BIC BI-200SM User manual

~. .
Instruction Manual
for
BI-200SM Goniometer
Ver.2.0
Brookhaven Instruments Corporation
750 Blue Point Road
Holtsville, New York 11742, U.S.A.
Phone: [phone]
FAX: [phone]
e-mail: [email protected]
www.bic.com

PLEASE READ
This is your instruction manual for your Brookhaven goniometer. Please read it carefully
before attempting to use the equipment. The INSTALLATION section describes initial
checks which must
be made to ensure proper operation.
DO NOT shine light directly into the photomultiplier when the high voltage is
attached and power is on. This will ruin the photomultiplier tube and void the
warranty. Align the system as described
in the manual. Brookhaven Instruments
is not responsible for photomultiplier tubes ruined by ignoring this warning.
DO NOT scratch the glassware. Alignment is degraded, especially at the lowest
and highest angles, by scratches and pits in the index matching vat and sample
cells. Follow carefully the instructions for cleaning vats and cells. Brookhaven
Instruments
is not responsible for glassware scratched by ignoring this warning.
11

COPYRIGHT NOTICE
Copyright (C), 1989 by Brookhaven Instruments Corporation. All Rights Reserved Worldwide. No part of this
MANUAL may be reproduced, transmitted, transcribed, stored in aretrieval system, or translated into any human or
computer language, in any form or by any means, electronic, mechanical, magnetic, optical, chemical, manual, or
otherwise, without the express written permission of Brookhaven Instruments Corporation, Brookhaven Corporate
Park, 750 Blue Point Road, Holtsville, New York 11742, U.S.A.
Third Printing
Catalog Number
August 1993 with changes to Alignment sections
BI-200SMMAN, Ver. 2.5
111

WARRANTY
Brookhaven Instruments Corporation (hereinafter known as BIC) warrants that the product is free from
defective material and workmanship.
Under the terms of this warranty BIC agrees to correct by repair, or at
BIC's election by replacement, any parts which prove to be defective through no fault of the user.
This warranty is limited to the original purchaser of the product.
The product shall beshipped, freight prepaid and insured in full, or delivered to afacility authorized by BIC
to render
the service provided hereunder, in either the original package or asimilar package affording an
equal degree of protection. The purchaser must contact BIC for instructions prior to returning the product.
The product shall not have been previously altered, repaired or serviced by anyone other than aservice facili-
ty authorized by BIC. The product shall not have been subjected to accident, misuse, or abuse, or operated
contrary
to the instructions contained in the operating manual or manuals.
BIC shall
not be liable for direct, indirect, incidental, consequential, or other types of damages resulting
from the use
of this product other than the liability stated above. Thesewarranties are in lieu of all other
warranties, expressed or implied, including, but not limited to, the implied warranties of merchantability or
fitness for aparticular purpose.
The BICwarranty extends for aperiod of 90 days. This period begins from the date of receipt of the equip-
ment, and
it applies only to the original purchaser. The warranty period is automatically extended to 1year
(except as noted below) from the date
of receipt of the equipment provided all invoices for said equipment,
including transportation ifapplicable,
are paid within 30 days after receipt of invoice.
The BICwarranty extends for aperiod not exceeding thewarranty period of the original equipment manufac-
turer where applicable.
The typical warranty period on printers and computer peripherals is 90days, and on
photomultiplier tubes it is 180 days. Please contact BICfor copies of applicable OEM warranties.
The risk of damage passes to the buyer upon receipt of all glassware associated with the goniometer and its
options and accessories includingvats, cells, filters, and lenses.
IV

TABLE OF CONTENTS
TABLE OF CONTENTS
Section
Introduction....... 1-1
II Specifications..................................................................................................... 2-1
III User's Configuration.......................................................................................... 3-1
IV Installation................. 4-1
IV-1 Unpacking &General Layout.. 4-1
IV-2 Laser Safety Features.................................... 4-4
IV-3 Alignment. 4-7
IV-4 Mounting PMT Housing 4-17
IV-5 Power and Signal Connections 4-18
IV-6 Temperature ControL 4-19
IV-7 Filtration/Circulation 4-22
VSample Preparation 5-1
V-1 Dust : 5-1
V-2 Filtration 5-2
V-3 Purification 5-4
V-4 Cell Cleaning 5-6
V-5 Solution/Suspension Preparation 5-8
VI PCS Measurements......... 6-1
VI-1 Measurement Conditions....... 6-1
VI-2 Making the Measurement.. 6-3
VI-3 Variations 6-6
VII .Intensity Measurements: Alignmenl 7-1
VII-1 Counting 7-1
VII-2 Laser Stability 7-3
VII-3 Angular Intensity Measurements 7-4
v

