ILLUMINATING Near-IR

totype near-IR “cuffs" thatfit over a per- son's fingerand measure the light trans- mitted through the fingertip have been proposed for noninvasive ...
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ILLUMINATING Near-IR Near-IR spectroscopy is fast becoming a useful analytical tool at industrial process lines, in biological and polymer research laboratories, in the field as a portable method, and for quality control of raw materials. Its speed, noninvasive nature, and minimal sample preparation requirements make it attractive for a variety of sample types including liquids, slurries, coatings, powders, and solids. The ability of near-IR wavelengths to penetrate into and sometimes through a sample has led to some astonishing experiments: In the past five years, near-IR spectroscopy has been used to determine pH in the caustic brines of hazardous waste tanks, and prototype near-IR "cuffs" that fit over a person's finger and measure the light transmitted through the fingertip have been proposed for noninvasive determination of blood glucose. The enormous progress in chemometrics and computing power that has been achieved in the past decade makes both exotic and routine applications possible. Near-IR spectrometers range from simplified process instruments that monitor only a few wavelengths characteristic of a single analyte to full-fledged research in-

Advances in component design and calibration softwarefitnear-IR for both research and routine use

ysis. Table 1 presents characteristics and components for a representative selection of near-IR spectrometers. For more information on individual products, send an e-mail message with one of the keywords listed at the bottom of the table in the subject line to our reflector service at [email protected]. For a more comprehensive list and more in-depth discussion of near-IR system components in general, see W. Fred McClure's Report on near-IR spectroscopy in the Jan. 1,1994, issue (Anal. Chem. 1994, 66,43A-53A).

struments that acquire spectra in the entire near-IR region (780-2526 nm) as well as mid-IR or UV-vis wavelengths. Some instruments can even perform near-IR imaging. We asked Mark A. Arnold of the University of Iowa, Lois Weyer of Hercules, and Patrick Treado of the University of Pittsburgh for their views on trends in near-IR instrumentation and applications and their advice for potential buyers. In the United States alone, there are well over 20 manufacturers of complete near-IR spectrometers and many more "third-party" vendors of components for sampling or detection and software packages for data anal-

Source optics Source optics differentiate commercial near-IR spectrometers into four major types: grating monochromator, Fourier transform (FT), acoustooptic tunable filter (AOTF), and light-emitting diode (LED). Perhaps because process-monitoring applications, whether on-line or at-line, make up one of the largest segments of the near-IR market, each of these spectrometer types is being pursued for adaptation to dedicated routine as well as research use. Each method has its strengths and tradeoffs with the others, and no one type is

Analytical Chemistry, December 1, 1995 735 A

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Review

Table 1 . Summary of representative products Product Company

SpectroChem 100 AnalytiChem P.O. Box 677 Rockville, MD 20848 301-924-3025

Genesis ATI Mattson 1001 Fourier Dr. Madison, Wl 53717 800-423-6641

Infra Prover Bran+Luebbe 1025 Busch Pkwy. Buffalo Grove, IL 60089 708-520-0700

Luminar 2000 Brimrose 5020 Campbell Blvd. Baltimore, MD 21236 410-931-7201

Price Type

$35,000 (complete system) Diffraction grating

$28,500 FT

ΙΝΑ FT

ΙΝΑ AOTF

Techniques

Transmission, reflectance

Transmission, reflectance

Optics

Diffraction grating with postdispersive detection using fiber-optic bundles to remote probes and cells

Fully sealed and desiccated Michelson corner-cube interferometer with internal HeNe wavelength refer­ ence; halogen source with CaF2 beamsplitter

Reflectance, transmission, transflectance Polarization interferometer

Reflectance, transmission, transflectance AOTF with software-selec­ table wavelength incre­ ments of 0.3-20 nm; dou­ ble-beam design with poly­ styrene reference

Detectors

I n As

Peltier-cooled InAs; LNgcooled InSb or InGaAs

Temperature-stabilized PbS

1 sample and 1 reference; Si (650-1050 nm);TEcooled InGaAs detectors for 900-1600 nm, 10001850 nm, or 1200-2200 nm

5 scans/s

1.1 s/scan

Up to 4000 discrete wavelengths/s in random access

1000-5000 nmwith InSb; 1000-3800 nm with InAs; 800-1700 nm with InGaAs 0.1 nmat 1000 nm

