Alliance Separations Module

Functionality
Warranty
2695
Options
Layout

©2007 Waters Corporation

 Alliance®
Alliance ® Warranty

Assemblies/Serviceable parts Warranty

Solvent manager drive mechanics 2 years or 200,000 injections

Sample manager drive mechanics 2 years or 200,000 injections

Seal pack assembly 1 year or 15,000 injections

All other assemblies 1 year

2
 Product Warranty
Period
General Product Warranty as it applies to any new instrument

Instrumentation Item(s) Instrumentation Component(s) Warranty Period

Electronic and Mechanical Total instrument except for maintenance 1 year (12months) from date of
Assemblies parts, operating supplies and expendable shipment, unless otherwise stated in
components. the user documentation (e.g., 2695s
have a 2-year warranty for the sample
manager and solvent manager drive
mechanisms)

Normal Wear and Maintenance As defined in the instrument Performance 90 days from date of shipment
Parts Maintenance Kit (if available)
Or for individual maintenance parts as listed
in the user documentation.

Operating Supplies and Autosampler vials, solvent and sample Warranted to function properly when
Expendables filters, and fuses. delivered.

Software Item(s) Software Component(s) Warranty Period

Software (Media Only) CDs and diskettes 90 days from date of shipment

Software Performance 90 days from date of shipment

3
 2695 Separations Module

 Alliance® Systems Support

 2695 Features

 Available Options

 Component Overview & Layout

 2695 Features

• Solvent Management vs. Pump • Detector flexibility

• Sample Management vs. Autosampler – UV (2)
– RI (1)
• Integrated Solvent & Sample Manager

2690XE
Base 2690 • Base 2690 plus:
 Quaternary GPV • Inline degasser
 120 sample vial capacity
— Std. 2ml vials with optional LVI • Column heater or Column heater/cooler
 Independent needle wash
• Sample Heater / chiller
 Independent plunger seal wash
 Helium Sparge - solvent conditioning*
 IEEE & RS232 controllable
 Floppy disk drive
 Solvent bottle tray*

5
 Options

 2695  Field Installable Column

Switching Valves
— Syringes – µL — 2 Position Regeneration
o 250µL - standard — 3 Position Selection
— 6 Position Selection
o 25µL, 2500µL
— Sample Loops – µL
o 100µL - standard
o Variable up to 2ML
— Bar Code Reader Upgrade
— Weight = ~130lbs
— Volume = <650µL
— # Samples - 120

 Column Heater
— Without Valve (default)
 Column Heater/Cooler

6
 Alliance Option Kits

 All options are field installable:

— Plunger Seal Wash (WAT270872)

— PerformancePLUS Degasser Tray (WAT270873)

— Sample Heater Cooler (WAT270802)

— Column Heater (186001863)

— Column Heater / Cooler (186001791)

o 3Column Switching valves
– Three-Column Select valve kit 205000162
– 2 Column regeneration valve kit 205000163
– Six-Column Select Valve kit 205000164

— Vial Bar Code (Discontinued) (176000114)

– 128/C, ASCII, Numeric Only (6-digits)

7
 Component Layout
Left Side

Right Side

Rear Panel

8
Alliance® Solvent Conditioning
— Tubing Flow Path

—Piston Drive

—GPV

—Degasser Assembly
oOld Style
oCurrent Style
Alliance Start Up Flow Chart
2695

10
Priming the Solvent
Manager
• Properly degas your
solvents before introduction

• Use solvent with the lowest

viscosity for initial priming

11
 Principal Primes
Solvent Manager

 Dry Prime:
— Opens the fluidic path to replace air with solvent, then performs a
prime.
 Wet Prime:
— Replaces solvent in the path from the reservoirs to V1 & V2 and then to
waste (V3). Used to change solvents in the system.
 Seal-Wash Prime:
— Lubricates each plunger & flushes away solvent or dried salts. Extends
the life the plunger seals.

 Needle-Wash Prime: Sample Manager

— Flushes the needle in the Sample Management system
preventing carryover or contamination. Extends the life of the
injector seals.

12
 Dry & Wet Prime

 Use “Dry” Prime when the system is dry.

 Use the “Wet” Prime to change solvents or if instrument has been

idle for a long period of time.
— Run slow flow following to replace with degassed solvent.

 Complete Remaining Prime Functions.