TABLE OF CONTENTS
VIII Intensity Measurements: Rayleigh Ratios 8-1
VIII-1 Corrections 8-1
VIII-2 Reference Intensity .. 8-3
VIII-3 Calibration 8-4
VIII-4 Rayleigh Ratios... 8-5
VIII-5 Toluene &Benzene 8-6
vi

General
Description
Organization
of this Manual
INTRODUCTION Page 1-1
Section I: INTRODUCTION
This manual describes the BI-200SM goniometer, version 2.0.
Version 2.0 differs in three ways from
the original goniometer.
First, an additional 2mm aperture
and mount are provided to
make the initial alignment
of the laser beam much easier.
Second, acompletely new, compact
and much improved detec-
tor optic
is provided. It is now much easier to view the align-
ment needle and.to make
the center of rotation adjustments.
All lenses
are coated achromats. This allows wavelength
changes with minimal
or no changes in alignment. Third, a
more universal filtration/circulation system
is provided. This
system
is an option for use with the index matching fluid. We
now use Teflon tubing and agear pump.
The BI-200SM
is designed for making precision measurements
of scattered laser light. The average, time-integrated intensity
(Classical), and the intensity fluctuations (QELS) can both
be
measured. From the average intensity measurements on a
polymer solution, one may calculate
the molecular weight,
radius
of gyration and second virial coefficient. From the
QELS measurements, one calculates diffusion coefficients,
particle size, and particle size distribution information.
The design
of the BI-200SM incorporates an open, modular
concept. This allows you,
the user, to modify the existing design
and to add your own components should the need arise. The
laser and detector rails
are industry standards. If you wish to
add optical components please contactBrookhaven for sugges-
tions with mounts for these rails.
The specimen cell assembly has
separate flow paths for the
index matching liquid and
the liquid used for temperature
control. Although the plumbing for these separate systems
is
standard, the options themselves--an external temperature
controller,
the BI-TCA or TCD, and the filtration/circulation
system, the BI-FC--are not.
If you have chosen to supplyyour
own temperature controller
or filtration/circulation system,
please-contact the factory for advice.
The sections in this manual
are organized into three groups:
the introduction, sections I-III; installation, section IV; and
measurement, sections V-VIII. Look
at section III for the
configuration
of your instrument. The options thatyou pur-
chased
are listed there as well as the high voltage setting for the

INTRODUCTION Page 1-2
photomultiplier tube. Parts of the goniometer are described in
Section IV -1. Laser safety features and precautions are de-
scribed in Section IV-2. Section IV-3
is the heart ofthis manu-
al. The alignment
of the goniometer is described in this sec-
tion.
If the goniometer is not properly aligned, then measure-
ments will not turn
out as well as expected. Pay particular
attention to this alignment section.
The last four sections
are devoted to measurements including a
measurement to verify alignment. Sample preparation
is dis-
cussed in Section V.
Poor sample preparation, especially for
low angle aqueous measurements,
is the leading cause of bad
light scattering results. Photon eorrelation spectroscopy (PCS)
measurements are discussed in Section VI. Amore complete
discussion
of PCS measurements is found in Brookhaven corre-
lator manuals. Intensity measurements are discussed in Sec-
tions VII and VIII.
It
is assumed thatyou are using the goniometer with aBrook-
haven signal processor, either aphoton counter
or correlator.
If you are using your own signal processor, please make the
appropriate revisions to the suggestions in this manual. Brook-
haven software has
been explicitly written for use with Brook-
haven goniometers and signal processors.
Please read the manual carefully. Every attempt has
been
made to be thorough. Designs do change, however, and
documentation
is not always perfect or current. Occasionally
an error
or omission is discovered. Ifyou find aproblem with
the instrument
or the manual, we would appreciate hearing
from you.

