Waters IC-Pak Column and Guard User Manual

[ Care and Use ManUal ]

IC-pak Column and guard Column

I. IntroduCtIon

Waters IC-Pak™ anion (A) and cation (C) columns are designed for use

in Ion Chromatography (IC) applications to separate ions.

a. Anion Columns

The stainless steel anion columns separate and quantify many

anions, such as F-, CI-, NO

-

, Br-, NO

2

ppb levels. Table 1 lists the characteristics of IC-Pak anion columns.

Table 1: Anion Column Characteristics

Anion Column Dimensions Particle Size Capacity

IC-Pak A 4.6 x 50 mm 10 µm 30 ± 3 µeq/mL

IC-Pak A HC

(High Capacity)

IC-Pak A HR

(High Resolution)

4.6 x 150 mm 10 µm 30 ± 3 µeq/mL

4.6 x 75 mm 6 µm 30 ± 3 µeq/mL

The packing material is a polymethacrylate resin with a quaternary

ammonium functional group. The columns are shipped in 1.3 mM

gluconic acid/1.3 mM boric acid (pH 8.5).

-

, HPO

3

2-

, and SO

4

2-

anions at

4

Contents

I. IntroduCtIon

II. InstallatIon

III. eluent and sample guIdelInes

IV. operatIon

V. Care and maIntenanCe

VI. orderIng InformatIon

VII. Warranty/serVICe

b. Cation Columns

The non-metallic cation columns separate and quantify Li+, Na+,

+

NH

, K+, Mg2+, Ca2+, Sr2+ and Ba2+ cations at ppb levels. T he Waters

4

cation guard column, placed in the solvent stream before the

sample injector, is used only to aid monovalent cation detection by

removing polyvalent cations from the solvent stream.

Table 2 lists the characteristics of IC-Pak cation and cation guard

columns.

IC-Pak Column and Guard Column 1

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COMPRESSION SCREW OR NUT

T

UBE

FERRULE

END MUST BE STRAIGHT
AND SMOOTH TO ACHIEVE
MAXIMUM COLUMN EFFICIENCY

CRITICAL DISTANCE TO BE DETERMINED BY
THE UNION OR COLUMN FITTING, ETC.

Table 2: Cation Column Characteristics

Cation Column Dimensions Particle Size Capacity

IC-Pak C 4.6 x 50 mm 10 µm 12.0 ± 0.2 µeg/mL

Guard 4.6 x 50 mm n/a 2.0 ± 0.2 meg/mL

The packing material is a styrene divinylbenzene resin with a

sulfonic acid functional group. The columns are shipped in 2 mM

nitric acid.

II. InstallatIon

Before attaching the column in the flow path:

1. Directly connect the HPLC injector to the detector by replacing the old

column with a zero-dead-volume union.

2. Flush the lines free of microparticulates and previous solvents. Flush

the injector loop if applicable.

3. Remove the union.

4. Install the column.

To prepare a new tubing/ferrule connection:

1. Scribe the circumference of the tubing at the desired break using either

a file with a cutting edge or a tube cutter.

2. Grasp the tubing on both sides of the scribe mark with cloth-covered

pliers (to prevent marring the tube surface), and gently work the tube

back and forth until it separates.

Note: Ensure that the tubing end is straight, open, and free of burrs.

3. Slide the compression fitting, followed by the ferrule (large end of the

taper first) over the tube.

Note: Properly bottom the tubing in the fitting seat. Otherwise, dead

volume could result in sample band spreading.

Figure 1: Ferrule and Compression Assembly (Stainless Steel Column)

a. Installing a Stainless Steel Column

Remove the end plugs from the column and save them for use when

the column is removed from the system and stored. The column

outlet is indicated by an arrow on the label (showing the direction

solvent should flow).

To install the column, thread the inlet and outlet fittings into the

column until finger tight, and then tighten the fittings 1/4-to-1/2

turn. Do not over-tighten. Over-tightening will damage the

connection. A properly prepared and assembled compression fitting

in good condition is all that is required.