13
 Solvent Management –
Serial Flow Path

Prime/Vent Valve

D A
Inlet Inlet
Checkvalve Checkvalve

Front B
C

14
 Piston Drive Tray

Vent Filters Piston Drive Motors

Plunger Driver Board

Accumulator Piston Drive

Checkvalve
Primary Piston Drive

Prime / Vent Valve

Top = Acc
Transducers Bot = Pri

Plunger Wash Pump

Checkvalve

15
External Tubing

2795
Only

16
 Solvent Conditioning
 Modified GPV assembly
— Internal accumulators (diaphragms)
— High Flow tubing - yellow (.040”)
— Standard tubing - black (.030”)
— Low Flow tubing - green (.020”)

There is a 5msec pause before

voltage is applied to the next
valve so that no more than one
valve is open at any time.

17
 Alliance Solvent Conditioning
• Sparge Assembly Tray
– Industry standard 1/8”
fittings

PerformancePlus Degasser Chamber

Recommended Max 5mls/min

Flow rate

Internal Volume 500uls

Internal Tubing 0.045”

• Current Style
Diameter Degasser Tray
Flush Volume (4x) 2mls
– 4 channel only

18
 Current Degasser

 Vacuum Pump runs at High Speed (400 RPM) until a

vacuum level of 0.9psia is reached.
— Once 0.9 is reached within 10 minutes, then the speed drops
down to 60 RPM

400 RPM

0.9psia

60 RPM
6.5psia
Vacuum motor RPM
Vacuum level PSIA

19
 Screen Hierarchy

Dual Mode Concept

Main menu screen Status screens

• Used to access main • Used for direct control
software

20
2695 Status Layout

Only the options

installed will be
displayed.

21
Direct Functions

22
Alliance® Solvent Manager

 Solvent Pump Tray

 Head Assembly –
Cross Section

 Online mixing is
accomplished in the head
assemblies

 Solvent enters the head

through the ‘J’ Tube
— First in = First out

 140ul plunger cavity volume

24
Flow
Path

Head
Assy.

25
 Stroke Volume

 Stroke volume is pre-set in the

“Default Separation Method” to
130uL.

 Selection of an alternative stroke

volume is recommended,
depending upon flow rate – refer
to the table below:

Flow range (ml / min) Stroke volume (µL)

0.010 – 0.530 25
0.531 – 1.230 50
1.231 – 3.030 100
3.031 – 10.000 130

26
 Bubble Detection

 Activates:
— 650psi or higher

 Compression / Decompression Ratio:

— 1 - 1.4 = Normal
— 1.4 -1.8 = Fair
— > 1.8 = Bubble Detection Occurs

 Bubble Recovery Mode

— Pre v2.02 only

27
 Operating Pressures

Flowrate setting Maximum Operating Pressure

0.001mL – 2.999mL 5000psi
3.0mL – 4.999mL (linear decline) 5000psi – 4000psi
5.0mL – 10mL 2000psi

Pressure 5
(kpsi)
4

0
1 2 3 4 5 6 7 8 9 10
Flowrate (mLs/min)

28
2695 Injection Flow Path

Injection Sequence
Sample Manager Main Components

Clear Tubing

Red Line
- solvent out Blue Line - solvent in

Seal Pack

30
Purge Cycle - Part I

Needle in stream
Position

31
Purge Cycle - Part II

32
Purge Cycle Part III (Compression Check)

Needle
in lower seal

33
Injection Cycle

V2 & V3 Open
to equilibrate
the Sample Loop

Needle in
Seal Position

34
Sample Withdraw - Part I

Needle in Vial

35
Sample Withdraw - Part II

Needle in Vial

36
Sample Injection

37
 Alliance® Sample Managers

 Components
 Inject Sequences
 2695 Sample Management
 5 carousels
— 24 vials each (120 total)
— Color coded and alphabetized (A-B-C-D-E)
 Rebuildable seal pack
 Std. Syringe 250µl
— (25 & 2500 optional)
 Std. 100µl sample loop
o Configurable options
 Vial detection
— Fiber optics
— Flashing red LED

Internal L/Inch L/cm

Diameter

.005” 0.3 0.118

.009” 1.04 0.41

.010” 1.29 0.507

.020” 5.15 2.03

(+/-)
.030” 11.58 4.06

.040” 20.6 8.1

39
 2695 Sample Manager

Carousel Drive Transducer Needlewash Pump

Syringe Drive
Col Htr Bd

V2

V3
Injector Assy.

V4

V1

Carrier Drive
Bar Code Reader

40
 New Style Injector

 Enhanced version
injector assembly
 Uses existing Seal Pack
Rebuild
 Backwards Compatible

41
 Transducer

 The system pressure transducer measures the operating

pressure. A software algorithm compares the primary head
pressure and the system pressure readings and regulates
the pre-compression step to balance the pressures,
providing a smooth, ripple-free flow.
Current

Obsolete

42
 2695 Needle wash

 The needle wash system consists of a 24 VDC diaphragm

pump and a 3-way solenoid valve (V4) on the input side of
the pump that opens to admit wash fluid and closes to
admit air.

