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J

audzems

:

J

ournal of

AOAC I

nternational

V

ol

.

99, N

o

.

4, 2016 

1113

Chloride in Milk, Milk Powder, Whey Powder, Infant

Formula, and Adult Nutritionals by Potentiometric Titration

Method: First Action 2016.03

G

reg

J

audzems

Nestlé USA, Inc., Quality Assurance Center, Chemistry Technical Services, 6625 Eiterman Rd, Dublin, OH 43017

T

ian

Y

an

and

W

an

X

in

Chinese Academy of Inspection and Quarantine Comprehensive Test Center, Beijing 100123, China

S

takeholder

P

anel on

I

nfant

F

ormula

and

A

dult

N

utritionals

E

xpert

R

eview

P

anel

for

SPIFAN N

utrient

M

ethods

Darryl Sullivan (Chair)

, Covance Laboratories

John Austad

, Covance Laboratories

Sneh Bhandari

, Silliker Laboratories

Esther Campos-Gimenez

, Nestlé

Adrienne McMahon

, Nestlé

Scott Christiansen

, Perrigo

Hans Cruijsen

, FrieslandCampina

Wil van Loon

, FrieslandCampina

Jon DeVries

, General Mills/Medallion Laboratories

Brendon Gill

, Fonterra

Don Gilliland

, Abbott Nutrition

Karen Schimpf

, Abbott Nutrition

Min Huang

, Frontage Laboratories

Estela Kneeteman

, National Institute of Industrial Technology

Bill Mindak

, U.S. Food and Drug Administration

Maria Ofitserova

, Pickering Laboratory

Shay Phillips

, Mead Johnson

Guenther Raffler

, Central Laboratories Friedrichsdorf–

Eurofins

Kate Rimmer

, National Institute of Standards and Technology

Melissa Phillips

, National Institute of Standards and

Technology

David Woollard

, Hill Laboratory

Jinchuan Yang

, Waters Corp.

Introduction

The presented method is a combination of AOAC First

Action methods

2015.07

(1) and

2015.08

(2). As both methods

were reviewed by the Expert Review Panel as equivalent, the

authors were asked to combine the methods into one method.

This combined method maintains the performance requirements

cited in each separate method single-laboratory validation

and therefore meets the

Standard Method Performance

Requirements

(3).

AOAC Official Method 2016.03

Chloride in Milk, Milk Powder, Whey Powder, Infant

Formula, and Adult Nutritionals

Potentiometric Titration Method 

First Action 2016

(Applicable to the determination of chloride in milk, milk

powder, whey powder, infant formula, and adult nutritionals

by potentiometry, with an analytical range of 0.35–1060 mg

chloride/100 g reconstituted product or ready-to-feed (RTF)

liquids).

Caution

: Consult Material Safety Data Sheets for all

substances that are required and considered

hazardous. Follow all laboratory safety precautions

and wear proper personal protective equipment.

A. Principle

Reconstitute powder samples by dissolving 25 g powder

sample in 200 g warm water (40°C); RTF products are ready

to use as they are. Precipitate proteins by adding precipitation

solutions I and II, and then centrifuge. Acidify the supernatant

with nitric acid solution. Titrate chloride ions against

standardized silver nitrate solution (0.1 M), potentiometrically

using a silver electrode to detect the end point.

B. Apparatus

Common laboratory equipment and, in particular, the

following:

(a) 

Analytical balance

.—Precision to 0.1 mg.

(b) 

Centrifuge

.—Tabletop with rotor for 50 mL conical

tubes, capable of operating at ≥12000 ×

g

.

(c) 

Centrifuge tubes

.—50 mL, conical, polypropylene.

(d) 

Pipets

.—1, 10, 20, 50, and 100 mL, Class A glass

volumetric or automatic (Eppendorf or equivalent).

Submitted for publication April 2016.

Adopted as a First Action Official Method by the Expert Review

Panel on SPIFAN Nutrient Methods.

Approved on: March 16, 2016.

Corresponding author’s e-mail:

greg.jaudzems@us.nestle.com

DOI: 10.5740/jaoacint.16-0123

OFFICIAL METHODS

6