Pike FlexIR Hollow Waveguide Bedienungsanleitung

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Jan. 1, 2012

Contents

Introduction

Unpacking Your FlexIR HWG Accessory

Packing List

Installing the FlexIR HWG with MCT Detector

Accessory Setup

MCT Liquid Nitrogen Filling and Stabilization

Installing the HWG Probe

Aligning the FlexIR Accessory

Optimizing MCT Pre-Amp Gain

Removing the FlexIR Accessory

Storage

ATR Probe

Zinc Selenide

Germanium

Diamond/ZnSe Composite

Diffuse Reflectance Probe

Specular Reflectance Probe

Suggested Measurement Settings

Example Applications

Precautions

SAFETY

HGW Probe Assembly Handling

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Introduction

The FlexIR Hollow Waveguide Accessory is an excellent tool for remote and specific area analysis of a

wide variety of samples. Visible surface contamination, small area material identification and bulky

materials too large to fit into the FTIR sample compartment are a few of the many samples and

application types for the FlexIR accessory.

The FlexIR Hollow Waveguide (HWG) Accessory is designed for high throughput, ruggedness and wide

spectral range. The FlexIR utilizes a custom optical design with diamond-turned focus optics providing

exceptional IR throughput. The new hollow waveguides are very durable and free from the typical

fracture problems encountered with polycrystalline and glass core fibers. The highly reflective HWG

fibers transmit maximum energy through the mid-IR spectral region  eliminating the need for multiple

fibers for a complete spectrum.

Available probes include ATR, diffuse reflectance, and specular reflectance. The ATR probe may be

configured with a zinc selenide, germanium, or diamond/zinc selenide composite crystal. The PIKE

Technologies FlexIR Hollow Waveguide Accessory is built and tested for optimum performance for your

FTIR spectrometer.

Figure 1: Optical Diagram of the MCT FlexIR Accessory

Beam returned

from sample

Integrated MCT Detector

Incoming Beam

HWG Probe

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Unpacking Your FlexIR HWG Accessory

In order for you to quickly verify receipt of your accessory, we have included a packing list. Please

inspect the package carefully. Contact PIKE immediately if any discrepancies are found.

WARNING: The hollow waveguide probes have a limited bend radius of 150 mm. A smaller radius bend

will break the probe.

Packing List

FlexIR Manual

FlexIR Hollow Waveguide Base

HWG Probe or Probes

PN 045-3000

PN 045-30XX

(based upon your order)

Quantity 1

Probe Attachment Screws

Wrench Set

Purge Tubing Kit

(for Mid-IR FlexIR)

Quantity 1

PN 025-3055

Quantity 2

Quantity 1

Funnel

Reference Cap

(to fill MCT Detector)

(Diffuse and Specular

Probes only)

Quantity 1

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Installing the FlexIR HWG with MCT Detector

Accessory Setup

Turn off the power to the FTIR spectrometer. Connect the interface detector cable of the HWG

accessory to the detector connector port of the spectrometer. Consult the FTIR manual for additional

information regarding the detector connector port and the proper software settings to select an

external detector.

The base optics of the Mid-IR FlexIR HWG Accessory fits into the sample compartment of the FTIR

spectrometer. The FlexIR HWG Accessory will include the baseplate mount for your FTIR spectrometer.

Place the accessory into the sample compartment of your FTIR and secure any lock-down screws.

MCT Liquid Nitrogen Filling and Stabilization

Fill the MCT detector with liquid nitrogen using the funnel included with the accessory.

WARNING: Wear safety goggles and protective clothing when handling liquid nitrogen. Exposure to

liquid nitrogen will cause severe skin or eye injury.