Goniometer
Detector Optics
Detector
NO Filter
Beam Focus
Sample Cell
Assembly
Cells
SPECIFICATIONS Page 2-1
Section II: SPECIFICATIONS
200mm turntable mounted on circular base with holes for
mounting to asupporting table. Manual
or motor driven selec-
tion ofangles with
0.01° steps. Rigid arm for mounting beam
alignment apertures and neutral density filter in common
holder and for mounting detector rail. Fine-thread screws for
center ofrotation adjustments.
Adjustable eyepiece for viewing scatteringvolume. Two
hundred micron wide slit with adjustments to determine center
of rotation. All lenses are coated achromats. Filterwheel with
narrow-band optical filters for laser wavelengths of633,514.5,
488nm, one open and two blank positions. Pinhole turret with
100,200 and
400}L pinholes for selecting coherence areas
(QELS measurements) and
1, 2and 3mm apertures for adjust-
ing intensity (classical measurements).
Selected photomultiplier tube (PMT), shielded housing, socket,
dynode chain, integral amplifier/discriminator.
The low voltage
power requirements
(± 5vdc) are supplied from aBrookhaven
correlator
or photon counter. Aseparate high voltage supply
(-1,500 to
-3,00Ovdc, 3mA, ±15mvdc for ±10% line voltage
fluctuations)
is required.
Aneutral density filter with an optical density
of 3.0 is mounted
on the rigid arm after alignment
is complete. This reduces the
main beam intensity by approximately afactor of1000 for
angles below approximately
8°.
A10cm focal length coated achromatwith adjustments is used
for focusing and steering the beam onto the center
of rotation.
Entrance and exit apertures block stray light.
Insulated, anodized metal potwith special glass vat for contain-
ing an index matching liquid. Inlet/outlet ports for circulating
index matching liquid. Inlet/outlet ports for circulating a
temperature.controlled fluid around the sample cell holders.
Temperature range approximately +5°C to
+80°C Cylindrical
and square cell holders. Alignment cell for use in determining
the center
of rotation.
Five, nominal 12mm outside diameter, round cells with Teflon
caps are provided as standard. Cells are nominally 55mm tall
and require aminimum of1.5mLofsample.

BI-LRM
BI-FC
BI-TCA
or TCD
BI-HV
BI-RC26
SPECIFICATIONS Page 2-2
Options
Laser rail and mounts for small, cylindrical HeNe lasers, 35mW
and lower power HeNe lasers with rectangular cross sections,
and most Argon-ion lasers. Includes laser rail of appropriate
length, foot with mounting holes and rail slider. Two adjustable
laser mounts included.
Gear pump, 47mm filter holder, set of filters, smooth-tip
forceps for handling filters, Teflon tubing
and connectors. For
use with most index matching fluids like toluene or decahydro-
napthalene (trade name, Decalin).
Temperature controllerwith external circulation. Stability of
±O.l°C over the range of temperatures suitable for use with
the BI-200SM. Proportional control with temperature select-
tion either analog (TCA)
or digital (TCD).
High voltage power supply suitable for use with BI-200SM.
Nominal 26mm outside diameter cylindrical cells with Teflon
stoppers. Best for wide angle measurements
and aqueous
suspensions.

CONFIGURATION Page 3-1
Section III: CONFIGURATION
Model Number: BI-200SM Goniometer SIN: 80451
Detector Type: BI-DS1 PMT SIN: HC1303
Dark Count Rate: 275 ±25 cps @24°C
OPTIONS
Correlator Type: PCI BI-9001 AT Di
Correlator SIN: 4001136
NOTES:
ORIGINAL PURCHASER: Prof. Sinha
ORGANIZATION: University of CA, San Diego
DELIVERY DATE: December
3, 2004

;r.; Brookhaven Instruments Corp.
!&!: GoniometerAlignment Software Ver. 3.15 Date: Dec
1, 2004
Time: 12:24:20
Sample
ID
Operator ID
Notes
2.0
U of CASan Diego setup
G.Comstock
633nm
~
0«
t::B
w.
~E
o ....
o
Z
0.0 .
................. __ A __ .. _ .. __ .. • .. _.._ ..
. .
-2.0..l::0~"""----L--'--'----'--~~-"""----:::':90~ ......... -'----'--"""--~--'----'- ......... 1-:-::8;:;:;O
degrees
"A" Dark Count Rate: 243 cps
"8" Dark Count Rate: 0 cps
Repeats: 5
Duration IRep: 1.0 sec
Dust rejection ratio: 1.33
Refractive Index of Sample Liquid: 1.474
Refractive Index of Sample Cell: 1.500
Refractive Index of Vat Liquid: 1.474
Pinhole size: 1 mm
Polarization Analyzer: None
Interference Filter: In
% Error % Error
Angle I'
I'· sin e=I Norm. to 90 Norm. to Avg.
15.00 66135 17117 0.64 0.56
20.00 49875 17058 0.30 0.22
30.00 34062 17031 0.14 0.06
45.00 24136 17067 0.35 0.27
60.00 19652 17019 0.07 -0.01
90.00 17008 17008 0.00 -0.08
120.00 19629 16999 -0.05 -0.13
135.00 24069 17019 0.07 -0.01
150.00 33873 16936 -0.42 -0.50
155.00 40124 16957 -0.30 -0.38