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993-9453 ;:"' 3 If, ()0

INSTRUCTIONS
MODEL 560
ATOMIC ABSORPTION SPECTROPHOTOMETER

Rev. April 1979

PERKIN-ELMER
Perkin~Elmer is a trademark of the Perkin~Elmer Corporation
NORWALK, CONNECTICUT, U.S.A.
Copyright 1982 - The Perkin-Elmer Corporation
All Rights Reserved
Printed in U. S. A.
TABLE OF CONTENTS

Section

1 INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1-1

2 INSTALLATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-1
A Eq u i pm en t . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 -1
1. Equipment Provided ...................... 2-1
2. Equipment Required But Not Supplied ........... 2-4
B. Installation Procedures ..................... 2-4
1. Removal of Wavelength Locking Device ....... 2-4
2. Burner-Nebulizer Installation ........ 2-6
3. Drain Trap Installation .................... 2-7
4. Burner Regulator Installation ............ 2-8
5. Lamp Installation ..................... 2-16
6. Sample Support Tray ....................... 2-17
7. Lamp and Burner Alignment ................. 2-17
8. Burner Compartment Door Removal, Replacement .. 2-17
9. Nitrous Oxide Supply and Accessories ....... 2-17
10. Rear Instrument Terminal Board ........... 2-19
11. Connecting a Heated Graphite Furnace ........ 2-20
12. Connecting the Model 560 to Line Power ...... 2-21
3 SPECIAL LABORATORY REQUIREMENTS ..................... 3-1

4 PRINCIPLES OF OPERATION ..................... 4-1

5 PERFORMANCE CHARACTERISTICS ..................... 5-1

6 SPECIFICATIONS ........................... 6-1

7 CONTROLS AND INDICATORS ......................... 7-1


A. Instrument Controls and Indicators ................ 7-1
1. Lower Right Front Panel ................. 7-1
2. Upper Right Front Panel (Display and
Keyboard) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
3. Upper Left Front Panel ...................... 7-8
4. Lower Left Front Panel ..................... 7-9
B. Digital Burner Control System ................... 7-10
C. Flowmeter-Type Burner Regulator Controls and
Indicators .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7-14

8 OPERATING INSTRUCITONS ....................... 8-1


A. Sample Analysis ....................... 8-1
B. Burner Regulator Operation ....... ~ .......... 8-2
1. Operation of the Digital Burner Control
System . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8- 2
2. Operation of the Flowmeter Gas Control System.8-7
3. Adjusting the Flame .......................... 8-12

4/79
TABLE OF CONTENTS (Cont.)

Section Page

C. Preliminary Instrument Procedures ................. 8-13


1. Analytical Methods Manual. .................... 8-13
2. Burner Head Installation .................... 8-13
3. Organic Solvents ............................. 8-13
4. Corrosive Solutions .............................. 8-14
5. Lamp Installation and Alignment ................. 8-14
6. Control Settings ......................... 8-15
7. Burner Alignment .............................. 8-16
8. Nebulizer Adjustment ......................... 8-17
9. Warm-Up . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-17
D. Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-18
1. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-18 1

2. Selecting the Number of Standards ............. 8-18


3. Selecting the Concentrations of Standards ..... 8-19
4. Calibration Procedure For Flame Analyses ........ 8-20
5. Calibration For Fast Peak Measurements ....... 8-22
6. Res lope . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-2 2
7. Expansion .. ., . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-23
8. Errors That May Occur During Calibration ....... 8-25
9. Averaging and Statistical Operations ........... 8-27
E. Special Determinations ........................ 8-29
1. Operating the Optional o Arc Background
2
Corrector o ............................. 8-29
2. Reading Fast, Peak Shaped Signals with a Heated
Graphite Furnace ...................... 8-31
3. Flame Emission Measurement ................... 8-32
4. Measurement of the Emission Spectra of a Lamp
Source . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-35
F. Additional Readout Devices .................... 8-35
1. Strip Chart Recorder ....................... 8-35
2. Printer-Sequencer ........................... 8-37
3. Model TR-2 Teletypewriter Readout, Communications
Interface . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-41
9 HAZARDS . . . . . .. 9 -1

10 MAINTENANCE INFORMATION ............................ 10-1


A. Obtaining Service ............................... 10-1
B. Maintaining the Burner ......................... 10-1
1. Burner Cleaning Schedule .................... 10-1
2. Cleaning the Burner Head Slot ................ 10-1
3. Cleaning the Burner After Use of Organic Samples.10-3
4. Cleaning the Burner After Use of High
Concentrations of Silver, Copper, or Mercury
Samples in an Acetylene Flame ............... 10-3
5. Cleaning the Burner Mixing Chamber ............. 10-3
C. Maintaining the Nebulizer ................... 10-4
1. Cleaning the Nebulizer and Sample Capillaries ... 10-4
2. Changing the Nebulizer ................... 10-5
3. Disassembly of the Nebulizer for Cleaning ...... 10-5
4/79
TABLE OF CONTENTS (Cont.)

Section

D. Care of Optics . . . . . . . . . . . . . . . . . . ,, . . . . . . . . . . . . . . . . . . . . 10-7


E. Opening the Electronics Compartment ............ 10-7
F. Opening the Photometer Compartment ............. 10-7
G. Replacing and Aligning the D Arc .............. 10-8
2
1. Lamp Replacementtl.,. e o 10-8
2. Aligning the D2 Lamp ................... 10-9
H. Replacement Parts List .................... 10-11

11 TROUBLE SHOOTING .......................... 11-1


A. Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-1
B. Hollow Cathode Lamp .................. 11-1
1. Lamp will not fit properly in the lamp mounting
bracket . . . . . . . . . . . . . . . . . . . . o e 11-1
2. Lamp connector will not fit the connection on the
instrument ......................... 11-1
3. Lamp will not light ...................... 11-1
4. Lamp current cannot be set to the desired
operating value 0 e 11-2

C. Display Does Not Respond ....................... 11-2


1. Display is completely lit and all indicator dots
are 1 it ... e e 0 11:- 2
2. Display is blank but warning lights are all on .. 11-2
3. The reading on the display will not change ..... 11-2
D. Calibration ....... o l l - 3
1. Calibration curves do not pass through zero ... 11-3
E. Indicator Dots On ....................... 11~3
1. OVER CAL dot on ... 0 11-3
2. KEYBOARD dot is lit ..................... 11-3,
3. The BKDG CORR dot is on ................ 11-3
4. BKGD CORR dot is blinking ................. 11-3
F. Results Questionable .......................... . 11-3
1. Results erroneously high ......... ~ ...... 11-3
2. Results erroneously low ............... 11-4
3. Cannot get suggested detection limits ....... 11-4
4. Cannot get close to the suggested sensitivity 11-4
G Re s u 1 ts No i s y ....... 11- 5
1. Display noisy with flame off ....... 11-5
2. Digital display is quiet with the flame off, but
noisy with the flame on or with the flame on and
solution aspirating ..................... 11-5
H Re s u 1 ts Dr i ft . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-7
1. Baseline drifts with flame on ........... 11-7
2. Readings drift or are not reproducible .... 11-7
I. Background Correction ...... 11-8
1. The BKDG CORR indicator dot above the digital
display front panel is blinking .......... 11-8
2. The D2 arc has less energy than the primary
source ... ......................... e 11-8
3. The Background Corrector does not provide
adequate correction .................... 11-8
TABLE OF CONTENTS (Cont.)

Section Page

4. The analytical results with background correction


are excessively noisy .................... 11-9
5. Sensitivity is lower in the AA-BG mode than in
AA mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-9
J. Flame Ignition and Gas Control ................. 11-9
1. If the gases do not ignite ................ 11-9
2. If the burner-nebulizer system flashes back .... 11-10

12 ERROR MESSAGES ..... 12-1

WARRANTY INFORMATION

13 Standard Absorption Conditions for Selected Elements 13


LIST OF ILLUSTRATIONS

Figure Page

2-1 Dimensional Diagram for the Model 560 with (A)


Digital-Type Burner Controls and (B) Flowmeter-
Type Burner Controls ........ ~2-3
2-2 Burner Compartment Installation ................. 2-5
2-3 Location of Spectrophotometer Leveling Screws .... 2-6
2-4 Connecting the Burner Head Safety Interlock
System . .. 0 0 0 0 G 0 'l 0 0 2-6
Q 0 0 0 0 0 e e 0 " 0 G c 0 0 0

2-5 Installation of the Interlock Drain Trap ........ 2-8


2-6 Drain Interlock Connector . . . . . . . . . . . . . . . . . . . . . . . . 2-8
2-7 Parts of the Connectors Used Between the Burner
Regulator and the Burner Nebulizer . . . . . . . . . . . . . . . 2-11
2-8A Installation Diagram for the Digital-Type Burner
Control System for the Model 560 ................ 2-12
2-8B Installation Diagram, Flowmeter-Type Gas Control
System for the Model 560 . . . . . . . . . . . . . . . . . . . . . . . . 2-13
2-9A Plumbing Schematic for the Model 560 Digital-Type
Burner Control System, Assembly Nos. 060-0206
through 060-0210 0 Cl 9 0 0 0 2~14
0 e G 0 8 0 & 0 II 0 0 G & 0 D 0 0 0 0 0 0 0 0 0 0 0 9

2-9B Plumbing Schematic for the Model 560 Flowmeter-


Type Control System, Assembly Nos. 060-0196
through 060-0200 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2-15
2-10 Electrical Connections between the Instrument and
the Flowmeter-Type Control System ..... , . . . . . . . . . . 2-16
2-11 Rear Instrument Terminal Board . . . . . . . . . . . . . . . . . . . 2-19
4-1 Model 560 Optical Schematic . . . . . . . . . . . . . . . . . . . . . . . 4-1
7-1 Right Front Control Panel . . . . . . . . . . . . . . . . . . . . . . . . . 7-1
7-2 Left Front Control Panel . . . . . . . . . . . . . . . . . . . . . . . . . 7-9
7-3 Burner Control Unit Controls . . . . . . . . . . . . . . . . . . . . . . 7-10
7-4 Flowmeter-Type Gas Controls . . . . . . . . . . . . . . . . . . . . . . 7-15
8-1 Relationship between Actual Flow Rates and Dis-
played Va 1 ue s. 0 II CJ Ii 0 0 IJ 8-3
0 0 0 0 0 0 0 a 0 0 e 0 0 0 0 0 fl

8-2 Flow Rates from Flowmeter Settings (Flowmeter-Type


Burner Control) .. ob"
o.,. e. 8-9 o o e o o

8-3 Lamp Compartment o . . . . . . . 0 o o o o o o o o 8 -14


8-4 Burner Compartment. o o o e". o e o o o. o. 8-16
8-5A One Standard - Linear Plot . . . . . . . . . . . . . . . . . . . . . . . 8-18
8-5B Three Standards - S-Shaped Plot (Calibration
Error) .. _.. o e o o fJ 1:1 o 8-18
8-6 Calibration Curve Using a Single Standard ....... 8-21
8-7 Calibration Curve Using Two Standards ......... 8-21
8-8 Calibration Curve Using Three Standards .......... 8-22
8-9 Resloping Example ............................ 8-22
8-10 Model PRS-10 Pr inter-Sequencer . . . . . . . . . . . . . . . . . . . . 8-37
8-11 Printout Showing Various Codes . . . . . . . . . . . . . . . . . . . 8-37
8-12 PRS-10 Printout Showing Averaging and Calibration.8-39
8-13 PRS-10 Uncovered . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8-40
8-14 Sequential Printout of Results Obtained with Model
TR-2 o o o'-~o o o o o 0 o " o o o o o o 8 -41
o e o o o a o o o o e o o o o e a o e o o o o o u o

8-15 Operator-Selected Data Format and Printout from


Program Tape Used to Generate Format ......... 8-41

4/79
LIST OF ILLUSTRATIONS (Cont.)

Figure

10-1 Burner Assembly 040-0146 . . . . . . . . . . . . . . . . . . . . . . 10-2


10-2 Nebulizer - Exploded View . . . . . . . . . . . . . . . . . . . . . 10-6
10-3 D2 Arc Lamp Cover . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10- 8
10-4 D2 Arc Lamp and Lens . . . . . . . . . . . . . . . . . . . . . . . . . . 10-10
10-5 Adjust Knobs . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-10
10-6A Model 560 Electrical Interconnection Diagram
(Sheet 1) 057-9140R . . . . . . . . . . . . . . . . . . . . . . . . . . 10-13
10-6B Model 560 Electrical Interconnection Diagram
(Sheet 2) 057-9140R . . . . . . . . . . . . . . . . . . . . . . . . . . 10-15
10-7 Electrical Schematic, Analog Circuit 560
0.5 . .7-9270E . . . . . . . . . . . . . . . . . . . . . " . . . . . . . . . . . . . . 10-17
10~8 Electrical Schematic, Background Corrector
Circuit (J9) 057-0331E . . . . . . . . . . . . . . . . . . . . . . . 10-19
10-9 Electrical Schematic, Recorder Interface
Circuit (JS) 057-0319D . . . . . . . . . . . . . . . . . . . . . . . 10-21
10-10 Electrical Schematic, A/D Converter Circuit
(J7) 057-0322E . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-22
10-11 Electrical Schematic, Processor Circuit (J6)
057-9170E . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-23
10-12 Electrical Schematic, ROM Circuit (JS)
057-9160C . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-24
10-13 Electrical Schematic, I/O Circuit (J4)
057-9180E . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-25
10-14 Electrical Schematic, TTY Interface Circuit
(J3) 057-0321E . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-26
10-15 Electrical Schematic, Printer Interface
Circuit 057-0320E . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-27
10-16 Electrical Schematic, +5 V, +15 V Unregulated
Power Supply (Jl) 057-0327D . . . . . . . . . . . . . . . . . . 10-28
10-17 Electrical Schematic, Control 057-0334D ....... 10-29
10-18 Electrical Schematic, Standard Gas Control
System 0 5 7- 0 4 0 0 E . . . . . . . . . . . . . . . . . . . . . . . . . . . . . l 0 - 31
10-19 Electrical Schematic, Keyboard Display
057-9130E ..... ., . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10-33
10-20 BC-3, Interconnection Diagram, 047-04020 ...... 10-35
10-21 BC-3, Power Supply Schematic, 047-94BOD ...... 10-36
10-22 BC-3, Interlock Display, 047-9630C ......... 10-37
10-23 BC-3, MPU Logic 047-9620E ................... 10-38

4/79
1 INTRODUCTION
The Perkin-Elmer Model 560 is an atomic absorption spectropho-
tometer which measures the concentration of metallic elements
in a variety of matrices. It provides integrated readings in
absorbance, concentration or emission intensity. The readings
are integrated over a period selected by the operator from 0.2
to 60 seconds. When used with flameless sampling devices, the
Model 560 can also measure peak height or integrated peak area.
Special keys are provided for calibration using up three stan-
dards and a blank. In addition, controls are included to fa-
cilitate automatic averaging and statistical treatment of re-
sults.
Using optional accessories, the readings can also be presented
on a laboratory recorder, printed on paper tape along with sample
identification by the PRS-10 Printer-Sequencer, or typed in re-
port form using the TR-2 Teletypewriter Readout. Part of the
TR-2 assembly provides an output compatible with EIA specifica-
tion RS-232C, which makes interfacing with computers or other
data logging devices possible.
The Model 560 is available in the assembly versions shown in
Table 1-1 below:
TABLE 1-1 - THE MODEL 560 ASSEMBLIES AVAILABLE

F lowme te r Type o 2 a~d Burner Drain


~
Model 560 Features Digital Type
Assembly Burner Controls Burner Controls ~ Dr 1 ve Inter lock Interlock

llOV, 60 Hz llOV, 50 Hz 220V, 50 Hz

$ @ Ell
060-0206 060-0206 060-0207

060-0208 060-0209 060-0210 @ Ill Cl

060-0197
"" <ID <ID Acey
060-0196 060-0196
--+--
@ Acey
060-0198 060-0199 060-0200
""

The Model 560 is listed with the U.S. Food and Drug Administra-
tion as an IVD instrument. This manual contafns--~fnfoiinaEion
required- by :Fi5.A for -such instruments.
This manual describes the procedures the operator of the Model
560 needs to run the instrument. Sections 2 and 3 provide in-
stallation procedures (although the instrument is usually in-
stalled by a Perkin-Elmer Service Representative) and information
on material and equipment needed to set up an atomic absorption
instrument in the laboratory. Information on principles of
operation, performance characteristics and specifications for
the Model 560 is provided in Sections 4, 5, and 6. Operation
and calibration instructions are given in Sections 7 and 8.
Servicing and maintaining the instrument and trouble shooting
advice are discussed in Sections 10 and 11. Error messages
are explained in Section 12.
4/79
1-2

The following publications are used in conjunction with this


manual and, with the two exceptions noted, are provided with
the instrument or can be obtained free of charge from Perkin-
Elmer.

1. "Preparing Your Laboratory for Perkin-Elmer Atomic Absorption


Spectrophotometers" (Brochure L-301). This brochure is in-
cluded in this manual (Section 3) .

2. "Atomic Absorption Spectroscopy" by w. Slavin, Wiley and


Sons, 1968. This book is available from Perkin-Elmer. Order
part no. 990-9628.

3. "Atomic Absorption Spectroscopy" by B. Welz, Ver lag Chemie,


1976. Available from Perkin-Elmer, Part No. ~93-9462.

4. "Analytical Methods for Atomic Absorption Spectroscopy" (part


no. 303-0152) is provided with the instrument.

5. Flameless sampling techniques with an HGA Graphite Furnace


are discussed in the HGA instruction manuals and in "Analytical
Methods for Atomic Absorption Spectroscopy Using the HGA
Graphite Furnace" (part no. 990-9972). These manuals are
supplied with the HGA accessory.

6. Atomic Absorption Newsletter. A free one-year subscription


is provided to the purchaser of an atomic absorption instru-
ment.

7. "Concepts, Instrumentation and Techniques in Atomic Absorp-


tion Spectrophotometry" by R.D. Beaty. A copy is supplied
with each instrument (part no. 993-9533).

4/79
2 INSTALLATION

2A. EQUIPMENT

2A,l. Equipment Provided

Table 2~1A and B lists the equipment supplied with the instru-
ment. Some items are different for each of the four assembly
versions of the Model 560. The major versions are shown in
Figure 2-lA and Bu below.

TABLE 2~1A ~ ITEMS SUPPLIED WITH THE MODEL 560


(with Standard Burner Controls)
Part No. Description

057-0040 Basic Instrument Assembly


057-0858 Standard Burner Regulator Assembly, 115V or
057-0859 Standard Burner Regulator Assembly, 230V
057-0049 Spare Parts Kit, 115.V (see below) or
057-0047 Spare Parts Kit, 230V (see below) or
057-0048 Spare Parts Kit, 115V with BGC (see below) or
057-0046 Spare Parts Kit, 230V, with BGC (see below)
040-0266 4" Flat Burner Head
057-0705 Burner and Shield Assembly
057-0947 Burner Installation Kit
057-1068 Burner Tray
057-1380 Cover Plate
057-1208 Dust Cover

The Spare Parts Kits (057-0046 through 057-0049) contain the


following:

Part No. Description

303-0152 "Analytical Methods for Atomic Absorption


Spectrophotometry" Manual. (Periodic supplements
are supplied free.)
303-0477 Recorder Cable
303-1435 Spacer Feet (3)
998-8985 Line Cord 220V or
998-8986 Line Cord 125V
990-8173 Glide Cushion (3)
990-9390 AA Newsletter Subscription Form. (The first
one-year subscription is free.)
993-9453 Instruction Manual
998-1776 Fuse l.4A @ 250 VAC (5) (For Spares Kit 057-0046)
or 998-0047 Fuse LOA, 3AG (5) (For Spares Kit 057-0047)
or 998-1615 Fuse 2.5A, 3AG, SLO-BLO (5) (For Spares Kit 057-0048)
or 998-1614 F'use 2.0A, 3AG, SLO-BLO (5) (For Spares Kit 057-0049)

The following parts are provided in the Burner Installation Kit


057-0947:

Part No. De script ion

040-0188 Burner Spares Kit


990-3193 Nut-Ferrule, 1/4-in. Brass (4)
303-0405 Apiezon Grease (1 Pkg.)
990-3094 Tubing Insert (6)
993-9533 "Concepts, Instrumentation and Techniques in Atomic
Absorption Spectrophotometry" by R. Beaty. A copy
is supplied free with each instrument.

4/79
2-2

TABLE 2-lA - ITEMS SUPPLIED WITH THE MODEL 560 (Cont.)


(with Standard Burner Controls)

The Burner Spares Kit 040-0188 includes the following:

Part No. Description

990-8265 Polyethylene Tubing (1 Pkg)


040-1276 End Cap Gasket, Rubber
040-1277 End Cap Gasket, Corkprene (2)
990-2038 Burner Head 0-Ring
990-2043 Blow-Out Plug 0-Ring
990-2237 Separator Screw 0-Ring
990-2239 Nebulizer 0-Ring

The following parts are provided for the installation of the Burner
Regulator:

Part No. De script ion

057-0559 Fuel Hose Assembly (Red)


057-0566 Nitrous Oxide Hose Assembly (Blue)
057-0567 Air Hose Assembly (Black)
990-3031 Outlet Bushing
990-3196 Tube Fitting

TABLE 2-lB - ITEMS SUPPLIED WITH THE MODEL 560


(with Optional Burner Controls)

Part No. Description

057-0040 Basic Instrument Assembly


047-0397 Optional Burner Regulator Assembly, 115y or
047-0398 Optional Burner Regulator Assembly, 230V
057-0049 Spare Parts Kit, 23~V with BGC
or 057-0048 Spare Parts Kit, 115V with BGC See Table 2-lA
or 057-0047 Spares Parts Kit, 23.0V for parts
or 057-0046 Spare Parts Kit, 115V breakdown.
040-0266 4" Flat Burner Head
057-0705 Burner and Shield Asssembly
057-0947 Burner Installation Kit (See Table 2-lA for parts)
057-1068 Burner Tray
057-1208 Dust Cover

The following parts are provided for installation of the


interlocked drain system:

Part No. De script ion

047-0365 Drain Assembly


047-0391 Drain Tube Assembly
990-4991 2 Gallon Plastic Carboy
990-3002 Hose Clamp (2)
047-0352 Drain Block Assembly
991-0167 Screw, #8-32 x 3/4 long
991-1320 Washer #8, Ext. Tooth

The folllowing parts are provided for the installation of the


Burner Regulator:

Part No. Description

057-0559 Fuel Hose Assembly (Red)


057-0566 Nitrous Oxide Hose Assembly (Blue)
057-0567 Air Hose Assembly (Black)
990-3031 Outlet Bushing
990-3196 Tube Fitting

4/79
2-15

I
\
RESTRICTOR
FUEL
FLOW 2 WAY
NEEDLE
VALVE SOLENOID FUEL
VALVE PRESSURE
REGULATOR

AIR-OFF-N 2 0 AIR-N 20-FLOW


VALVE NEEDLE VALVE

f
l
FUEL SHUT OFF
TOGGLE VALVE

~
i1 t
n
3WAY
FUEL
FLOW METER
I
AIR-N 2 0
FLOWMETER n
SOLENOID
VALVE
t
CHECK CHECK
VALVE VALVE
l l
IGNITER@
............
0~2F~~0
OUT o
l
............
0N~~ OUT ............
NEB0 0

............ 0AIRIN ............


~~0
Fig. 2-9B - Plumbing Schematic for the Model 560 Flowmeter-Type
Control System, Assembly Nos. 060-0196 thorugh 060-0200.

4/79
2-16

MODEL 560

STANDARD
GAS CONTROL

D
1 P610 to J610 (Gray Cable) 2 Burner Compartment to J604
Connector INTERLOCK (Gray Cable)
Connector
Fig. 2-10 - Electrical Connections between the Instrument and the
Flowmeter-Type Control System

5) Locate the tubing harness which extends from the bottom


of the burner compartment of the spectrophotometer. The
black gas tubing and the thin white igniter tubing are
partially wrapped with a translucent white plastic spiral.
6) Connect the tubing (step 5) to the appropriate gas fittings
on the rear panel of the burner regulator. (The connections
are shown in Figure 2-8B.)
7) Connect the gray cable (Fig. 2-10) which extends from
P610 IGNITER on the rear panel of the regulator to the
IGNITER connector, on the rear panel of the instrument.
8) Make sure the POWER switch on the front panel of the
regulator is OFF and plug in the burner regulator power
cord.
9) Set the fuel and oxidant source regulators to the pressures
shown in Table 8-3Ao

2B,5. Lamp Installation


Both single and multi-element source lamps are used for atomic
absorption determinations. A list of the source lamps available
is provided in Price List PL-311.

4/79
2-17

Insert the lamp in the lamp holder so that the lamp envelope
is held in place by the two retaining springs (see Fig. 8-3).

Note: If the Perkin-Elmer Universal Lamp Mount is used,


install the lamp and lamp mount as described in the in-
structions, 993-9099, provided with the mount.

2B,6. Sample Support Tray

The sample support tray, designed to hold containers of solutions


or solvent for aspiration, is held by supporting brackets below
the burner assembly. It may be hung in position at several levels
on the brackets.

To remove it for cleaning or disposing of spilled liquids, lift


it without tilting in order to disengage its supporting hooks
from the brackets attached to the instrument.

2B,7. Lamp and Burner Alignment

Refer to Sec. 8C. These procedures are followed each time the
insturment is set up for measurement.

2B,8. Burner Compartment Door Removal, Replacement

The burner compartment door (Fig. 2-1) may be removed from its
hinges as follows: Lift up on the door so the pivot of the
bottom hinge is lifted out of the hinge, then pull the bottom
of the door outward and downward, away from the instrument and
remove the door.

To replace the door, align the upper hinge pivot on the door
with the hole in the upper hinge, then push up on the door to
insert the pivot into the hinge. Align the lower hinge pivot
with the hole in the lower hinge and allow the door to drop into
position.

2B,9. Nitrous Oxide Supply and Accessories

When refractory elements are to be determined, the high tempera-


ture combination of nitrous oxide and acetylene is required.

Note: It is generally inadvisable to use nitrous oxide to


determine elements which are best determined with air. Air
is less expensive than N2 0; also, a number of elements will
show poorer sensitivity and greater ionization interference
in the nitrous oxide flame.

The use of nitrous oxide requires a number of accessories and


precautions:

1) A size no. 1 N O cylinder contains about 14,000 liters and


will last for to to 12 hours of burning time.

4/79
2-18

2) Use the blue N?O hose assembly (057-0566) only to connect


the cylinder to the burner regulator (see Fig. 2-8A or 2-
8B) .
3) A nitrous oxide pressure regulator is required. This is
available (with an integral heater) from Perkin-Elmer as
Part No. 303-0204 (105-125 V) or 303-0349 (200-240 V) or
from the gas supplier. -
Cautions: When installing or using nitrous oxide, the
following precautions must be observed:
a) Nitrous oxide must not be permitted to flow in lines
that have been contamianted by oil. Like oxygen,
nitrous oxide and oil form a combination that may lead
to spontaneous combustion or explosion.
b) The standard burner head must be replaced with the
nitrous oxide burner head, Perkin-Elmer part number
040-0277. The nitrous oxide burner head instructions
should be strict followed.
c) Heat the pressure regulator to avoid freezing.

d) Ensure that the drain trap is correctly in-


stalled as described in Section 2B,3. The
drain hose should be periodically checked
for wear. Do not kink the drain tube.
e) When the nitrous oxide or air/acetylene flame is used,
the flame shield should be in place. Wear tinted
safety glasses if looking at the flame directly without
the shield. Prolonged exposure to the unshielded
radiation from the flame can lead to eye fatigue and
possible damage.
f) Ventilate areas where nitrous oxide is used or stored.
N2o is an asphyxiant and is a potential hazard when
used in a confined space.