43
 Solvent Select Valves

Three Position Six Position Two Position

Select Valve Select Valve Regeneration Valve

• Example of plumbing • Used on 2nd Generation • Regenerant used to keep

– Column Alliance Column Heater. off-line column
– Waste for HT flushing equilibrated
• New Column Heater works
– Restrictor for MS with 2695, 2695D, 2795 • Regenerant pump
Flow Injections and 2796. – 510, 515, 600, etc

44
Sample Heater Cooler

 4º – 40ºc

 Temperature
degradation
point = 29º

 Rear Panel with

Sample Heater
Cooler Removed

45
Sample Heater / Cooler
Current Style

Temperature
Probe

2” Internal Fan for

circulation

2 – 4”
External
Fans

Heater Chiller
Engine

See Service
Side Mounted Note:
Control Bd. for
easier access 2690 Heater
Chiller Update
46
 Original Alliance Column Heater

 4 column capacity
 Preheat tube
—  1ml not necessary
– Coil red line in column heater
—  Install preheat tube and coil red line
 See Service Note:
— Repair of Alliance Column Heaters
 Externally connected
— Interconnect cable
– Column heater interconnect board

Do not connect or remove while live

Damage to COMM port on CPU will occur

47
Old, New, and Newest

48
2nd Gen Col Htr & Column
Heater/Cooler
• 2 columns up to 300mm w/guard columns
• A grommet for mounting a calibrated thermister for
qualification
• A smaller door hinge allows tubing to be routed out the
right side
• No pre-heater tubing
• The switching valve has been moved forward for easier
access
– Alliance Column Heater/Cooler
– From ambient –15°C up to 65° C
– Internal power supply to drive the heater cooler engine
– Separate power switch on right side
– Alliance Column Heater
– Ambient to 65° C
– Similar heater coil for convection heating
• Both models:
– Interface 2695, 2695D and 2795, (minimum Rev. 2.02)
– Common PCB, includes valve driver circuit

49
2695 Diagnostics
 Diagnostics

2690 2695

51
Run Samples Diagnostics

52
Compression Check & Adjust Seals

53
Other Diagnostics

54
Other Tests

55
Other Tests - cont.

56
Other Tests - cont.

57
 Service Utilities

Password = 1147

See Service
Note on
Transducers

Seal Wash
Pump
Activation

• Default at start-up
• Not necessary with
current vacuum sensor

Contact Global Service Support before making adjustments

58
 Alliance® Service Procedures
—PM Procedures
oPM Test
—Calibration Protocol
 Plunger Drive Assembly

Follow steps closely

Indicates
Direction of
Solvent Flow

1/8” – ¼”
Turn Only

60
 Check Valve Summary
New Desc. Old Desc. Material P/N (2) PM Kit Application Used With

PerformancePLU PerformancePLU Ruby 700000254 Y Standard Check 2695, 2795,

S R/S CV Cart. S Sapphire CV Sapphire Valve 515, 600,
(2) Cart. (2) 1/8 1525

PerformancePLU PerformancePLU Ceramic 700002399 N Option – sticking 2695, 2795,

S C/C CV Cart S Ceramic CV issues, wide range 515, 600,
(2) Cart. (2) of flow rates 1525

2X95 R/S CV 2690 Inlet CV Ruby WAT270941 N Option – Lower 2695, 2795
Cart. (2) (2) /Sapphire Internal Volume
1/16”

2X95 C/C CV Separations Ceramic/Cer 700002761 N Option – sticking 2695, 2795

Cart. (2) Module Ceramic amic. 1/16” issues, lower
CV Cart. (2) internal volume

Discontinued Separations Ceramic 700002333 N Discontinued Replaced by

2X95 Ceramic Module Ceramic 1.75 700002761
CV CV Cart. (2)

Ceramic Ball & Seat = Cartridge will

have ‘C’ stamped on it.

