Acclaim Surfactant Column Data Sheet - Cromlab€¦ · pesticides, detergent powders, petro-leum...
Transcript of Acclaim Surfactant Column Data Sheet - Cromlab€¦ · pesticides, detergent powders, petro-leum...
Colum
ns A c c l a i m ® S u r f a c t a n t C o l u m nA S i m p l e S o l u t i o n t o D i f f i c u l t C h a l l e n g e s
Acclaim Surfactant columns arehigh-efficiency specialty silica columnsfor separating anionic, nonionic, andcationic surfactants:
• Ideal selectivity for separation of
anionic, nonionic, and cationicsurfactants
• Excellent peak shapes for cationic
surfactants
• Improved resolution for ethoxylated
surfactants
• Compatible with highly aqueous
mobile phases
• Methods compatible with various
detectors
• Broad range of applications
Ideal Selectivity for the Separation ofAnionic, Nonionic, and CationicSurfactants
The Acclaim Surfactant columnis a new column designed for, andideally suited to, the separation of avariety of different surfactants. Thiscolumn incorporates a proprietarysilica-based bonded phase that offersideal selectivity and unprecedentedcapacity for separating cationic,nonionic and anionic surfactants in asingle run. The simple, volatile mobilephases are compatible, with massspectrometry detection which
facilitates the application of thiscolumn to trace-level analyses ofsurfactants in various matrices, includ-ing pharmaceutical formulations andenvironmental samples.
Surfactants are widely used inindustrial, agricultural, and pharmaceu-tical markets, in products as diverse aspesticides, detergent powders, petro-leum products, cosmetics, and pharma-ceuticals. Their separation and identifi-cation can be a challenge due both tothe diversity of surfactants and com-plexity of the sample matrix.
Peaks:
1. Xylene sulfonate
2. Lauryldimethylbenzyl ammonium chloride
3. Octylphenoxyethoxyethyl dimethylbenzyl ammonium chloride
4. Triton X-100
5. Decyl sulfate
6. Dodecyl sulfate
7. C10-LAS
8. C11-LAS
9. C12-LAS
10. C13-LAS
mV
Minutes0 5 10 15 20 25 30 35 40
1
2
3
4
5
6
710
98
2
Figure 1. Separation of a mixture of surfactants showing remarkable selectivity.
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Figure 2. Analysis of a cationic surfactant showing excellent peak shape.
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Dimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile,
(B) 0.1 M NH4OAc, pH 5.4Gradient: 25–85% A in 30 min,
then hold at 85% A for 10 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 25 µLDetection: ELSD
Peaks: 1. Xylene sulfonate2. Triton X-1003. Decyl sulfate4. Dodecyl sulfate5–8. Dodecylbenzene sulfonate
Dimensions: 4.6 × 150 mmMobile Phase: Acetonitrile/0.1M NH4OAc, pH 5.4 v/v
40/60 for Acclaim Surfactant column60/40 for Symmetry C18 (Waters) column
Temperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 5 µLDetection: ELSD
Sample: Lauryldimethylbenzylammonium chloride (1000 ppm)
The separation of surfactants istypically accomplished using HPLC.Reversed-phase and ion-exchangechromatography are the most popularapproaches, but normal-phase and size-exclusion chromatography are alsoused, depending on the application.Although many HPLC stationaryphases are available and have been usedfor the analysis of surfactant formula-tions, none of these columns have beendesigned specifically for this applica-tion, nor are they capable of separatinganionic, nonionic, and cationic surfac-tants in a single chromatographic run.Figure 1 shows the difference betweena conventional C18 column and theAcclaim Surfactant column for theseparation of a mixture of anionic andnonionic surfactants. The AcclaimSurfactant column provides excellentseparation, whereas the C18 columnfails to resolve all the surfactants underthe same conditions.
Excellent Peak Shapes for CationicSurfactants
Reversed-phase chromatography,using a C18 column, is often used forthe separation of anionic surfactants.When analyzing cationic surfactants,however, it is often difficult to obtainsharp, symmetrical peaks due primarilyto the presence of free silanols. Thenovel bonding chemistry of theAcclaim Surfactant phase allows foreffective deactivation of free silanolstoward positively charged cationicsurfactants, resulting in excellent peakshapes, as shown in Figure 2. Bycomparison, a C18 column tested undersimilar conditions demonstrates anextended retention time and peak tailing.