4/79
2-19

2B,10. Rear Instrument Terminal Board

1 Cutout for Printer or RS-232C


Connector
2 BASELINE Correction Terminals
3 Remote RESLOPE Terminals
4 Remote SEQUENCE INHIBIT
Terminals
5 Common Ground for Sl, S2, S3
6 Remote S3 Terminals
7 Remote S2 Terminals
8 Remote Sl Terminals
9 Remote AZ (Auto Zero)
Terminals
10 Remote READ Terminals
11 1 Volt Recorder Terminals
12 10 mV Recorder Terminals

Figure 2-11 - Rear Instrument Terminal Board

BASELINE Connections

When working at very high scale expansion levels, using a


Heated Graphite Furnace such as the HGA-500, remote contact
closure of these terminals prior to the atomization cycle
enables the Model 560 to compensate for any slight variations
in electrical baseline. Connect these terminals to the BASE-
LINE connections on the Heated Graphite Furnace controller.

RSLP Connections

These connections duplicate the Reslope key function on the


instrument keyboard, and are activated by remote contact
closure (for example, by an Auto Sampling Accessory) between
the contact and circuit ground.

SEQ # INHB

When activated by remote contact closure at the time a reading


is printed, these connections inhibit the printing and in-
crementing of a sequence number for sample measurements on
the PRS-10 Printer Sequencer.

Note: Closure of these contacts inverts the normal arrange-


ment for printed sequence numbers. No sequence numbers are
printed for sample measurements, but sequence numbers will
be printed for -calibration data.

4/79
2-20

S3, S2, Sl, AZ and READ Connections

These terminals duplicate the corresponding control functions


on the instrument keyboard, and are activated by remote con-
tact closures to ground. There is a single ground connection
for Sl, S2, and S3.

1 V and 10 mV Recorder Connections

The two sets of connections provided are for the connection


of a 1 V or 10 mV recorder. The readout signal varies from
0 to 10 V or 0 to 100 mV, depending on the pair of connections
used, equivalent to the range 0 to 9999 on the display.

TTY Socket*

With the Communications Interface Accessory installed, this


socket enables a Teletype to be connected for the printing
of reports. The signals available at this socket are de-
scribed in the Communications Interface instructions.

PRS Socket*

This socket is provided for connecting a PRS-10 Printer Se-


quencer Accessory. Requires the installation of the Printer
Interface accessory circuit board in the instrument.

2B,ll. Connecting a Heated Graphite Furnace

When a Heated Graphite Furnace Accessory such as a Model HGA-500,


HGA-400, HGA-2200, HGA-2100 or HGA-76B is used, the HGA controller
transmits a READ impulse to the Model 560 so that a measurement
is taken at the appropriate point in the atomization cycle. The
HGA-500 or HGA-400 has an additional facility for triggering Base-
line Offset Correction.

The cable (Part No. 290-0280) supplied with an HGA-2100** or


HGA-2200 has a white and black lead at each end. A black lead
is capped at one end; remove the cap. The HGA-76B connector cable
is a shielded white wire with a plug at the HGA end and a blue
and black lead at the spectrophotometer end. The HGA-500 or
HGA-400 cable comprises four leads. Connect the appropriate cable
as follows:

*This socket is not supplied unless the corresponding accessory


is installed.
**With an HGA 2100. Connect a ground lead between the recorder
ground connection and TB303, terminal 4 on the HGA-2100. Cable
290-0280 includes a suitable ground lead. HGA-2100's shipped
before July 1974 have a different cable. Modify the cable or
use other cable to make the connection described here. If
necessary, contact a Perkin-Elmer Service representative for
assistance.
4/79
2-21

a) HGA-500 or HGA-400 To Model 560

Red and Blue wires to READ Output READ Input


Grey and Black wires to BASELINE BASELINE Input
Output
To Model 560 READ INPUT
b) HGA-2100/2200 TB3
White to SIG
White to Pin 1 Black to Ground ( ~)
Black to Pin 2
To Model 560 READ INPUT
c) HGA-76B Plug Connection PR
Blue to SIG
Blue to Pin 1 Black to Ground ( ~)
Black to Pin 2

2B,12. Connecting the Model 560 to Line Power

When all other connections have been made, make sure the instrument
POWER switch is set to OFF, then plug in the power cord.

4/79
SAMA

( Al 2.1-1972

SCIENTIFIC APPARATUS MAKERS ASSOCIATION

Recommended Practice

Guidelines for the


Purity and Handling of Gases
Used in Atomic Absorption Spectroscopy

Scientific Apparatus Makers Association


1140 Connecticut Avenue, N.W.
Washington, D.C. 20036
FOREWORD
(

The Scientific Apparatus Makers Association is a voluntary national trade association


representing the . major segments of the scientific instrument industry. Founded in 19 I 8 to
promote a domestic industry which expanded rapidly during World War I, SAMA has worked
consistently to assist in the strengthening and expansion of United States production and
distribution of scientific and industrial instruments, apparatus and equipment.

Because of the diversity of the products and markets of its member companies, SAMA from
virtually the time of its inception has found it expedient to organize into various product-oriented
sections. This organization permits groups of member companies to focus more specifically on their
particular problems and primary interests through section programs and activities, and at the same
time benefit from the larger participation in the general association meetings and activities.

At present there are seven operating sections in SAMA, which are:

Analytical In strum en t Optical


Laboratory Apparatus Process Measurement and Control
Measurement and Test Instrument Scientific Laboratory Furniture
Nuclear Instrument and Equipment

The Association and its sections are active in the development and promotion of both
domestic and international standards. Technical standards are published by SAMA; and cooperative
programs are maintained with the Instrument Society of America, American Society of Testing and
Materials, and other standards-making organizations. SAMA sponsors several committees of the
American National Standards Institute and has representatives serving on working committees of
the International Standards Organization and the International Electrotechnical Commission.
Liaison is also maintained with the General Services Administration, Department of Commerce, and
the Department of Defense in the promulgation of federal and military standards and specifications.

The following material was developed within the Analytical Instrument Section by a Task
Group on Atomic Absorption Spectrophotometers. The material was completed in October, I 972.

This material is not copyrighted and may be quoted in purchase specifications.

Scientific Apparatus Makers Association


1140 Connecticut Avenue, N.W., Washington, D.C. 20036
Scope and Purpose Acetylene 99.6 -99.8%
Oxygen .01 .1%
This recommended practice is intended to provide manu- Nitrogen .02 .2%
Phosphine .001 .04%
facturers and users of Atomic Absorption Spectrophoto-
Sulfur Compounds
meters guidelines for the purity and handling of gases. It (Calculated as H1S) .0003 .0008%
describes the general purity requirements for gases used in Chlorine 00002- ,0001%
atomic absorption spectrophotometers and contains infor- Hydrogen Trace
mation on handling, gas volume requirements for normal Methane Trace
operation, and several other points which may be useful in
establishing a working analytical system.
The acetylene supplier does not include acetone vapor in
This recommended practice ctoes not describe completely his calculation of purity, and in actuality, acetone is by far
safety precautions for the handling of gases. The supplier of the major contaminant.
compressed gases generally will supply information for safe
handling of gas cylinders.

Hydrogen
Acetylene
Hydrogen is usually obtained in 1A cylinders (3) containing
Acetylene is usually obtained in size IB cylinders (!) about 5500 liters (STP). An air-hydrogen flame requires
containing about 9000 liters (STP) of gas dissolved in about 15 liters per minute, and therefore, a cylinder will
acetone. An air-acetylene flame requires about 5 liters per last for about 6 hours of continuous operation. Hydrogen is
minute, whereas a nitrous oxide-acetylene flame requires available in several purity grades. The extra dry grade
about 15 liters per minute. Therefore a single lB acetylene (99 .9+%) is satisfactory for atomic absorption work.
cylinder will last from I 0 to 30 operating hours, depending Hydrogen cylinders are used at high pressure arrd should be
on the proportion of N 2 0 to air flame use. handled with care at all times.

Acetylene is dissolved in acetone because it cannot be


compressed as a dry gas to greater than about 30 PSI
Air
without special precautions to prevent explosive decom-
position. To provide a margin of safety, acetylene should
Air suitable for A.A. analysis can be obtained either from
not be used at above 15 PSI, outside of the cylinder. As
compressed air cylinders or from a compressor unit. Use of
acetylene is removed from a cylinder, it is accompanied by
compressed air cylinders has two potential disadvantages:
acetone vapor. The ratio of acetone vapor to acetylene
vapor increases as the acetylene is depleted. For some
elements, absorption sensitivity will change as the ratio of I. Occasionally cylinder air has gone through a liquifica-
acetone to acetylene changes. Therefore it is good practice tion stage during which the oxygen to nitrogen ratio can
to switch to a full cylinder when the pressure falls to change. Therefore it is not uncommon to find other than
between .75 and 100 PSI. Since the acetylene is in solution, 20'% oxygen in air cylinders. This can provide a potential
the pressure drop is not linear with gas removal, and a safety hazard and can cause burner operation and analytical
pressure of 75 PSI indicates a nearly empty cylinder, results to vary.
assuming the cylinder is at room temperature .. Acetylene
cylinders should be used and stored only in an 'upright
2. A standard #1 size air cylinder contains about 6200
position to avoid the possibility of acetone filling the valve
liters at standard temperature and pressure (STP). A premix
or regulator.
burner-nebulizer system uses about 20 liters/minute, and
therefore one cylinder will last about five hours. Unless an
Acetylene should not be allowed to come in contact with instrument is used only a few hours per day, changing
copper, silver or mercury, as these metals can form unstable cylinders becomes a nuisance.
acetylides. (2) Wet acetylene produces explosive acetylides
with copper. Pure copper should not be used for acetylene
Because of these limitations, a compressor is generally used.
plumbing. The rate of formation of acetylides is increased
An air compressor should be chosen that will provide at
by the presence of air or carbon dioxide. The acetylide is
least 30 liters per minute at a pressure of 40 PSI. It is
formed much less rapidly on brass than copper.
desirable to have a surge tank to provide a smoother flow.
It is also desirable to have a water and oil trap between the
Suitable acetylene has a minimum purity specification of compressor and the burner-nebulizer gas control box to
99.6%, the actual assay being about 99.8%. A nominal keep oil and. water droplets out of the flow metering
analysis is given in the following table: system.
Nitrous Oxide consumption rate varies widely, depending on the particular
application. Argon is available in several purity grades.
Nitrous oxide is usually obtained in size IA cylinders (4) Either the prepurified grade (99 .998%) or the high purity
containing about 15,000 liters (STP). The nitrous oxide is grade (99.995'/r) is satisfactory for atomic absorption work.
in the liquid stale, initially at a pressure of about 750 PSI. Argon cylinders are used at high pressure and should be
A nitrous oxide acetylene flame requires about 20 liters handled with care at all times.
N 2 0 per minute, and therefore a single IA cylinder will last
just a little over 12 hours of continuous operation. Since
the nitrous oxide is in liquid form, the pressure guage does Nitrogen
not give any indication of how much N 2 0 remains in the
cylinder un ti! the pressure starts to fall rapidly as the Nitrogen is usually obtained in size IA cylinders (6)
residual gas is drawn off. containing about 6500 liters (STP). Nitrogen is generally
used as a flame diluent to provide a relatively cool flame,
When nitrous oxide is removed from the cylinder at this and the consumption rate varies widely, depending on the
rate, the gas expanding in the cylinder pressure regulator particular application. Nitrogen is available in several purity
cools the regulator diaphragm so that sometimes it freezes, grades. Either the high purity grade (99.9%) or the extra
causing a lack of regulation. It is therefore advisable to heat dry grade (99 .7%) is satisfactory for atomic absorption
the regulator, using either a built-in heater or an externally work. Nitrogen cylinders are used at high pressure and
supplied source of heat such as a lamp or electrical should be handled with care at all times.
resistance tape.

All lines carrying nitrous oxide should be free of grease, oil


or other organic material, as it is possible for spontaneous
combustion to occur. Cylinders of nitrous oxide should be
considered high pressure cylinders and should be handled
(1) Cylinder valve outlet CGA No. 510 (some suppliers use
with care at all times.
CGA No. 300)
(2) V. F. Brameld, M. T. Clark, A. P. Seyfang, Jour. Soc.
Argon Chem. Ind. 66, 346 (1947).
(3) Cylinder valve outlet CGA No. 350.
Argon is usually obtained in size lA cylinders (5) contain-. (4) Cylinder valve outlet CGA No. 1320.
ing about 7000 liters (STP). Argon is generally used as a (5) Cylinde; valve outlet CGA No. 580.
flame diluent to provide a relative!y cool flame, and the (6) Cylinder valve outlet CGA No. 580.

2
4 PRINCIPLES OF OPERATION

The two books listed below provide a general background on


the principles of operating the Model 560:

(1) w. Slavin, Atomic Absorption Spectroscopy, Wiley and Sons,


1968. (P-E part no. 990-9628)
(2) B. Welz, "Atomic Absorption Spectroscopy", Verlag Chemie,
1976 (P-E part no. 993-9462)

A schematic of the optical system is shown in Fig. 4-1.

MONOCHROMATOR

M6

M4
PRIMARY SOURCE

SAMPLE COMPARTMENT

Fig. 4-1 - Model 560 Optical Schematic


5 PERFORMANCE CHARACTERISTICS

The sensitivity of the instrument in detecting metallic


elements is shown in Tables 5-1 and 5-2 below:

TABLE 5-1 - STANDARD CONDITIONS FOR ATOMIC ABSORPTION

STANDARD CONDITIONS FOR ATOMIC ABSORPTION

SBW FLAME SENS. SBW FLAME SENS.


ELEMENT A (nm) ~ GASES CHECK(a) ELEMENT A (nm) ~ GASES CHECK(a)

Ag 328.l 0.7 A-Ac 3 Nd 463.4 0.2 N-Ac 500 (b)


Al 309.3 0.7 N-Ac 45(b) Ni 232.0 0.2 A-Ac 7
As 193.7 0.7 A-Ac 40 Os 290.9 0.2 N-Ac 45
As 193.7 0.7 N-Ac 45 p 213.6 0.2 tN-Ac 15000
As 193.7 0.7 Ar-H 7 Pb 283. 3 0. 7 A-Ac 25
Au 242.8 0.7 A-Ac 12 Pd 247.6 0.2 A-Ac 12
B 249.7 0.7 N-Ac 2000 Pr 495.1 0.2 N-Ac 2500 (b)
Ba 553.6 0.2 N-Ac 20(b) Pt 265.9 0.7 A-Ac 90
Ba 553.6 0.2 A-Ac 225(b) Rb 780.0 2.0 A-Ac 5 (b)
Be 234.9 0.7 N-Ac 1.2 Re 346.0 0.2 N-Ac 700

Bi 223.1 0.2 A-Ac 18 Rh 343.5 0.2 A-Ac 15


ca 422.7 0.7 A-Ac 3. 5 RU 349.9 0.2 A-Ac 25
ca 422. 7 0. 7 N-Ac 2. 5 (b) Sb 217.6 0.2 A-Ac 25
Cd 228.8 0.7 A-Ac 1.2 Sc 391.2 0.2 N-Ac 20(b)
co 240.7 0.2 A-Ac 7 Se 196.0 2.0 A-Ac 25

er 357.9 0.7 A-Ac 4 Se 196.0 2.0 Ar-H 12


cs 852.1 2.0 A-Ac 15 (b) Si 251.6 0.2 N-Ac 85
cu 324.7 0.7 A-Ac 4 Sm 429.7 0.2 N-Ac 400(b)
Dy 421.2 0.2 N-Ac 40(b) Sn 286.3 0.7 N-Ac 200
Er 400.8 0.2 N-A(! 45 (b) Sn 286.3 0.7 A-Ac 180

Eu 459.4 0.2 N-Ac 25(b) Sn 286.3 0.7 A-H 70


Fe 248.3 0.2 A-Ac 6 Sr 460.7 0.2 A-Ac 6 (b)
Ga 287.4 0.7 N-Ac 65 Sr 460.7 0.2 N-Ac 4 (b)
Gd 407.9 0.2 N-Ac 800(b) Ta 271.5 0.2 N-Ac 725
Ge 265.l 0.2 N-Ac llO Tb 432.6 0.2 N-Ac 400(b)

Hf 286.6 0.2 N-Ac 700 (c) Tc 261.5 0.2 A-Ac 120


Hg 253.6 0.7 A-Ac 350 Te 214. 3 0. 2 A-Ac 45
HO 410.4 0.2 N-Ac 50(b) Ti 365.3 0.2 N-Ac 85
In 303.9 0.7 A-Ac 35 Tl 276.8 0.7 A-Ac 25
Ir 264.0 0.2 A-Ac 400 Tm 371.8 0.7 N-Ac 16 (b)

K 766.5 2.0 A-Ac 1.8 u 358.5 0.2 N-Ac 2300(b)


La 550.1 0.2 N-Ac 2000 (b) v 318.4 o. 7 N-Ac 75
Li 670.8 O.i A-Ac 1. 5 w 255.l 0.2 N-Ac 500
LU 336.0 0.2 N-Ac 300 (b) y 410.2 0.2 N-Ac 85(b)
Mg 285.2 o. 7 A-Ac 0.3 Yb 398.8 0.2 N-Ac 5 (b)

Mn 279.5 0.2 A-Ac 2.5 Zn 213.9 o. 7 A-Ac 0.8


Mo 313.3 0.7 N-Ac 25 Zr 360.1 0.2 N-Ac 475
Mo 313. 3 0.7 A-Ac 40
Na 589.0 0.2 A-Ac 0.7 A-Ac = Air-Acetylene
Nb 334.4 0.2 N-Ac 1700(b) N-Ac = Nitrous oxide-Acetylene
Ar-H = Argon-Hydrogen-Entrained Air
A-H = Air-Hydrogen

(a) Metal concentration (g/ml) in aqueous solution which will give a


reading of approximately 0.2 absorbance units.
(b) Addition of a large amount of an easily ionizable material (e.g.
1000 g/ml potassium as the chloride) may be required to control
ionization.
(c) Fluoride added to obtain the sensitivity check value shown.
5-2

TABLE 5-2 - SENSITIVITY CHECKS FOR THE HGA GRAPHITE FURNACE

HGA
ELEMENT GRAPHITE FURNACE*t

Al 0.05
As 0.04
Au 0.04
Ba 0.03
Bi 0.02

Cd 0.003
Co 0.03
Cr 0.007
Cu 0.01
Fe 0.01

In 0.05
Ir 0.3
Mn 0.005
Mo 0.025
Ni 0.04

Pb 0.025 (283nm)
Pb 0.016 (217nm)
Pd 0.04
Pt 0.18
Sb 0.04

Se 0.06
Si 0.14
Sn 0.14 (286nm)
Sn 0.08 (224.6nm)
Te 0.025

Ti 0.21
v 0.15
Zn 0.0007

* All data were obtained using pyrolytically coated tubes, rapid heating and gas flow
interrupt.

t The sensitivity check data given above are the metal concentrations ( g/ml) in aqueous
solution which will give a reading of approximately 0.2 absorbance units when 20 J.11
are used. Greater sensitivity can be obtained by using larger solution volumes.

4/79
6 SPECIFICATIONS
Monochromator: Littrow grating system. Focal length 267 mm.
Wavelength range 190-870 nm. covered by dual-blazed grating,
1800 line/mm (45,700 lines/inch). Ruled area 64 x 72 mm blazed
at 235 nm and 600 nm. Resolution settings of 0.2, 0.7 and 2 nm
switch-selectable. Dispersion: 1.6 nm/mm (nominal). Wide-range
photomultiplier detector with UV-transmitting window. Wavelength
read on three-digit counter.
Photometer: Double-beam, time shared system. Protected from
corrosive atmosphere "AC" system (lamp light chopped by rotating
sector while flame light is unchopped). Minimum spectral band
width - 0.2 nm (nominal). Source current adjustable to 50 mA.
Optional Deuterium Arc Background Corrector also operates with
a double-beam, time-shared system and includes Automatic Inten-
sity Control of the deuterium arc source.
Readout: Results shown on 6-digit electronic display with range
of 9999 counts and two zero positions for use with adjustable
decimal. Readout is linear in absorbance, concentration, or
emission intensity with variable scale expansion of O.OlX to
lOOX. Automatic zero setting and automatic concentration cali-
bration (with up to three standards) are push-button actuated.
Ability to take a number of readings and average them, display
the average and calculate and display the coefficient of vari-
ation and standard deviation and resolope the calibration curve
with a single additional standard are built-in. Informative
error messages are displayed to alert the analyst to improper
instrument calibration. Peak height and integrated peak area
modes are provided for use with fast peak-shaped signals.
Integration time variable from 0.2 to 60 sec in nominal 0.2-sec
intervals. Overrange indication for expansion, calibration,
absorbance, and display. Function indicator and display checks
in LAMP and SET UP modes. Direct connnection provided for labo-
ratory recorder with separate recorder control allowing contin-
uous or "noise-free" integrated readings on recoraer (as per
the digital display), or continuous readings in absorbance, or
continuous readings with display calibration and variable time
constant.
Sample area: 22 cm wide, 21 cm deep. Open to the front through
a removal flame shield of about 7% light transmission. Sample
tray, 21 cm wide and 12 cm deep, adjustable to three separate
heights.
Wavelength drive: (Optional module) .5 nm/min. scan speed.
6-2

Burner: Premix design, stainless steel mixing chamber coated


with an inert plastic; plastic-coated flow spoiler, auxiliary
air inlet; 5 angle to ensure proper drainage; check valve;
burner mount is adjustable in vertical and horizontal directions
(with scale reading provisions) and angularly without scale
reading. Adjustable stainless steel nebulizer (corrosion re-
sistant nebulizer available); 10-cm all-titanium single-slot
burner head supplied.
Standard Burner Control: contains individual pressure and
flow controls and meters for oxidant and fuel. T-valve to
switch oxidant from air to nitrous oxide or other gas. Flame
is ignited only on air-based flames with pushbutton actuated
glow plug. Also contains burner head safety interlock system
and automatic fuel flow change when switching to nitrous oxide-
acetylene flame.

Optional Burner Control: includes microprocessor to measure


oxidant and fuel flows to provide automatic checking for safe
flow ratios and to sense burner head, flame and burner drain.
Also includes automatic gas sequencing in addition to the
features of the standard burner control.

Weight: 70 kg (150 lb.) net; 125 kg (270 lb.) gross.

Power requirements: 105-125 or 200-240 volts, 50/60 Hz, 150


watts.

Dimensions 41 cm high; 56 cm deep; 88 cm wide.

4/79
7 CONTROLS AND INDICATORS
7A. INSTRUMENT CONTROLS AND INDICATORS
7A, 1. Lower Right Front Panel (Fig. 7-1)
POWER On-Off Switch - Controls line .Power to the instrument. The
digital display will light only when the power is on.
SIGNAL Control Switch - Four switch positions determine how the
data measured by the instrument are shown on the display. The
remaining two are used in setting up the initial instrument
parameters:

@
SIGNAL MODE RECORDER BKGO CORR POWER
TC1 TC2 AABG ON
AA,. ,. BG
TC3

"TC4

OFJ'

1. Digital Display and Indicators 12. CHK (Check) Key


2. Ait (Au to Zero) Key and Signal Dot 13. PRNT (Print) Key and Sigma Dot
3. Sl Key and Signal Dot 14. Numerical Keyboard
4. S2 Key and Signal Dot 15. CE (Clear Entry) Key
5. SJ Ke~ and Signal Dot 16. Electronics Compartment
6. AVErage Key and Signal Dot Access Screws
7. Coefficient of Variation Key and 17. SIGNAL Control Switch
Signal :-)ot 18. READ Key and Signal Dot
8. Stan dare :>eviation Key and 19. MODE Control Switch
Signal Dot 20. RECORDER Control Switch
9. RSLP (Res lope) Key and Signal Dot 21. BKGD CORR (Background
10. t (Time) Key Corrector) Control Switch
11. EXPansion Key and Signal Dot 2 2. POWER Toggle Sidtch

Fig. 7-1 - Right Front Control Panel


4/79
7-2

SIGNAL Control Switch continued:

LAMP - When the SIGNAL switch is set in this position, no


reading is shown on the display (to test that the digit
segments turn off at the proper time). All indicator dots
remain lighted. The ENERGY/LAMP meter on the left front
panel shows the hollow cathode lamp current directly in
milliamperes when the AA/BG rocker switch is in the AA
position. The lamp current can be adjusted with the knob
below the ENERGY/LAMP meter.

SET UP - This position displays relative energy on the ENERGY/


LAMP meter and disconnects the automatic gain control. The
wavelength is peaked on the desired line and the lamp position
is adjusted to provide maximum energy when the switch is on
this setting. (All parts of the digital display and all
indicator dots are lit to test that they work.)

ABSorbance - In this setting, the instrument displays data in


absorbance (absorbance-seconds for peak area) Expansion factors
set with other controls do not affect the digital display or the
output to the recorder, but the automatic gain control does
operate when the SIGNAL switch is in this position.
CONCentration - In this position, the instrument displays
atomic absorption data in units of concentration or with fixed
scale expansion. Expansion values can be chosen from 0.01
to lOOX, or 1, 2, or 3 standards can be used to calibrate the
instrument to read directly in concentration. The automatic
gain control is operating when the SIGNAL switch is set in
this position.

EMission CHOP - Flame emission measurements made with the


SIGNAL switch in this position are automatically modulated.
The emission reading can be displayed directly in units of
concentration or with fixed scale expansion. Expansion values
can be set from 0.01 to lOOX, or 1, 2, or 3 standards can be
used to calibrate the instrument to read in concentration.
The automatic gain control does not operate in this SIGNAL
switch setting.

EMission - Lamps and other emission sources where the signal


is already modulated are measured with the SIGNAL switch on
this setting. The reading can be displayed directly in units
of concentration or with an expansion factor. On this setting,
the automatic gain control does not operate.

MODE Control Switch - The settings on this switch determine how


the measurement results are shown on the digital display:

CONTinuous - Readings are integrated over the time determined


by the operator and automatically updated on the display at
the end of each integration period. The integration time is
variable from 0.2 to 60 seconds in nominal 0.2-second increments.
7-3

MODE Control Switch continued:


\
HOLD - Each reading must be initiated by pressing the.READ
button, or by an accessory connected to the (Remote) READ
terminals at the back of the instrument. There is a 2-
second delay before integration begins for the time
selected by the operator.

PK HT (Peak Height) - When a measurement is initiated by


pushing the READ button or by an accessory connected to
the (Remote) READ terminals on the back of.the instrument,
the instrument will display the highest reading obtained
during the time selected by the operator.

PK AREA - When a measurement is initiated by pushing the


READ button or by an accessory connected to the (Remote)
READ terminals at the back of the instrument, the instru-
ment will display the sum of the readings taken during the
integration time selected by the operator.

RECORDER Control Switch - The following six switch positions


determine how the data measured by the instrument are trans-
mitted to the recorder. At some positions, it allows data
to be sent to the recorder in a format either the same as or
different from the format of the display.

ABSorbance - At this setting, the data sent to the recorder


are presented in terms of absorbance. Scale expansion,
curvature correction factors, and the MODE control switch
setting do not affect the signal sent to the recorder. The
time constant is equivalent to TCl (see Table 7-1). (When
taking emission measurements, data with an expansion of lX
are sent to the recorder.)

INTegrate - When the RECORDER control s~ritch is set in this


position, scale expansion and curvature correction applied
to the signal sent to the digital display also apply to the
signal sent to the recorder. The type of signal is deter-
mined by the position of the MODE control switch.

If the MODE switch is set on HOLD, PK HT or PK AREA,


the recorder pen will remain at rest until the completion
of a read cycle. The pen rises to a point on the chart
equivalent to the value on the digital display, holds
the position for three seconds and returns to its
original position.

If the MODE switch is set on CONTinuous, a continuous


signal is sent to the recorder, and the recorder pen
will move continuously along the chart. The time constant
is equivalent to TCl.
7-4

RECORDER Control Switch continued:

TCl, TC2, TC3, and TC4 (Time Constant Settings 1 through 4) -


These four switch position settings send a continuous signal
with varying time constant (damping) values from the instru-
ment to the recorder. Curvature correction and expansion
factors apply to the signal recorded when the switch is on
any of these four settings. The damping, or random noise
suppression, and the minimum aspiration time required (see
Table 7-1) increase from settings TCl to TC4.