1/8” = PEEK Gaskets

1/16” = Black Gaskets
61
Rebuilding the Head and Seal Wash
Chamber • Seal Wash Face Seals
– Not Replaced
• Seal Wash Plunger Seal
(WAT270160)
• 2- Seal Wash Tube seals
(WAT270669)
(Not in 2695 PM kit)
WAT271017

• Face Seals (WAT270163)

– 4 = 2 in each head
• Plunger Seal (WAT270789)
– 2 = 1 in each head

62
 Service Procedures

 Head seal replacement

— Plungers seals Orange, Floraloy G material
— Face seals Standard seal
Good for most
applications
• Seal wash chamber seal replacement Mix of organic / H2O

– Plunger seals Black, GFP material

– Face seals Optional seal

– Tube seals Good for 100% organic

Clear, UHMWPE material
• Seal pack rebuild
Optional seal
– HP seals / misc. components
Good for 100% organic

63
 2695

Sample Manager
 2695 Performance Maintenance Kit

P/N# WAT270944

 Solvent filter WAT007272 1

 Oriented plunger WAT270488 2
 Check valve cartridges 289000144 2
 Face seals WAT270163 4
 Plunger seals WAT270789 2
 Seal pack rebuild kit w/needle WAT271019 1
 Seal wash tube seal WAT270668 4
 Seal wash plunger seals WAT270160 2
 Syringe WAT073109 1
 Battery WAT080443 1
 Filter Retainer 405001171 1
 Solvent filters WAT025531 4
 Filter insert WAT088084 1

65
 Performance Maintenance
Visit Features

 During the Performance Maintenance Visit the FSE will check

whether the current version of firmware is installed
— If the instrument is not at current revision, the FSE consults
with customer to advise about the features/benefits of the
latest version
— The FSE reviews the error log (Alliance) or trace log (ACQUITY)
for potential issues
o During a corrective repair event the FSE can review the logs to help
troubleshoot the issue

66
 Specialty Tools

Seal Extraction Tool 2695 Seal Insertion Tool

WAT039803 WAT270969

Standard Seal
High Insertion Tool and
Pressure
Seal Insertion
Seal Guide
Tool & Bullet WAT024923

WAT045427

67
Old Seal Pack Rebuild

68
 Original 2695 Injector

• Be sure to wet the Needle and Seal

Pack before assembling.
• Internal needle volume approximately
80µL.

~2mm

.044”
.057”
60° .020”

.015”

69
New Style 2695 Injector
Injector- 700002789
Injector Upgrade Kit- 700002790
Spare Seal Pack- 700002791

70
Injector Removal

Remove/Install
Sample Loop
using 2- 5/16”
wrenches
through the slot
in the Injector
Assembly

71
Seal Pack / Needle Removal

In all pictures, Old Design on

Left – New Design on Right

72
 Seal Pack Adjust
 The 2695 determines the top and bottom of the lower seal in
motor steps relative to the STREAM position. From these it then
derives the SEAL position.

 The correct needle position depends on the particular needle, and

seal pack assemblies. Any change in these assemblies will
therefore require a new adjust seals operation to reprogram the
2695 for the correct step counts.
73
Hands On exercise – PM

 Complete PM on 2695

o Rebuild Solvent Manager

• Check Valves
• Head Seals
• Seal Wash Seals
• In-Line Filter

o Rebuild Sample Manager

• Rebuild Seal Pack &
Needle
• Replace Syringe
• Rebuild V1
• Replace Battery

 Re-initialize
 Static Leak Test
 Seal Pak Adjustment

74
 Qualification

 Flow rate Accuracy

— Using a 10ML & 25ML Flask measure 0.5, 1.0 & 5.0mls/min
 GPV Testing
— Review procedure
 Injection Accuracy
— Fill a 2ml vial with pre-slit septum's with water
— Zero balance and record weight
— Perform 6 - 50µL injections
— Zero balance and record weight
— [(w1-w2) / 6] x 1000 = µL per injection
 Sample Heater / Cooler Temperature Accuracy
— Using a calibrated thermocouple, place over the center of the
carousel and close door.
Make sure probe does not make contact with any surfaces.

75
Troubleshooting Common
Errors
 General Troubleshooting

 There is no instant cure for any problems encountered

— Good old fashion troubleshooting.
— Take your time to understand the problem.
— Check the simple things first.
— Understand chemistries, flow rates, solvent conditioning and etc.

 Use error code handout as a reference

— Company Confidential

 Slower flowrate than programmed

— Measure battery - 3 volts?
— Proper contact

77
 Software Update Loading Errors

 Test function of disk drive:

— Create method, export method to disk, delete method from memory
then import method
— Change position of disk protection tab
 Program disk?
— Perform checksum on disk
— Try transferring all files to newly formatted floppy disk and retry
installation
 Errors from new CPU PCB.
— “Fatal error.”
– Immediately after installation or next power up.
— A “clear ram” must be performed on a fresh software load
immediately after loading software.
– A “clear ram” may be needed on software updates only if error occurs.
– Back up programs before clearing ram.