Prepare a new tubing/ferrule connection (Figure 1) when a new

column is connected or when a damaged compression screw or worn

ferrule are removed.

Note: The tubing distance beyond the ferrule may differ for different

column types. Re-size the tubing to the correct distance by replacing

the ferrule.

IC-Pak Column and Guard Column 2

b. Installing Non-Metallic Columns

Remove the end plugs from your column and save them for use when

the column is removed from the system and stored. The column

outlet is indicated by an arrow on the label (showing the direction

solvent should flow).

To install the column, thread the inlet and outlet fittings into the

column until finger tight, and then tighten the fittings 1/4-to-1/2

turn. Use caution with non-metallic columns. Over-tightening these

fittings may cause damage which results in a leaking connection.

A properly prepared and assembled compression fitting in good

condition is all that is required.

[ Care and Use ManUal ]

COMPRESSION SCREW

.021-inch (i.d.)

TEFZEL TUBING

TEFLON® FACE

BEVEL

FERRULE

STAINLESS STEEL

FAC E

FROM SOLVENT

RESERVOIR

PUMP

Inj

OPTIONAL
GUARD-PAK
AND HOLDER

IC-PAK

A

COLUMN

DETECTOR

TO WASTE

HIGH SENSITIVITY

NOISE FILTER

PUMP

Inj

HIGH SENSITIVITY

NOISE FILTER

ELUENT

EDTA/ HNO

3

GUARD COLUMN Inj

IC-PAK C

430/431

PUMP

Inj

HIGH SENSITIVITY

NOISE FILTER

ELUENT

EDA/ HNO

3

Inj

IC-PAK C

430/431

To replace a fitting:

1. Use a sharp razor blade to make a long tapering cut in the tubing as

shown in Figure 2. Alternately, if tubing is not in short supply, stretch

the tubing (after warming over low heat) between two sets of pliers and

cut the tube at thinnest point. The resulting taper will slip through the

fittings more easily.

2. Pass the tubing through the compression screw and ferrule. Be sure the

stainless steel side of the ferrule is facing the screw. Pull the tubing

with pliers to ensure the bevel or taper is completely past the ferrule.

Figure 5: IC Systems for Divalent Cation Analysis

III. eluent and sample guIdelInes

a. Preparing the Eluent Requirements

3. Hold the ferrule with a second set of pliers and give the tubing a half

twist to lock the ferrule. Cut the tubing flush with the end of the ferrule.

Figure 2: Ferrule and Compression Assembly (Non-Metallic Column)

c. Configuring the Column In the System

Install stainless steel or non-metallic anion columns relative to the

other major components as shown in Figure 3.

Water-miscible organic solvents, which may be used as modifiers to

reduce hydrophobic interaction between sample and packing, must

not exceed the concentrations listed below.

IC-Pak A Columns 12% acetonitrile in water

IC-Pak C and Guard Columns 10% acetonitrile in water

Note: Organic solvent concentration should not exceed 20%. It is

possible, however, to use organic solvents up to 50% concentration

by gradual introduction via gradient method. Perform solvent

changeovers at 0.1 mL/min over 6 hours. Dedicate column to use in

the organic concentrations over 20%.

Use high performance liquid chromatography (HPLC) grade solvents

that have been filtered to remove microparticulate matter greater

than 0.45 µm in size. Filtering will ensure optimum long-term

performance of the column. Vacuum filtration, sonication, or sparging

may be used to remove dissolved gas which could affect results.

Before filtering or clarifying any solvents, flush the filters with

100 mL of the eluent. Discard the filtered eluent. Surfactants used to

treat some filters may otherwise affect analysis.

Figure 3: IC System for Anion Analysis

Install cation columns with a guard column for detecting monovalent

cations (Figure 4) or without a guard column for polyvalent cations

(Figure 5).

Figure 4: IC Systems for Monovalent Cation Analysis

IC-Pak Column and Guard Column 3

An in-line filter may be used to remove particulates in the solvent

and contaminants which the 0.45 µm filter does not remove.

Note: Do not use tetrahydrofuran (THF) or methanol with IC-Pak A columns.