TABLE 7-1 - MINIMUM ASPIRATION TIME

RECORDER Control Recommended Minimum


Settin_g_ As_E_iration Time

TCl 1 to 2 sec
TC2 6 sec
TC3 17 sec
TC4 55 sec

BKGD CORR (Background Corrector) Switch - In instruments which


have an optional built-in D2 (deuterium) Arc Background
Corrector accessory, the position of this switch determines
whether power is applied to the deuterium lamp. (The control
is present on all instruments to facilitate installation if
the Background Corrector is added later.)

AA - When the switch is set at this position, the instrument


takes normal atomic absorption measurements with the primary
source (hollow cathode lamp, EDL, etc). The D2 arc is not on.

AA-BG - At this position, the background corrector accessory,


including the D2 arc source, is turned on and measurements
taken at this setting are automatically background corrected.

BG - At this setting the hollow cathode source is off and


measurements of the background only are made with the D2 arc.
This setting is useful in studies where the background itself
is to be measured. Lamps with external power sources such as
electrodeless discharge lamps (EDLs), must be turned off
separately, blocked, or removed from the instrument in order
to obtain measurements of background only.

7A,2. Upper Right Front Panel (Display and Keyboard) (See Fig. 7-1)

The area above the control switches includes a numerical keyboard,


function keys, the READ key, the digital display and indicator
lights. Their functions are described. below.

Note: None of the keys operate if the SIGNAL switch is in the


SET UP or LAMP positions.
7-5

READ Key and Indicator - Momentary depression of this key ini-


tiates a measurement or read cycle. When the cycle is com-
pleted, the results will appear on the display in the form
selected by the operator. The READ indicator lights when
measurement begins and goes out upon completion of the cycle.
A read cycle cannot be initiated:
a) if the SIGNAL switch is set to SET UP or LAMP, or
b) if a numeric entry is pending (the display shows the KEY-
BOARD indicator).
Pressing another key or pressing READ again will interrupt
the read cycle and the new task will be performed.
Digital Display - Shows the analytical result with up to four
significant digits (six digits if the leading two are zeroes).
A pending numerical entry also appears on the display until
it is assigned to the memory by pressing a function key, or
cleared by pressing CE (clear entry). The display also pre-
sents error messages, a full explanation of which is included
in Section 12.
BKGD CORR Indicator - When the BKGD CORR switch is set to either
the AA-BG or BG position the indicator comes on. The indicator
will flash if the background corrector signal falls below a
usable level in the AA-BG mode. (The attenuator control located
in the lamp compartment should be moved to the "IN" position
to alleviate this condition. Refer also to Section 8E,l.)
KEYBOARD Indicator - Lights when the value displayed is a key-
board entry and not an analytical result.
AVERAGE Indicator - Lights to indicate that the value displayed
is the average of several determinations.
OVER CAL Indicator - The indicator lights when the displayed
result is more than 5% greater than the most concentrated
standard used to calibrate the instrument. This measurement
result may be invalid. Either dilute the sample or use a more
concentrated standard and recalibrate.
Function Keys
AZ - Pressing the key in the CONT or HOLD MODE causes the indi-
cator to flash and initiates a read cycle, the result of which
is then set to zero and taken as the zero calibration point.
In PK HT or PK AREA, pressing this key causes the displayed
reading to be set to zero; the indicator does not light.
7-6

Sl - With a numerical entry pending on the display, pressing Sl


stores the value as the actual concentration of the first
standard. The instrument reverts to reading in absorbance.
Any previous calibration for Sl, S2, or S3 is erased and
their indicators go out.

With no prior numerical entry:

a) in CONT or HOLD, and CONC or EM, pressing Sl initiates


a read cycle, terminating in a single-standard calibration.
Sl light flashes during the read cycle and stays on at
the end of the cycle if calibration is successful. If
an error occurs, the light goes off and an error message
is displayed.

b) in PK HT or PK AREA, and CONC or EM, pressing this key


causes a single-standard calibration to be performed using
the absorbance value (or emission signal) which produced
the number on the display. Sl light comes on if calibration
is successful, or goes out if unsuccessful.
c) in ABS the key is ignored.

S2 - Is used in the same way as Sl but for the second standard.


If the calibration attempt is unsuccessful, calibration remains
at the Sl level and an error code is displayed; the 82 indicator
does not light. Following calibration with S2, any change
to S2 causes the calibration to revert to the Sl level. 82
concentration must be greater than Sl .

S3 - Is used in the same way as Sl, 82 but for the third standard.

RSLP - Reslope. An Sl, S2, or 83 calibration must be extant


or this key is ignored. Pressing RSLP causes the slope of
the calibration curve to be adjusted, without the necessity
of running all the standards again. The reslope factor reverts
to 1 if Sl, S2, or S3 is changed or reapplied.

AVE - Average. Following a numerical entry between 2 and 99,


pressing this key causes the designated number of readings
to be averaged and the average displayed. AVE indicator lights
when the key is pressed and goes out when the key is pressed
again to cancel.

A) CONT MODE: Instrument continuously takes specified number


of readings, averages then and displays the average. Press
A/Z, Sl, 82, S3 or RSLP to initiate specified number of
readings and average them. The instrument is then cali-
brated, based on the computed average.
7-7

B) HOLD MODE :
a) Press READ to initiate specified number of readings,
which are then averaged and the average displayed.
b) Press A/Z, Sl, S2, S3 or RSLP to initiate specified
number of readings, and average them. The instrument
is then calibrated, based on the computed average.
C) PK HT or PK AREA MODE: Press READ to initiate a single
reading. After the specified number of READ entries, the
results are averaged and the average displayed. A/Z, Sl,
S2, S3 or RSLP requests are ignored until an average has
been obtained. Pressing A/Z, Sl, S2, S3 or RSLP with an
average displayed will cause that value to be used for
calibration.
CV - Coefficient of Variation. Following an AVEraging operation,
press CV to display the coefficient of variation of the results.
Press CE to restore the average display. If the PRNT indicator
is on, pressing CV causes the CV to be printed following the
average printout. Press CV again to cancel the CV mode.
SD - Standard Deviation. Used precisely the same as CV, except
that the SD is displayed or printed. Press SD again to cancel
the SD mode.
t Key - Unless instructed otherwise, the instrument uses a 0.5-
second integration time in taking measurements. This interval
determines the approximate duration of the read cycle. To
change the integration time, enter the time interval desired
from 0.2 to 60 seconds, using the numerical keyboard. Then
depress the t key. The interval selected* will be stored in
the instrument and used for each measurement taken until a
different interval is entered by the operator or until the
instrument is shut off.
The operator can check the integration time setting by pressing
and holding the CHK key and then pressing the t key. The inter-
val will then be shown on the display. If no entry was made,
the built-in time of 0.5 second will be displayed.
If an integration time of less than 0.2 second or greater than
60 seconds is selected, an error code will appear on the dis-
play and all actions will be ignored by the instrument until
the entry is cleared using the CE Key.
EXPansion Key and Indicator Dot - This key allows the operator
to store a fixed scale expansion factor (between O.OlX and
lOOX) in the instrument memory. When the SIGNAL switch is
set on CONC, EM CHOP, or EM, the factor is automatically applied

*The instrument will "round off" the time selected to the nearest
machine cycle (approximately 0.18 sec).
7-8
to the measurement results shown on the digital display. The
dot alongside this key lights when an expansion factor has
been stored in the instrument memory and is being applied.
(When the SIGNAL control switch is set on ABSorbance, the ex-
pansion factor is ignored and the indicator is turned off.)
An entry made with the EXPansion key erases the previously
set expansion factor.
If the factor is less than 0.01 or greater than 100, an error
code will be displayed. The incorrect entry must then be clear-
ed with the CE key.
If the Sl standard rather than an expansion factor has been
applied, pressing EXP and CHK keys simultaneously will display
the expansion factor needed to produce the concentration value
assigned to SL
CHK (Check) Key - When this key is pressed together with one
of the function keys, the value stored with that key will be
shown on the display.
PRNT (Print) Key and Indicator Dot - When the key is depressed,
it connects the instrument to an optional external logging
device such as a printer or a teletypewriter. When data are
being transmitted, the indicator dot beside the button will
light. The indicator dot will go out if the data output rate
of the instrument is too fast for the data logging device to
accommodate.
If a sample sequence number is required in addition to the
analytical data, on the printer or teletypewriter, enter the
starting number and press PRNT to initiate printing.

Numerical Keyboard - The keyboard consists of 10 numerical keys,


0 through 9, a decimal point key and a Clear Entry (CE) key.
Momentary depression of any of the numerical keys or the decimal
point key:
(1) stops a read cycle in progress;
(2) shows the value selected on the digital display;
(3) causes the KEYBOARD indicator dot on the panel to light.
The information displayed is then either entered into memory
by pressing a valid function key (Sl, S2, S3, t, EXP) or is
cleared by pre~sing the CE key.
7A,3. Upper Left Front Panel (See Fig. 7-2)
WAVELENGTH Counter - Indicates the wavelength setting of the
monochromator in nanometers (nm).
COARSE/FINE ADJUST Knobs - Manually changes the wavelength setting
of the monochromator. The changes are indicated on the WAVELENGTH
counter.
7-9

SLIT Width Control - Used to


select a spectral slit width
for the monochromator. The
three NORMAL width settings
(0.2, 0.7 and 2.0 nm) are
used for flame analysis applica-
tions. The three ALTernate WAVELENGTH DRIVE FIN ADJUSJ

width settings (0.2, 0.7 and


2.0 nm) are used for operation WAV.ELEHGJH
nm
with the HGA Graphite Furnace
or for operation with other
devices that require a restricted
beam size. Wider slits permit
lower GAIN control settings and
tend to reduce noise f luctua-
tion. Relatively narrow slits
are required to block spectral
lin~s close to those being used
so that they will not reduce the
sensitivity of the analysis or
bend the working curve. Recom-
mended slit width settings are
specified in the Analytical
Methods Manual.
WAVELENGTH DRIVE Switch - Turns on
the (optional) automatic wave-
length drive accessory. (Scanning
speed is 5 nm/min.)

7A,4. Lower Left Front Panel


(See Fig. 7-2)
AA/BG Rocker Switch - Used to select
the type of source energy monitored
on the ENERGY/LAMP Meter. This
switch is spring-loaded and must
be held in the BG position manually. 1 WAVELENGTH Drive Switch
In the AA position, the energy (optional)
from a source located in the lamp 2 Optics Compartment Access
compartment is shown. In the BG Screw
position, the energy from the D2 3 FINE ADJUST Wavelength
arc background source is shown. Control
4 WAVELENGTH Counter
ENERGY/LAMP Meter - Indicates the 5 COARSE ADJUST Wavelength
energy level of the reference Control
beam of the instrument or the 6 SLIT Width Selector
current supplied in milliamps 7 ENERGY/LAMP Meter
to the hollow cathode lamp source. 8 AA/BG Energy Selector
The meter indicates lamp current Switch
when the SIGNAL control switch 9 GAIN Control
(on the right control panel) is 10 LAMP Current Control
set on LAMP and the AA/BG rocker
switch is set on AA. Fig. 7-2 - Left Front Control
4/79 Panel
7-10

LAMP Control - This control adjusts the current supplied to the


hollow cathode lamp source. Increase the current by turning
the control clockwise.

GAIN Control - Changes the voltage applied to the photomultiplier


detector. Increasing the GAIN setting (clockwise rotation)
causes the ENERGY/LAMP meter needle to move right. The con-
trol is active only when the SIGNAL control is on the SET
UP, EM CHOP, or EM position. When the SIGNAL control is on
the ABS or CONC position, this manual control is overridden
by the automatic gain control.

7B. DIGITAL BURNER CONTROL SYSTEM (See Fig. 7-3)

A. FUNCTIONS OF CONTROLS

INTERLOCKS
1 FUEL Display
FLAME
AIR HEAD
2 OXIDANT Display
N10 HEAD 3 OXIDANT Flow Control
DRAIN 4 FUEL Flow Control
5 FLAME Button
FUEL OXIDANT
6 Panel Retaining Screws
7 Keyboard
8 INTERLOCKS Status
Lights



Figure 7-3 - Burner Control Unit Controls

~ Selects AIR oxidant and acetylene

~
(C 2 H2 ) fuel operation. When this gas
combination is selected, the indicator
to the left of the key lights. Air/
c 2 H2 is the default gas selection.

4/79
7-11

FiOl Selects nitrous oxide (N 0) oxidant


and C H fuel operation.
2
If this
~
2
selection is used when igniting the
flame, flame ignition occurs on an
AIR/C 2 H mixture, followed by a change-
2
over to N 0/C H after 15 seconds.
If this gas c8m~ination is selected,
2
the indicator to the left of the key
lights.

~ Press to display and adjust the flow


~
setting of the selected oxidant (air
or nitrous oxide) prior to igniting
the flame. Key has no function once
the flame is ignited. Following flame
shutdown and closing of the oxidant
supplies, press to depressurize the
line of the oxidant selected.

~ Press to display and adjust the fuel


~ flow setting prior to igniting the
flame. Key has no function once the
flame is ignited. In N o;c H mode,
2 2 2
the flow shown is the boosted flow.
Following flame shutdown and closing
of the acetylene cylinder, press to
depressurize the fuel line.

OVERRIDE A) Press to override the optical flame


sensor. The light to the side
of the key indicates when the
override is in e f feet. (Used only
with certain sampling accessories
that interrupt the sensor beam).
Press again to cancel the override.

B) Pressing the OVERRIDE button (light


on) also defeats the microprocessor
flow checking functions, and enables
any fuel/oxidant ratio to be selected.
This feature is provided for users
of hydrogen/argon* mixtures, for
which different ratios may be
required in some cases.

*A special accessory control unit is required for these gases.

4/79
7-12

FLAME Pressing FLAME ON/OFF starts the com-


ON/OFF bustion gases flowing in the ignition
sequence: OXIDANT/FUEL - IGNITION.
If the flame fails to light first time,
an E3 message is displayed. Press
FLAME ON/OFF again to clear the error
message and repeat the sequence. To
extinguish the flame, press FLAME
ON/OFF to shut down in a safe sequence.

FUEL Display Displays two digits that show the


actual fuel flow rate in arbitrary
units on a scale of 0 to 99 (Refer
also to Figure 8-6). With N 2 o;c H
2 2
the digits show the boosted flow values.
When the flame is on, the digits are
shown. When the flame is off, the
fuel flow setting is displayed when
the CHK FUEL key is pressed.

OXIDANT Display Displays two digits that show the


actual oxidant flow rate in arbitrary
units on a scale of 0 to 99 (Refer
also to Figure 8-6). When the flame
is on, the digits are shown. When
the flame is off, the oxidant flow
setting is displayed when the CHK OXID
key is pressed.

FUEL and OXIDANT The knobs are used to vary the settings
Adjust Controls of needle valves in the respective
fuel and oxidant lines. Turn the knobs
counterclockwise to increase flow.
To read the flow rates, observe the
digits when the flame is on, or press
CHK FUEL or CHK OXID when the flame
is off.

B. FUNCTIONS OF INTERLOCK LIGHTS

FLAME Light: When the light is on, the .flame is burning


and the flame sensor is active. If the flame
goes out the interlock system will shut off
the gases. If the sensor receives insuffici~nt
energy (e.g. because the beam is obstructed
by sampling accessories or if an argon/hydrogen
flame is used)* the sensor interlock may
be disabled by pressing the OVERRIDE key.

4/79
7-13

AIR HEAD Light: Turns on if a burner head is installed, with


an air/C 2 H2 burner head interlock pin in
place. Ignition will not occur if the light
is off (unless the N o HEAD light is on).
2
N 0 HEAD Light: This light is turned on when the longer
2
burner head interlock pin is in place, in-
dicating that a N o burner head is installed.
2
N2 o will not flow unless the light is on
(except when the CHK OXID key is pressed).

DRAIN Light: Turns oh if the drain is connected and there


is fluid in the trap. If the light is off
the flame will not light, and gases will not
flow.

Note: If any one of the interlocks is not complete when


Tgnition is attempted, the corresponding indicator light
will flash for approximately 10 seconds and will then be
extinguished.

C. DESCRIPTION OF ERROR CODES

The microprocessor is programmed to detect certain invalid fuel:ox


oxidant ratios (and shuts down the flame if such combinations
are selected), and also performs checks for satisfactory flows
and flame conditions. If an error is diagnosed an error message
of the form 'E digit ' is displayed on the fuel or oxidant
display (if the fault lies with the fuel or oxidant flow). If
the fault is due to an invalid flow ratio, or is caused by the
flame sensor, then E is displayed on the left hand display digits
and the error number is displayed on the right. The explanations
of these messages are given below.

Importan.J:: The system will ~diagnose error conditions


if the OVERRIDE key has been pressed and the OVERRIDE light
is on. Exercise extra care when using the OVERRIDE mode.

Note: Error checking is performed immediately following the


Tgnition sequence. If an error is detected, the flame will
then shut down.

El FLAME TOO LEAN (With nitrous oxide


only, not with air). The fuel to
nitrous oxide oxidant ratio is~ 0.70,
indicating that the gas mixture is
excessively lean. The error message
occurs only with nitrous oxide, and
remains on the display until either
the CHK OXID or CHK FUEL key is pressed.
Check the gas pressure settings and
flow rates before attempting to re-
light the flame.
4/79
7-14

E2 FLAME TOO RICH


The fuel to oxidant ratio is too high
(~ 0.95 with air oxidant or ~ 1.50
with N o oxidant). The error message
2
remains on the display until either
the CHK OXID or CHK FUEL key is pressed.
Check the gas pressure settings and
flow rates before attempting to relight
the flame.

E3 FLAME SENSOR
The optical flame sensor will generate
an E3 if the sensor receives insufficient
energy from the flame, either because
the flame has gone out, or because
the sensor beam is obstructed. The
error is cleared by pressing either
of the CHK OXID or CHK FUEL keys, or
by pressing FLAME ON/OFF.

E4 GAS FLOW TOO LOW


The oxidant or fuel flow is below 10
units. The error is displayed on either
the fuel or the oxidant display, depending
upon which flow is too low. The message
will remain on the display until the
appropriate CHK key (fuel or oxidant)
is pressed.

7C. FLOWMETER-TYPE BURNER REGULATOR CONTROLS AND INDICATORS*


(See Fig. 7-4)

FUEL PRESSURE Gauge - Registers gas pressure of fuel at the FUEL


FLOWmeter.

FUEL FLOWMeter - Indicates fuel gas flow rate in arbitrary units


(See Table 8-3) for settings.) All readings are taken from
the center of the flowmeter ball.

OXIDANT Flowmeter - Indicates oxidant gas flow rate in arbitrary


units. (See Table 8-3 for settings.) All readings are taken
from the center of the flowmeter ball.

OXIDANT PRESSURE Gauge - Registers pressure of oxidant supplied


to the nebulizer.

OXIDANT Pressure Regulator - Controls pressure of oxidant supplied


to the nebulizer.

OXIDANT FLOW Needle Valve - Adjusts auxiliary oxidant flow rate.

FUEL FLOW Needle Valve - Adjusts fuel flow rate.

*Model 560 assembly numbers 060-0196 through 060-0200


4/79
7-15

1 FUEL PRESSURE Gauge


2
3
FUEL Toggle Valve
FUEL FLOWMeter
0
4 OXIDANT FLOWmeter CD

mliiTE

5 IGNITE Button
6 OXIDANT PRESSURE Gauge
7 OXIDANT PRESSURE Regulator
8 POWER ON/OFF Switch and
Indicator Light
9 OXIDANT FLOW
10 OXIDANT Selector Valve
11 FUEL FLOW
H,O
12 FUEL PRESSURE Regulator
PERKIN-ELMER

3-d''--

Figure 7-4 - Flowmeter-Type Gas Controls

FUEL PRESSURE Regulator - Controls pressure of fuel at the FUEL


FLOWmeter.
Oxidant Selector Valve - Selects oxidant and turns it on or OFF.
The burner head safety interlock pin must be properly installed
before the oxidant can be switched from AIR TO N2o. Although
the valve can be turned to the N2o position, N2o will not
flow unless the pin is installed.
FUEL Toggle Valve - Turns fuel gas on (straight out position)
and off (parallel to panel).
IGNITE Button - Momentary push button for the ignition of flame
gases. Ignition will occur only when the oxidant selector
valve is in the AIR position and the safety interlock pin
on the burner head hold-down cable is connected.
POWER Switch and Signal Light - Controls line power to the burner
regulator. When the regulator is connected to line power
and the POWER switch is in the ON position, the signal light
alongside is lit.

4/79
8 OPERATING INSTRUCTIONS
8A. SAMPLE ANALYSIS
The following steps summarize the basic analytical procedure
used with the Model 560. The steps below are explained in detail
in the sections that follow. Once the set up and analysis routines
become familiar, measurement will taken just a few minutes.
If an error message is displayed, refer to Section 12 for the
explanation.
1) Prepare samples and standards. Consult "Analytical Methods
for Atomic Absorption Spectroscopy", supplied with the instru-
ment for data on each element.
2) Plug in the power cord, turn the GAIN control fully counter-
clockwise, turn on the power, install the appropriate lamp
and burner head. (Refer to Section 8C~)
3) Turn the SIGNAL control switch to LAMP. Set the lamp current
(as read on the ENERGY/LAMP Meter) to the proper value with
the LAMP current control. (See Section 8C,6.)
4) Turn the SIGNAL control switch to SE"I' UP. Set the slit to
the proper value. Set the wavelength to the proper value,
and peak the wavelength setting. Align the lamp. Optimum
wavelength setting and lamp alignment are indicated by ENERGY/
LAMP meter needle movement to the right. Close the lamp
compartment door.
5) Set the SIGNAL control switch to CONC (EM CHOP for flame
emission measurements) and the MODE control switch to HOLD.
6) Set the BKGD CORR switch to AA. (To take background corrected
readings, see Section 8E,l.)
7) Set up the gas controls and ignite the gases. (Refer to
Section 8B.)
8) Select an integration time by entering the desired value
through the numerical keyboard and pressing the t key. (The
initial integration interval is set at 0.5 seconds when the
instrument is turned on.)
9) Aspirate a blank solution and press the AZ key to zero the
display.
10) To calibrate the instrument (see Section 8D):
a) Enter the desired value for Standard 1 through the numerical
keyboard and press the Sl key.
b) Repeat (a) for S2 and S3 if these standards are also used.
c) Aspirate Sl and press the Sl key.
d) Repeat (c) for S2 and S3, if used. The standards must
be aspirated in order of increasing concentration, when
calibrating the instrument.
8-2

11) Aspirate a sample solution and press the READ button. The
indicator dot above the READ button will be lit until measure-
ment is complete. The interval depends on the selection
made in step 8.

BB. BURNER REGULATOR OPERATION

8B,l. Operation of the Digital Burner Control System

Cautions: 1. Do not use oxygen in the burner.

2. Use new tubing only for lines supplying nitrous oxide


to the Burner Contror-and to the instrument. Do not, under
any circumstances, introduce nitrous oxide into gas lines
or equipment contaminated with oil. Nitrous oxide can cause
spontaneous combustion of oil with dangerously explosive
results.

Prepare the instrument, including the burner and nebulizer for


operation. Connect gas supplies to the Burner Control as de-
scribed in Section 2. Tables 8-1 and 8-2 and Figure 8-1 provide
data on pressure and flow settings for various fuel/oxidant com-
binations for the range of burner heads.

A. GAS ~RESSURE SETTINGS

Recommended tank outlet pressures are indicated in Table 8-1


for the commonly used gases. The maximum figures must not be
exceeded.

TABLE 8-1 - RECOMMENDED PRESSURE SETTINGS

GAS LINE OR TANK OUTLET PRESSURE

C2H2 6 69 kPa (10 psig)

H2 * 138 kPa (20 psig)

Air 275 kPa to 600 kPa max. (40 psig to 85 psig max.)

N 0 or Ar* 275 kPa to 600 kPa max. (40 psig to 85 psig max.)
2

*A speical accessory control is required for these gases.

4/79
8-3

z
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0
IO 0 IO 0 IO 0
(\J (\J

'U!W/l 'MOl.:I

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~
(X)

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tO en
!::::
(!)
0

[SJ IO Cl

z ~
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v a_
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ro
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0
ro
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Fig. 8-1 - Relationship between Actual Flow Rates and Displayed


Values
4/79
8-4

B. GAS FLOWS

The flow rates required for a "normal" flame will vary with the
type of burner head that is installed, the nature of the solvent,
and the fuel-oxidant combination in use. These factors are
summarized in Table 8-2. Values shown for flow are in arbitrary
units, corresponding to the values displayed on the Burner Control
displays. The relationship between "flow units" and flow rates
for different gases is shown in Figure 8-2.

TABLE 8-2 - FLOW SETTINGS FOR THE RANGE OF BURNER HEADS

Aqueous Solutions Organic Solutions


Burner Head Fuel Ox id. Fuel Ox id. Fuel Ox id.

10 cm (1 slot) C2H2 Air 30 55 18 55


(040-0266)

10 cm (3 slot) C2H2 Air 32 55 18 55


(040-0289)
H2 Argon* 20 60 - -
Nitrous Oxide C2H2 N 0 45** 40 33 40
2
(5 cm)
(040-0277) C2H2 Air 20 40 12 40

H2 Air 50 35 - -

* Use override
**Flow after automatic c 2 H2 boost

C. SETTING UP AND IGNITING THE FLAME

a) Air/Acetylene Operation

1) Set the POWER switch on the BURNER CONTROL unit to ON.


Switch the spectrophotometer on.

2) Verify that a suitable burner head is installed, and that


the drain is properly connected (Section 2). Ensure that
the burner head safety interlock pin is correctly installed.
When the installation is satisfactory the DRAIN light, and
the AIR HEAD light will turn on.

3) Set the acetylene tank output pressure to 69 kPa (10 psig).

Imlortant: Change the tank when the tank pressure


fa Is to 520 kPa (75 psig) . If the pressure falls
below this level, acetone may be carried over into
the burner regulator, possibly damaging valves and
tubing. Such damage is not covered by the instru-
ment guarantee.

4/79
2-8

c) Keep water in the drain tube trap and submerge the


end of the drain tube at least 13 cm (5 inches) in ./
the water (see Section 6C,l, step 5). Do not kink the
drain tube.
d) Do not leave the flame unattended.
2C,2. Burner-Regulator Operation - Burner-Regulator 303-0678
(Fig. 2-3A) and 303.:..0692 (Fig. 2-3B)

Prepare the burner-nebulizer for operation

Caution: DO NOT USE OXYGEN IN THE BURNER

If a nitrous oxide burner head is installed, refer to the instructions


(990-9631) supplied with the burner head.

Caution: Do not, under any circumstances, introduce nitrous


oxide into gas lines or equipment contaminated with oil.
Nitrous oxide can cause spontaneous combustion of oil, with
dangerously explosive results. Thoroughly degrease all lines
and equipment suspected of oil contamination before introducing
nitrous oxide into them.

Table 2-2 and Figure 2-5 provide data on pressure and flowrneter
settings for various fuel-oxidant combinations with Perkin-Elmer
burner heads.

a) Air-Acetylene Operation

1) Verify that a suitable burner head is installed in the burner


chamber and that the drain tube is properly installed (see
Sec. 6C,l, steps 5 and 6). For models with the burner head safety
interlock, make sure a single click is heard when connectin~ the
burner head interlock pin.

2) Make sure the FUEL SHUT OFF valve is in the closed (right
angle) position.

3) Set the acetylene cylinder regulator output pressure at


.85 kg/sq cm (12 psig).

4) Set the air supply output pressure at 2.8 to 5.2 kg/sq cm


(40 to 75 psig).

5) Turn the N2 0-AIR valve to AIR and set the N20-AIR PRESSURE
regulator for a gauge reading of 2.1 kg/sq cm (30 psi).

6) Set the AUXILIARY N2 0-AIR valve for a flowrneter reading of


9. 0.

7/74 \
2-9

7) Open the FUEL SHUT OFF valve and quickly set the FUEL
PRESSURE regulator for a gauge reading of .56 kg/sq cm
(8 psi). Then adjust the needle valve beneath the FUEL
FLOW flowmeter to bring the upper white (plastic) float
ball to read approximately 9.0 on the flowmeter.

8) Ignite the burner flame by pressing in the IGNITE button


and holding it in until the flame is lit.