1
2 3
4
5
67
8
1
3
4, 5 2, 8
6 7
mV
Minutes0 5 10 15 20 25 30 35 40
Acclaim Surfactant
Symmetry® C18 (Waters)
mV
Minutes0 5 10 15 20
Acclaim Surfactant
Symmetry C18 (Waters)
3
Figure 3. Improved resolution between oligomers in ethoxylated surfactants.
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Figure 4. Analysis of a strongly hydrophilic hydrotrope.
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Dimensions: 4.6 × 150 mmMobile Phase: Acetonitrile/0.1 M NH4OAc, pH5.4
v/v 40/60 for Acclaim Surfactantv/v 50/50 for Symmetry C18 (Waters) column
Temperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 10 µLDetection: UV, 225 nm
Sample: Triton X-100 (1000 ppm)
Dimensions: 4.6 × 150 mmMobile Phase: Acetonitrile/0.1 M NH4OAc,
pH 5.4 v/v 30/70Temperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 5 µLDetection: UV, 225 nm
Sample: Sodium xylene sulfonate (1000 ppm)
Improved Resolution for EthoxylatedSurfactants
As a consequence of its novelcolumn chemistry, the Acclaim Surfac-tant column exhibits a unique polaritythat provides significantly improvedresolution for individual oligomers ofethoxylated surfactants compared withconventional C18. Figure 3 provides acomparison between the AcclaimSurfactant column and a conventionalC18 for the characterization of TritonX-100. The Acclaim surfactant columnexhibits significantly improved resolutionbetween the oligomers.
Compatible with Highly AqueousMobile Phase Conditions
High-density C18 columns areoften unsuitable for analyzing stronglyhydrophilic hydrotropes, such assodium naphthalene sulfonate andxylene sulfonate. The problem arisesbecause these analyses require a highlyaqueous mobile phase that often leadsto undesirable “dewetting”. Asillustrated in Figure 4, the novelchemistry of Acclaim Surfactantcolumn provides excellent resolutionbetween isomers of xylene sulfonate,while under the same condition littleor no retention is observed on theconventional C18 column.
Methods Compatible with VariousDetectors (ELSD, UV, MS ConductivityDetection)
UV absorbance is the mostpopular detection method in HPLC, dueto its ease of use and sensitivity(Figures 3–5 and 18–20). The drawbackwith this approach is that the analytemust have a chromophore to bedetected and many surfactants do not.
Although refractive index (RI)detection is a universal detectionmethod, capable of detecting allanalytes, it is incompatible withgradient methods, exhibits low sensitiv-ity, and thus is only used when otherdetection methods are not applicable.
AU
Minutes0 10 20 30
Acclaim Surfactant
Symmetry C18 (Waters)
AU
0 5 10 15
Acclaim Surfactant
Minutes
Symmetry C18 (Waters)
Evaporative light-scatteringdetection (ELSD) is not only a univer-sal detection method, but also iscompatible with gradient methods andis far more sensitive than RI. In addition,methods developed with ELSD can beeasily transferred to LC-ESI-MSapplications with little or no modifica-tions, because both detectors share thesame mobile phase requirements(Figures 1, 2, 8, 11–14 and 16–22).
Mass spectrometry (MS) is aninherently sensitive and universalmethod and has become the widelyaccepted tool for characterization oforganic compounds. The soft ionizationtechniques, such as electrosprayionization (ESI), have greatly increased
the applicability of MS detection tosurfactant analysis. As shown inFigures 6, 10, and 15, the AcclaimSurfactant column can be used for theanalysis of anionic, cationic, andnonionic surfactants using LC-ESI-MSand ammonium acetate eluents.
Suppressed conductivity detec-tion can also be used for surfactantanalysis and provides certain advan-tages for analyzing trace levels ionicsurfactants in complex matrices.Figures 7 and 9 show the separation ofvarious anionic and cationic surfactantson the Acclaim Surfactant column,using a borate buffer and acetic acidmobile phases, respectively.
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Figure 5. Analysis of sodium dodecylbenzene sulfonate (LAS).
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Dimensions: 4.6 × 150 mmMobile Phases: Acetonitrile/100 mM NH4OAc, pH 5.4,
v/v 70/30 for Acclaim Surfactantv/v 50/50 for Acclaim PA(Waters) column
Temperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 5 µLDetection: UV, 225 nm
Figure 6. Analysis of sodium lauryl sulfate using LC-ESI-MS.