Pour a small amount of liquid nitrogen into the funnel and wait for it to drain into the Dewar of the

detector. Add additional small amounts of liquid nitrogen until the detector is filled. Allow the detector

to stabilize for about 10 minutes and then top it off with a final amount of liquid nitrogen to completely

fill the liquid nitrogen Dewar. A lit green LED light indicates the Dewar contains liquid nitrogen and is

beginning the detector cooling process or is sufficiently cooled. It is not an indication that the accessory

is necessarily ready for use. Be sure to wait a 10 minute equilibrium time after the Dewar has been

completely filled. Observing a stable interferogram is another indication that the HWG accessory is

ready for measurements. An insufficiently cooled detector will produce a low and unsteady signal. The

red LED light indicates the accessory is not ready for use. If the red LED is illuminated during use check

that the detector Dewar is filled with liquid nitrogen.

Installing the HWG Probe

The next step is to install the HWG probe. Insert the black probe connector end into the base optics and

secure with hex screws provided with the accessory as shown on the following page.

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Aligning the FlexIR Accessory

This accessory has been pre-aligned on the same make as your spectrometer. In most cases, little to no

further alignment is necessary. To assess the need for additional alignment, check the energy when in

the monitor mode of the spectrometer software. When using the specular or diffuse reflection probe,

slide the reference cap over the probe tip before monitoring the energy. No reference cap required for

ATR probes.

The alignment procedure requires that the IR beam pass through the hollow waveguide(s) and return

the beam through the hollow waveguide to reach the detector. Prior to adjusting the mirrors as

explained below a closed loop must be established. In other words, the alignment process for a diffuse

reﬂectance or a specular reﬂectance probe requires that the probe tip be positioned gently touching the

diffuse reference disk or a specular mirror embedded in the reference cap included with the probe,

respectively. For an ATR probe, no reference or mirror is required. Simply be sure the ATR crystal surface

is clean.

Open the FTIR bench setup software display to monitor the interferogram signal strength. Please refer

to your FTIR software manual for details of this operation. Reduce the size of the FTIR aperture to

achieve acceptable interferogram signal strength. If your FTIR does not have an aperture, use an IR

beam-limiting screen placed at the right or left side of the FTIR sample compartment to reduce the

energy to an acceptable level.

Optimize the signal by adjusting the input mirror (Figure 3), which directs the IR beam into the hollow

waveguide(s), located below the installed probes. Rotate slowly the screws, positioned on the diagonal,

one at a time while maximizing the signal by monitoring the energy displayed through the FTIR software.

Figure 2: Assembled FlexIR Accessory

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After adjusting the input mirror optimize the position of the output mirror, which redirects the returned

beam into the detector. Adjust the two screws located on the top of the accessory (Figure 3). This mirror

and the resulting focus on the detector is extremely sensitive to small movements of the positioning

screws. A turn of less than a quarter of a complete rotation will drastically change the amount of energy

striking the detector, which may be monitored through the FTIR software.

Figure 3: Locations of mirror alignment ports

Repeat the adjustment of the input and output mirror two to three more times if increases in

performance are observed, to fully optimize the accessory. The positioning of the MCT detector has

been optimized for the speciﬁc bench and probe type. In general, the position of the MCT detector does

not require adjustment. In the event different probe types are in use, the position/alignment of the MCT

detector may slightly improve signal performance. Adjust the MCT detector position in the left or right

direction by loosening the screw located on the detector base rigging as shown in Figure 4. After

adjustment, retighten the screw to secure the detector.

Figure 4: Illustration of MCT detector alignment point

Input Mirror

Adjustment Screws

Output Mirror

Adjustment Screws

Detector Positioning Screw

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Optimizing the MCT Pre-Amp Gain

The MCT pre-amp gain has been adjusted at the PIKE manufacturing facility. It most likely will not

require further adjustment. However, adjustments may be required especially if using different probe

types which exhibit large relative energy differences reaching the detector. For example, the gain is set

higher for a diffuse reﬂectance probe compared to an ATR probe.

Figure 5: Illustration of MCT detector alignment point

The gain should be adjusted to allow 50% of total energy counts or voltage registering on the detector.

To adjust the gain, remove the gain cap from the front of the base optics. Access the gain screw using a

small screwdriver.

Removing the FlexIR Accessory

Turn off the power to the FTIR spectrometer.