9) Before shutdown, aspirate H2 o for a few minutes. If organic


solutions have been aspirated, follow the procedure in Sec.
3B,4 for cleaning the burner.
10) Close the FUEL SHUT OFF valve first, then turn the N20-AIR valve
to the OFF position. For models with the burner head safety inter-
lock, close the FUEL SHUT OFF valve first, and press in the Safety
Interlock Release button (item 8, Fig. 2-3B) before turning
the N20-AIR valve to OFF. If high concentrations of silver,
mercur~ or copper salts have been nebulized, follow the pro-
cedure in Sec. 3B,5.

b) Nitrous Oxide - Acetylene Operation

Note: For models with the burner head safety interlock, make
sure a double click is heard when connecting the burner head
interlock pin.

1) Set the nitrous oxide cylinder regulator pressure at 2.8 kg/sq cm


(40 psig).

2) Carry out steps 1 to 5 of the Air-Acetylene procedure.

3) Set the AUXILIARY N2 0-AIR valve for a flowmeter reading of 5.5.

4) Open the FUEL SHUT OFF valve and quickly set the FUEL PRESSURE
regulator for a gauge reading of .56 kg/sq cm (8 psi). Then
adjust the needle valve beneath the FUEL FLOW f lowmeter to
bring the lower (steel) float ball to read approximately 5.0
on the flowmeter.

5) Ignite the burner flame by pressing in the IGNITE button and


holding it until the flame is lit.

6) Turn the N 0-AIR valve quickly from AIR to N2o.


2
7) Adjust the flame as described in the instructions for the
N20 burner head (990-9631).

8) Before shutdown, aspirate H20 for a few minutes and turn the
N20-AIR valve quickly from N20 to AIR. If organic solutions
have been aspirated, follow the procedure in Section 3B,4 for
cleaning the burner.
5/74
2-10

9) Close the FUEL SHUT OFF valve first, then set the N2 0-AIR
valve to the OFF position. For models with the safety inter-
lock, close the FUEL SHUT OFF valve first, and press in the
Safety Interlock Release button (item 8, Fig. 2-3B) before
turning the N2 0-AIR valve to OFE'. If high concentrations
of silver, mercury or copper salts have been nebulized, follow
the procedure in Section 3B,5.

Table 2-2 - Initial Pressure and Flowmeter Settings

A. Pressure Settings

Gas Line or Cylinder Burner Regulator


C2H2 .85kg/sq cm (12 psig)
.56kg/sq cm (8 psi_g)
H2 1. 4 ( 2 0) 1. 06 (15)
C3Hg 0.7 (10) . 43 ( 6)
AIR 2. 8 - 7.0 (40-100) 2.1 (30)
N20 or ARGON 2.8 (40) 2.1 ( 3 0)

B. Flowmeter Settings - Burner-Regulator 303-0678 and 303-0692

Burner Ox id. Aqueous Organic


Fuel
Head Fuel Oxid. Fuel Ox id.

4-in. (1 slot) C2H2 AIR 9.0 9.0 3.0 6.0


(3 03-0418) H2 AIR 6.0* 4.0 --- ---
3-S lot C2H2 AIR 10.5 10.5 6.5 10.0
(3 03-0401) H2 ARGON 4.5 9.0 --- ---
C3H8 AIR 2.0 4.5 --- ---
Nitrous Oxide C2H2 N20 5.o* 5.5 4.0* 5.5
{303-0419) C2H2 AIR 5.0 6.0 3.0 5.0
2-in. ( 1 slot) C2H2 AIR 5 .5 6.0 3.0 5 .5
3 03-0420 H2 AIR 6.0* 4.0 --- ---

*Setting for the lower (steel) of the two flowmeter balls.

11/73
2-11

15
HYDROGEN
ACETYLENE (NYLON BALL)
(NYLON BALL) .56 Kg/sq cm
13 .56 Kg/sq cm
(Bpsig)
(Bpslg)

II
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9

0::
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4 8 12 16 20 24 28 32 36 40
LITERS /MINUTE

Fig. 2-5 - Flow Rates from Flowmeter Settings for Burner-


Regulator 303-0678 and 303-0692

2C,3. Adjusting the Flame

1) Allow three to five minutes warm-up of the burner system.


If the flame is uneven, shut it off and clean the burner
head slot (see Sec. 3B,l). Check the burner alignment
by following the procedure in Sec. 3B,l.

2) A fuel-lean (oxidizing) mixture gives a blue, hotter flame;


a fuel-rich (reducing) mixture gives a yellow, cooler flame.
Adjust the Auxiliary Oxidant (air or nitrous oxide) control
to provide the flame condition recommended in the Analytical
Methods Bood for the element to be determined.

Additional fine adjustments may be necessary to obtain optimum


sensitivity. Aspirate a standard of the element of interest
and adjust fuel or oxidant flow to obtain a maximum reading,
zeroing the readout with a blank solution after each adjustment.

5/74
8-5

4) Set the air supply pressure to between 275 kPa and 600 kPa
(40 to 85 psig).

5) Press AIR/C H 2 to select the desired gas combination.


2
The light to the left of the key will light.

6) Press CHK OXIDant, and set the displayed digits to the


desired value (refer to Table 8-2) using the knob below
the OXIDANT digits.

7) Press CHK FUEL and set the displayed digits to the desired
value (refer to Table 8-2) using the knob below the FUEL
digits.

8) Press FLAME ON/OFF to ignite the flame. An automatic


sequence starts the gases flowing for a pre-determined
period before ignition occurs.

Note: When gases are connected the flame may not


1T9ht the first time owing to air in the supply
lines. Repeat the ignition procedure until the
flame ignites.

9) After flame ignition, allow the burner head to warm up.


The flame should appear uniform and stable throughout
its length. If it is not, cleaning of the burner or
burner head may be required, as described in the
spectrophotometer instructions (refer to "Maintenance").

10) If necessary, reset the acetylene pressure to 69 kPa


(10 psig).

b) Nitrous Oxide/Acetylene 0peration

1) Set the POWER switch on the BURNER CONTROL unit to ON.


Switch the spectrophotometer ON.

2) Verify that the N 0/C?.H 2 burner head (Part No. 040-0277)


2
is installed, and thaE the drain is properly connected
(Section 2). Ensure that the burner head safety interlock
pin is correctly installed. When the installation is
satisfactory the DRAIN light and the N o HEAD light will
2
turn on.

3) Set the acetylene tank output pressure to 69 kPa (10 psig).

Imortant: Change the tank when the tank pressure


lalis to 520 kPa (75 psig)~ If the pressure falls
below this level, acetone may be carried over into
the burner regulator, possibly damaging valves and
tubing. Such damage is not covered by the instrument
guarantee.

4/79
8-6

4) Set the air supply to between 275 and 600 kPa (40 to 85
psig) .

5) Set the nitrous oxide tank output regulator to between


275 and 600 kPa (40 to 85 psig).

6) Press N o;c H 2 to select nitrous oxide operation. The


2 2
light to the left of the key will light.

7) Press CHK OXIDant, and set the displayed digits to 40


using the knob below the OXIDANT digits.

8) Press CHK FUEL and set the displayed digits to 45 (boosted


c 2 H2
setting) using the knob below the FUEL digits.

9) Press FLAME ON/OFF to ignite the flame. An automatic


sequence starts the gases flowing for a pre-determined
period before ignition occurs. An air/acetylene flame
is automatically followed by a switchover to N o;c H
2 2 2
after 15 seconds.

Note: When gases are first connected, the flame may


not"'light for the first time owing to air in the supply
lines. Repeat the ignition procedure until the flame
ignites.

10) After flame ignition, allow the burner head to warm up.
The flame should appear uniform and stable throughout
its length. If it is not, cleaning of the burner or
burner head may be required, as described in the
spectrophotometer instructions (refer to "Maintenance.")

Note: If it is desired to switch to N o;c H opera-


2 2 2
tion after first using an air/C H flame, use the
2
following procedure. With an airJC/.H flame burning,
2
set the c 2 H? flow to 20 units and tfie air flow to
40 units. Press the N o;c H key. The acetylene
2 2 2
flow will be boosted automatically to approximately
45 units, and the oxidant selector will switch auto-
matically from air to N o.
2
D. FLAME FLOW ADJUSTMENTS

Once the flame is ignited, the fuel and oxidant gas flows may
be adjusted if desired. With air/acetylene, a fuel-lean (oxidizing)
mixture gives a blue, hot flame; a fuel-rich (reducing) mixture
gives a yellow, cool flame. An N o;c H 2 flame should have a
2 2
rose-red inner core approximately 1 to 2 cm (1/2 to 3/4-in.)
high. Any other adjustment to flow requires that measurements
be taken, as described in the instrument optimization procedures.

4/79
8-7

E. FLAME SHUTDOWN PROCEDURE

1) When the analyses are complete, and before shutting down


the flame, aspirate water for a few minutes. If organic
solutions have been aspirated, follow the cleaning procedures
outlined in the instrument manual to clean the burner.

2) Press FLAME OFF to extinguish the flame. The system follows


a predetermined shutdown sequence to extinguish the flame
safely.

Caution: Unstable acetylides, which are especially


11kery to explode when permitted to dry may be
formed when nebulizing high concentrations of silver,
copper or mercury salts in an acetylene flame.
Thoroughly flush the burner mixing chamber and waste
drain tubing with water immediately after this kind
of analysis and inspect the burner mixing chamber
visually to be sure all traces of residue have been
removed.

3) At the end of the working day, or if the instrument is to


be idle for an extended period of time, close the acetylene,
nitrous oxide (if in use) and air s_ylinder (tank) valves.
Then press CHK OXID and CHK FUEL long enough to depressurize
the acetylene, nitrous oxide and air lines.

8B,2. 0.P..eration of the Flowmeter Gas Control System

Prepare the burner for operation.

Cautions:: 1) Do Not Use Ox_ygen in the Burner.

2) Use new tubing for lines supplying nitrous oxide to


the burner regulator and the instrument. Do not, under
any circumstances, introduce nitrous oxide into gas lines
or equfpment contaminated with oil. Nitrous oxide can
cause spontaneous combustion of oil, with dangerously
explosive results.

Table 8-3 and Figure 8-2 provide data on pressure and f lowmeter
settings for various fuel-oxidant combinations with Perkin-Elmer
burner heads.

a) Air/Acetylene (Air/C H ) Operation


2 2

1) Verify that a suitable burner head is installed in the


burner chamber and that the drain tube is properly in-
stalled (see Sec. 2B,3 and Sec. 8C,2). Make sure the
safety interlock pin is installed.

4/79
8-8

TABLE 8-3 - INITIAL PRESSURE AND FLOWMETER SETTINGS

A. Pressure Settings

Gas Line or Cylinder Burner Regulator

C2H2 82 kPa (12 psig) 55 kPa (8 psig)

H2 140 kPa (20 psig) 100 kPa (15 psig)

c 3 H8 70 kPa (10 psig) 40 kPa (6 psig)

AIR 340 - 590 kPa (50-85 psig) 210 kPa (30 psig)
-
N 0 or ARGON Z80 kPa (40 psig) 210 kPa (30 psig)
2

B. Flowmeter Settings

Burner Fuel Ox id Aqueous Solns. Organic Solns


Head Fuel Oxid. Fuel Oxid.

4-in. (1 slot) CzHz AIR 32 55 13 37

(040-0Z66) H2 AIR 60 28 - -

3-Slot CzH2 AIR 45 70 30 60

(040-0Z89) Hz ARGON 20 60 - -

C3H8 AIR 9 29 - -

Nitrous Oxide C2HZ N 0 55* 40 52 38


2
(040-0Z77) C2HZ AIR 25 40 15 28

2-in. (1 slot) CzH2 AIR 25 40 15 28

(040-0Z90) Hz AIR 50 40 - -

*Trri'al flow (start at 25 when switching from air to N2o fuel


flow will automatically be boosted to 55)

4/79
~mmh1mm~~mm-fat1-~~m~-.l- BURNER-REGULATOR '-
::::i:::::::<:t:::i::;:,::=:. . ,.=7"='~ GAS FLOW CALIBRATION __
8oJtill.illlli1~~~~~~~~~~~~~~~~~~~~!11ifil~~~filfilfilttffiiliilijftili
70------+-----~

en
z
0
en
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0
a:::
w
; 1~ 11~~mw~~~~::~~JH~~~~@~iruJ@1 I
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0
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LL

0 2 4 6 8 10 12 14 16 18 20 22 24 26 28 30 32

GAS FLOW (liters/minutes)

Fig. 8-2 - Flow Rates from Flowmeter Settings


(Flowmeter-Type Burner Control)
4/79
8-10

2) Make sure the FUEL Toggle valve is in the closed


(parallel to panel) position.

3) Set the acetylene cylinder regulator output pressure


at 80 kPa (12 psig)

Important: Change the tank if the pressure in the


acetylene cylinder falls below 520 kPa (75 psig).
If the tank is not changed when the pressure drops to
this level, acetone which can damage valves or tubing,
may be carried into the burner regulator. Such damage
is not covered by the instrument guarantee.

4) Set the air supply output pressure at 280 to 550 kPa


(40 to ~o psig).

5) Turn the Oxidant Selector valve to AIR. Set the OXIDANT


FLOW needle valve for a flowrneter reading of 55*.

6) Adjust the FUEL FLOW needle valve to bring the float ball
to approximately 32* on the flowmeter.

7) Ignite the flame by pressing the IGNITE button and holding


it until the flame is lit. After ignition, minor adjust-
ments in the flame condition may be necessary. (See
Section 8B,3.)

8) Before shutdown, aspirate H o for a few minutes. If


2
organic solutions have been aspirated, follow the pro-
cedure in Sec. lOB,3 for cleaning the burner.

9) To extinguish the flame, close the FUEL Toggle valve


first, then turn the N2 0-AIR valve to the OFF position.

Caution: Unstable acetylides, which are especially


likely to explode when permitted to dry, may be
formed when nebulizing high concentrations of silver,
copper, or mercury salts in an acetylene flame.
Thoroughly flush the burner mixing chamber and waste
drain tube with water immediately after this kind of
analysis and inspect the burner mixing chamber visually
to be sure all traces of residue have been removed.
(See Section lOB,4.)

*These settings are for use with the single-slot, 4-in. burner
head.

4/79
8-11

10) Close the acetylene cylinder valve and open the FUEL
Toggle valve to bleed the acetylene line until the
gauges on the acetylene cylinder read zero, then close
the FUEL Toggle valve.

b) Nitrous Oxide/Acetylene (N 2 o;c 2 H2 ) Operation

1) Set the nitrous oxide cylinder regulator pressure at 280 kPa


( 40 ps ig)

2) Carry out steps 1 to 4 of the Air/Acetylene procedure, mak-


ing sure a nitrous oxide/acetylene burner head is properly
installed.

3) Turn the Oxidant Selector valve to N


2
o.
4) Set the OXIDANT FLOW needle valve for a flowmeter reading
of 35.

5) Turn the Oxidant Selector valve to AIR

6) Open the FUEL Toggle valve and adjust the FUEL FLOW needle
valve to bring the float ball to approximately 25 on the
flowmeter.
7) Ignite the burner flame by pressing in the IGNITE button
and holding it in until the flame is lit.

8) Allow the burner head to warm up for a few minutes then,


turn the Oxidant Selector valve quickly from AIR to N2o.
The acetylene flow is automatically increased. After
switcho.ver, minor adjustlflents in the flame condition
may be necessary. (See Section 8B,3.)

9) While aspirating a standard solution of the element to be


determined, adjust the fuel flow to obtain maximum absorption.

10) Before shutdown, aspirate water for a few minutes then turn
the oxidant selector valve quickly from N2o to AIR. If
organic solutions have been aspirated, follow the procedure
in Sec. lOB,3 for cleaning the burner.

11) To extinguish the flame, close the FUEL Toggle valve


first, then set the oxidant selector valve to the OFF
position.

Caution: Unstable acetylides, which are especially


likely to explode when permitted to dry,. may be
formed when nebulizing high concentrations of silver,
copper, or mercury salts in an acetylene flame.
Thoroughly flush the burner mixing chamber and waste
drain tube with water immediately after this kind of
analysis and inspect the burner mixing chamber visually
to be sure all traces of residue have been removed.
(See Section lOB,4.)

4/79
8-12

12) Close the N o and acetylene cylinder valves, then set the
2
oxidant selector valve at N o and turn on the FUEL Toggle
2
valve on the gas control unit to bleed the N o acetylene
2
lines. Close the oxidant selector valve and the FUEL Toggle
valve when the gauges on the N o and actylene cylinders read
2
zero.

8B,3. Adjusting the Flame

a) Air/Acetylene

1) Allow several minutes warm-up of the burner system. If


the flame is uneven, shut it off and clean the burner
head slot (see Section lOB,2). Check the burner alighment
by following the procedure in Sec. 8C,7.

2) A fuel-lean (oxidizing) air/acetylene mixture gives a


blue, hotter flame; a fuel-rich (reducing) air/acetylene
mixture gives a yellow, cooler flame. Adjust either the
OXIDANT FLOW or the FUEL FLOW control to provide the flame
conditions recommended in the Analytical Methods Manual
for the element to be determined.

b) Nitrous Oxide/Acetylene

Adjust the FUEL FLOW Needle valve until the reaction zone
(rose red inner cone) of the flame is 1 to 2 cm (1/2 to
3/4 in.) high. The outer zone {plume) will be 30 to 35 cm
(12 to 14 in.) high.

Note: When first ignited, the flame may separate or split


forming a "V" along the burner slot if the burner head
did not reach an equilibrium temperature with air/acet-
ylene operation. As the fuel flow is adjusted and the
burner head warms up, the "V" will close and form a normal
flame suitable for analysis. This may take several minutes.

Additional fine adjustments may be necessary to obtain optimum


sensitivity. Aspirate a standard solution of the element of
interest and adjust the fuel or oxidant flow to obtain a maximum
reading. Zero the meter with a blank solution after each adjust-
ment.

4/79
8-13

8C. PRELIMINARY INSTRUMENT PROCEDURES

8Ctl. Analytical Methods Manual

Ref er to the "Analytical Methods for Atomic Absorption


Spectroscopy" (303-0152) section on Standard Conditions
for data on lamp source, wavelength and slit settings,
fuel and oxidant control settings., Chemical glassware,
reagents and other materials used in sample preparation
will be required, and samples and standards can be pre-
pared as discussed in the Analytical Methods manual.

8Ci2. Burner Head Installation

Install the burner head recommended in Table 8-2 or 8-3B


for the fuel/oxidant combination used as follows:
1) Push the head into the chamber (see Fig. 10-1) so
that the slot in the base of the head engages the
positioning pin on the left side of the burner chamber
neck .. Tighten the retaining ring (item 16, Fig. 10-1).

2) Connect the burner head hold-down cables (item 5, Fig.


8-4) to the retaining clips below the burner chamber.
i

3) Insert' the safety interlock pin into the safety interlock


at the base of the burner compartment as shown in Fig.
2-4.

8C,3. Organic Solvents

If organi~ solvents are to be used, see the General Information


section in the Analytical Methods Manual and "Burner Operating
Notes - Using Organic Solvents".

Aspirated organic solvents tend to increase the yellowness of


the flame. It is desirable to compensate by reducing fuel flow
and also oxidant flow.

Burn organic solvents as follows:

1) Replace the standard gasket, 040-1276 (Fig. 10-1, item 3),


in the burner mixing chamber with Corkprene gasket 040-1277,
provided.

Use the following procedure for the standard burner head


(040-0266) only.

2) Light the burner and set the air flow to 55.

3) Set the fuel flow at 32.

4/79
8-14

4) Aspirate an organic solution and adjust the fuel flow


until the flame is as blue as possible without lifting
off the edges of the burner head.

If other burner heads are used, light the flame with the flows
specified for the particular head in the Analytical Methods
Book. Reduce the fuel flow until the flame is as blue as
possible without lifting off the edges of the burner head.

After completing work with organic solutions, replace the


standard chamber gasket (item 3, Fig. 10-1).

Use the recommended burner cleaning procedure in Section


lOB,3 after aspirating organic solutions.

8C,4. Corrosive Solutions

If highly corrosive solutions are to be used, replace the


standard nebulizer with the accessory corrosion resistant
nebulizer (303-0404). See Section lOC,2 for instructions
on changing the nebulizer.

8C,5. Lamp Installation


and Alignment (See Fig.
8- 3)

Install the recommended


lamp source:

1) Position the lamp so that


it is held by the two
springs in the lamp holder.
The--focus of the optical
system is located in the
plane defined by the axes
through the centers of
the two lamp alignment
knobs. All source lamps
should be positioned so
that the light emitting
portion is in that plane. 1 Pin
Perkin-Elmer Intensitron 2 Hold-down Screw
hollow cathode lamps are 3 Alignment Knobs
correctly positioned when 4 D Attenuator Control
2
the alignment knobs on the 5 Retaining Spring
lamp holder are centered 6 Lamp Connector
7 Photometer Screws

Fig. 8-3 - Lamp Compartment


4/79
8-15

between the two mica wafers in the lamp. Perkin-Elmer


electrodeless discharge lam s should be positioned with
the connector end 7 cm 2 3 4 in) from the center axis
through either alignment knob.

2) Open the lamp compartment door, loosen the hold-down screw


(item 2, Fig. 8-3), and push the lamp holder against both
stops in the lamp compartment floor. The forward stop must
be in the base of the holder. Secure the holder with the
front and rear hold-down screws.

3) Turn the LAMP current control fully counterclockwise.

4) Plug in the lamp connector.

8C,6. Control Settings

1) Make the following control settings:

Right Panel Left Panel

POWER - ON AA/BG Switch - AA


SIGNAL - LAMP GAIN - Turn fully counterclockwise
2) Turn the LAMP current control clockwise until the ENERGY/
LAMP meter shows the proper value indicated on the lamp
label for continuous or DC operation. One meter division
equals 1 mA. (The element source lamp in the spectro-
photometer is continuously (D.C.) powered.) Depending
on the age of the lamp used, the correct current setting
is listed either as 11 continuous 11 , 11 303/3 05/3 06/ 4 03 11 ,
11
303/403 11 or 11 303 11 on the lamp label.

3) Change the SIGNAL control switch to SET UP. Set the slit to
the proper value. Adjust the COARSE ADJUST wavelength control
to obtain the correct setting on the WAVELENGTH counter. (See
the Analytical Methods Manual for proper slit and wavelength
settings for the element of interest.)

4) Turn the FINE ADJUST wavelength control slowly to obtain


the maximum needle deflection to the right on the LAMP/
ENERGY meter. If necessary, adjust the GAIN control while
turning the FINE ADJUST waveletigth control to keep the
needle on scale.

5) Turn the two alignment knobs on the lamp holder (Fig. 8-3)
to maximize (needle to the right) the ENERGY/LAMP meter
reading (lamp emission).
6) Close the lamp compartment door.
4/79
8-16

8C,7. Burner Alignment

When the burner is correctly


aligned, the slot in the
burner head is parallel to
and slightly below the
sample beam.

l~ Set the SIGNAL control


to ABS, set the MODE
switch to CONTinuous
and set the display to
zero with the AZ key.
Set the integration
time to 0.5 sec. by
entering 0.5 on the
keyboard, then de-
pressing the t key.

2) Raise the burner head


with the Vertical Adjust
Knob (item 7, Fig. 8-4)
until absorption is
indicated on the display.

3) Slowly lower the burner


head with the Vertical
Adjust Knob until it is
just below the source
beam (with the display
again at zero). 1 Screw Holes for Microsampling
Accessory Mount
4) Ignite the gases accord- 2 Screw Holes for HGA-2100 Mount
ing to the procedure in 3 Photometer Windows
Section 8B,l or 8B,2. 4 Retaining Ring
5 Hold-down - Safety Interlock Cable
5) Aspirate a standard 6 Rotational Adjust Knob
which provides an 7 Vertical Adjust Knob
absorbance of 0.2 to 0.6 B Horizontal Adjust Knob
absorbance units, and
adjust the position of Fig. 8-4 - Burner Compartment
the burner head by turn-
ing the Horizontal Adjust Knob (item 8, Fig. 8-4) until the
maximum absorbance is indicated.

6) Turn the Rotational Adjust Knob (item 6, Fig. 8-4) to obtain


maximum absorbance.

Note: Ordinarily, the horizontal and rotational align-


ment procedures need be carried out only when changing
burner heads.
4/79
8-17

BC,8. Nebulizer Adjustment

The nebulizer will require adjustment if it is dismantled, or


if it is necessary to restore normal functioning of the instru-
ment, or to optimize performance when changing solvents.

To adjust the nebulizer:

1) Prepare the spectrophotometer for sample aspiration as


described earlier in this section. Select an element
that requires a blue (oxidizing) air/acetylene flame and
a WAVELENGTH control setting ahove 250 nm (refer to the
Analytical Methods Manual). Recommended elements are
Cu, Mg, Ni (341.5 nm), Pb (283.3 nm). Do not use Ca,
Sr, Ba, Pd, Pt, Rh, Ru, Au or Ir, or other elements
whose absorbance is sensitive to changes in the fuel-
air ratio.

Important: Do not adjust the nebulizer when


using a nitrous oxide-acetylene flame.

2) Aspirate a standard. Keep the free end of the sample


capillary in the standard. Loosen the locking ring
(item 12, Fig. 10-2) and slowly turn the knurled
nebulizer knob (item 1, Fig. 10-2) counterclockwise.
Stop turning the knurled knob when the nebulizer air
blows back into the standard (small bubbles appear
at the end of the capillary tubing in the standard) .

3) Keep the end of the capill~ry in the standard and


slowly turn the knurled knob clockwise. Watch the dis-
play while turning the knob; the reading will increase
as aspiration begins. Continue to turn the knob clock-
wise slowly until the reading displayed stops increasing
and starts to decrease. This reversal indicates the
point of maximum absorption. Return to this setting
and turn the locking ring against the knob to lock the
setting.

8C,9. Warm-Up

For most analyses, operation of the instrument may begin


without lamp warm-up. The double beam and automatic gain
control features compensate for most variations in the lamp
output. Whert using electrodeless discharge lamps (EDLs)
allow 5 to 10 minutes warm-up.

4/79
8-18

8D. CALIBRATION
8D,l. Introduction
The readout of the Model 560 may be calibrated directly in units
of concentration using a two-step process. First, enter the
concentrations(s) of the standard(s) being used. Second, aspirate
a blank plus each standard and press the appropriate standard
button. The System equates the absorbance of each standard with
the actual concentration, and constructs an appropriate calibration
curve.
The selection of the number of standards, and their concentrations,
is most important. Some useful guidelines are given below.
8D,2. Selecting the Number of Standards
The Standard Conditions pages of the Analytical Methods manual
indicate the linear working range for each element (i.e. the
concentration range over which absorbance is linearly proportional
to concentration).
a) If the analyte concentration of all the samples to be analyzed
falls within the linear range, then calibration should be
performed with a single standard.

0.4 0.4

0.3 0.3

w w
u u
z z
<! <!
~ 0.2 ~ 0.2
0 0
en en
CD CD
<! <!

0.1 0.1

0 2 3 4 0 2 3 4
CONCENTRATION CONCENTRATION

Fig. 8-SA - One Standard - Fig. 8-SB - Three Standards -


Linear Plot S-Shaped Plot (Calibration Error)

4/79
8-19

b) If the analyte concentration in the samples is expected to


exceed the linear range, then either two or three standards
are recommended, depending on the degree to which the linear
range is exceeded. As a general rule, if the analyte con-
centrations are expected to be less than three times the
linear range, two standards are adequate. If the concen-
trations are expected to exceed three times the linear range,
use three standards*.
It is important to note that it is not necessarily an advantage
to use more standards than the number recommended, and sometimes,
the use of too many standards could give rise to erroneous or
misleading results. For example, when operating within the
linear range, one standard will give a linear plot as shown in
Figure 8-SA. If three standards are used over the same range,
the resulting calibration curve could appear S-shaped, as shown
in Figure 8-SB, and will not be accepted. The Model 560 is
programmed to recognize invalid calibration attempts, and will
display an error message when such an attempt is made. A full
explanation of calibration errors is given in Section 12.
8D,3. Selecting the Concentrations of Standards
If one standard is to be used, the concentration of Sl should
be higher than the most concentrated sample, and should not
exceed the upper limit of the linear range. The calibration
curve then becomes a straight-line plot, with the autozero point
as the origin.
If multiple standards are to be used, the selection of their
concentrations usually depends on .whether the analyst requires
a constant maximum relative error, or a constant maximum absolute
error. With the former, all results will be accurate to within
a specified percentage of the analyte concentration. With the
latter, all results will be accurate to within a specified con-
centration over the selected concentration range.
For constant maximum relative error, select the number of standards
required, with concentrations such that
S2 has 3x the concentration of Sl
and S3 has 2x the concentration of S2.

