiona, oaargoacy action
aay bo aocoasary ia order to aove a
leaking cylinder, to a location where
it can vent oafely, or it oay have to
bo rcsoved f roo a building and brought
eutdoora. tn ouch inatancaa, aa
eaorgency plan should bo put into
offoct:
1. Properly warn all personnel
required to evacuate a building or
aection of a building*
2. Shut off electrical power to
prevent ignition of a leaking flaa-
mablo
3. Dotaraine the abort eat route so
the point of gaa dlapoaal.
A. Obtain satisfactory conveyance,
ouch an a hand truck, to novo tha
cylinder aviftly.
5. Peat the area whora the cylinder
ia venting to prevent taaparing by
unauthorised personnel.
Such an oaargency plan can function
efficiently only if a trained safety
crew ia educated in the proper hand-
ling of gaa cylinders, with training
ia tho procedures to bo followed in
caaea of osargancy with all tho g*saa
handled by tho facility. £a.uipaent
ouch aa self-contained gaa masks
must bo available for *^**"<11ng toxic
gasea or for handling asphyxiating
gaaoa in cloao confinati. Esarganciei
involving fln-nnbla gasea aunt bo
managed with tho ucaoat care in order
to prevent ignition. The afteraath
ef sroaa leakage ia axtreaely iaport
AH *ra*a aoat bo adaquately vented
before the restoration of pover ia
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CASK (cant)
Section No. A
Revision No. 1
Date: 06/01/3F
Page 10 of 12
coses of flasmable-gas leakage. Areas
contaainated by corrosive gases oust bo
adequately vented and completely washed
down-to prevent subsequent degradation
of delicate instruments, electrical
contacts, ace.
Handling of Corrosive Cases
Corrosive gases should bo scored for tho
shortest possible periods before use,
preferably less then throe months.
Storage areas should bo as dry as possible.
A good supply of water should bo available
to handle oaergency leaks. Moot corro-
sive gases «r«a bo absorbed ia water.
Corrosive gases should not bo stored ia
areas containing instruments or other
devices sensitive to corrosion. Those
gases should be segregated as CO typo,
and rotated so that tho oldest stock is
used first. The saalleat cylinders
possible should be used to ensure rea-
sonable turnover of cylinders. Cylinders
used and then> put back in storage should
have all appurtenances reaoved froa tho
valve outlet and should preferably bo
flushed with dry nitrogen or air to
keep thea ia good working order.
Uhen corrosive gases are being used, Che
cylinder valve stem should bo worked
frequently Co prevenc "freezing." The
valve should bo closed when tho cylinder
is not in use. Regulators and valves
should be closed when the cylinder is
not in use and flushed with dry air or
nitrogen after use. Such control
devices should not bo left on a cylinder,
except when it is in 'frequent use.
Vhan corrosive gases are to bo dis-
charged into a liquid, a trap, check
valve, or vacuum break device should
always be employed to prevenc danger-
ous suck-back.
Occasionally a valve otea does boeoao
frosen and cannot be turned. Thin
condition aay bo corrected by first
plugging the cylinder valve outlet
with a solid plug, gaskatod cap, or a
closed needle valve, loosening the
volvo packing nut, t id than trying
eo cum the valv_o stun nanunlly with
a corroccly fitted wrench (no longer
than 8 inches), or by slightly tapping
cho wrench with a light cool. Once
the scea is turning freely, shuc the
valve, tighten the packing nut, and
safety vent the gas crapped in tho
valve pore. This operation should be
dona ia a hood or out of doors. If
tha cylinder valve cannot bo unfrozen
by ehis procedure, ask the supplier foi
indorsation or return cho cylinder.
General precautions for handling,
storing, and using compress>td gases
is presented separately ia Attachaenc
One. You may post it ia your work
area as a daily reaindar.
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PZECXDTIONS Dt BAMfiUSC
OF COiffSlSSED CASZS ZH IBS
LABOKAIOBX (coat)
Section No. A
Revision No.~T
Date: 06/01/52"
Page ll~oT IF
use when working vith toxic
gases. Those masks obould bo placed
la convenient locations ia areas net
likely to become contaminated, and
obould bo approved by tho U.S. Bureau
of Mines for, tho oorrlco intendod.
Those involved.in the handling of
compressed gases should bocomo
familiar with the proper application
aad Uaitatioaa of the various typoa
of aaalta aad raspiration aido avail-
oblo.