WARNING: Do not disconnect the detector cable before turning off the FTIR. Failure to do this may

cause damage to the FTIR and/or FlexIR electronics.

Remove the signal/power cable from the FTIR spectrometer and remove the FlexIR accessory from the

sample compartment.

Storage

Place the FlexIR ﬁber optic accessory into the plastic bag provided to protect its optics from dust.

Gain Adjustment Screw

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ATR Probe

The ATR probe may be used to measure solids, liquids, and powders. Intimate contact between the

sample and the ATR crystal is required to obtain a quality spectrum. To use, collect a background

spectrum of a clean ATR crystal. Next, place the ATR tip on the sample and exert pressure to obtain good

contact and collect the sample spectrum.

The ATR probe is sealed up to 60 mm beyond the ATR probe tip. Do not submerge the probe into a

liquid deeper than 60 mm. Double score lines are etched on the probe head to indicate the maximum

immersion allowed. Isopropyl alcohol, a mild solvent, is recommended for cleaning the ATR crystal using

a cotton swab.

Zinc Selenide

Zinc Selenide (ZnSe) is a general-purpose ATR material. It has limited use with strong acids and alkalis.

The acceptable pH range is 5 through 9. Additionally, complexing agents such as ammonia and EDTA will

erode its surface because of the formation of complexes. The maximum temperature range for the ZnSe

probe is ambient to 95 °C.

Germanium

Germanium (Ge) has been used extensively in the past as a higher refractive index material for samples

that have a high refractive index such as carbon ﬁlled samples. Due to its higher refractive index, spectra

collected with a Ge ATR crystal are weaker in spectral absorbance compared to spectra collected with

ZnSe or diamond/ZnSe composite ATR crystals. The acceptable pH range is from 1 to 14. The maximum

temperature range for the Ge probe is ambient to 95 °C.

Diamond/ZnSe Composite

Diamond is one of the most rugged optical materials. It can be used for the analysis of a wide range of

samples including acids, bases, and oxidizing agents. Diamond is also scratch and abrasion resistant. Its

disadvantage is the intrinsic absorption from approximately 2300 to 1800 cm-1. The maximum

temperature range for the diamond/ZnSe probe is ambient to 60 °C.

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Diffuse Reflectance Probe

The diffuse reﬂectance probe is suitable for solid samples with diffuse surfaces only. Do not submerge

the diffuse reﬂectance probe in powders or liquids as the tip is without a protective window and

damage to the probe will result.

In collecting a background spectrum, insert the probe tip into provided reference cap. If probe fits

tightly or cannot bottom out on reference loosen set screw on side and insert probe cap. Tighten set

screw to provide enough drag/friction to hold the reference cap in place, yet allow the cap to be

removed. Next the sample spectrum is collected after positioning the probe either touching or within

0.4 mm from the sample. The probe tip is delicate. Avoid exerting a strong pressure on the tip end. The

maximum temperature for the diffuse reflectance probe is 95 °C.

Specular Reflectance Probe

The specular reﬂectance probe is ideal for smooth non-diffuse surfaces. In collecting a background

spectrum, insert probe into provided reference cap. If probe fits tightly or cannot bottom out on

reference loosen set screw on side and insert probe cap. Tighten set screw to provide enough

drag/friction to hold the reference cap in place, yet allow the cap to be removed.

Generally, a specular reﬂectance spectrum is collected by collecting a background spectrum using the

reference cap with an embedded mirror. Next the sample spectrum is collected after positioning the

probe either touching or within 0.4 mm from the sample. The probe tip is delicate. Avoid exerting a

strong pressure on the tip end. Do not submerge the probe tip in a powder or a liquid as this will result

in damage to the probe. The maximum temperature for the specular reflectance probe is 95 °C.

Suggested Measurement Settings

Wavelength Range: 4000 to 700 cm-1 (actual range of HWG Accessory MCT version: 5000 to 700 cm-1)

Velocity: Select appropriate speed for MCT detector for your spectrometer Resolution: 4 to 8 cm-1

Actual measurement parameters will vary based on the experimental conditions and sample material.

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