*With three standards it is frequently possible to determine


accurately analyte concentrations up to ten times the limit
of the linear range, and in some cases even higher concentrations
can be determined. However, the accuracy of the determinations
may be degraded if too large a concentration range is used.
If the accuracy obtained is insufficient, a change in analytical
conditions may be required. For example, one of the alternative
wavelengths given in the Analytical Methods manual may provide
lower sensitivity, or the burner head may be rotated to reduce
sensitivity, or the samples may have to be diluted further.

4/79
8-20

Regardless of whether two or three standards are used, the most


concentrated standard should have equal or greater concentration
than the most concentrated sample.

For constant maximum absolute error, the standards should be


equally spaced over the concentration range expected, i.e. S2
= 2 x Sl, and S3 = 3 x Sl. Again, the most concentrated standard
should have equal or greater concentration than the most con-
centrated sample.

8D,4. Calibration Procedure For Flame Analyses

1) Make up the appropriate numbers of standards, with the re-


commended concentrations.

2) Set up the instrument as described in Section 8C.

3) Select CONC and HOLD.

4) Enter the concentration of the first (lowest concentration)


standard, and press Sl. Then enter the concentrations of
S2 and S3, if multiple standards are to be used.

Notes: (A) Four full digits may be entered, and a decimal


point, to set any value between .0000 and 9999. If re-
quired, two additional leading zeroes are permitted before
the four digits in order to position the decimal, e.g.
values of .001234 or 0.01234 are permitted.
(B) The number of decimal places in the result is deter-
mined by the position of the decimal in the entry of Sl.
However, the position of the decimal for S2 and S3 is also
determined by the entry for Sl, so the values of the other
standards must be considered when entering the value for
Sl. For example, if Sl were 5.000, than S2 could not be
entered as 10.0, as this would in effect be a 5-digit
number (10.000) and only 4 digits are allowed (see Note
(A) above). Sl should have been entered as 5.0 or 5.00.
(C) The concentration entries for Sl, S2 and S3 must be
entered in order of increasing concentration.

5) Key in the desired integration time and press T.

6) Aspirate a blank solution and press the AZ key to initiate


the READ cycle. Continue to aspirate the blank until the
AZ indicator stops flashing and the READ light goes out.

4/79
8-21

0.5
0.7

0.4 0.6

Sl 0.5
w w
~ 0.3 u
<! ~ 0.4
ID
0:: ID Sl
0
gi 0.2 s:
0::

ID
0.3
<!
<!
0.2
0.1
0.1
A/Z A/Z
0 2 3 4 0 2 3 4 5 6 7 8 9
CONCENTRATION CONCENTRATION

Fig. 8-6 - Calibration Curve Fig. 8-7 - Calibration Curve


Using a Single Standard Using Two Standards

7) Aspirate the first standard and press Sl to start the READ


cycle. When the READ indicator is extinguished and the Sl
lamp stops flashing and remains on, calibration using Sl
is established (Figure 8-6).

8) If two standards are being used, aspirate S2 and press S2


to start the READ cycle. When the READ indicator is extinguished
and the S2 lamp stops flashing and remains on, calibration
using S2 is established. (See Figure 8-7.)

9) If a third standard is being used, establish calibration


for S3 as described in step 8. Figure 8-8 shows a typical
three-standard calibration curve.
Note: Standards must be aspirated in order of increas-
ing concentration-;-and their concentrations must be
entered in the same sequence. If an error message is
displayed refer to Section 12.

With the appropriate calibration curve established, the Model 560


is able to convert non-linear absorbance readings of the samples
directly into concentrations which are then displayed.

4/79
8-22

1.8
SLOPE = Original Calibration Factor r"
r
1.5

S2 7
7,,,/y-
r

,
w 1.2 ~ S2
7
u
z z
<t <t
~ 0.9 00
0::
0 0
(f) (f)
00 00
<t 0.6 <t
Sl

A/Z
0 4 12 24 0 8 16
CONCENTRATION CONCENTRATION

Fig. 8-8 - Calibration Curve Fig. 8-9 - Resloping Example


Using Three Standards

8D,5. Calibration For Fast Peak Measurements

Peak height or peak area measurements are calibrated to read


in units of concentration in the same way as the CONT and HOLD
modes are calibrated, but with a slight difference.

First, enter the values for Sl, S2, and S3 in the usual manner.
Then, analyze the AZ, Sl, S2, or S3 standard as appropriate,
pressing the READ key to obtain the absorbance reading. When
the READ indicator goes out and a value is displayed, press the
corresponding AZ, Sl, S2 or S3 key to cause calibration to take
place.

8D, 6. Re slope

The "Reslope" facility of the Model 560 enables the slope of


the calibration curve to be adjusted, without the necessity of
running all the calibration standards again.

In the normal calibration operation, the system computes an


equation where concentration is a function of absorbance:

C = f (A)

where C=concentration, A=absorbance and f represents the


functional relationship between concentration and absorbance.
In Reslope, the equation is modified to:

C = K f (A)

4/79
8-23

where K is the reslope factor necessary to restore the function


to its original value following a change in slope.

Note: The Reslope facility is designed to compensate for


small changes in sampling conditions, such as flow changes
or nebulizer adjustments, or matrix differences between the
standards used to set up the calibration and the samples.
If larger changes occur, resloping will improve the results,
although a complete recalibration may be advisable in such
cases.

The Reslope facility may be used at any stage during the analysis
of samples, to ensure that the calibration curve is still appli-
cable*. For example, if for any reason the physical properties
of the samples is thought to be changing (through evaporation
or some other reason) leading to a slight general change in
concentration, then the Reslope facility may be useful.

Before Resloping it is advisable to auto zero, in case the base-


line has drifted. Therefore, proceed as follows:

1) Aspirate a blank (preferably the same blank as before) and


press AZ. Continue to aspirate until the READ indicator
is extinguished and the AZ indicator stops flashing.

2) Enter the concentration of the standard to be used for Reslop-


ing. It is recommended that this standard be somewhere in
the middle of the concentration range. For example, if three
standards are being used, then 82 would be useful as the
Reslope standard, being approximately half the concentration
of 83. To enter the concentration of the Reslope standard,
key in the concentration value and press RSLP.

3) Aspirate the Reslope standard and press RSLP. Continue to


aspirate the standard until the RSLP lamp stops flashing
and stays on, and READ is extinguished. The System has now
redefined the slope of the calibration curve based on the
single RSLP determination (see Figure 8-9).
8D,7. Expansion

The absorbance reading is multiplied by an expansion factor to


obtain the displayed result. This expansion factor may either
be entered via the keyboard, or computed automatically by the
system. It is important to differentiate between the two.

*For a single-standard calibration (Sl only) it is unnecessary


to use the Reslope facility, as recalibration using Sl will
work equally well. However, Reslope may be used if desired.

4/79
8-24

A) Computed Expansion During Calibration

In the CONC or EM SIGNAL mode, the absorbance reading is


multiplied by a computed expansion factor to produce the
concentration reading. The decimal point is ignored when
determining the expansion factor. The maximum permitted
expansion factor is lOOx.

For example, if a standard Sl has a concentration of 40.


ppm (as entered on the keyboard) and gives a measured ab-
sorbance of 0.008, then the instrument will compute an ex-
pansion factor of 40+ 8 = 5, and will display the result
as 40 ppm. However, if the concentration of Sl was entered
as 40.0, the instrument would compute an expansion factor
of 400 + 8 = 50, and the result would be displayed as 40. 0
ppm. Thus, entering 40.00 as the concentration of Sl would
produce an expansion factor of 500, and the instrument would
display an error code E-10 (overexpand).

The computed expansion factor may be displayed by pressing:

lcHKj (ExPj
The expansion factor is only meaningful if the plot is linear,
i.e. one expansion factor applies throughout the calibration
range. {This implies that only a single-standard calibration
will produce a useful expansion factor). If the calibration
curve is non-linear, the Model 560 will display only the
expansion factor computed for Sl.

B) Scale Expansion Factors, Entered Via the Keyboard

A scale EXPansion factor may be entered directly, via the


keyboard, by keying in the desired expansion factor (between
O.OlX and lOOX) followed by EXP.

Such an entry overrides any computed calibration curve.

IN CONC or EM, the instrument will multiply every subsequent


absorbance reading by this value.

In the ABS mode, the EXPansion factor entered via the key-
board is not implemented immediately, but is stored pending
the selection of the CONC or EM mode.

For an explanation of the error codes that may occur during


calibration, refer to Section 8D,8 and Section 12.

4/79
8-25

8D,8. Errors That May Occur During Calibration

If an error occurs during calibration, the instrument will dis-


play the appropriate error message and wait until corrective
action is taken by the analyst. The error message must be cleared
by pressing CE. The following is a detailed explanation of cali-
bration errors and their most common causes.

A) Expansion Factor Greater Than 100 (ElO)

When a standard is aspirated, an ElO error will be displayed


if the instrument is required to compute an expansion factor
greater than lOOx. This error code is rare, and usually
only happens when the blank is aspirated accidentally instead
of the standard. For example, if the concentration is entered
as 1000. and the measured absorbance is 0.005, the calculated
EXPans ion factor would be 1000 + 5 (ignoring the decimals)
= 200x. As the maximum permitted EXPansion is lOOx, an ElO
will be displayed. In general, the reasons for this kind
of ElO are:

a) The standard is far too dilute for the concentration value


that has been entered (e.g. blank is being aspirated
instead of the standard).

b) The sensitivity of the system is too low. Ensure that


the burner and nebulizer are adjusted correctly for maximum
absorption. Perform SET UP and ensure that the lamp
alignment is correct. Also, verify that the correct
wavelength has been used.

c) The concentration value entered was too high. Press CHK


and the relevant standard key to verify that the correct
entry was made.

Note: If the System can reduce the EXPansion by ignor-


ing one or more of the least significant digits after
the decimal, it will do so. In the above example,
no error is produced if the concentration entry is
1.000, 10.00 or 100.0 as the System will interpret
these values as 1.00, 10.0 or 100.

An ElO will also be displayed if an attempt is made to


expand a negative absorbance value, and again it probably
means that the wrong standard has been aspirated. (A
negative absorbance means that the sample has less absorption
than the blank used for autozero).

4/79
8-26

B) Standards Out of Sequence (Ell)

The concentration values must be entered in order of increas-


ing concentration and the standards must be aspirated' in
the same sequence.

C) S-Shaped Calibration Curve (El2)

In some instances it is possible for the data to describe


an S-shaped curve (see Figure 8-5). If this occurs, the
System will not establish calibration using the most recently
determined standard, and El2 will be displayed.

The most frequent causes of this error are the use of too
many standards within the linear range and improperly pre-
pared standards.

D) Reslope Standard Out of Range (El3)

If the absorbance of the standard used in Reslope is higher


(+5%) than the absorbance of the most concentrated standard
used in the initial calibration, an E-13 error will be dis-
played. For best results the Reslope standard should be
approximately in the middle of the calibrated range.

E) S2, S3 Values Do Not Follow Sl Format (El4 and E59)

As described in Section 8D,4, the value entered for the con-


centration of Sl determines the number of digits that may
be entered for 82 and S3.

For example, if Sl is entered as:

5.000 (which is equivalent to 4 digits.)


then 10.0

will not be accepted as the value of S2, as this is interpreted


as a 5 digit number. Sl should have been entered as 5.00
or 5.0. An E59 will be displayed in this case.

If Sl, S2 and S3 are entered correctly, for example:

Sl 5.00
S2 10.00
S3 20.00

and used to calibrate, then changing Sl to 6.000 will cause


an El4 to be displayed if recalibration using S2 and S3 is
attempted.

4/79
8-27

8D,9. Averaging and Statistical Operations

A) Averaging

The Model 560 has the facility to take a predetermined number


of readings, average them and display the result or print
the result on an external printer. When the number on the
display is an averaged result the AVERAGE light comes on.
On an external printer the letters AV are printed next to
the averaged result; a sequence number is printed for the
average only, and not for the individual results. To initiate
averaging, proceed as follows:

1) Enter the number of determinations for which the average


is required, by pressing:

Number of results)
( to be averaged (n)
2 to 99

2) If the results are to be printed on a PRS-10 Printer


/Sequencer, enter:

(Starting Sequence)
Number IPRNTI
The PRNT indicator will light.

3) Aspirate the sample:

a) In the CONT mode, the Model 560 will take the required
number of results and then calculate and display the
average automatically. If PRNT is pressed the in-
dividual readings and averaged results will be printed.

b) In the HOLD mode, press the READ key once to initiate


'n' readings. The average will then be calculated,
displayed and printed.

c) In the PK HT or PK AREA modes, press the READ key


n times to take n readings. After the nth reading
the average is calculated, displayed and printed.

Note: If a standard is aspirated instead of a


sample, and the relevant standard key (Sl, S2 or
S3) is depressed, the system will first compute
the average absorbance of the determinations,
and then use the average absorbance for cali-
bration.
B) Statistical Calculations

Using the CV or SD keys, the Model 560 is able to compute


and display the coefficient of variation (CV) or the standard
deviation (SD) for the averaged result obtained in Paragraph
A) above. If a printed CV or SD is required, the PRNT button
4/79
8-28

must be depressed (indicator on) before depressing the


CV or SD key. Only if the PRNT button is pressed will
the CV or SD indicator come on.

a) To Calculate the Coefficient of Variation (CV)

1) To display the CV, without printing results, calculRte


the average as described in Paragraph A) above so
that the average is displayed and the AVERAGE indicator
comes on, then press:

The display will change to show the coefficient varia-


tion. Press CE to remove the CV before attempting
any further operations.

2) To print the CV using a PRS-10 printer, select PRNT*+


before pressing CV. The CV indicator will light.
Calculate the average as described in Paragraph A)
above, then the CV will be printed, and presented
on the display.

b) To Calculate the Standard Deviation (SD)

1) To display the SD, without printing results, calculate


the average as described in Paragraph A) so that the
average is displayed and the AVERAGE indicator comes
on, then press:

The display will change to show the SD. Press CE


to remove the SD before attempting any further opera-
tions.

2) To print the SD, first select PRNT.*+ Then enter:

~
The SD indicator will light. Calculate the average
as described in Paragaph 8D,9(A). The printer will
print the average followed by the SD~

Note: In HOLD or CONT, if a standard is aspirated


instead of a sample, the CV or SD will be calculated,
and displayed or printed, but the sequence number
is not printed or incremented. In PK HT or PK AREA,
the average is computed and a sequence number is
printed and incremented. ~

*After obtaining the CV or SD, press CE to remove the displayed value


before releasing the PRNT key. If PRNT is released before the CV
or SD display is cleared it will be necessary to press CE before
continuing.
+Also press PRNT to enable data output to an RS-232C device.
4/79
8-29

8E. SPECIAL DETERMINATIONS


(
8E,l. Operating the Optional D Arc Background Corrector
2

The D2 (Deuterium) Arc Background Corrector is included in some


assembly verions (see Table 1-1) of the Model 560 or it can be in-
stalled at a later date by a Perkin-Elmer service engineer.

a) Background <:orre*cted MeaSl!E,ements

Notes: 1. Use of the D Arc Background Corrector is not


recommended at wavelengtfis longer than 390 nm unless an
order-sorting glass filter (such as Corning no. 0~52) is
placed in the sample beam window in the left side of the
. sample compartment. Such a filter blocks second order
radiation from the deuterium source. (The maximum usable
wavelength of the D2 Background Corrector with the Corning
no. 0-52 filter is ~30 nm.)
2. For most element source lamps used at wavelengths less
than 350 nm, the automatic intensity adjustment system
equalizes the n 2 lamp energy and the element source lamp
energy. For some hollow cathode lamps at wavelengths greater
than 300 nm and for some electrodeless discharge lamps, the
D2 lamp energy will be less than the element lamp energy.
Background correction will still be effective. Often the
imbalance can be reduced by using the next wider slit width
or reducihg the element lamp current somewhat, or both.
Some loss of sensitivity may result.

1) Prepare the instrument for measurement as described in


Section BA. To provide optimum performance for all types
of light sources used, the Model 560 background corrector
will automatically select one of two. modes of operation when
the BKGD CORR switch is in the AA-BG mode. If an Electrode-
less Discharge Lamp is used, the EDL will be operated with
continuous power (the optimum mode of operation for EDLs)
and the EDL and deuterium arc lamp signals will b~ electron-
ically separated. If a hollow cathode lamp is used, the
power to the lamp will automatically change from continuous
application to pulsed application, providing hollow cathode
and deuterium arc lamp signals which are separated in time.
In addition, the peak current to the hollow cathode lamp
will be adjusted to approximately 1.5 times that used for
continuous operation to provide optimized performance level
with background correction. The lamp current meter calibra-
tion will also be changed automatically when a hollow
cathode lamp is used in the AA-BG mode so that the same
current settings used in other modes may also be used in
the AA-BG mode. Under these operating conditions, there
may be a slight difference in sensitivity between results
obtained with and without background correction, particu-
larly for the more volatile elements (e.g., lead, cadmium,
etc.). This very slight reduction in sensitivy should have
no effect on performance.

4/79
8-30

Note: Recent EDL power supplies are capable of


supplying modulated power if desired. This is
achieved by connecting the modulation cable directly
to the (hollow cathode) lamp socket in the base
of the lamp compartment. Additional details are
furnished in the EDL Power Supply Instructions.

2) Turn the BKGD CORR switch (item 14, Fig. 7-1) to AA-BG.
The dot alongside the BKGD CORR indicator above the digital
display will light. For preliminary or approximate determina-
tions (where highest accuracy or precision is not required) ,
the system is operable 30 seconds after it is turned on.
However, for maximum precision and stability, the instrument
and the deuterium (D 2 ) lamp should be allowed to warm up for
3 to 4 minutes.

3) The BKGD CORR indicator dot will blink if the background


corrector power falls below a minimum usable level. In
that event, move the filter attenuator control located
in the lamp compartment (item 1, Fig. 8-3) to the IN postion.
Allow about one minute for the Automatic Intensity Control to
automatically readjust the power to the o2 lamp to an optimum
value. If the dot continues to blink after the attenuator is
positioned, there is not sufficient light from the lamp used
for the element of interest and simultaneous background
correction cannot be used for this particular measurement.
However, it may be possible to effect background correction by
taking readings in the AA and BG modes and using the difference
between those readings to obtain corrected values.

Note: Do not use the attenuator screen unless the indicator


shows it is required. Always position the attenuator control
in the OUT position at the start of a determination. Use
of the attenuator when not required may cause poorer perfor-
mance and reduce the life of the o2 lamp.

4) The o 2 lamp energy can be checked by holding the AA/BG energy


selector switch (item 8, Fig. 7-2) in the BG position and read-
ing the relative energy of the o2 lamp on the ENERGY/LAMP
meter alongside the energy selector.

b) Background Only Studies

1) Prepare the instrument for measurement as described in


Section SA. Do not install a lamp. If an Electrodeless
Discharge Lamp (EDL) or any other lamp with an outside
power source is installed, turn if off, or remove it from
the lamp compartment, or block the lamp emission manually
by inserting an opaque object in front of the lamp. If
a hollow cathode lamp powered by the instrument power
supply is being used, its power will automatically be
turned off in this mode, and it need not be removed or its
emission blocked.

4/79
8-31

2) Turn the BKGD CORR switch (item 14, Fig. 7-1) to BG.
The dot alongside the BKGD CORR indicator above the digital
display will light. Preliminary or approximate determina-
tions can be made 30 seconds after the system is turned on.
However, for maximum precision and stability, the instru-
ment and the deuterium (D ) lamp should be allowed to warm
2
up for 3 to 4 minutes.

3) Make sample measurements in the normal manner. However,


the readings will indicate only the level of background
present, not the ainoun t of atomic absorption.

8E,2. Reading Fast, Peak Shaped Signals with a Heated Graphite


Furnace

A) Normal HGA Operation


The Model 560 can measure peak shaped signals over a selected
period of time in two ways. When the MODE control switch is
set on PK HT, the instrument measures the highest value produced'
during the interval selected by the operator. When the PK AREA
mode is selected, the instrument measures the area under the
peak during the interval chosen. (Calibrating the display to
read directly in concentration is slightly different than for
flame determinations. See below.)

The optional Heated Graphite Furnace assembly can be installed


in place of the flame sampling components on the Model 560 when
extremely small samples have to be measured or when very low
detection limits are required. When the instrument and a recorder
are connected to the HGA Controller as described in Section 2B,ll,
the HGA Controller will automatically start the measurement cycle
coincident with the start of the HGA Atomize cycle. If a Perkin-
Elmer recorder is used it is also automatically controlled so
that .it starts several seconds be fore the HGA Atomize cycle and
stops about 30 seconds after atomization is complete.

1) Se.t the Model 560 MODE control switch to PK HT or PK AREA.

2) Using the numerical keyboard, enter the desired measurement


interval (between 0.2 and 60 seconds) and press the t key.
The interval should be adjusted after observing the pattern
of peaks produced by standards in the same concentration
range as that expedted in the sample. The interval should
begin before the peak appears and end only after the recorder
pen has returned to the baseline.

3) Pipet a blank solution into the furnace and press the Program
Start button on the HGA.

4) After the indicator dot above the READ button goes out,
signaling the end of the measurement cycle, press the AZ
(Auto Zero) key. This stores the result obtained in the
instrument memory so that subsequent results (and the signal
sent to the recorder) will be offset by the value obtained.
4/79
8-32

5) Turn the signal control switch to CONCENTRATION

6) Enter the desired value for Sl through the numerical keyboard.

7) Pipet the least concentrated standard to be used to calibrate


the instrument and press the Program Start button on the
HGA.

8) After the indicator dot above the READ button goes out, press
81 to store the measurement result in the instrument memory.
The instrument will equate this result with the value stored
in step 6. Repeat steps 6, 7, and 8 for 82 and S3, if ne-
cessary, in order of increasing concentration.

Note: If the dot above the READ button goes off before
the end of the Atomize cycle on the HGA, it will be ne-
cessary to wait until the end of the cycle before pressing
the AZ, Sl etc. keys.

9) Measure the samples by pipetting them into the furnace and


pressing the Program Start button on the HGA.

B) Automatic Baseline Offset Correction with the HGA-500 or HGA-400

The microprocessor-controlled HGA-500 or HGA-400 includes a


facility for automatic baseline correction (B.O.C.), to com-
pensate for slight variations in the electrical zero of the
baseline. This feature is especially useful when using high
scale expansions with an Auto Sampler, under changing baseline
conditions.

The HGA-500 or HGA-400 BASELINE terminals must be connected to


the BASELINE connections on the Model 560 in order to generate
the desired baseline offset signal.

As described in the HGA-500 or HGA-400 instructions, generate


an analysis cycle with BASELINE correction occuring at some
point towards the end of the char cycle. Following the pro-
cedure of Paragraph A) above, pipette a blank and press
START/STOP to start the cycle.

The Model 560 will first perform a baseline offset correction


(BOC) during the char cycle, then auto zero (AZ) following
atomization of the blank. During subsequent READ cycles using
actual samples, the Model 560 will not only compute the
correct concentrations using the auto zero value, but each
concentration is also corrected for any slight variations in
baseline, using BOC.

8E,3. Flame Emission Measurement

Measurements in emission can be made either at a fixed wavelength


or by scanning a spectral region of interest utilizing the optional
Wavelength Scan Accessory 057-0207) with output to a recorder.
Refer to the Analytical Methods Manual section on Flame Emission
for general information on flame emission measurements.
4/79
8-33

a) Measurement at a Fixed Wavelength


1) Prepare the instrument for operation as described in
Section 8A. If a hollow cathode lamp is installed in
the lamp compartment, unplug it. Remove, turn off or
manually block emission from an electrodeless discharge
lamp.

2) Set the SIGNAL control switch to EM CHOP. Set the


SLIT width for the resolution desired.

3) With the WAVELENGTH counter at the approximate analytical


wavelength of interest, aspirate a blank solution and
press the AZ key to zero the display. The cycle is
complete when the indicator dot alongside the AZ key
stops flashing.

4) Aspirate the most concentrated standard solution,


optimize the wavelength setting to provide maximum
energy, and adjust the GAIN control as necessary to keep
the ENERGY/LAMP meter reading on scale.

5) After the wavelength setting has been optimized, adjust


the GAIN control while aspirating the most concentrated
sample or standard to be used to provide a reading of
about 40 divisions on the ENERGY/LAMP meter.

6) Using the numerical keyboard, enter the desired measure-


ment interval between 0.2 and 60 seconds and press the
t key.

7) Set the MODE control switch to the position desired,


aspirate a blank solution and zero the display by
pressing the AZ key.

8) Follow the directions in Section 8D,l to calibrate


the display to read directly in concentration.

Note: Calibration curves for flame emission


measurements may not be as accurate over ex-
tended concentration ranges as the calibra-
tion curves for atomic absorption measurements.
Before making sample determinations, make sure
the flame emission calibration curve to be used
is sufficiently aqcurate over the concentration
range of the samples.

9) After processing 8 to 10 samples, changing the gain


or changing the MODE control setting, check zero by
aspirating a blank solution. Also occasionally aspirate
a standard to check the calibration or RECALibrate.

4/79
8-34

b) Measurement with the Wavelength Scan Drive Accessory


1) Prepare the instrument for operation as described
in steps 1 and 2, above, and connect a recorder to
the instrument.

2) Set the WAVELENGTH counter to a position slightly ~


below the analytical wavelength of interest.
Scanning occurs from shorter to longer wavelengths.

3) Completely block the left hand burner compartment


window (item 3, Fig. 8-4) with a nonflammable object
(see Caution) and zero the display.

Caution: USE AN OPAQUE NONFLAMMABLE OBJECT (E.G.


A METAL RULER) TO BLOCK THE WINDOW. NEVER INSERT
A HAND OR FLAMMABLE OBJECT INTO THE BURNER COMPART-
MENT WHEN A FLAME IS BURNING.

4) Aspirate the most concentrated standard or sample to


be used in the analysis. Manually scan the wavelength
region of interest, adjusting the GAIN control, if
necessary, to keep the ENERGY/LAMP meter reading on
scale.
5) Adjust the WAVELENGTH control for the strongest emission
signal in the wavelength range to be examined. Set the
ENERGY/LAMP meter reading with the GAIN control to about
40 divisions.
6) Remove the solution, then zero the display and the recorder
baseline.

7) Follow the directions in Section 8D,l to calibrate


the display to read directly in concentration.

8) Rotate the WAVELENGTH control to return to the starting


position. Push the accessory SCAN button on to obtain
an emission scan. After completing the scan, push the
button to off.

9) After processing 8 to 10 samples, changing the gain or


changing the MODE control setting, check zero by aspi-
rating a blank solution. Also occasionally aspirate a
standard to check the calibration, or RECALibrate.

10) Aspirate other standards and sample solutions, operating


the wavelength drive and manual WAVELENGTH control as
in step 8.

4/79
8-35

8E,4. Measurement of the Emission Spectra of a Lamp Source

1) Prepare the instrument for operation as described in Section


BA. No flame is used.

2) Install and align the lamp.

3) Set the SIGNAL control switch to EMission and set the


WAVELENGTH counter to a position just below the wavelength
region to be examined. Scanning occurs from shorter to
longer wavelengths. (The scan speed is preset to 5 nm/min.)

4) Set the SLIT control to the desired value and the RECORDER
control switch to TCl or TC2.

5) Block the lamp beam with an opaque object placed in front


of the lamp face and zero the display and the recorder base-
1 ine. Unblock the beam.

6) Manually scan the wavelength region of interest and adjust


the GAIN control if necessary to keep the ENERGY/LAMP
meter reading on scale.

