Appl i cati o n No te 014

Measuring Salt Content in Canned

Vegetables Using Manual Titration
Water Analysis Instruments, Thermo Fisher Scientific

Key Words
Salt analysis, manual titration, canned vegetables, food analysis, titration of
chloride.

Goal
The following application note describes how to reliably measure the salt
content in canned vegetables by manual titration to mV endpoint using
a Thermo Scientific™ Orion™ Chloride Ion Selective Electrode (ISE) or a
Thermo Scientific Orion Silver Billet Electrode.

Introduction Required Reagents and Solutions

Salt analysis is a routine task in food analysis, and • 0.1M Silver Nitrate Solution
titration of chloride (Cl-) is a common technique to
• .1M NaCl (sodium chloride) Standard (Cat. No.
0
determine the sodium chloride (NaCl)/salt content in
941706)
food. In this note, Cl- in ground peeled tomatoes is
manually titrated by silver nitrate (AgNO3) to a fixed • ptimum Result B Filling Solution (Cat. No.
O
millivolt reading on a Thermo Scientific Orion chloride 900062) for chloride ion selective electrode; or, silver
ion selective electrode (ISE) or by a Thermo Scientific chloride pH filling solution (Cat No. 900011) for
Orion Silver Billet electrode. This method produces results silver billet electrode
comparable to autotitration or ion chromatography (IC)
• Ionic Strength Adjuster (ISA) (Cat. No. 940011)
methods, yet is simple and inexpensive.
• Deionized water (DI) of conductivity <2 µS/cm
Recommended Equipment
• hermo Scientific™ Orion Star™ A211 pH meter, Star
T
A214 pH/ISE meter or equivalent

• rion 9617BNWP Chloride ISE or Orion 9780SC

O
Silver Billet electrode with 91CBNC cable

• Orion Stirrer Probe (Cat. No. 096019)

• Swing Arm Stand (Cat. No. 090043)

• Electrode Polishing Strip (Cat. No. 948201)

• 10 mL burette, burette clamp, ring stand

2 Solutions Preparation % salt g or mL liquid food mL of pureed solid food
Prepare or purchase AgNO3 titrant solution of 0.1M. To
0.1 12.5 125
prepare: weigh approximately 8.5g AgNO3 and dissolve
in 500 mL DI. Store in a brown or opaque bottle. 0.25 5.0 50
Standardize as indicated below. 0.50 5.0 50
0.75 20* 20
Meter Setup
Connect Orion electrode and the stirrer probe to the 1.0 20* 20
meter. In Setup, select the mV mode, set read type to 5.0 4* 4
continuous, and set the stirrer speed to 3. Refer to the 10.0 2* 2
Orion meter user guide for more details.
*Prepare like for a solid sample (50g sample plus 450 mL
Electrode setup, storage, soaking, and rinsing DI), then use this volume of prepared sample.
See the electrode user guide or instruction sheet.
Sample titration
Electrode Performance Check Prepare samples as detailed above. Prepare one to three
See Standardization of Titrant section, below. Alternately, replicates of each sample as desired. Titrate the sample, as
analyze a QC sample. described above. Record the volume of titrant used (Vs).
Calculate the salt (sodium chloride) content of the sample
Titration setup
using the equations on the following page. After each
Secure the burette on the clamp. Fill the burette with
titration, rinse the electrode and stirrer with DI, wipe with
AgNO3 solution (titrant) and adjust the level to the
a lint-free wiper, and rinse again with DI. Tap to remove
zero mark.
excess water drops.
Standardization of Titrant
Quality Control (QC)
Add 3.0 mL of 0.1M NaCl standard, 50 mL of DI, and 1
Recommended QC procedures may include: titrant
mL ISA to a 100 mL beaker. Rinse the electrode and
standardization, analysis of chloride standard or QC
stirrer with DI. Immerse the electrode and stirrer at least
sample, duplicates, matrix spike, and/or blank titration.
one inch below the liquid level in the beaker. Tap to
release bubbles trapped on the surface of the electrode. Accuracy can be improved by performing a blank
Turn on the stirrer. titration. Place 50 mL of DI into a 150 mL beaker. (If
solid samples are titrated, use 100 mL of DI). Add 1 mL
Adding AgNO3 titrant from the burette, titrate at
ISA for each 50 mL DI. Titrate. Subtract the volume
moderate rate until the mV reading is near 240 mV.
required to reach endpoint in the blank titration (Vb)
(Note: mV reading will start low and increase as titrant is
from the sample titration volume. See Calculations on the
added). Allow time for the reading to stabilize before
following page.
adding more titrant. As endpoint is approached, the
reading will take longer to stabilize. Start to add titrant
slowly until the reading just exceeds 260 mV (or 290 mV
for silver billet). This is the endpoint of the titration. See
an example titration curve on the following page. Record
the volume of titrant used (Vt). Repeat the
standardization procedure if required by user’s protocol.
Calculate the titrant concentration (T) as indicated on the
following page.

Sample Preparation and Preservation

Liquid samples: Measure with a pipet (mL) or with a scale
(gram, g). Record exact amount. Transfer to a 150 mL
beaker and add DI water to the 50 mL mark on the
beaker. Add 1 mL ISA.