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: Acetonitrile/0.1 M NH4OAc,
pH 5.4 v/v 75/25Temperature: 25 °CFlow Rate: 1 mL/min (0.2 mL/min to
mass spectrometer)Inj. Volume: 25 µLDetection: MS (ESI negative, probe 300 °C,
cone 20 V needle 2.5 KV,SIM 265.2, span 0.3 m/z)
Peak: Sodium lauryl sulfate (1 ppm)
Broad Range of Applications
Anionic SurfactantsAnionic surfactants account for
60% of surfactant use in the UnitedStates, where they are popular ingredi-ents in detergent powders. This popular-ity arises because of their effectivenesscompared with other surfactants inparticulate soil removal, especially fromnatural fabrics, and because they areeasily spray-dried.
Linear alkylbenzenesulfonates(LASs) are the most widely usedsurfactants, due to their low cost andrapid degradation under aerobic condi-tions. The synthesis of LAS typicallyleads to a mixture of positional isomersthat results in a very complex samplematrix that can be a challenge to separateeffectively by chromatography. Tosimplify quantitative analysis, isocraticconditions are often used to produce onlysingle peaks for the same size homo-logues species. As shown in Figure 5,LAS can be separated on the AcclaimSurfactant column into simple, singlepeaks corresponding to a homologousseries, whereas the Acclaim PA columngives more complex chromatograms.
Alkyl sulfates are the sulfuric acidesters of linear alcohols. They arefrequently employed as additives incosmetics and detergents. Figure 6shows the analysis of lauryl sulfate,a major ingredient in shampoo, on anAcclaim Surfactant column usingLC-ESI-MS and an ammoniumacetate eluent.
Alkylether sulfates are preparedby adding oxyethylene groups to analcohol that is then sulfated. Oxyethy-lation enhances water solubility andfoaming, making these surfactantsideal components in shampoos anddetergents. Figure 7 shows the analysisof laureth sulfate using suppressedconductivity detection.
AU
Minutes0 5
C10-LAS
C13-LAS
C11-LAS
C12-LAS
C10-LAS
C13-LAS
C11-LAS
C12-LAS
10 15 20 25
Acclaim Surfactant
Acclaim PA
Abun
danc
e
Minutes0 5 10 15 20
Figure 7. Analysis of ammonium laureth sulfate using conductivity detection.
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Column: Acclaim Surfactant, 5 µmDimension: 4.6 × 150 mmMobile Phase: Acetonitrile/0.5 M H3BO4
and 20 mM NaOH v/v 55/45Temperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 10 µLDetection: Suppressed CD (AMMS III)
Sample: Ammonium laureth sulfateµS
Minutes0 10 3020
0
4
5
Cationic SurfactantsCationic surfactants are used as
fabric softeners, corrosion inhibitors,and antimicrobial agents. The mostpopular cationic surfactants includealkyl quaternary ammonium salts,benzylalkylammonium salts, pyridiniumsalts, ester quats, ethoxylated quats, andquaternary imidazolium compounds.
Figures 8–12 present examples ofchromatographic analysis using theAcclaim Surfactant column.
Figure 8. Separation of cationic surfactants using ELSD.
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile, (B) 0.1 M NH4OAc, pH 5.4Gradient: 25–85% A in 30 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 25 µLDetection: ELSD
Peaks: 1. Lauryl pyridinium chloride2. Lauryldimethylbenzyl ammonium chloride3. Octylphenoxyethoxyethyl dimethylbenzyl
ammonium chloride4. Cetyltrimethylammonium chloride5. Cetylpyridinium chloride
1
2
3
4
5
mV
Minutes0 10 3020
Figure 9. Separation of cationic surfactants with suppressed conductivity detection.
Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile
(B) 20 mM acetic acidGradient: 20–50% A in 15 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 10 µLDetection: Suppressed CD (AMMS III)
Peaks: 1. Lauryl pyridinium chloride2. Lauryldimethylbenzyl ammonium chloride3. Octylphenoxyethoxyethyl dimethylbenzyl
ammonium chloride4. Cetyltrimethylammonium chloride5. Cetylpyridinium chloride
Figure 10. Analysis of quats using LC-ESI-MS.