13. Vhoa. raturciag cylinders, clooo
tho valve before abipaene, loaviag
oome poaitive prasouro in tbo cy-
liader. K«place any valve outlot
and protective capo originally
shipped vi'th tao cyliader. Mark
or label the cyliader "ompty"
(or utilize 'standard DOT "eapty"
labels) aad store in a designated
area for return to tho supplier.
16. Before uuiag cyliadora, read
all label information and data
sheets associated vith the gas
being used. Observe all applicable
safety practices.
17. Eye baths, safety shavers,
gas auks, respirators, and/or
rususcitators should be located
nearby but out of tho iracdiato
aroa that is likaly to bocoso
coataainatod in the ev«nc of a
largo release of gao.
IS. Fire oxtinguishera, prefer-
ably of tho dry choaical typo,
should be kept clooo at brrad and
should be chocked periodically
to assure eh«is proper operation.
Tho user of conpressod gases should
become faailiar with tho first-aid
cathodo to bo employed in cases of
ovorezpoouro or bvmo caused by a
Sao. A plant doctor obould bo
familiar vith whatever further creat-
aaato may bo necessary. Unnecessary
delay ia the treataent of a patieat
overcome by a toxic gas or burned
by a corrosive gas could cause tho
patieat peraaaeat daaage aad night
oven result ia death. Authorized
personnel should odainister first aid;
hovovor, they should not take it upoe
themselves to adsinister medical
treatments. A physician should bo
contacted immediately.
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gyr ONE
CCfTBAL PRECAUTIONS IS BA2DLZKC
Of COXPSESSO CASES DC THE
UkBOSAXORt
Section No. A
Revision No. __!__
Date: 06/01/82
Page 12 of 12
Scmo general precautions for haadliag,
storing, aad using cospreaaod gasaa
follow.
1. B«vor drop cylinders or paralc thes
eo strike oasa other violently.
2. Cylinders aay bo stored la tbo opaa.
but should bo procoecad from eha ground
beneath to prevent rusting. Cylinders
My bo stored la eha nun, except la
localities vharo extreaa tasparaeuraa
prevail; la tha auto of curtain gaaeo,
eha supplier'a rocesaeadatiba for
shading should bo obaerved. If lea or
snov accusulates on a cyllndar, chav
ac rooa cesperacura or with vaear at a
te^aratuxa not axcaedlag 125°f.
3. Tha valve-protoctioa cap ahould bo
loft on oach cylinder until le haa beaa
securod agnfnte a vail or boneh, or
placed la a cylinder otaad, and la
raady to bo used.
4. Avoid dragging, rolling, or oilding
cylinders, oven for a short distance.
They should be novod by using a suitable
hand track.
S. Kevar tsspar vith safety devlcos la
valves or cylinders.
6. Do not store full and oapty cylinders
together* Serious suck-back can occur
when aa espty cylinder la attached to
a prassurixed oyotc
7. So part of a cylinder ahould bo sub-
jected to a tosperaturo higher tbaa 122°?.
A flasa should never bo permitted to coma
la contact vita any part of a cosprassod
gao cylinder.
8. Cylinders should act be subjected
to artificially created lev teapera-
turoo (-20 T or lover), olaco aaay
typos of otaol vlll lose their
ductility aad ispact strength at low
tosporatureo. Special atainlais steel
eyliodara'arft available for lev tea-
peraturo uao.
9. Do not place cylinders vhere they
aay bacoao part of aa electric circuit
When electric are-veldiag, precautions
oust bo taken to prevent striking aa
arc ogainst a cyliadar.
10.. Bead aad ground Ml cylinders,
lines, aad oquipaeat used vlth
flasaabla coepressad gases.
11. Uso coopresaed gases only la voll-
voatilated area. Toxic, flaasabla, ygd
corrosive gases should bo handled la
a hood. Only snail cylinders of toxic
gooes ahould bo used.
12. Cylinders should bo used la rotatit
as received froa the supplier. Storage
areas should bo see up to perslt invont-
cry rotaeloa.
13. Vhea discharging gas into a liquid
a trap or suitable check valve should b<
used to prevent liquid froa getting
back into the cylinder or regulator.
14. Vhea using compressed gases, vear
appropriate protective equipment, such
as mfaE? fogglss or face shield,
rubber gloves, aad safety shoes, tfall-
veasUUtsd barricades should bo us ad la
excreaaly hazardous operations, such
aa ia the handling of fluorine. Cad
easka ^'-Uti b« kept available for
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Section No. 8
Revision No."~T
Date: 06/01/5F
Page 1 of 2
APPENDIX B
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