HP 6890 series User manual
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2
Linearity
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3
The filters are mar ed on the edge with the transmission wavelength.
Each filter has a mirrored sideĊwhich must face the flame when
installedĊand a colored surface.
The sulfur filter is blue/purple and transmits at 393 nanometers.
The phosphorus filter is yellow/green and transmits at 525 nanometers.
The HP 6890 FPD uses an inert fused silica insert liner in the transfer
line. This allows fused silica columns up to 530 ID to run right to the
base of the flame, minimizing sample tailing or loss on chemically active
sites. The liner is also compatible with standard pac ed columns.
The FPD flame produces considerable water vapor. The detector must be
operated above 120°C to prevent condensation.
Unnecessarily high temperatures can cause thermal decomposition of
many thermally labile phosphorus and sulfur compounds.
Detector temperature can have a significant effect on sulfur sensitivity. If
analyzing compounds with high boiling points, the detector temperature
should be set to 25°C above the final oven temperatureĊif allowed by the
temperature limit of 250°C.
Temperature set below 120C
Air or hydrogen flow set at or set at
Ignition failure
4
Detector shutdown
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Column installation
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6
Changing wavelength filters
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WARNING
7
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8
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Installation Printed circuit board Ignitor and heater
9
Lit off et " ! !
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Lit off et
Lit off et
! # # # !
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Procedure: Changing the Lit offset setpoint
Lit offset
ąCONFIGURE FRONT DET
Mkup ga type N2
Lit off et 2.0 <
Electrometer On
1. Press [Config][Front Det] or [Config][Back Det].
2. Scroll to Lit off et and enter a number.
The default is 2.0 A.
Enter 0 to disable the automatic reignite function.
The set oint range is 0 to 99.9 A.
10
Flame ignition sequence
$!) !%/$!- *" /$! "'(! %#)%/%*) (!/$* . *) /$! )!3/ +#! %. 0.! /$!
0/*(/%''4 +!-"*-(. /$%. .!,0!)!
0-). '' !/!/*- #.!.5%- $4 -*#!) (&!0+5*"" --%!- -!(%).
*)
!/. %- "'*2 /* ((%)
0-). /$! #'*2 +'0# %#)%/*- *)
(+. /$! $4 -*#!) "'*2 "-*( /* ((%)
!.!/. /$! %- "'*2 /* /$! %- "'*2 .!/+*%)/
!.!/. /$! $4 -*#!) "'*2 /* /$! $4 -*#!) "'*2 .!/+*%)/
0-). /$! (&!0+ #. *)
*(+-!. /$! .%#)' $)#! 2%/$ /$! Lit offset 1'0! " /$!
$)#! %. #-!/!- /$) Lit offset !'-!. /$! "'(! *) '%/ " %/ %.
'!.. !'-!. /$! "'(! *"" )*/ '%/
*- /$%. +-*!.. /* 2*-& /$!-! (0./ ! !)*0#$ %- +-!..0-! /* /$!
+)!0(/%. (* 0'! /* +-*1% ! ((%) "'*2 ! -!*((!) .0++'4
+-!..0-! *" +.%
Lighting the flame
Manual
ą FRONT DET (FPD)
Temp 250 250
H2 low 50.0 50.0
Air low ā60.0 60.0
Mode:Col+mkup=const
Combined low 15.0
Mkup (N2) 50.0 50.0
Flame O <
Output 0.0
Flame
Automatic
!
Lit o set !
12
Electrometer on/off
T e Configure Detector control table contains an Electrometer
On/Off setpoint.
If the photomultiplier tube is
exposed to room light with the electrometer on, the tube will be destroyed
!
Always turn t e electrometer off before removing t e PMT ousing to
avoid destroying t e tube.
Electrometer data rates
Analog output for t e FPD can be presented at eit er of two speeds. T e
faster speed allows minimum peak widt s of 0.004 minutes, w ile t e
standard speed allows peak widt s of 0.01 minutes.
Procedure: Using fast peaks
If you are using t e feature, your integrator must be fast
enoug to process t e data coming from t e GC. It is recommended t at
your integrator bandwidt be at least 15 Hz. To use fast peaks:
CONFIGURE SIGNAL 1
Fast peaks On < 2.
1.
Digital output to t e C emStation is available at 11 speeds from 0.1 Hz to
200 Hz, capable of andling peaks from 0.001 to 2 minutes wide. Output
to an INET integrator is available at 20 Hz. Consult Signal Handling" in
t e volume for a discussion of t e different rates.
T e feature does not apply to digital output.