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: Acetonitrile/50 mM NH4OAc,
pH 5.4 v/v 60/40Temperature: 25 °CFlow Rate: 1 mL/min (0.2 mL/min to
mass spectrometer)Injection Vol.: 25 µLDetection: MS (ESI positive, probe 300 °C,
cone 30 V, needle 2.5 kV, SIM 332.4,360.4, 374.4, 388.5, span 0.5 m/z)
Peak: Benzyl dimethyl hydrogenatedtallow ammonium chloride (10 ppm)
Minutes151050
1 2
3
4
5
µS
Minutes0 5 10 15
C18
C15 C17
C16Abun
danc
e
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6
Figure 11. Separation of ethoxylated quats.
Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: Acetonitrile/0.2 M NH4OAc, pH 5.4 v/v 40/60Temperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 25 µLDetection: ELSD
Sample: Ethoquad 18/25 (500×)
Figure 12. Separation of quaternary imidazolinium compounds.
Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile
(B) 0.1 M NH4OAc, pH 5.4Gradient: 25–85% A in 30 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 10 µLDetection: ELSD
mV
Minutes0 10 35255 20 30 4015
2-Hydroxyethylbenzyl coco imidazolinium chloride
Diethyl heptadecyl imidazolinium ethylsulfate
mV
Minutes0 10 255 20 3015
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21117
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Nonionic SurfactantsNonionic surfactants account for
about 40% of the worldwide consump-tion of surfactants. Most nonionicsurfactants are considered low-foamingproducts, have good cold watersolubility, and low critical micelleconcentration. Their compatibility withcationic fabric softeners makes thempreferable in certain formulations.Figures 13–16 show chromatographicanalyses of three individual nonionicsurfactants using the Acclaim Surfac-tant column.
Figure 13. Analysis of PEG monoethyl ether (MW-550).
Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile
(B) H2OGradient: 5–20% A in 25 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 10 µLDetection: ELSD
Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile
(B) H2OGradient: 40–65% A in 30 min,
then hold at 65% A for 5 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 10 µLDetection: ELSD
Figure 14. Analysis of NEODOL 25-7.
R—(OCH2CH2)nOH
R = C12 to C15n ~ 7
NEODOL 25-7
mV
Minutes0 10 3020 35
Figure 15. Analysis of Triton X-100 using LC-ESI-MS.
Minutes0 8 204 16 2412
C8H17 (OC2HCH2)nOH
n ~ 10Triton X-100
Abun
danc
e0 2 4 6 8
Minutes
mV
10 12 14 16 18 20 22 25
Inj. Volume: 25 µLDetection: MS (ESI positive, probe 300 °C,
cone 20 V, needle 2.5 kV, SIM 312.2, 356.2,400.4, 444.4, 488.4, 532.4, 576.5, 620.6, 664.6,708.6, 752.5, 796.6, 840.7, 884.7, 928.7, 972.7,1016.8, 1060.7, 1104.7, span 0.5 m/z)
Peak: Triton X-100 (100 ppm)
21118
21079
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: Acetonitrile/50 mM
NH4OAc, pH 5.4 v/v 45/55Temperature: 25 °CFlow Rate: 1 mL/min (0.2 mL/min
to mass spectrometer)
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Polyethylene Glycols (PEGs)Polyethylene glycols (PEGs) are
often nonsurfactant impurities found inethoxylated surfactants, typically in therange of 1–10%. The oligomer distribu-tion is similar to, but broader than thatof the surfactant. Figure 17 illustratesthe exceptional resolution of theAcclaim Surfactant column for indi-vidual oligomers in various PEGs.
Figure 16. Analysis of ZONYL FSO fluorosurfactant.
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile, (B) H2OGradient: 40–70% A in 30 min, then
hold at 70% A for 5 minFlow Rate: 1 mL/minInj. Volume: 10 µLDetection: ELSD
Figure 17. Separation of different polyethylene glycols.
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile, (B) H2OGradient: 3–15% A in 20 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 10 µLDetection: ELSD
mV
Minutes0 5 10 15 20
PEG-600
PEG-400
PEG-300
RfCH2CH2O(CH2CH2O)xH
Rf = F(CF2CF2)yx = 0 to about 15y = 1 to about 7
Zonyl FSO fluorosurfactant
mV
Minutes0 10 3020 35
9
Figure 18. Analysis of a shampoo.