7) Adjust the WAVELENGTH control for the strongest emission


signal in the wavelength range to be examined, and set
the ENERGY/LAMP meter reading to a maximum value of 40
scale divisions.

8) Block the lamp beam as described in step 5, zero the


display and unblock the beam. The display should be
zeroed each time the GAIN is adjusted.

9) Calibrate or apply an expansion factor to the display.

10) Rotate the WAVELENGTH control to return to the starting


position. Push the SCAN button to on to obtain an emission
scan. After the scan is complete push the button off.

BF. ADDITIONAL READOUT DEVICES

BF,l. Strip Chart Recorder

There are two sets of recorder terminals at the rear of the


instrument. One set is labeled 1 V, the other 10 mv. Table
8-4 sununarizes the signal ranges for each set of terminals and
their equivalents on the Model 560 display.

4/79
8-36

TABLE 8-4 - RECORDER SIGNAL RANGES

Recorder RECORDER Signal Reading


Output Control to on
Terminals Settin9 Recorder 1 Dis:elay

10 mV ABS 0 - 20 mV -2
INT, TCl, TC2, TC3, TC4 0 - 99.99 mV 0 - 9999 3

1 v ABS 0 - 2 v -2
INT, TCl, TC2, TC3, TC4 0 - 9.999 v 0 - 9999~

1
Signals over 10 mV (1 V) are offscale on 10 mv (1 V) recorder
range. Actual (onscale) reading may be obtained on recorder by
using 100 mV (10 V) range on a multirange recorder.
2
Recorder signal varies from 0 - 20 mv (0 - 2 V) , but the
display reading depends on setting of SIGNAL control. With
SIGNAL control at ABS, display reading varies from 0. 000 to 2.000
absorbance units; at CONC, display reading can vary from 0 to
9.999, depending on the standard concentrations used for cali-
bration or the scale expansion factor used.
3
Regardless of decimal point position.

As indicated in Table 8-4, the signal to the recorder can be


transmitted in terms of absorbance with no scale expansion,
curvature correction or calibration factors applied, even
though these factors have been applied to the digital display.
Also, both continuous and integration outputs are possible.
See Section 7A,l for descriptions of the RECORDER and MODE
control switches and the recorder output options they provide.

When an integrated reading format is selected,


a trace like the one shown in the accom-
panying sketch is obtained. After the
READ button is pressed and the indicator
dot goes out, the pen rises rapidly to
the appropriate signal level, holds this
level for 3 seconds, then drops back to
recorder or electrical zero.

Note: Do not use a recorder range of less Time


than 10 mV full scale if using the 10 mV
terminals (or 1 V, if using the 1 V terminals). Instead use
the controls on the instrument to expand the reading. If a
recorder range less than 10 mv (1 V) is used, smooth recorder
traces will not be obtained owing to the design of the D/A
converter in the Model 560.

4/79
8-37

1000 -C.Uul
10 J l v 3 2 0 MEASUREMENT
1 0 U2 l' 4 o V ~ WITH SEQUENCE #
1 0 iJ J J1 E:. h ~ ERROR CODE
iou4 udJ7 I
v JIJU ~ AUTOZERO
.J ':i iJ l ---+-- Sl CALIBRATION
1: J 0 li ~ S2 CALIBRATION
2L UU ii. ~ S3 CALIBRATION
10u5
lUG6
1J07
l L 'l U
J.Js
"I , U '.! C
I
---+-- OVER-CALIBRATION
1 Ov,J <:. l j
10G9 l 7
I
[I :J
l 011) j ) L
1 L' JU Ii S ~ RESLOPE CALIBRATION
l Lil j 4. 'J 3
1 0 l :! 1 (J. 4 j

1 Paper Feed Button Fig. 8-11 - PRS-10 Printout Showing


Various Codes. Lines with Codes,
Fig. 8-10 - Model PRS-10 Including Auto Zero, Are Printed
Printer-Sequencer in Red

8F,2. Printer-Sequencer
The PRS-10 Printer Sequencer (Fig. 8-10) provides a printed record
of the analytical results from the Model 560. The printout (Fig.
8-11) may include up to 10 digits of information generated by
the Model 560, of which four may be a sequence number and six
the results of a measurement. When five or six digits are utilized
to record a measurement, the first one or two will be zeros, only
for correct decimal point placement. In addition to the digits,
the decimal point is properly positioned and a minus sign is
printed for negative results.
Codes are printed to identify calibration or statistical measure-
ments. (status codes) and to indicate the occurrence of error
conditions (error codes). Where multiple error conditions exist
simultaneously, up to two error codes may be printed out on the
same line. On any line on which a status code is printed, the
sample sequence numbers are not indexed (no sequence numbers are
printed). Sample sequence numbers are indexed and printed when
an error code is printed.

4/79
8-38

Using the PRS-10


1) Make sure there is enough paper in the PRS-10. If not, re-
place the paper roll as described below. The paper is colored
red at the edges when the supply is nearly depleted.
2) Set up the Model 560 to make the desired measurements.
3) When the Model 560 is ready to make sample measurements,
proceed as follows:
a) If sequence numbers are desired on the PRS-10 printout,
enter the starting number (up to 4 digits) on the Model
560 keyboard, then push PRNT. The indicator dot alongside
the PRNT button will go on.
Note: Each time a sample measurement is recorded,
the sequence number is incremented by 1. Sequence
numbers are neither printed nor incremented during
calibration measurements.
b) If sequence numbers are not wanted, push PRNT on the Model
560. The indicator dot alongside the PRNT button will
go on.
The PRS-10 will print out each reading taken with the
Model 560. The PRS-10 will stop operating and the dot
next to the PRNT button will go off if the Model 560 MODE
switch is set on CONT and integration time less than 0.5
second is entered. The indicator dot also will not light
i the PRS-10 printed circuit board is not installed.
4) As data are recorded, all valid sample measurements are printed
out in black. If Averaging is selected, sequence numbers
are printed for the averaged result only. Calibration measure-
ments or readings taken when an error condition exists are
printed in red. Status codes, used to identify calibration
measurements, statistical operations and error conditions
are as follows:
Red zeroes - printed out when the Model 560 is auto zeroed
I - first standard (Sl) concentration
II - second standard (S2) concentration
III - third standard (S3) concentration
AV - averaged result
SD - standard deviation
CV - coefficient of variation
RS - reslope
C - over-calibration (possible error condition)
ER - error condition (error message - refer to
Section 12)

4/79
8-39

5) Figure 8-12 illustrates


an example of calibration
printout from the Model
560 with autozero and two
standards (81, 82), using \). 7Ll l
averaged readings. The lJ. (u1
l', 7 JO
following points are of L, 7 v l ~v
SAMPLE DETERMINATION
u. 1 u
in te re s.t: ll .-Ju U I
CV
$[;
U,Jj3
AUTOZERO CALIBRATION
u .l.1 v (:'.
a) The individual readings l.. rjQ(.'
WITH THREE DETER-
MINATIONS SHOWING
are printed in units ~'' i_:, IJ IJ
('<,.,. 06
AV
CV
COEFFICIENT OF
VARIATION AND
STANDARD DEVIATION
of concentration, but !..-1L:ll.Jo
2
so
the average in each :; j (,

l. 3 0 lJ
CALIBRATION USING
case is calculated us- PRINTEIJ
IN RED
(J. j

.., , C:C1=>.IU
rl (j
AV
AVERAGED VALUE OF
THREE DETERMINATIONS
ing the absorbance values v. 21 CV OF Sl, WITH CV AND SD
'J'J ,_, J\..l u so
for the individual read- .J ' LI..; ') ~,' !J cu
ings. The average J, CG 9 i! l
..... v(.:;l ~ l
Cu
Ch
CALIBRATION USING
AVERAGED VALUE OF
absorbance is then con- .J. u l:.) d
e, 1 s
AV THREE DETERMINATIONS
OF S2, WITH CV AND SD
CV
verted to a concentra- , 1J '..! r, ~IJ '.:>
"~
tion value. O, vli!4 ")u
U,1;0487
V,LJG490 SAMPLE DETERMINATION
lvJ Li, 1 L4 ci ':i
USING THE TWO-STANDARD
AV CALIBRATION
u. 37 CV
b) C (over-calibration) ij((Ji) 1b Si:

is shown for each measure-


ment of 82 because the
results are above the
range of the highest
standard previously Fig. 8-12 - PRS-10 Printout
used (0.005 for 81 in Showing Averaging and Cali-
this example) . bration

6) Push the paper feed button (Fig. 8-10) to advance the paper.
After the button is pushed there is a 1.5 second delay to
allow the mechanism to attain operating speed. The paper
will continue to advance until the button is released.
7) To turn off the PR8-10, push the PRNT button. The indicator
dot associated with the PRNT button will go out.
Paper Replacement
Use Perkin-Elmer replacement paper, part no. 023-1202 (package
of 10 rolls).

4/79
8-40

To install a new paper roll,


swing the front panel of the
PRS-10 out from the top as
shown in Fig. 8-13. Swing
the top cover up and to the
back. (The covers are held
in place by magnetic catches.)
If a small amount of paper
is left but it is desired
to replace the roll before
it runs out completely, cut
the paper where it comes off
the roll, before it enters
the print mechanism. Care-
fully, pull out the paper
remaining in the print mech-
anism.

Lift the old roll out of the


paper support taking care
not to drop the metal spindle
through the center of the
roll into the printer. Insert
the spindle through the new
roll and install the new roll 1 Top Cover
as shown in Fig. 8-13 so the 2 Reel Release
paper feeds from the bottom 3 Black Paper Guide (hidden)
of the roll. Feed the paper 4 Magnetic Catch
up over the black paper guide,
5 Front Cover
over the shiny metal plate 6 Tear-off Bar
stamped with a directional
arrow (under the wire guide)
Fig. 8-13 - PRS-10 Uncovered
and down into the slot just
in front of the arrow. Feed
the paper into the slot as far as possible, then swing up the
front cover and, with the Model 560 POWER switch on, push the
paper feed button on the front of the PRS-10. Hold the paper
down in the slot until the printer feed rolls grip it, then re-
peatedly push the feed button until the end of the paper comes
out from under the tear-off bar at the front of the printer.
(It may be necessary to manually guide the paper under the tear-
off bar.) The paper is now installed. Close the covers. Make
sure the paper feeds up the ramp, over the top cover.

Ribbon Replacement

Use Perkin-Elmer replacement two-color ribbon, part no. 023-1201.

4/79
8-41

0 ,1Js
0. 376 0 ,739
1.390
lO 3 I ,237 3.00 s
107 6,94 c 3,50
l 0 ,40 0 ,373 !09 112
101 '.),50 5 p:,1)0 17 ,2.6P.V
I ,545 l II II 3 p,,l)OAV
105 0 z 10 ,53 17 ,26 114
,QI)
110 5,Q I as E:
21l 00 s 17 ,25
05 :.. II 5 z1.74AV ""10"\,.t11
\7 .21 7 .99 116
05 21072 c 15 .s2A.V \.. 1.-l'lloll,.?l'l\1
117
e.\lO
os z 21 72 c is.s2 ~11CI' 110\\ t1C
21.78 c 15 ,52 "11"1.- 11so\\l' ~s11
\5 ,53 ot11C " 1'111'\.. t1G
"1 1t1\..'
l\};11 a ,aooa \
11011 a ,5aao s
.,1s1111
co11c"'"it'
aa 1-
G '~Gil $
\".~\)\) $
1>1'1'1-' \. a s
c\l o ,oa "s r.\\a s \ .o"~
50
5.ao s o 2
?I.-.. a ,ao t.s 150\ s 0 ,396 'z."'\)
t*-11"'1\ 5.00 $ 30 .o \ ,531 Q \~1.
t,'01'01\ll \ 15'00~ 5 I ,909\ ..
0. 11 b \
11
30 o .o\01 'O
11'110"\\ll 2
"1"110"\\ll 3 3 10 113!1 ~.\~
.t.s,1
I .1 o3 ,.1
",1""1l" 1 ,0 lb I I ,99 0 ,3
I 10 4 3 o .uozb \'
2 20 .~11
0 '3q" \ .10\'2.
3 3.111
",.?4 r~.,,o9 ~
"

Fig. 8-14 - Sequential Printout Fig. 8-15 - Operator-Selected


of Results Obtained with Model Data Format and Printout from
TR-2 Program Tape Used to Generate
Format

To install a new ribbon, swing the front panel of the PRS-10 out
from the top as shown in Fig. 8-13. Swing the top cover up and
to the back. (The covers are held in place by magnetic catches.)
Press the handles next to the ribbon reels in, toward the paper
roll, to release the reels and lift the old reels and ribbon from
the printer. Install the replacement ribbon, threading it the
same way as the old ribbon. (A threading diagram is provided
on the back of the black paper guide which is exposed when the
paper roll is lifted from its holder and held toward the front
of the instrument.) The ribbon is now installed. Close the
covers. Make sure the paper feeds up the ramp, over the top
cover.

8F,3. Model TR-2 Teletypewriter Readout, Communications Interface

The Model TR-2 Teletypewriter Readout (part no. 060-0063 for


105-125V, 60 Hz; 060-0064 for 200-240V, 50 Hz) provides a printed
report of the analytical results from the Model 560. The data
can be presented sequentially, as shown in Fig. 8-14, or in a
format selected by the operator (Fig. 8-15), and can be punched
into a paper tape for computer handling.

4/79
8-42

Included as part of the Model TR-2 are a standard Model 33 Tele-


type and a Communciations Interface (P-E part no. 060-0061).

The Communciations Interface, which is also available separately,


allows connecting the Model 560 to a variety of peripheral equip-
ment, including teleprinters, cathode ray tubes, paper tape
punches, computers, and Bell System Data-phones. It is intended
to be compatible with equipment conforming to specification
RS-232C of the Electronics Industry Association.

Instruction Manual 993-9188 describes the installation and opera-


tion of the Model TR-2 System, including the Teletype and
Communications Interface; instruction manual 993-9189 applies
to the Communications Interface as a separate accessory for the
Model 560.

4/79
9 HAZARDS

Possible hazards that could harm the user or result in


damage to the instrument appear in boxed statements at
appropriate places throughout this manual.
10 MAINTENANCE INFORMATION

lOA. OBTAINING SERVICE

All servicing should be performed by a Perkin-Elmer service


representative.

Burner and nebulizer maintenance and other maintenance pro-


cedures are described in this section.

lOB. MAINTAINING THE BURNER

lOB,l. Burner Cleaning Schedule

The nature of the samples aspirated determines the burner clean-


ing interval. In ordinary operation, the burner will need
infrequent cleanings (see Fig. 10-1). If high concentrations of
silver, copper, or mercury salts have been nebulized ihto an
acetylene flame, clean the burner chamber immediately after use
by following the procedure in Sec. lOB,4. Recondition the burner
chamber after working-with organic samples as described in Sec.
lOB,3. When samples with high solids content are aspirated,
clean the burner at least daily.

lOB,2. Cleaning the Burner Head Slot

The burner should provide an even flame over the length of the
burner slot. An uneven flame may indicate the slot needs clean-
ing. With the flame off and air on, carefully work along and
through the slot with a single-edge razor blade. Do not nick
the edges of the slot.

Cleaning stubborn deposits from the burner head slot may require
removing the burner head from the burner chamber. Proceed as
follows:

1) Extinguish the flame, turn off the gases and let the burner
cool.

2) Disconnect the hold-down cables (and the safety interlock)


from the chamber. Loosen the retaining ring (item 16, Fig.
10-1) and pull out the burner head.

3) Carefully work through the slot with a razor blade. Remove


scrapings from inside and outside the burner head.

4) The burner head can also be soaked overnight in detergent


and then rinsed with deionized water and blown dry with a
clean air supply.
10-2

1 Burner Chamber 040-0144 16 Retaining Ring 040-1290


2 End Cap Lock Nut 040-1246 17 a-ring 990-2038
3 Gasket (Rubber) 040-1276 18 Burner Head Pin 040-1287
4 End Cap Insert 040-1245 19 Blow-out Plug 040-1263
5 End Cap 040-1243 20 a-ring 990-2043
6 Nebulizer Assembly 303-0352* 21 Blow-out Plug Spring 040-1128
7 Nebulizer Clamp 040-1278 22 Blow-out Plug Cap 040-1120
8 Clamp Screw 040-1282 23 Mounting Screws 040-1329
9 Clamp Washer 040-1283 24 Hold-down Cable Clip 303-1638
10 Gas Fitting 990-3401 25 Accessory Bracket support Screw
11 Waste Fitting 303-1278 991-0146
12 Flow Spoiler 040-0140 26 Drain Block Assembly, 040-0352*
13 Flow Spoiler Screw 040-1275
14 Flow Spoiler a-ring 990-2237
15 Burner Head 040-0266* [includes
safety interlock cable and pin
assembly (040-0276) in place of
one hold-down cable]

~uded with the Model 560, but not part of Burner Assembly 040-0146

Fig. 10-1 Burner Assembly 040-0146


4/79
10-3

5) Remount the burner head in the burner chamber. Tighten


the retaining ring finger tight. Make sure the head is
firmly seated in the chamber and cannot rotate. Reconnect
the hold-down cables and safety interlock.

lOB,3. Cleaning the Burner After Use of Organic Samples

If aqueous samples are aspirated after organic samples such as


oil or MIBK extracts, the absorption signal produced can be
noisy and erratic. After aspiration of organic samples, follow
this procedure to prevent contamination of subseauent aqueous
samples.

1) For 5 minutes, aspirate an organic solvent known to be


miscible with the samples that have just been aspirated.

2) Aspirate acetone for five minutes.

3) Aspirate 1% HN0 3 for five minutes.

4) Examine the burner chamber. If deposits have formed, dis-


assemble and clean the burner as described in Sec. lOB,5.

5) Empty the waste drain tube and collection vessel and refilJ
them with water.

lOB,4. Cleaning the Burner After Use of High Concentrations


of Silver, Copper, or Mercury Samples in an Acetylene Flame

Unstable acetylides, which are especially likely to expiode


when permitted to dry, may be formed when nebulizing high
concentrations of silver, copper, or mercury salts into an
acetylene flame. Thoroughly flush the burner mixing chamber
and waste drain tube with water immediately after this kind
of analysis, and inspect the burner mixing chamber visually
to be sure that all traces of residue have been removed.

lOB,5. Cleaning the Burner Mixing Chamber

1) The mixing chamber may be cleaned either after removal of


the chamber assembly from the spectrophotometer or while
mounted on the instrument, depending on its condition.

2) Follow the procedure in Sec. lOB,2 for removing the burner


head from the instrument.

3) Try to clean the chamber by pouring about 200 cc of water


in the neck. If this method is unsuccessful, the chamber
must be dismantled, cleaned, and reassembled as described
in the steps below. '
10-4

4) Refer to Fig. 10-1. Unscrew the nebulizer clamp screw


(item 8) and remove the nebulizer assembly (item 6); then
unscrew the end cap lock nut (item 2) and remove the end
cap (item 5) and gasket (item 3).

Important: Removal of the end cap (item 5) or of


the retaining ring (item 16) exposes a plastic
covered surface. Be careful not to damage this
coating by any sort of impact.

5) Loosen the two mounting screws (item 23) on the right


side of the chamber and lift it off the mount.

6) To dismantle the chamber, unscrew the flow spoiler


mounting screw with its 0-ring (items 13 and 14), then
reach in and remove the flow spoiler (item 12). Unscrew
the blow-out plug cap (item 22) to remove the blow-out
plug (item 19), spring (item 21) and 0-ring (item 20).

7) Deposits in the burner head and mixing chamber can be


removed with detergent solution and a bottle brush.

Important: Do not soak the stainless steel mixing


chamber in acid or use kitchen-type cleansers. Avoid
damage to the plastic lining of the mixing chamber
from abrasive tools.

8) After cleaning, rinse thoroughly with deionized water and


replace the flow spoiler and blow-out plug assembly.

9) Install the chamber on the mount and tighten the two mount-
ing screws.

10) Replace the end cap and tighten the lock nut finger tight.
Replace the nebulizer assembly and burner head. Check the
burner alignment and align if necessary.

lOC. MAINTAINING THE NEBULIZER

lOC,l. Cleaning the Nebulizer and Sample Capillaries

A low absorbance reading with a clean burner head slot may be


due to an obstruction in the nebulizer or sample capillary.
Aspirate pure solvent with the flame on until the absorbance
reading is satisfactory for a subsequent standard.

Note: If a longer sample capillary is used, the rate


of sample uptake and sensitivity will decrease.

If solvent aspiration fails to clear the sample capillary or


nebulizer capillary, push a wire (provided with the spectrophotom-
eter) through the capillaries from the inlet side. Move the
wire in and out.
10-5

Important: Use only the cleaning wire provided (303-0135)


to clean the capillary. Other wire may be burred and
damage the nebulizer.

For deposits which do not yield to either of these measures, the


nebulizer may be disassembled for cleaning (see Sec. lOC,3).

lOC,2. Changing the Nebulizer

1) Remove the nebulizer oxidant tubing from the nebulizer


installed in the spectrophotometer.

2) Loosen the nebulizer clamp screw (item 8, Fig. 10-1) on the


end cap.

3) Remove the nebulizer from the end cap and install the
replacement nebulizer, making sure the nebulizer 0-ring
(item 12, Fig. 10-2) is in position.

4) Secure the nebulizer with the nebulizer clamp screw.

5) Replace the oxidant tubing. To attach the sample capillary,


first insert a cleaning wire into the sample capillary.
Then insert the wire into the nebulizer capillary and slide
the sample capillary along the wire until it is firmly in
place. Remove the wire.

Important: When using the corrosion-resistant


nebulizer (303-0404), do not attempt to remove
the sample capillary. It is an integral part
of the assembly.
6) Adjust the nebulizer for maximum sensitivity as described in
Section 8C,8.

lOC,3. Disassembly of the Nebulizer for Cleaning

Important: The cleaning procedure of Sec. lOC,l usually


suffices to restore the nebulizer to satisfactory working
order. The disassembly described here is seldom needed.
The performance characteristics of a nebulizer are likely
to be modified by disassembly.

Disassembly (See Fig. 10-2)

1) Remove the nebulizer from the burner as in Sec. lOC,2.

2) Unscrew and remove the Jcnurled knob (item 1) and washer


(item 3).

3) Carefully pull out the needle assembly (item 4). Inspect


the inner end for deposits and clean if required.
10-6

4) Remove the 0-ring (item


12), unscrew and remove
the front end cap (item
11), and pull out the
venturi section (item 10).

5} If necessary, remove the


insert (item 8) by push-
ing it out with a wooden
probe.

6) Clean components as
required with a suitable
solvent; 0-rings may be
cleaned with soap and
water.
1 Knurled Knob 303-1460* Assembly (See Fig. 10-2)
2 Locking Ring 303-1456*
3 Washer 303-1802 l} Lubricate the 0-ring on
4 Needle Assembly 303-0354 the insert (i tern 7) and
5 0-ring 990-2101 the 0-ring on the needle
6 Spring 303-1806 assembly (item 5) with a
7 a-ring (2) 990-2239 bit of grease such as
8 Insert 303-1812 Apiezon L.
9 Nebulizer Body 303-0353
10 Venturi 303-1810 2) Slide the needle assembly
11 Front End Cap 303-1808 into the insert as far as
12 0-ring 990-2239 it will go; the needle tip
should protrude from the
Fig. 10-2 - Nebulizer - Exploded small aperture in the in-
View sert end.

3) Insert these assembled components into the left end of the


nebulizer body (as shown in Fig. 10-2), and install the
washer and knurled knob.

4) Install the venturi over the needle tip; put on and tighten
the front end cap (itemll). Slip the 0-ring (item 12) over
the protruding end of the venturi.

5) Install the nebulizer in the burner as described in Sec.


lOC,2 and adjust the aspiration rate as.described i~
Section 8C,8. Lock the setting by turning the locking
ring counterclockwise against the knurled knob.

*Some nebulizers may have coarser threads (identified by the


straight parallel grooves on the knurled knob and locking
rings.) The part numbers for the items with coarser threads
are 303-1809 (item 1) and 303-2049 (item 12).
lOD. CARE OF OPTICS

1) Avoid making fingerprints on the windows of the sample


compartment or on the face of the source lamp.

2) When the covers are removed, do not touch the reflecting


surfaces of mirrors or gratings.

3) If dust collects on the optical surfaces, blow it off


carefully with a clean and dry air bulb. Do not rub
the surfaces with a cloth.

4) Window surfaces only may be cleaned with a tuft of cotton


moistened with a dilute solution of mild liquid detergent
followed by several rinsings with deionized water.

5) If mirror surfaces become dirty (e.g., from exposure to


labo~atory ~apors~ cleaning should be done by a Perkin-Elmer
service engineer. If a service engineer is not available,
a skilled technician may clean the surf aces by careful use
of clean cotton moistened with a clean solvent such as
alcohol. Quick drying of the surfaces is important. DO
NOT RUB OPTICAL SURFACES. Care must be taken to avoid
scratches, which require resurfacing the mirrors.

Important: Never touch or clean the grating surfaces.

lOE. OPENING THE ELECTRONICS COMPARTMENT

Caution: Disconnect the power cord whenever the


instrument cover is removed. Potentially dangerous
voltages are present within the instrument.

To gain access to the electronics compartment (behind the right


front control panel), unscrew the four screws (shown in Fig. 7-1)
on the sides of the panel. Carefully slide the electronics com-
partment forward.
To close the compartment, be sure no wires are caught and
carefully slide the electronics compartment back into the
instrument and secure with the screws.

lOF. OPENING THE PHOTOMETER COMPARTMENT


To gain access to the photometer compartment (in the top section
of the spectrophotometer) unscrew the screw above the WAVELENGTH
counter, and two screws (items 7, Figure 8-3) in the area of
the lamp compartment.

Note: This cover must be lifted to gain access to the o2 arc.

4/79
10-8

Lift the cover (hinged at the rear of the instrument) and allow
the cover to be supported by the chain at the right rear corner
of the photometer compartment, to hold the cover open.

lOG. REPLACING AND ALIGNING THE D2 ARC

Caution: Do not look at the o 2 arc when it is on. The


ultraviolet light can cause serious eye damage.

lOG,l. Lamp Replacement

1) Make sure the instrument power is off and that the power
cord is disconnected.
2) To gain access to the D2 arc lamp in the photometer compart-
ment (top section of spectrophotometer), unscrew and remove
the hexagonal setscrew above the WAVELENGTH counter (see Fig.
7-2, item 2). Also unscrew and remove the screw on the
lip of the lamp compartment (see Fig. 8-3, item 9). Lift
the cover (hinged at rear of instrument). A brace at the
right rear corner of the photometer compartment should be
engaged to hold the cover open.

3) Remove the primary source (lamp) mount and the long mount
hold-down screw.

4) Unplug the D2 arc lamp


connector (item 2, Fig. 10-3).

5) Unscrew the two arc lamp


cover screws (item 1, Fig.
10-3) and remove the arc
cover.

6) Loosen the two arc retain-


ing setscrews (item 4, Fig.
10-4) .

7) Twist the o 2 arc lamp (item


3, Fig. 10-4) 90 counter-
clockwise so that the arc
face (item 2, Fig. 10-4)
faces the front of the instru-
ment. Remove the lamp.

1 Arc Lamp Cover Screw 8) Carefully place the new lamp


2 Arc Lamp Connector in the arc holders with the
3 Arc Lamp Cover arc face facing the front
of the instrument.
Fig. 10-3 - D2 Arc Lamp Cover

4/79
10-9

9) Tighten the two arc retaining screws (item 4, Fig. 10-4)


so that the lamp is held securely, but can still be
rotated. Then gently twist the lamp 90 clockwise so
that the arc face (item 2, Fig. 10-4) faces the lens
(item 1, Fig. 10-4).

10) Adjust the lamp gently by hand so that the arc face is
aligned and centered with the lens (item 1, Fig. 10-4)
and as parallel to the lens as possible. Adjust the
height of the D2 arc lamp so that the bottom of the arc
face is about 5.0 cm (2 in.) above the D2 base plate.

11) Carefully slide the D2 lamp cover (item 3, Fig. 10-3)


back into place over the D2 lamp. Secure the lamp cover
with the two lamp cover screws removed in step 5 (item 1,
Fig. 10-3).