1000-2500 nm; 10002200 nm with fiber optics

650-1050 nm;900-1600 nm; 1000-1850 nm; 1200-2200 nm 1-3 nm; 2-6 nm; 3-7 nm; 5-10 nm, respectively

Yes

Yes

Yes

First and second derivatives

PLS, PCR

PLS, PCR, discriminate analysis

PLS, PCR, cluster analysis

PLS, PCA, PCR, KNN

No Yes

Yes ΙΝΑ

386 DX or higher PC; RS-232 communications; full data acquisitions and manipulation

386 PC standard, 486 PC optional; Ethernet communi­ cation, data acquisition and processing software; selfdiagnostics; process control language

Validation kit; NIST stan­ dards; bar code readers, remote switching probe for liquids; AOTF, filter, and grating systems also avail­ able

Fiber-optic probes, 16-channel multiplexer

403 ac NIR624

404 ac NIR625

Performance Spectral acquisition time 2 s

Spectral range

1000-2500 nm

Resolution

1 nm at 1000 nm; 2 nm at 2000 nm

Statistical functions Derivatives/data pretreatment Nonlinear regressions (PLS, PCR, etc.) Multiple linear regression Statistical fit diagnostics (overfitting) Data system

Yes Yes

Yes

IBM-compatible 386 or higher PC running Windows

386 or higher PC running Windows 3.1 or higher; RS232C communications; full data acquisition, manipula­ tion, reporting, and pro­ grammable control

Special features

Available as lab, process, or portable system

Options and accessories

Fiber-optic cables, probes, cells, battery pack

18 χ 17 in. footprint; exter­ nal beam for fiber-optic accessories Validation kit with manual and check standards; fiber­ optic probe for analysis of liquids and powders

Reader service number E-mail reflector keyword

401 ac NIR622

ΙΝΑ = Information not available at presstlme

736 A Analytical Chemistry, December 1, 1995

402 ac NIR623

ΙΝΑ

Quantum 1200 Plus LT Industries 6110 Executive Blvd. Rockville. MD 20852 301-468-6777

MagnaIR Nicolet 5225 Verona Rd. Madison, Wl 53711 800-356-8088

UV/Vis/NIR On-Line Instruments 130 Conway Dr. Bogart. GA 30622 800-852-3504

$43,000+ Grating monochromator Vis/near-IR Reflectance, transmission, transflectance Fast scan grating mono­ chromator; high-energy throughput

ΙΝΑ FT

$31,000 Double-beam, double-grating scanning monochromator Reflectance, transmission, transflectance Double-beam double mono­ chromator with W/halogen source; high-intensity lamp available

Reflectance, transmission, transflectance Michelson interferometer; quartz-halogen source; quartz, CaF 2 , or XT-KBr beamsplitters

Lab/Process Analyzers Perstorp Analytical/ NIRSystems 12101 Tech Rd. Silver Spring, MD 20904 800-343-2036 ΙΝΑ $40,000+ Holographic grating mono­ Grating monochromator chromator, Vis/Near-IR UV-vis/near-IR Transmission, reflectance, Transmission, reflectance, immersion diffuse reflectance Lab: Predispersive singleDouble-beam double beam diffraction grating. monochromator with Process: Vibration-isolated W/halogen and deuterium diffraction grating; pre/postsources; holographic grat­ dispersive monochromaings at 360 lines/mm for tors; dual-channel design; near-IR fiber-optic interface Peltier-cooled PbS for near- Si (400-1100 nm); PbS (1100-2500 nm); IR InGaAs (900-2200 nm) Lambda 900 Perkin Elmer 761 Main Ave. Norwalk, CT 06859 800-762-4000

Si, PbS. InGaAs single detectors; Si, InGaAr 256and 512-element array detectors

D-TGS (12,500-350 c m - 1 ) ; MCT (11,700-600 c m - 1 ) ; PbSe (13,000-2000 cm" 1 ); InSb (11,500-1850 c m - 1 ) ; PbS (10,000-4200 cm - 1 )

PMT for UV-vis; PbS for near-IR

Up to 5 full scans/s corres­ ponding to 6000 discrete wavelengths/s

Up to 50 full scans/s

ΙΝΑ

1200-2400 nm; 400-2400 nm expansion; 900-1800 nm; 400-800 nm 1 nm in near-IR; 0.3 nm in visible

400-2500 nm

185-2600 nm

Scan rates to 9600 nm/min for near-IR with 0.04-10 s integration; integration to 999 s 185-3300 nm