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile
(B) 0.1 M NH4OAc, pH 5.4Gradient: 25–80% A in 30 min,
then hold at 80% A for 15 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 10 µLDetection: ELSD, UV
Figure 19. Analysis of a laundry washing detergent.
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile
(B) 0.1 M NH4OAc, pH 5.4Gradient: 25–80% A in 30 min,
then hold at 80% A for 15 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 5 µLDetection: ELSD, UVSample Prep: Dilute 10× with 70% acetonitrile,
then filtered through 0.2-µm membrane
Analysis of Surfactants in ConsumerProducts
Figures 18–22 demonstrate theapplicability of the Acclaim Surfactantcolumn for analyzing a variety ofconsumer products, such as shampoo,laundry detergent, dish washing liquid,mouthwash, and fabric softener.
Reproducible ManufacturingTo meet the exacting needs of our
customers, each Acclaim Surfactantcolumn is manufactured to stringentspecifications to ensure column-to-column reproducibility. Each column isshipped with a lot validation sheetshowing the test results and specifica-tions for the lot of bonded silica packedinto the column. In addition, eachcolumn is individually tested andshipped with an individual test chro-matogram validating the columnperformance, with respect to selectivity,capacity, and efficiency.
mV
Minutes0 10 3020 35 40 455 15
Laureth Sulfate
25
UV, 225 nm
ELSD
Minutes0 10 3020 35 40 455 15 25
UV, 225 nm
ELSD
Dodecylbenzene sulfonate
Dodecylbenzene sulfonateand Laureth sulfate
10
Figure 20. Analysis of a dishwashing liquid.
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile
(B) 0.1 M NH4OAc, pH 5.4Gradient: 25–80% A in 30 min, then hold at 80% A for 10 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 10 µLDetection: ELSD, UVSample Prep: Dilute 10× with 70% acetonitrile,
then filtered through 0.2-µm membrane
Figure 21. Analysis of a mouthwash.
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 x 150 mmMobile Phase: (A) Acetonitrile
(B) 0.1 M NH4OAc, pH 5.4Gradient: 25–80% A in 30 minTemperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 20 µL (direct injection)Detection: ELSD
Peaks: 1. Sodium sacchrin and benzoate2. Domiphen bromide3. Cetylpyridinium chloride
Figure 22. Analysis of a fabric softener.
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Column: Acclaim Surfactant, 5 µmDimensions: 4.6 × 150 mmMobile Phase: (A) Acetonitrile
(B) THF(C) 0.1 M NH4OAc, pH 5.4
Gradient: 40% A/10% B/50% C to 75% A/ 10% B/75% C in 20 min,then hold for 10 min
Temperature: 30 °CFlow Rate: 1 mL/minInj. Volume: 20 µLDetection: ELSD
Peaks: Methyl bis[ethyl(tallowate)]-2-hydroxyethyl ammonium methyl sulfate (500×)
Minutes0 10 3020 35 405 15
Dodecylbenzene sulfonate
25
UV, 225 nm
ELSD
Dodecylbenzene sulfonateand laureth sulfate
Minutes0
mV
10 3020
1
2
3
Minutes0
mV
10 3020
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ORDERING INFORMATION
To order in the U.S., call (800) 346-6390 or contact the Dionex Regional Officenearest you. Outside the U.S., order through your local Dionex office or distribu-tor. Refer to the following part numbers.
Product Description Part Number
Acclaim Surfactant Analytical Column (4.6 × 150 mm) ............................063201Acclaim Surfactant Analytical Column (4.6 × 250 mm) ............................063203Acclaim Surfactant Guard Cartridges (4.3 × 10 mm), 2 ea ........................063215Acclaim Guard Kit (holder and coupler) ....................................................059526Acclaim SST Guard Cartridge Holder ........................................................059456Guard to Analytical Column Coupler .........................................................059457
SPECIFICATIONS
Starting Material:Ultrapure silica
Particle Size:5 µm
Particle Shape:Spherical
Particle Size Distribution (40/90):1.2
Total Carbon Content (%):12%
Endcapped:Yes
Metal Impurity (ppm) Na, Fe, Al:<10.0
Pore Volume (mL/g):0.9
Average Pore Diameter (Å):120
Surface Area (m2/g):300
pH range:2.5–7.5
Temperature:<60 °C
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Acclaim and AAMS are registered trademarks of Dionex Corporation.
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