12) Plug the D2 lamp connector (item 2, Fig. 10-3) into the
D2 lamp socket as shown in Fig. 10-3.

13) Replace the lamp mount and the two mount hold-down screws.

lOG,2. Aligning the D2 Lamp

1) Connect the Model 560 power cord, turn on the instrument


power, and wait several minutes for warm-up.

2) Set the BKGD CORR control switch to AA-BG and wait 30


seconds for warm-up.

3) Set the wavelength to 260 nm.

4) Hold the AA/BG rocker switch alongside the ENERGY/LAMP


meter in the BG position while performing steps 5 through
10.

5) Set the SIGNAL control to SET UP and adjust the ENERGY/


LAMP meter reading to between 10 and 20 divisions with
the GAIN control.

6) Loosen the two adjust lock setscrews (item 4, Fig. 10-5).

7) Rotate the In/Out adjust knob (item 1, Fig. 10-5) until


the ENERGY/LAMP reading is maximized. Use the GAIN
control to keep the meter needle below the control point
(about 40 divisions) if necessary. Retighten the adjust
lock setscrews.
10-10

1 Lens 1 In/Out Adjust


2 Arc Face 2 Vertical Adjust
3 Arc Lamp 3 Horizontal Adjust
4 Arc Retaining Setscrews 4 Adjust Lock Setscrews
5 Upper Retaining Arm
6 Lower Retaining Arm

Fig. 10-4 - D2 Arc Lamp and Lens Fig. 10-5 - Adjust Knobs

8) Loosen (turn counterclockwise) the top vertical adjustment


knob (item 2, Fig. 10-5) while tightening (turning clockwise)
the bottom vertical adjustment knob. If the meter reading
decreases, retighten the top adjustment knob while loosening
the bottom adjustment knob until the meter reading is
maximized. If the meter reading increases, continue to
loosen the top vertical adjustment knob while tightening
the bottom adjustment knob to maximize the meter reading.

9) Loosen (turn counterclockwise) the left horizontal adjustment


knob (item 3, Fig. 10-5) and tighten (turn clockwise) the
right horizontal adjustment knob (item 3, Fig. 10-3). If
the meter reading decreases, retighten the left adjustment
knob while loosening the right adjustment knob until the
meter reading is maximized. If the meter reading increases
when the left knob is loosened, continue to loosen the left
adjustment knob while tightening the right adjustment knob
until the meter reading is maximized.
10-11

10) Repeat steps 7, 8, and 9 until the meter reading is


maximized.
Note: If the D arc lamp is not properly positioned
as described in 2 Sec. lOG,l, steps 9 and 10, it
may not be possible to reach a maximum reading
before the adjustment knobs reach their maximum
travel. In that event, the lamp must be repositioned
as described in Sec. lOG,l steps 1 through 5 and
steps 9 through 13. After repositioning, the lamp
must be realigned as described in Sec. lOG,2.

lOH. REPLACEMENT PARTS LIST

Part No. Description


040-0188 Burner Spares Kit (includes 990-2239
Nebulizer Tubing, Polyethylene, 1 Pkg.)
250-6519 1/2-in. Drain Tubing (6 ft)
998-1614 Slo-blo Fuse, 2.0 Amp, 3AG (5), 115V
998-1604 Slo-blo Fuse, 1.0 Amp, 3AG (5), 230V
057-0557 Air/Argon Hose Assy., Black
057-0566 N20 Hose Assy., Blue
057-0559 Fuel Hose Assy., Red
990-3898 Coupling, Oxidant Hoses
990-3032 Coupling, Fuel Hoses
990-8986 Line Cord, 115V or
998-8985 Line Cord, 230V
303-0477 Recorder Cable Assembly
057-0168 Sample Tray
303-0352 Nebulizer
303-0404 Nebulizer Corrosion Resistant (Plastic)
303-0299 Nebulizer Corrosion Resistant (Pt-Rh)
040-0266 10 cm Flat Burner Head (1 Slot)
040-0289 3 Slot Burner Head
040-0277 Nitrous Oxide Burner Head
IOOK" SIJ\'::J~E e=t.MP A/Ll CCliWERTER TIMlr'>IG DIAGRAM

-t-15V GATE GENER.;,TQR


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GND~
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Rl4 RAMP GENE?.ATOR &. VOLTAGE COMPARATOR
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I I t50V 1.5 INHIBIT COUNTER FOR OVER R,>,NGEING
2.1 SIGN..:.L INT. HOLDS
~;~tW - 2.2 FLAG PPS l/0 CONVERSION COMPLETED
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2. FACTORY ADJUST Rl7 FOR


+ISV LOGIC R21 A GATE GENERATOR PERIOC
s~,f 1.IBK IC12
50V,2w or 180MS 5MS,IF REDUIREL.
USE ONLY TYPE CC CERMET FILM
FIXED RESISTOR.
j , FACTORY ADJUST RI FOR THE PEAK
i/6~.3 HEIGHT MODE TO BED TO+IO%MORE
m ,17 THAN THE CONT MODE,IF KEQUIRED.
IN825A
tl5V o=520X -+ ~~fc~NR~~ nis~ ~CE~6~~roj~L5~~~WiR 1
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57.6K F2,2 CONVERSION COMPLETED
~~1:.~
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50Vf

Fig. 10-10 Electrical Schematic, A/D Converter Circuit (J7) 057-0322E (Rev. H)
4/79
- I< 2'JL!<.L
30(+-~L~A _
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---1<2ori10!~:.
1< 18 1/05- 06_
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---<1<14 1/02_____ -

--1.(24~---

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IC I
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--~ 2, ~G_1~_ - --------
_ 9)A(BIO__ ' +5 v
--!< I AS I A /-B1-1 - - - - - ..
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SIG G N D l ___ l --~ 27( NC
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-----,.( 10 4---Ncl USED ON ,111111111


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PWRGN+r----<1L,__=R__,\ ~~p~~~ -,r -II' _, __ ,__ ,__ , __ ,___ -

---< 97 _Jj
----k 98~+1 I Io+svi
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4.7 .I .1 T
MFD MFD MFD
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Fig. 10-12 - Electrical Schematic, ROM Circuit (JS) 057-9160C (Rev. BJ