Solid samples: Weigh about 50 g of sample. Record exact

weight to 0.01 g. Place into blender or food processor.
Add 450 mL of DI water. Blend until smooth and liquid.
Using a wide-mouth pipet or graduated cylinder, transfer
an amount of the well-mixed sample to a 150 mL
beaker. Add DI water to 100 mL mark on the beaker.
Add 2 mL ISA.
Results 3
Salt Analysis in Ground Peeled Tomatoes by Manual Titration
Endpoint Volume* ppm Salt (sodium % Salt (sodium Sodium (mg per 66
Sample Weight (g)
(mL) chloride) in sample chloride) in sample g serving)
Sample 1 4.33 3.83 5060 0.506 % 131
Sample 2 4.15 3.68 5070 0.507 % 132
Sample 3 4.10 3.68 5130 0.513 % 133
* The endpoint volume of the blank Mean 5090 0.509 % 132
(0.10 mL) has been subtracted RSD 0.8 %
Spike Sample Recovery 97.2 %

Raw Data

Comparison of Manual Titration with Other Methods

ppm Salt (sodium chloride) in % Salt (sodium chloride) in Sodium per serving (mg per
Method
sample sample 66 g serving)
Manual Titration 5090 0.509 % 132
Autotitration 5020 0.502 % 130
Ion Chromatography 4860 0.486 % 126
RSD 2.4 %

Calculations
1. T
itrant concentration (T)
T = VCl × MCl ÷ Vt
Example: 3.00 mL × 0.100 M ÷ 3.06 mL = 0.0980 M titrant
T = concentration of silver nitrate titrant (M, mol/L)
VCl = volume of sodium chloride standard (mL)
MCl = molarity of the sodium chloride standard (M, mol/L)
Vt = volume of titrant used at the end point for titrant standardization (mL)
2. % Salt (sodium chloride) concentration in the sample (C%) as % NaCl*
C% = 5.844 × T × (Vs - Vb) ÷ (W × DF)
Example: 5.884 × 0.0980M × (3.93 – 0.10 mL) ÷ (51.5 g × 0.103) = 0.414% salt
C% = concentration of sodium chloride in the sample (%)
Vs = volume of titrant used at the end point for sample titration (mL)
Vb = volume of titrant used at the end point for blank titration (mL), if blank titration performed.
W = weight of sample (g)
DF = dilution factor; mL of sample titrated ÷ total mL of pureed sample, e.g. 51.5 g sample ÷ (450 mL + 51.5)
= 0.103.
3. ppm Salt (sodium chloride) concentration in the sample (Cppm) as ppm NaCl*
Cppm = 58440 × T × (Vs - Vb) ÷ (W or V × DF)
Example: 58440 × 0.0980M × (3.93 – 0.10 mL) ÷ 5.30 mL = 4140 ppm or mg/L salt
Cppm = concentration of salt (sodium chloride) in the sample (ppm, mg/kg, or mg/L)
V = volume of sample titrated
4. S odium* per serving (Cserving) as mg sodium per serving of food
Cserving = Cppm × 0.3934 × S ÷ 1000
Example: 4140 ppm × 0.3934 × 66 mL ÷ 1000 = 107 mg Na per 66 mL serving
Or, Cserving = C% × 3.934 × S
Example: 0.414% × 3.934 × 66 g = 107 mg Na per 66g serving
Cserving = sodium per serving of food (mg per serving of food)
S = weight or volume of one serving (g or mL)

*assumes that the sodium and chloride in the sample come from salt, NaCl
Example of a Titration Curve for Salt by Silver Billet Electrode
Titration of Salt (NaCl) mL Titrant mV mV change per mL change

Appl i cati o n No te 014

350 700
2.00 172.6
325
600 2.50 198.5 51.8
2.75 241.1 170.4
300
Silver billet endpoint, 500 2.80 260.4 386.0

mV change per mL change

275
290 mV at 2.85 mL 2.85 290.5 602.0
mV on Silver Billet

400
2.90 318.4 558.0
250
3.00 344.3 180.0
300
225 3.04 349.5 130.0
200
200

100
175

150 0
2 2.2 2.4 2.6 2.8 3 3.2
mL silver nitrate titrant added

titration curve mV change per mL change

References
1. Sodium Chloride in Canned Vegetables. AOAC Official Method 971.27 – 1976. www.aoac.org

2. EPRI FGD chemistry and analytical methods handbook rev 1, volume 2, Method 4, O4-1—O4-27. www.epri.com

Visit www.thermoscientific.com/water for additional information on Thermo Scientific Orion products, including
laboratory and field meters, sensors and solutions for pH, ion concentration (ISE), conductivity and dissolved oxygen
analysis plus spectrophotometry, colorimetry and turbidity products.

To purchase an Orion chloride electrode, ISE meter and other related products, please contact your local equipment
distributor and reference the part numbers listed below.

Product Description Part Number

Thermo Scientific Orion Star A214 pH/ISE Benchtop Meter STARA2140
Meters Thermo Scientific Orion Star A211 pH Benchtop Meter STARA2110
Thermo Scientific Orion Versa Star pH/ISE Benchtop Meter VSTAR40A
Thermo Scientific Orion Chloride Ion Selective Electrode 9617BNWP
Electrodes
Thermo Scientific Orion Silver Billet Electrode 9780SC
Thermo Scientific Orion NaCl Standard, 0.1M 941706
Thermo Scientific Orion Optimum Results B Filling Solution 900062
Solutions
Thermo Scientific Orion Electrode Filling Solution 900011
Thermo Scientific Orion ISE Ionic Strength Adjuster (ISA) 940011
Thermo Scientific Orion Stirrer Probe 096019
Accessories Thermo Scientific Orion Swing Arm Stand 090043
Thermo Scientific Orion Electrode Polishing Strip 948201

thermoscientific.com/water

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