Caution
13
( ( (#! *'#' "$*! ,) ),$ $*(#( $# ,) (*!*'
!)' # ) $)' ,) %$(%$'*( !)' *( ) $%)"*" (
!$,( $' )( !"#)( ' &*) '#) %'$'"# $ )( ))$'
( #(('!- $"%'$"(
))$' "$*#)( # ) %$()$# # ( ) - ) )
# )'( ()%$#) ( *)$")!!- () - )
) ()%$#)
,$ (#! ##!( # ),$ !)'$")' $'( ' *( $# $'
) $#)'$! )! '*#( ) ))$' ,! ) '$#) )
$%')( # (%! /(#! $#!- "$ -%! )!( $' *! ,+0
!#) '
ą FRON DE (FPD)
Output 178.9
ą BACK DE (FPD)
emp 250 250
H2 flow 50.0 50.0
Air flow ā60.0 60.0
Mode:Col+mkup=const
Combined flow 15.0
Mkup (N2) 50.0 50.0
Flame Off <
Output 119.2
) .$# ( ((# )$ ) '$#) ) %$()$# # / ) )-%
"(") ,!! !' $ $+'' )( %'(( $# ('$!! )$ )
Instrument !# # %'(( #)' '$!! )$ ) F det !# %'((
$-% # (!) Sig only FPD
14
Gas Type Suggested Flow
for Sulfur
Suggested Flow
for Phosphorus
Carrier gas
(hy rogen, helium, nitrogen, argon)
Packe columns 10 to 60 mL/min 10 to 60 mL/min
Capillary columns 1 to 5 mL/min 1 to 5 mL/min
Detector gases
Hy rogen 50 mL/min 150 mL/min
Air 60 mL/min 110 mL/min
Carrier + makeup 60 mL/min 60 mL/min
Supply pressure: Air supply pressure must be at least 90 psi for the ignition sequence.
All others, a equate to achieve esire flows.
Detector Temperature
Below 120°C, flame will not light
Set temperature about 25°C higher than highest oven temperatureĊlimit is 250°C.
Lit offsetą[Config] [Front Det] or [Back Det]
If the etector output with the flame on minus the output when the flame is off falls below
this value, the FPD attempts to reĆignite twice. If output oes not increase by at least this
much, the etector shuts own.
The recommen e setting is 2.0 pA.
A setting of 0 or [Off] isables autoignition.
15
Hydrogen flow, L/ in
Air flow, L/ in
Press [On] to ignite fla e
Turn off for packed colu ns.
For capillary colu ns, see
makeup gas flow mode below.
Te perature, C
To change makeup gas type,
press [Mode/Type]:
To view makeup gas or change Lit offset, press
[Config][Front Det] or [Config][Back Det]:
Select the appropriate gas.
ą FRONT DET (FPD)
Temp 250 250 <
H2 flow 50.0 50.0
Air flow ā60.0 60.0
Mkup (N2) 50.0 50.0
Fl me Off
Output 0.0
Displays output value.
Makeup gas flow mode:
If colu n di ensions are specified, the control table will also include one of these:
F DET MAKEUP MODE
*Const m keup flow
Col+m keup=const <
Mode:Col+mkup=const
Combined flow 0.0
M keup flow 0.0
Mode: Const m keup <
Mkup flow 0.0 Off
To change makeup mode,scroll to Mode: and press [Mode/Type].
Make a selection and enter the appropriate flow values.
ąĄCONFIGURE FRONT DET
Mkup g s type N2 <
Lit offset 2.0
Electrometer On
ąFRONT DET MAKEUP GAS
Helium <
*Nitrogen
Press [Front Det] or [Back Det].
Makeup gas type
It is not necessary to turn the electro eter
on or off unless you are perfor ing a
aintenance procedure.
16
Procedure: Using the FPD
Verify that all dete tor gases are onne ted, a olumn is installed, and the
system is free of leaks. Che k the oven temperature, inlet temperature,
and olumn flow. Use Figure 3 as a guide when operating the FPD.
Verify that a olumn is installed or the FPD olumn fitting is plugged
before turning on the air or hydrogen. An explosion may o ur if air and
hydrogen are allowed to leak into the oven.
1. Press [Front Det] or [Ba k Det] to open the FPD ontrol table.
2. Set the dete tor temperature. The temperature must be greater than
120C for the flame to light.
3. Change the hydrogen flow rate, if desired, and press [Off].
4. Change the air flow rate, if desired, and press [Off].
5. If you are using , turn off the makeup gas and
pro eed to Step 7.
6. If you are using :
a. Verify that makeup gas type is the same as that plumbed to your
instrument (next to Mkup line of ontrol table). Change the gas
type, if ne essary.
b. If your apillary olumn is and is onne ted to an EPC
inlet, hoose a new flow mode, if desired, and set the makeup gas
flow or ombined flow.
. If your apillary olumn is or is onne ted to a nonEPC
inlet, enter a makeup gas flow. Only onstant flow is available.
7. S roll to Flame and press [On]. This turns on the air and hydrogen
and initiates the ignition sequen e. On ignition, the signal in reases.
Typi al levels are 4 to 40 pA in sulfur mode, 10 to 70 pA in phosphorus
mode. Verify that the flame is lit by holding a old, shiny surfa e, su h
as a mirror or hromeĆplated wren h, over the vent exit. Steady
ondensation indi ates that the flame is lit.
WARNING
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