78
 Solvent Delivery Issues

 Bubble detected
— Criteria: >650psi and C/D ratio >1.8
 Check:
— Tubing connections
— Degasser
— Chamber efficiency (flow rate)
— Stroke length not excessive
— Seals, check valves
 Loss of prime
— < 25psi system pressure
— Criteria: 50 cycles
 Solvent delivery hardware fault
 Plunger homing overpressure
— Transducer out of range

79
 Static Leak Test Fails

 SLT is an automated ramp and decay for solvent delivery

system
— Accumulator ramps to 5000psi
— Primary ramps to 4000psi
— Refer to service note
 Criteria
— %Volume = <20% (compress solvent to pressure)
— Decay rate <300psi/min (measures decay)
 Check the obvious first
— 100% MeOH
— Degas solvent, run in continuous mode or 100% Sparge
— Prime system at slower flow and for longer
— Check fittings
— Use new SS pin plug
— Seals, check valves - re-energize seals
— Rinse and wipe off head face seals
— Check Prime / Vent Valve (may be rebuilt using WAT270936)
 Dead end at outlet of System Transducer

80
Static Leak Cont.

 If system is ramping up but not in sufficient time try using

RS232
- Type in edit pumprampdecayconfiguration, Then
change the following parameters
- CoarseFineDeltaPress(200) change to 100
- DecayAcquisitionTime(1.5) change to 3
- MxPctCompression(20) change to 40
- Then try test again

81
 Sample Management Issues

 Compression test
— Ramp and decay for sample loop area
— Parameters set using methanol, 100ul sample loop and 250ul
syringe

— Parameters: 2690
2695
– Compression pressure 300psi 100psi
– Compression volume 20ul 20ul
– Decay time 1.0 min 1.0 min
– Delta decay 50psi 50psi

82
Alternate Compression
Parameters
• For systems containing a larger Syringe,
– Refer to service note

Parameter Description Range Typical Value

Compression Pressure Sets the target pressure for the 30 to 300 psi 300 psi
compression check (2 to 20 bar) (20 bar)
Compressible Volume Sets the maximum volume that
25 ul syringe the syringe is displaced to 1 to 15ul 15ul
250ul syringe produce the compression 5 to 30ul 20ul
2500ul syringe pressure 5 to 100ul 50ul
Decay Time Sets the amount of time that .01 to 5.0 min 1.0 min
the system is kept at the
compression pressure
Maximum Delta Decay Sets the maximum difference in 10 to 100 psi <50 psi
pressure between the beginning (0.7 to 7 bar) (<3.45 bar)
and the end of the decay time
See Service Note
11/11/1999 Under
2690
83
 Compression Test Fails
- What to Do ?
 System is low volume
— Leaks are not always visible
 Manually purge valves and syringe
— Observe syringe barrel during purge
 Be sure Degasser is on
 Check fittings, syringe, tubing
 Pin plug V3 outlet when compressing to verify or eliminate
V3 failure
— Observe waste tubing during compression test for obvious V3
failure
— New style V3 introduced – see Service Note:
– Improved V3 Solenoid for 2690

84
 Sample Management
- Issues
 LVI’s breaking
— Refer to release notes for specific vial info
— Program needle offset (method specific)
 Ghost peaks:
— Refer to modified frit service note
— Attempt all traditional methods first
— Modified frit retainer (WAT035362)
– Needle wiper to increase seal wash volume
– There are risks

See Service Note

06/24/1998
Under 2690
85
 Sample Management
- Issues
 Seal Pack Geometry Fault:
— Indicates Injector Sensor Bracket may need adjustment
— Failed seal pack adjustment
— Top, bottom, width
 Test failed?
— 1000psi <3ml, prefer 1- 1.5ml/min
— Degas continuous
— Check sensor bracket height for 5/16”
— Test high pressure valves
— Rebuild S/P, energize seal pack seals

86
 Fatal Error

 Operating software error

 System locks up
 Re-power, maybe temporary glitch
 Check for loose cables, IC chips
 Check voltages
— Battery also
— New CPU / software load
– Perform “clear 8”
 Last effort before CPU replacement
— “Clear 0”

87
Questions?

88
Resources
 Worldwide Service Support
— Technical Inquiries
 www.waters.com
o 1-800-252-4752 x:8070
o Fax: 1-508-252-8469 — Waters Elite Support Center
— Service Notes Databases
— Operators Manuals
 Support Tools
— Applications and Brochures
— Startup & Troubleshooting Video
— Webcasts — FAQs
— White Paper — Graphical Parts Locator
— ESM (online)
— Service Notes

89
2695 Specifications

90