4/79
me I bI l P,RTOF
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10 9
~~~ 8 7

f'IQT[t
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Fig. 10-14 Electrical Schematic, TTY Interface Circuit (J3) 057-0321E (Rev. H)

4/79
10-28

-I
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95
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L_ - - -- - - - -- - - - - _J

Fig. 10-16 - Electrical Schematic, +5 V, +15 V Unregulated


Power Supply (Jl) 057-0327D (Rev. C)
4/79
10-31
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SLO-BLO 5 I 6 II
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POWER
RED GRN

Fig. 10-18 Electrical Schematic, Standard Gas Control System


057-0400E (Rev. C)

4/79
10-33

!-'------------------------
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+7v +7V +7V

15_Li"
tC3 IC3 IC IC3

02 03 04 06
2N4403 2N4<l 03 2N4403 2N'l403

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NOTES
L UNLESS OTHERWISE'SPECIFIED
I 1' L___ __
11. :~~ ~~~~rio:,.s ~cw1:T~~~s, ~2._%,

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err I THfi'U CRIS Afi'E HPSQf\;>465"0 L.E Q !>.
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Fig. 10-19 Electrical Schematic, Keyboard Display 057-9130E (Rev. D)

4/79
Pen- o 4 J J _ !:'f l_~t. :_1

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I
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PNEUMATIC ASSY
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),J./ST/!V.Af.-Vr

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L 6LK

B ~A }To "'"1 (oS1H72 eo.)

FLAME SENSOR

Fig. 10-20 BC-3, Interconnection Diagram 047-0402D (Rev. C)

4/79
J4
N047-0177

8
220 v---"-''-"---
7 ~'f_Y..-__
AC IN 20 O V _ _!;;IJ&::ll~L__)
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s
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NOTES
UNLESS OTHERWISE Sl'ECIFIEO
o. ALL RESISTORS ARE IN OHMS,:I::~,
ANO RATEO AT !:!lWATTS.

b. !~ii ~~~~T~~~Evc:m~'it~[::~sTIC
1 CAPACITORS ARE RATED AT _-_VOLTS.

Fig. 10-21 BC-3, Power Supply Schematic 047-9480D (Rev. F)

4/79
+SV
c
JI ICI
FLAME II 12 5
2.2K IC 1
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OVERRIDE 14
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2.2 K 0
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CR2 .....J
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Cz H2,N2 0 6 NOTE:
I
I. S 2 TO BE ALTERNATE ACTION.
Dl~AIN '3

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Fig. 10-22 - BC-3, Interlock Display, 047-9630C (Rev. B)

4/79
Cl/

oi9
4
+sv " ROM 00<17-1785 ICI 1:
AA BURNER CONT Fi'OL SPARE SPARE SPARE
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Fig. 10-23 BC-3, MPU Logic 047-9620E (Rev. D

4/79
11 TROUBLE SHOOTING

A. Introduction ..... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-1


B. Hollow Cathode Lamp ....................... 11-1
1. Lamp will not fit properly in the lamp mounting
bracket . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-1
2. Lamp connector will not fit the connection on the
instrument . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-1
3. Lamp will not light .......................... 11-1
4. Lamp current cannot be set to the desired
operating value . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-2
C. Display Does Not Respond ....................... 11-2
1. Display is completely lit and all indicator dots
are lit . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-2
2. Display is blank but warning lights are all on .. 11-2
3. The reading on the display will not change ....... 11-2
D. Calibration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-3
1. Calibration curves do not pass through zero ... 11-3
E. Indicator Dots On . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-3
1. OVER CAL dot on . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-3
2. KEYBOARD dot is lit ...................... 11-3
3. The BKDG CORR dot is on ..................... 11-3
4. BKGD CORR dot is blinking ..................... 11-3
F. Results Questionable ............................ 11-3
1. Results erroneously high ............... 11-3
2. Results erroneously low ................ 11-4
3. Cannot get suggested detection limits .......... 11-4
4. Cannot get close to the suggested sensitivity ... 11-4
G. Results Noisy ... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11-5
1. Display noisy with flame off .............. 11-5
2. Digital display is quiet with the flame off, but
noisy with the flame on or with the flame on and
solution aspirating ................ 11-5
H. Re s u 1 ts Dr i ft . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11- 7
1. Baseline drifts with flame on ................ 11-7
2. Readings drift or are not reproducible ....... 11-7
I. Background Correction ....................... 11-8
1. The BKDG CORR indicator dot above the digital
display front panel is blinking ............ 11-8
2. The D arc has less energy than the primary
2
source . 11-8
3. The Background Corrector does not provide
adequate correction ............ 11-8
4. The analytical results with background correction
are excessively noisy ...................... 11-9
5. Sensitivity is lower in the AA-BG mode than in
AA mode . 11-9
J. Flame Ignition and Gas Control .......... 11-9
1. If the gases do not ignite ........... 11-9
2. If the burner-nebulizer system flashes back ..... 11-10
11 TROUBLE SHOOTING

llA. INTRODUCTION

The following suggestions are included to help the operator


determine systematically whether difficulties experienced with
the spectrophotometer are due to a malfunctioning of the
instrument, improper settings of the instrument controls, or
improper analytical techniques.
If, after checking the instrument against the symptoms described
below, the source of the difficulty appears to be due to a mal-
functioning of the instrument, it is strongly recommended that
the operator of the instrument or other responsible personnel
contact the local Perkin-Elmer service representative. Servicing
of an instrument by other than Perkin-Elmer service representatives
will render the warranty null and void.

llB. HOLLOW CATHODE LAMP

llB,l. Lamp will not fit properly in the lamp mounting bracket

An Adapter Kit (Perkin-Elmer part no. 303-0870) is required for


use with lamps with diameters smaller than 2 inches..

llB,2. Lamp connector will not fit the connection on the instrument

Lamps other than the Perkin-Elmer Intensitron series may need


special connecting cables in order to be used with the instrument.
All Intensitron lamps are equipped with the proper connections.

llB,3. Lamp will not light

a) Make sure the instrument is plugged in, turned on, and warmed
up. If line voltage is low, operate the power supply from a
variable transformer set to give the appropriate voltage.

b) Be sure the lamp current knob is not fully counterclockwise.


c) Be sure the BKGD CORR switch is not set on the BG
position. Hollow cathode lamps are turned off when
the switch is set to this position.

d} Check other lamps to determine if the failure to light


is characteristic of the instrument or of the individual
lamp.
11-2

llB,4. Lamp current cannot be set to the desired operating


value

a) If the instrument is being run with a voltage regulator,


make sure that the regulator has a sinusoidal rather than
a square wave output. Regulators which provide a square
wave output may not provide sufficient voltage to light
certain lamps which require a very high starting voltage.
A suitable regulator is available from Perkin-Elmer (part
no.: 997-0214 for 105-130 V, 60 Hz; 997-0215 for 105-130 V,
50 Hz; or 040-0053 for 190-260 V, 50 Hz).

b) If the lamp formerly could be run at the proper current,


inability to reach the desired current setting can be an
indication that the lamp is starting to deteriorate. The
lamp can sometimes be temporarily regenerated by running
it several hours or by using a Lamp Current Reverser
(303-0395) and running it at 5 mA.

llC. DISPLAY DOES NOT RESPOND

llC,l. Display is completely lit and all indicator dots are lit

The SIGNAL switch is on the SET UP position. Switch to ABS, CONC,


EM CHOP or EM.

llC,2. Display is blank but warning lights DUHall on

The SIGNAL switch is on the LAMP position. 6ZLWFK to ABS, &21&


EM &+23 or EM.

llC,3. The reading on the display will not change

a) The integration time selected is too long.

b) The scale expansion set is too low for analysis (expansion


can be set as low as [ 

c) Keyboard indicator dot is on, indicating that a number has


been entered through the keyboard.

Clear the entry with CE Key or use the appropriate key ('t',
Sl, etc.) to store the entry in the instrument memory.

d) CV or SD indicator dot is on. Press CE to clear the SD


or CV display, and allow the display to function again.

e) If pressing a function key or the CE key does not clear


the display, check that some external accessory (connected
to the remote terminals at the rear of the instrument) is
not shorting one key on. All entries will be ignored until
the short is cleared.
11-3

llD. CALIBRATION
Errors that may occur during calibration are described in Section
8D,8 and in 6HFWLRQ 12.
llD,l. Calibration curves do not pass through zero
a) =HUR improperly adjusted.
=HUR the instrument ZKLOH aspirating a blank solution.
b) Contaminated reagents or solvent were used in the preparation
of standards.
To correct this condition, determine the standard curve vs.
a reagent blank.

llE. INDICATOR '276 21


llE,l. 29(5 CAL dot on
The value on the display is more than 5% greater than the highest
standard used for calibration. Use a standard of higher con-
centration or dilute the sample.
llE,2. KEYBOARD dot is lit
The number on WKH display was entered through the numerical
keyboard and is not an analytical value.
llE,3. The BKDG &255 dot is on
The ' arc source for the background corrector accessory has
been WXUQHG on.
llE,4. BKGD &255 dot is blinking
The background corrector power is below a usable level. Position
the attenuation screen in front of the arc. 6HH 6HFWLRQ 8E,l.)

llF. 5(68/76 48(67,21$%/(


llF,l. Results erroneously high
a) Corrections were not made for reagent blank. =HUR the in-
strument while aspirating a blank solution.
b) An ionization interference is present in the standard or
blank, but due to the presence of an excess of an easily
ionized component in the sample solution, the ionization
is partly overcome.
11-4

Add a relatively large amount of an easily ionized element


to the blank, standards and the samples.
c) 6WDQGDUG solutions have deteriorated or have been improperly
PDGH concentrations are actually lower than the calculated
values.
d) Background absorption (molecular absorption, light scattering,
etc.) is present. This can occur when determining trace
levels of an element in the presence of a large concentration
of a second element, and is particularly likely to be a
problem below  nm or where a high concentration refractory
matrix is encountered. 8VH a non-absorbing wavelength or,
in the case of molecular absorption, go to a higher tempera-
ture flame. If background absorption is hindering the analysis,
it may be advantageous to use the Deuterium Arc Background
Corrector.
llF,2. Results erroneously low
a) Chemical or matrix (bulk, viscosity) interferences are present.
b) 6WDQGDUG solutions are improperly made.
c) Blank solution is contaminated.
llF,3. Cannot get suggested detection limits
a} Insufficient scale expansion and integration time are being
used.
b) The sensitivity for analysis is too low, due to incorrect
flame conditions or because of the use of an incorrect wave-
length.
c} The lamp current is too low for desired stability.
llF,4. Cannot get close to the suggested sensitivity
a) The analysis is being performed on the wrong spectral line.
Many elements have nearby lines, each with different sen-
sitivities. 6HH the Analytical Methods Manual.)
b) Nebulizer sensitivity may vary from one unit to another.
c) Sensitivities with the corrosion resistant nebulizer tend
to be lower than with the standard stainless steel nebulizer.
d) Be sure that the proper flame, as recommended in the Analytical
Methods Manual, is being used. Many elements exhibit very
different sensitivity values with different flames.
11-5

e) Check flame conditions. Many elements are very sensitive


to the fuel-oxidant ratio.

llG. 5(68/76 12,6<

llG,l. Display noisy with flame off

a) Be sure a lamp has been installed in the instrument


(for Atomic Absorption analysis).

b) 6FDOH expansion may be too great for the analytical


conditions selected.

c) Check line voltage; the noise can be due to low voltage


or line transients.

d) May be due to weak lamp emission or lamp arcing. If weak


emission is the source of the problem, it can sometimes
be solved by using a Lamp Current. Reverser. If this does
not solve the problem, it may be necessary to increase
the operating current of the lamp to a value consistent
with the maximum rated current for the lamp and with the
degree of sensitivity loss (if present) which can be
tolerated. If this does not decrease the noise level,
one of the following should be tried:

(1) If consistent with acceptable analytical results,


use one slit setting higher (larger) than recom-
mended.

(2) With the conditions described it may be necessary


to replace the lamp in order to obtain satisfactory
performance.

llG,2. Digital display is quiet with the flame off, but noisy
with the flame on or with the flame on and solution
DVSLUDWLQJ

a) Results are sometimes noisy when determining elements in


the far ultraviolet range (for example when determining
As or 6H  because the flame is highly absorbing. 6RPHWLPHV
using the background corrector accessory will improve results
with these elements.
11-6

b) Another freauent cause is weak lamp emission accompanied


by intense emission from the flame or solution components
causing a high photomultiplier noise level. It can be
corrected by one of the following:

(1) Increase the operating current for the lamp to a


value consistent with the maximum rated current
for the lamp and with the degree of sensitivity
loss (if present) which can be tolerated.

(2) 8VH one slit setting smaller than recommended.

(3) 8VH a new, brighter lamp.

(4) Try a different absorbing wavelength, using the data


given in the Analytical Methods Manual.

(5) In cases where a major solution component is producing


intense emission from the flame, it may be advantageous
to remove that component from the solution by chemical
procedures.

c) If aqueous solutions are aspirated after organic samples


such as oil or MIBK extracts, the absorption signal pro-
duced may be noisy and erratic. Follow the procedure
outlined in 6HF lOB,3 to prevent or eliminate this con-
tamination.

If the instrument has been used extensively with viscous


or organic samples, the burner chamber should be taken
apart and cleaned.

d) To ascertain whether the difficulty is with the instrument,


try several lamps from among copper, magnesium, or some
other element with an absorbing wavelength between 
and  nm where absorption is not dependent on flame
conditions.

e) Check the lamp current setting, slit setting, and fuel and
oxidant flow rates.

f) Make sure the burner is draining properly.

g) Check the nebulizer visually for corrosion around the tip.

h) Check the adjustment of the nebulizer capillary.

i) Check the burner head. It may need cleaning.


11-7

j) Check the acetylene cylinder pressure. It should be


above 520 kPa (75 psig).
k) Check the air pressure. It should be 210 kPa (30 psig).

1) Check the air line filter, especially if there is an


excessive amount of sodium emission in the flame (yellow
flicks). The emission can also be due to contaminated
acetylene.

llH. 5(68/76 DRIFT

llH,l. Baseline drifts with flame on

The double beam system of the spectrophotometer should compen-


sate for any variation in the emission intensity of the lamps.
A drift in the zero or baseline can be caused by one of the
following:

a) Burner not warmed up. The burner should be warmed up


while aspirating a blank solution for 3 to 5 minutes.

b) Blocked capillary.

c) Burner not draining properly.

d) Lamp not positioned properly in holder.

e) At high scale expansions, a slight amount of baseline


drift is to be expected.

llH,2. Readings drift or are not reproducible

a) Check burner head and nebulizer capillary for clogging.

b) Check sample capillary for leaks (punctures).

c) Check nebulizer capillary for corrosion.

d) Check the adjustment of nebulizer capillary.

e) Make sure the burner is draining properly, and that the


burner was warmed up at the start of the run.

f) Make sure the burner waste drainage is not backing up


into the burner chamber.

g) Check the acetylene cylinder pressure and air pressure.


Acetylene cylinder pressure should be above 520 kPa
(75 psig). Air pressure should be  kPa (30 psig).
11-8

h) Check cleanliness and constancy of air supply.

i) The temperature of the solutions can be changed if they


have been placed near the burner area for too long.

j) With certain Electrodeless Discharge Lamps (EDLs)


sensitivity may vary during the first few minutes
of operation. As a rule of thumb, it is good
practice to allow EDLs to warm-up for at least
5 to 10 minutes before starting an analysis.

llI. BACKGROUND CORRECTION


llI,l. The BKGD CORR indicator dot on the digital
GLVSOD\ front panel is blinking

The background corrector power is too low for proper operation.


Position the attenuator screen in front of the arc. 6HH 6HFWLRQ
BE,l.)

llI,2. The D2 arc has less energy than the primary source

a) Check to be sure that the attenuator screen is set on the


out position (see Section BE,l).

b) Check to be sure that the D2 arc is properly aligned. (See


Section lOG,2 for alignment instructions.)

c) For some very bright primary sources (particularly EDLs)


or when operating at wavelengths greater than 300 nm, it
may be necessary to reduce the power to the primary source
or, if consistent with the sensitivity requirements of the
analysis, work at one slit setting larger than recommended
in the Analytical Methods Manual.

d) If the background corrector has been used extensively,


replace the D2 arc (see Section lOG for replacement
instructions).

llI,3. The Background Corrector does not provide adequate


correction

a) Check the amount of background using the BG only position


on the AA/BG energy selector switch on the left front
control panel. As the amount of background increases the
ability of the instrument to correct becomes less. Do
not attempt to correct for more than 1 absorbance unit of
background. (See Section 8E,l for use of the Background
Corrector.)
11-9

b) Check to be sure that the D2 arc is properly aligned


(see Section lOG for instructions).

c) Check to be sure that the primary source is in the


proper position and is aligned (see Section 8C,5 for
instructions) 

llI,4. The analytical results with background correction


are excessively noisy

a) Expect a moderate increase in baseline noise when the


background corrector is turned on.

b) The noise may become excessive if the background corrector


does not provide enough energy (see 11!,2 above).

c) Check the amount of background in the samples using the


BG position on the AA/BG energy selector switch. Expect
increased noise with increased background; don't
attempt to correct for more than one unit of background
absorbance. (See Section 8E,l for use of the Background
Corrector. )

llI,5. Sensitivity is lower in the AA-BG mode than in AA mode

To obtain a higher signal-to-noise ratio when the background


corrector is used, the hollow cathode lamp current is auto-
matically pulse modulated and run at a higher peak current in
this mode, leading to a slight decrease in sensitivity for
some elements.

llJ. FLAME IGNITION AND GAS CONTROL

llJ,l. If the gases do not ignite

a) Check that the fuel and oxidant supplies are turned on,
that all burner regulator controls are properly set,
and that correct pressure and flow rates have been
established. (See Section 8B.)

b) Make sure the burner head is in place and that the pin
on the hold-down cable is properly inserted in the
safety interlock at the base of the burner. If these
conditions are not met, the built-in automatic safety
features will prevent ignition. Also, check that the
drain system is properly installed. If the accessory
drain interlock is installed, the gases will not ignite
unless the drain interlock is connected.
11-10

c) After an extended shutdown (overnight or longer) air


may have diffused into the fuel line supplying the
igniter, and ifnition may not occur until the air has
been expelled by using several IGNITE cycles.

d) Be sure that ignition is being attempted on an air


based flame.

llJ,2. If the burner-nebulizer system flashes back

a) Check for proper flows of fuel and oxidant.

b) Be sure that the gases are connected to the proper


gas inlets on the burner regulator.

c) Be sure the drain hose is connected to the burner and


that there is water in the trap.

d) Check to be sure that there are no leaks and that the


blowout plug (item 19, Fig. 10-1) is properly seated.

e) If using tank air for an air/acetylene flame, check


with the supplier to be sure that it does not contain
an excess of oxygen.
SECTION 12 ERROR MESSAGES

12A. INSTRUMENT ERROR MESSAGES

ERROR CODES EXPLANATION

E-O(X) ERRORS THAT OCCUR DURING THE RUNNING OF SAMPLES.


CATEGORY

A message in this category is displayed instead


of a sample reading, and remains until the display
is updated with the next reading. If a PRS-10 printer
is connected the error code for the erroneous sample
is printed in red.

E-01 Result greater than 9999 (overrange).


Explanation: The range of the display is four digits,
with the possibility of up to two
additional leading zeroes. If the
instrument measures, or calculates,
a larger value, this error is displayed.
Causes: 1) Scale expansion too high.
2) Zero setting incorrect.
3) Sample concentration higher than
expected.
4) Standard used for calibration
was too dilute.

E-02 A) Absorbance range exceeded.


Explanation: The measurement range of the instrument
is approximately 2 absorbance units.
The total includes any off set that
has been removed through autozeroing.
Causes: Samples too concentrated.

B) Electronics Saturated.
Explanation: In the emission mode, the signal is
greater than the dynamic range of
the instrument.
Causes: 1) Standard used to set the GAIN
of the System was too dilute.
2) GAIN value entered via the keyboard
was too high.
Remedy: 1) Aspirate a more concentrated standard
and reset the System GAIN.
2) Enter a smaller GAIN value. (Refer
to the description of the key
function, Section 7).

4/79
12-2

E-04 Error in Calibration Function.


Explanation: An invalid calibration curve has been
computed, with a consequent erroneous
result.
Cause: The concentrations of the standards
or the blank used to perform the calibration
were grossly erroneous. The System
detected an error when it computed
the concentration for this particular
sample. Void all results using that
calibration.
Remedy: Remake the standards, and recalibrate.

E-05 Out of Legitimate Range of Calibration Function.

Explanation: Result falls considerably outside


the concentration range formed by
the blank and the most concentrated
standard.
Cause: Highest concentration standard was
more dilute than the sample.
Remedy: Recalibrate using standards covering
a wider range or dilute the sample.

E-06 Coefficient of Variation Greater than 99%.


Explanation: The Model 560 will only display Coefficients
of Variation up to 99%.
Cause: Samples close to or equal to the concentration
of the blank are being analyzed, with
consequent low mean values. since
CV = (SD x 100) ~ Mean Value, a zero
or near-zero mean value will result
in a very large CV value that has
no meaning.
Remedy: Use the Standard Deviation, which
is insensitive to low mean values.

E-l(X) CALIBRATION ERRORS.


CATEGORY

Error messages in this group are displayed only


during calibration (using Sl, S2 or S3) or during
RESLOPE. The error message remains on the display
until CE is pressed to remove it.
12-3

E-10 Over expand.


Explanation: 1) After Sl is pressed, the computed
expansion factor is greater than
100.
2) Absorbance value to be expanded
is negative.
Cause: Generally, the blank has been aspirated
instead of the appropriate standard.

Remedy: Recalibrate using the proper standard


or enter a smaller value for Sl.

E-11 Standards Out of Sequence.


Explanation: The concentration values for the
standards must be entered in order
of increasing concentration, and
the standards must be aspirated in
the same order.
Cause: Standards not aspirated in the same
sequence as their concentration entries.

E-12 S-Shaped Calibration Curve.


Explanation: The line used to describe the data
points is S-Shaped. The system has
no tolerance for lines with a slope
inversion. (Refer to Section 8D,2).

Causes: 1) Standards used for calibration


have been prepared incorrectly.
2) Three standards have been used
over a linear range. Owing to
truncation of results or System
noise, the resulting data points
do not fall precisely on a straight
line.
Remedy: If Cause 1), Prepare correct standards.
If Cause 2), Repeat the calibration
using a single, or at the most two,
standards.

E-13 Reslope Standard Out of Range.


Explanation: The absorbance of the Reslope standard
is higher than that of the most concentrated
standard.
Cause: The absorbance of the RESLOPE standard
is excessive. It must fall within
the range of the standards used in
the initial calibration.
Remedy: A RESLOPE standard near the middle
of the standard concentration range
is recommended for the best results.
12-4

E-14 S2 or S3 Values Do Not Follow Sl Format.

Explanation: The location of the decimal point is


not compatible with the entry for Sl.

Cause: As discussed in Section 8D,4, the values


of S2 and S3 standards must be con-
sidered when entering the concentration
value for Sl. This error will be found
and indicated if a new value is entered
for Sl which makes S2 and S3 invalid,
and then calibration is attempted using
these incompatible values of S2 and
S3.

Example: If Sl, S2 and S3 are entered correctly,


e.g.

Sl 5.00
S2 10.00
83 20.00

and used to calibrate, then changing


Sl to 6.000 will cause an El4 to be
displayed if recalibration using S2
and S3 is attempted.

Remedy: Re-enter a correct value for Sl.

E-5(X) ENTERED VALUES OUT OF ALLOWED RANGE


CATEGORY

These errors are largely self-explanatory, and are


displayed immediately if a value is entered which
is outside the permitted range of values for the
function. The erroneous value is not stored. Press
CE and enter a correct value.

E-50 Too many digits. (Should be not more than 4 digits).

E-51 Time not in the allowed range. (0.2 thru 60 seconds).

E-52 Expansion factor not in the allowed range. (0.01


thru lOOX)

E-59 S2 or S3 Values Do Not Follow Sl Format

Explanation: The location of the decimal point is


not compatible with the entry for Sl.
12-5

Cause: As discussed in Section 8D,4 the position


of the decimal in Sl determines the
values that are acceptable for,S2 and
S3, as the display will not permit
more than 4 digits.

Example: If Sl was entered as 5.000, then an


attempt to enter 10.0 for S2 will
display an E-59. Sl should have been
entered as 5.0 or 5.00.

Remedy: Re-enter an acceptable value for Sl.

E-6 INVALID NUMERICAL ENTRY


CATEGORY

These errors are an extension of the E-5(X) series,


but occur for specific functions when the entered
value is outside the permitted range, or equals O,
or is fractional. Only integers are permitted for
these functions. The error message remains on the
display until cleaned by the CE key. The erroneous
value is not stored.

E-63 Number of samples to be averaged is not in the range


2 through 99.

12B. DIGITAL-TYPE BURNER CONTROL ERROR MESSAGES

The microprocessor is programmed to detect certain invalid fuel:


oxidant ratios (and shuts down the flame if such combinations
are selected), and also performs checks for satisfactory flows
and flame conditions. If an error is diagnosed an error message
of the form 'E <digit> ' is displayed on the fuel or oxidant
display (if the fault lies with the fuel or oxidant flow). If
the fault is due to an invalid flow ratio, or is caused by the
flame sensor, then E is displayed on the left hand display digits
and the error number is displayed on the right. The explanations
of these messages are given below.

Important: The system will not diagnose error conditions


if the OVERRIDE key has been pressed and the OVERRIDE light
is on. Exercise extra care when using the OVERRIDE mode.

El FLAME TOO LEAN (With nitrous oxide


only, not with air). The fuel to
nitrous oxide oxidant ratio is ~ 0.70,
indicating that the gas mixture is
excessively lean. The error message
occurs only with nitrous oxide, and

4/79
12-6

remains on the display until either


the CHK OXID or CHK FUEL key is pressed.
Check the gas pressure settings and
flow rates before attempting to re-
light the flame.

E2 FLAME TOO RICH


The fuel to oxidant ratio is too high
(~ 0.95 with air oxidant or ~ 1.50
with N o oxidant). The error message
2
remains on the display until either
the CHK OXID or CHK FUEL key is pressed.
(The OVERRIDE key is functional but
will not clear the display.) Readjust
the flow rates.

E3 FLAME SENSOR
The optical flame sensor will generate
an E3 if the sensor receives insufficient
energy from the flame, either because
the flame has gone out, or because
the sensor beam is obstructed. The
error is cleared by pressing either
of the CHK OXID or CHK FUEL keys, or
by pressing FLAME ON/OFF.

E4 GAS FLOW TOO LOW


The oxidant or fuel flow is below 10
units. The error is displayed on
either the fuel or the oxidant display,
depending upon which flow is too low.
The message will remain on the display
until the appropriate CHK key (fuel
or oxidant) is pressed.

4/79
B
(5)

Standard Atomic Absorption Conditions for B

Wavelength Slit Relative Sensitivity Sensitivity Linear


Noise Check Range
(nm) (nm) (mg/L) (mg/L) (mg/L)

Flow spoiler data:


* 249.7 0.7 1.0 13,0 600.0 400.0
* 208.9 0.2 6.8 27.0 1200.0

1. Recorrunended Flame: Nitrous oxide-acetylene, reducing (rich, very red)

Standard Flame Emission Conditions for B

Wavelength Slit Flame


(nm) (nm)

249.7 0.2 Nitrous oxide-acetylene

January 1982
P!FRKH\J -t:.LIV1ER
B

Standard Conditions

-2-

STCX:KSTANDARDSOLUTION

BORON, 5000 mg/L. Dissolve 28.60 g of boric acid, H sBO s, in deionized water
and dilute to 1 liter with deionized water, STORE IN A POLYETHYLENE BOTTLE.

ALTERNATIVE SAMPLING TECHNIQUES

Boron can also be determined utilizing the HGA and the ICP. With the HGA, an
approximate detection limit of 15.0 g/L can be obtained. With the ICP, an
approximate detection limit of 4.0 g/L can be obtained. Refer to the General
Information section for additional details on the use of the HGA and the ICP.

January 1982
PER~'\:IN--ELMER
Al
(13)

Standard Atomic Absorption Conditions for Al

Wavelength Slit Relative Sensitivity Sensitivity Linear


Noise Check Range
(nm) (nm) (mg/L) (mg/L) (mg/L)
-------------~---------------------------------------------------------------------
Flow spoiler data:
* 309.3
396.2
0.7 1. 0
1.0
1. 1
1 1
50.0 100.0
0.7 55.0 150.0
308.2 0.7 1.0 1.5 70.0 150.0
* 394.4 0.7
0.2
0.89 2.2 100.0
150.0
237.3 1. 7 3.3
236.7 0.7 1.8 4.8 200.0
* 257.5
256.8
0.2
0.2
1.2 6.7
7.8
300.0
350.0
1.9

1. Recommended Flame: Nitrous oxide-acetylene, reducing (rich, red)


2. Table contains HCL data. EDL sensitivity values approximately the same.
3. Data collected with an alkali salt (0.1% or more) added to control ionization.

Standard Flame Emission Conditions for Al

Wavelength Slit Flame


(nm) (nm)

396.2 0.2 Nitrous oxide-acetylene

January 1982
PERl''\:IN-ELf\JlER
Al

Standard Conditions

-2-

STOCK STANDARD SOLUTION

ALUMINUM, 1000 mg/L. Dissolve 1.000 g of .Al wire in a mi,nimum amount of (l+l)
HCl, adding a small drop of mercury as a catalyst. Dilute to 1 liter with 1% (v/v)
HCl. Filter the solution to remove the mercury.

LIGHT SOURCES

Both Electrodeless Discharge Lamps (EDLs) and Hollow Cathode Lamps are
available for aluminum. EDLs provide greater light output and longer life than
Hollow Cathode Lamps. For aluminum, both EDLs and Hollow Cathode Lamps
provide approximately the same sensitivity and detection limit.

INTERFEREINCES

Ionization should be controlled by the addition of an alkali salt (0.1 % or more


potassium or lanthanum as chloride) to samples and standards. The aluminum signal
is reported to be enhanced in the presence of iron, titanium, fluoroborate and
acetic acid. Silicon slightly depresses the aluminum signal.

DOUBLETS

The 309.3 nm, 237.3 nm and the 257.5 nm aluminum lines are actually doublets
(309.27 nm/309.28 nm, 237.31 nm/237.34 nm, 257.51 nm/257.54 nm).

ALTERNATIVE SAMPLING TECHNIQUES

Aluminum can also be determined utilizing the HGA and the ICP . With the HGA, an
approximate detection limit of 0.01 g/L can be obtained. With the ICP, an
approximate detection limit of 20.0 g/L can be obtained. Refer to the General
Information section for additional details on the use of the HGA and the ICP.

January 1982
PE '~.(''"'"'1.
.ll j Ll\11ER
Ca
(20)

Standard Atomic Absorption Conditions for Ca

Wavelength Slit Relative Sensitivity Sensitivity Linear


Noise Check Range
(nm) (nm) (mg/L) (mg/L) (mg/L)

Flow spoiler data:


422.7
* 239,9 0.7 1.0 0.092 4.0 5.0
* 0.7 14.0 13 .o 600.0 800.0

Impact bead data:


422.7 0.7 1.0 0.085 5.0 2.0
239,9 0.7 14.0 13 .o 600.0 800.0

1. Recommended Flame: Air-acetylene, oxidizing (lean, blue)


2. Sensitivity with a flow spoiler & N20-C2H2 flame at 422.7 nm: 0.048 mg/L

Standard Flame Emission Conditions for Ca

Wavelength Slit Flame


(nm) (nm)

422.7 0.2 Nitrous oxide-acetylene

January 1982
Ca

Standard Conditions

-2-

STOCK STANDARD SOLUTION

CALCIUM, 500 mg/L. To 1.249 g of primary standard calcium carbonate, CaCO 3,


add 50 mL of deionized water. Add dropwise a minim1,1m volume of HCl (approx-
imately 10 mL), to effect complete solution of the CaC03. Dilute to 1 liter with
deionized water.

LIGHT SOURCES
I
When using the calcium 2.39.9 nm line, the use of a multi-element (Ca-Mg) or (Ca-
Mg-Al) hollow cathode lamp with a quartz window is recommended.

FLAME ADJUSTMENT

The absorption of calcium is dependent on the fuel/air ratio and the height of the
light beam above the burner. Although maximum sensitivity is obtained with a
reducing (fuel-rich) flame, an oxidizing (fuel-lean) flame is recommended for
optimum precision.

OTHER FLAMES

Calcium determination appears to be free from chemical interferences in the


nitrous oxide-acetylene flame. Ionization interferences should be controlled by the
addition of alkali salt (O.l % or more potassium as chloride) to samples and
standards. It is probably preferable to determine calcium in a nitrous oxide-
acetylene flame, especially in samples containing large amounts of silica.

INTERFERENCES

Slight ionization occurs in the air-acetylene flame, and can be controlled by the
addition of an alkali salt (0.1 % or more potassium as chloride) to samples and
standards. Calcium sensitivity is reduced in the presence of elements which give
rise to stable oxysalts. These elements include aluminum, beryllium, phosphorus,
silicon, titanium, vanadium, and zirconium. This effect is reduced by the addition of
0.1-1.0% lanthanum or strontium.

ALTERNATIVE SAMPLING TECHNIQUES

Calcium can also be determined utilizing the HGA and the ICP. With the HGA, an
approximate detection limit of 0.05 g/L can be obtained. Refer to the General
Information section for additional details on the use of the HGA and the ICP.

January 1982
PERr<~N i=.LN12=.R
... v
(23)

Standard Atomic Absorption Conditions for V

Wavelength Slit Relative Sensitivity Sensitivity Linear


Noise Check Range
(nm) (nm) (mg/L) (mg/L) (mg/L)
-----------------------------------------------------------------------------------
Flow spoiler data:
* 318.4
306.6
0.7
0.2
1.0
2.4
1.9
4.6
90.0
200.0
200.0
200.0
* 306.0
305.6
0.2
0.2
1. 5
2.0
4.7
6.2
200.0
300.0
400.0
500.0
437,9 0.2 3.8 7,9 350.0
438.5 0.2 1. 9 8.4 400.0
* 370.4
390.2
0.2
0.2
1.8
2. 1
11.0
13,0
500.0
600.0
320.2 0.2 3.4 13,0 650.0

1. Recommended Flame: Nitrous oxide-acetylene, reducing (rich, red)


2. Data collected with an alkali salt (0.1% or more) added to control ionization.

Standard Flame Emission Conditions for V

Wavelength Slit Flame


(nm) (nm)

437,9 0.2 Nitrous oxide-acetylene

January 1982
PERKIN-ELMER
v
Standard Con di ti ons

-2-

STOCK STANDARD SOLUTION

VANADIUM, 1000 mg/L. Dissolve 1.000 g vanadium metal in a minimum volume of


HN03 and dilute to! liter with 1% (v/v) HN03.

INTERFERENCES

Ionization should be controlled by the addition of an alkali salt (0.1 % or more


potassium as chloride) to samples and standards. An excess of Fe, Al, Ti, or H 3P0 4
increases the vanadium signal. Samples and standards should be matrix-matched to
control these interferences.

TRIPLETS

The 318.4 nm vanadium line is actually a triplet (318.3 nm/318.4 nm/318.5 nm).

ALTERNATIVE SAMPLING TECHNIQUES

Vanadium can also be determined utilizing the HGA and the ICP. With the HGA, an
approximate detection limit of 0.2 g/L can be obtained. With the ICP, an
approximate detection limit of 5.0 g/L can be obtained. Refer to the General
Information section for additional details on the use of the HGA and the ICP.

January 1982
PERKIN-ELMER
Cr
(24)

Standard Atomic Absorption Conditions for Cr

Wavelength Slit Relative Sensitivity Sensit1vity Linear


Noise Check Range
(nm) (nm) (mg/L) (mg/L) (mg/L)
-----------------------------------------------------------------------------------
Flow spoiler data:
* 357.9 0.7 1.0 0.078 4.0 5.0
* 359.4 0.7 1.2 0 .10 5.0 7.0
360.5 0.7 7.7 0. 14 7.0 1.0
425.4 0.7 8.8 0.20 12.0 7.0
427.5 0.7 10.0 0.27 15.0 1.0
* 429.0 0.7 6.9 0.38 20.0 5.0
Impact bead data:
357.9 0.7 1.0 0.041 2.0 3.0
359.4 0.7 1.2 0.054 2.5 4.0
360.5 0.7 7.7 0.068 3.0 3.0
425.4 0.7 8.8 0. 11 6.0 4.0
427.5 0.7 10.0 0. 14 8.0 3,0
429.0 0.7 6.9 0.20 12.0 3,0

1. Recommended Flame: Air-acetylene, reducing (rich, yellow)


2. Sensitivity with a flow spoiler & N20-C2H2 flame at 357,9 nm: 0.31 mg/L

Standard Flame Emission Conditions for Cr

Wavelength Slit Flame


(nm) (nm)

425.4 0.2 Nitrous oxide-acetylene

January 1982
PERKli\J EL!'V1ER
Cr

Standard Conditions

-2-

STOCK STANDARD SOLUTION

CHROMIUM, 1000 mg/L. Dissolve 3.735 g of potassium chromate, K 2CrO i+,


in deionized water and dilute to l liter with deionized water.

FLAMES

The determination of chromium requires a fuel-rich (yellow) air-acetylene flame.


The absorption is sensitive to the fuel-to-air ratio. The sensitivity and stability are
improved by using the three-slot burner head and a slightly luminous flame.

The nitrous oxide-acetylene flame reduces or eliminates many chemical and/or


matrix interferences that occur in the air-acetylene flame, but sensitivity is
reduced.

INTERFEREINICES

The absorption of chromium is suppressed in the air-acetylene flame by the


presence of iron and nickel. If the analysis is performed in a lean flame, the
interference can be lessened but the sensitivity will also be reduced. The addition
of 2% ammonium chloride (NH 4Cl) to sample and standard solutions controls the
interference caused by iron. An excess of phosphate will depress the chromium
response and can be overcome by the addition of calcium. Cr (VI) and Cr (III) exhibit
different sensitivities. It is recommended that if Cr (III) is present, it be oxidized to
give Cr (VI).

ALTERNATIVE SAMPLING TECHNIQUES

Chromium can also be determined utilizing the HGA and the ICP. With the HGA,
an approximate detection limit of 0.01 g/L can be obtained. With the ICP, an
approximate detection limit of 5.0 g/L can be obtained. Refer to the General
Information section for additional details on the use of the HGA and the ICP.

January 1982
PERKll'J ELrv1ER
Mo
(42)

Standard Atomic Absorption Conditions for Mo

Wavelength Slit Relative Sensitivity Sensitivity Linear


Noise Check Range
(nm) (nm) (mg/L) (mg/L) (mg/L)
-----------------------------------------------------------------------------------
Flow spoiler data:
* 313.3 0.7 1.0 0.67 30.0 40.0
317.0 0.7 1.1 1. 1 50.0 30.0
319.4 0.7 1.0 1. 4 65.0 60.0
* 390.3 0.7 10 2.9 150.0
315.8 0.7 0.94 3.5 150.0
* 320.9 0.2 0.76 7.4 350.0
311. 2 0.2 0.77 18.0 850.0
1. Recommended Flame: Nitrous oxide-acetylene, reducing (rich, red)
2. The Mo signal is depressed by the presence of Ca, Sr, Fe and sulfate.

Standard Flame Emission Conditions for Mo

Wavelength Slit Flame


(nm) (nm)

390.3 0.2 Nitrous oxide-acetylene

January 1982
Mo

Standard Conditions

-2-

STOCK STANDARD SOLUTION

MOLYBDENUM, 1000 mg/L. Dissolve 1.840 g of ammonium heptamolybdate


tetrahydrate, (NH 4)sM010244H 20, in! liter of 1% (v/v) NH40H.

OTHER FLAMES

An air-acetylene flame can also be used to determine molybdenum. However,


interferences will be greater when using :this flame. With air-acetylene, the
molybdenum sensitivity is 0.9 mg/L for 1% absorption at the 313.3 nm line.

INTERFERENCES

Calcium, strontium, iron, and sulfate interfere with molybdenum determination by


depressing the signal. These interferences can be controlled by the addition of
0.5% aluminum chloride, 2% ammonium chloride, or 0.1 % sodium sulfate to
samples and standards.

ALTERNATIVE SAMPLING TECHNIQUES

Molybdenum can also be determined utilizing the HGA and the ICP. With the HGA,
an approximate detection limit of 0.02 g/l can be obtained. With the ICP, an
approximate detection limit of 8.0 g/L can be obtained. Refer to the General
Information Section for additional details on the use of the HGA and the ICP.

January 1982
PERKIN-ELr\/1ER
Cd
(48)

Standard Atomic Absorption Conditions for Cd

Wavelength Slit Relative Sensitivity Sensitivity Linear


Noise Check Range
(nm) (nm) (mg/L) (mg/L) (mg/L)

Flow spoiler data:


* 228.8 0.7 1.0
0.90
0.028
11. 0
1.5
500.0
2.0
* 326 .1 0.7

Impact bead data:


228.8 0.7 1 0 0.016 0.75 1.0
326. 1 0.7 0.90 6. 1 250.0

1. Recommended Flame: Air-acetylene, oxidizing (lean, blue)


2. Sensitivity with a flow spoiler & N20-C2H2 flame at 228.8 nm: 0.11 mg/L
3. ~able contairis HCL data. EDL Ben~itivity values slightly (<10%) better.

Standard Flame Emission Conditions for Cd

Wavelength Slit Flame


(nm) (nm)

326.1 0.2 Nitrous oxide-acetylene

January 1982
Cd

Standard Conditions

-2-

STOCK STANDARD SOLUTION

CADMIUM, 1000 mg/L. Dissolve 1.000 g of cadmium metal in a minimum volume


of (1 +1) HCl. Dilute to 1 liter with 1% (v/v) HCl. THIS ELEMENT IS TOXIC AND
SHOULD BE HANDLED WITH EXTRA CARE.

LIGHT SOURCES

Both Electrodeless Discharge Lamps (EDLs) and Hollow Cathode Lamps are
available for cadmium. EDLs provide greater light output and longer life than
Hollow Cathode Lamps. For cadmium, both EDLs and Hollow Cathode Lamps
provide approximately the same sensitivity and detection limit.

INTERFEREINICES

High concentrations of silicate interfere in determining cadmium.

ALTERNATIVE SAMPLING TECHNIQUES

Cadmium can also be determined utilizing the HGA and the ICP. With the HGA, an
approximate detection limit of 0.003 g/L can be obtained. With the ICP, an
approximate detection limit of 4.0 g/L can be obtained. Refer to the General
Information section for additional details on the use of the HGA and the ICP.

January 1982
PERt'\!0.J -ELIVlER
Sb
( 51)

Standard Atomic Absorption Conditions for Sb

Wavelength Slit Relative Sensitivity Sensitivity Linear


Noise Check Range
(nm) (nm) (mg/L) (mg/L) (mg/L)

flow spoiler data:


* 217 .6
206.8
0.2
0.2
1.0
2.0
0.55
0.85
25.0
40.0
30.0
50.0
* 212.7
231.2 0.7 0.67 1.3 60.0 50.0
* 0.7 1.4 12.0 650.0

Impact bead data:


217.6 0.2 1.0 0.35 15.0 30.0
206.8 0.2 2.0 0.51 25.0 40.0
231.2 0.7 o.67 0.79 40.0 50.0
212.7 0.7 1. 4 8.0 400.0
-----------------------------------------------------------------------------------
1. Recommended Flame: Air-acetylene, oxidizing (lean, blue)
2. Sensitivity with a flow spoiler & N20-C2H2 flame at 217.6 nm: 1.8 mg/L
3. Table cont~ins EDL data. HCL sensitivity values slightly (<10%) poorer.

Standard Flame Emission Conditions for Sb

Wavelength Slit Flame


(nm) (nm)

259.8 0.2 Nitrous oxide-acetylene

January 1982
Sb

Standard Conditions
'

-2-

STOCK STAINIDARD SOLUfION

ANTIMONY, 1000 mg/L. Dissolve 2.743 g of potassium antimony! tartrate


hemihydrate, K(SbO)C 4 H 4 0 6 Y2H 2 0 in deionized water and dilute to ! liter with
deionized water. THIS ELEMENT IS VERY TOXIC AND SHOULD BE HANDLED
WITH EXTRA CARE.

LIGHT SOURCES

Both Electrodeless Discharge Lamps (EDLs) and Hollow Cathode Lamps are avail-
able for antimony. EDLs provide greater light output and longer life than Hollow
Cathode Lamps. For antimony, both EDLs and Hollow Cathode Lamps ixovide
approximately the same sensitivity and detection limit.

INTERFERE!NICES

A decrease in absorption occurs with increasing acid concentration. To avoid this


effect, matrix-match the acid concentration of the samples and standards.

ALTERNATIVE SAMPLING TECHNIQUES

Antimony can also be determined utilizing the HGA, the ICP, and the MHS. With
the HGA, an approximate detection limit of 0.15 g/L can be obtained. With the
MHS, an approximate detection limit of 0.1 g/L can be obtained. Refer to the
General Information section for additional details on the use of the HGA the ICP,
and the MHS.

January 1982
PERKIN-ELIV1ER
Te
(52)

Standard Atomic Absorption Conditions for Te

Wavelength Slit Relative Sensitivity Sensitivity Linear


Noise Check Range
(nm) (nm) (mg/L) (mg/L) (mg/L)
---~-------------------------------------------------------------------------------
Flow spoiler data:
* 214.3 0.2
0.2
1.0
0.66
0.43
4.4
20.0
200.0
20.0
* 238.6
225.9
* 0.2 0.49 18.0 800.0

Impact bead data:


214.3 0.2 1. 0 0.33 15.0 25.0
225.9 0.2 0.66 3,7 150.0
238.6 0.2 0.49 13. 0 550.0

1. Recommended Flame: Air-acetylene, oxidizing (lean, blue)


2. Sensitivity with a flow spoiler & N20-C2H2 flame at 214.3 nm: 1.5 mg/L
3, Table contains HCL data. EDL sensitivity values slightly (<10%) better.

Standard Flame Emission Conditions for Te

Wavelength Slit Flame


(nm) (nm)

238 ,3 0.2 Nitrous oxide-acetylene

January 1982
PERKIN-ELi\t1ER
Te

Standard Conditions

-2-

STOCK STANDARD SOLUTION

TELLURIUM, 1000 mg/L. Dissolve 1.000 g of tellurium metal by slowly adding a


minimum volume of concentrated HNO 3. Dilute to about 50 mL with deionized
water. Redissolve the precipitate with a minimum volume of concentrated HCl.
Heat to expel oxides of nitrogen, cool, and dilute to 1 liter with 1% (v/v) HCl.
THIS ELEMENT IS VERY TOXIC AND SHOULD BE HANDLED WITH EXTRA
CARE.

LIGHT SOURCES

Both Electrodeless Discharge Lamps (EDLs) and Hollow Cathode Lamps are avail-
able for. tellurium. EDLs provide greater light output and longer nfe than Hollow
Cathode Lamps. For tellurium, both EDLs and Hollow Cathode. Lamps provide
approximately the same sensitivity and detection limit.

INTERFEREINICES

The tellurium signal is affected by large excesses of Ca, Cu, Si, Na, Zn, and Zr;
therefore, matrix-matching is important.

ALTERNATIVE SAMPLING TECHNIQUES

Tellurium can also be determined utilizing the HGA, the ICP, and the MHS. With
the HGA, an approximate detection limit of 0.1 g/L can be obtained. With the
MHS, an approximate detection limit of 0.02 g/L can be obtained. Refer to the
General Information section for additional details on the use of the HGA, the ICP,
and the MHS.

January 1982
PER~\:ll'J r Ll'V1ER
Bi
(83)

Standard Atomic Absorption Conditions for Bi

Wavelength Slit Relative Sensitivity Sensitivity Linear


Noise Check Range
(nm) (nm) (mg/L) (mg/L) (mg/L)
-----------------------------------------------------------------------------------
Flow spoiler data:
* 223. 1 0.2 1. 0 0.45 20.0 20.0
306.8 0.7 1. 9 1.3 50.0 100.0
* 206.2 0.1 1.6 3.7 150.0
* 227.7 0.7 0.94 6. 1 300.0

Impact bead data:


223.1 0.2 1.0 0. 19 10.0 15.0
306.8 0.7 1.9 0.55 25.0 50.0
206.2 0.7 1.6 1.6 70.0 50.0
227.7 0.7 0.94 2.7 100.0

1. Recommended Flame: Air-acetylene, oxidizing (lean, blue)


2. Sensitivity with a flow spoiler & N20-C2H2 flame at 223.1 nm: 2.1 mg/L
3. Table contains HCL data. EDL sensitivity values approximately the same.

Standard Flame Emission Conditions for Bi

Wavelength Slit Flame


(nm) (nm)

223. 1 0.2 Nitrous oxide-acetylene

January 1982
PERKIN--ELMER
Bi

Standard Conditions

-2-

STOCK STANDARD SOLUTION

BISMUTH, 1000 mg/L. Dissolve 1.000 g of bismuth metal in a minimum volume of


(1+1) HN03. Dilute to 1 liter with 2% (v/v) HN03.

LIGHT SOURCES

Both Electrodeless Discharge Lamps (EDLs) and Hollow Cathode Lamps are
available for bismuth. EDLs provide greater light output and longer life than
Hollow Cathode Lamps. For bismuth, both EDLs and Hollow Cathode Lamps
provide approximately the same sensitivity and detection limit.

DOUBLETS

The 223.1 nm bismuth line is actually a doublet (222.8 nm/223.1 nm).

ALTERNATIVE SAMPLING TECHNIQUES

Bismuth can also be determined utilizing the HGA, the ICP, and the MHS. With the
HGA, an approximate detection limit of 0.1 g/L can be obtained. With the MHS,
an approximate detection limit of 0.02 g/L can be obtained. Refer to the
General Information section for additional details on the use of the HGA, ICP, and
the MHS.

January 1982
PERKIN~ELl\l1ER

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