ASH ANALYSIS

PHÂN TÍCH TRO

GVHD: Phạm Thị Hoàn

hoanpt@hcmute.edu.vn
CONTENT

01 Introduction

Ash Contents in Foods 02

03 Role of Ash analysis

Sample Preparation 04
05 Method: Dry Ashing

Method: Wet Ashing 06

3
WHAT IS ASH?
4
 INTRODUCTION

Ash refers to the inorganic residue remaining after either

ignition or complete oxidation of organic matter in a foodstuff.

5
 INTRODUCTION

The ash content is a measure of the total amount of

minerals present within a food

The mineral content is a measure of the amount of specific

inorganic components present within a food

Ca Na K Cl
6
CONTENT

01 Introduction

Ash Contents in Foods 02

03 Role of Ash analysis

Sample Preparation 04
05 Method: Dry Ashing

Method: Wet Ashing 06

99
ASH CONTENTS IN FOOD

10
CONTENT

01 Introduction

Ash Contents in Foods 02

03 Role of Ash analysis

Sample Preparation 04
05 Method: Dry Ashing

Method: Wet Ashing 06

11
11
 ROLE OF ASH ANALYSIS

✓ To proximate the nutritional evaluation.

✓ Ashing is the first step in the preparation of

food sample for specific elemental analysis.

12
CONTENT

01 Introduction

Ash Contents in Foods 02

03 Role of Ash analysis

Sample Preparation 04
05 Method: Dry Ashing

Method: Wet Ashing 06

13
13
 SAMPLE PREPARATION

✓ It needs to be very carefully

chosen a weight of sample
so that it represents the
original materials

A 2–10 g sample generally is used

for ash determination

14
 SAMPLE PREPARATION
✓ Milling, grinding to reduce the size of sample
→ contamination by microelements
Most grinders and
mincers are of steel
construction

Distilled-deionized
water always should
be used in dilutions
15
 SAMPLE PREPARATION
✓ Plant Materials should be dried in two stages (i.e.,
first at a lower temperature of 55◦C, then a higher
temperature). Plant material with 15% or less
moisture may be ashed
without prior drying.

16
 SAMPLE PREPARATION

✓ Fat and Sugar Products

Animal products, syrups, and spices
require treatments prior to ashing
because of high fat, moisture
(spattering, swelling), or high sugar
content (foaming) that may result in
loss of sample.

17
 SAMPLE PREPARATION

✓ Fat and Sugar Products

Meats, sugars, and
syrups need to be
evaporated to dryness
on a steam bath or
with an infrared (IR)
lamp.

18
 SAMPLE PREPARATION

✓ Fat and Sugar Products

Smoking and burning may occur
upon ashing for some products
(e.g., cheese, seafood, spices).
Allow this smoking and burning
to finish slowly by keeping the
muffle door open prior to the
normal procedure
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ASHING METHOD

Dry Ashing Wet Ashing

22
 DRY ASHING - Definition

Dry ashing is incineration at high temperature

(525°C or higher).

24
 DRY ASHING - Definition

Dry ashing refers to the use of a muffle furnace

capable of maintaining temperatures of 500–600°C.

CxHyOzNn → CO2 + H2O + NxOy

25
DRY ASHING - Instrumentation
crucibles

muffle furnaces 26
DRY ASHING - Instrumentation

tongs

eyewear gloves desiccator

27
 DRY ASHING – Procedures
Step
Weigh a crucible with sample
1
Step Predry the moist sample over the
2 flame
Step Place the sample in muffle furnace at
3 500-550°C for 4-6 hours (or more)
Step Carefully remove the silica crucible from
4 muffle furnace (T<250°C)

Step Keep crucible in desiccator for cooling,

5 after cooling take a final weight

AOAC Methods 900.02 AOAC (Association of Official Analytical Chemists)

28
DRY ASHING – Calculation

The ash content is calculated as follows:

% ash (wet basis)

𝑚𝑎𝑓𝑡𝑒𝑟 𝑎𝑠ℎ𝑖𝑛𝑔 − 𝑚𝑐𝑟𝑢𝑐𝑖𝑏𝑙𝑒

%𝐴𝑠ℎ = ∗ 100
𝑚𝑠𝑎𝑚𝑝𝑙𝑒 (𝑤𝑒𝑡)

30
DRY ASHING – Calculation
The ash content is calculated as follows:
% ash (dry basis)

𝑚𝑎𝑓𝑡𝑒𝑟 𝑎𝑠ℎ𝑖𝑛𝑔 − 𝑚𝑐𝑟𝑢𝑐𝑖𝑏𝑙𝑒

%𝐴𝑠ℎ = ∗ 100
𝑚𝑠𝑎𝑚𝑝𝑙𝑒 (𝑑𝑟𝑦)

𝑚𝑠𝑎𝑚𝑝𝑙𝑒 (𝑑𝑟𝑦) = 𝑚𝑠𝑎𝑚𝑝𝑙𝑒 (𝑤𝑒𝑡) ∗ 𝐾

Where, K – dry matter coefficient = % total solid/100

31
 DRY ASHING
safe method

01 no added reagents
or blank
time required 02
ADVEN-
01 DISAD TAGES little attention/ a lot
VEN- 03 of samples
expensive
02 TAGES can be used in
equipment 04
other analyses
03
loss of the Volatile elements at risk of being lost include As, B,
volatile elements Cd, Cr, Cu, Fe, Pb, Hg, Ni, P, V, and Zn.
32
ASHING METHOD

Dry Ashing Wet Ashing

34
 WET ASHING - Definition
Wet ashing is a procedure for oxidizing organic
substances by using acids and oxidizing agents
or their combinations.

Its primary use is

preparation for specific
mineral analysis

35
 WET ASHING - Reagents
Combinations of the following acid solutions are
used most often:
1) nitric acid (HNO3),
2) sulfuric acid (H2SO4) -hydrogen peroxide
(H2O2),
3) perchloric acid (HClO4).

36
WET ASHING – Procedures
Accurately weigh a dried, ground (1g)
01 sample

Add 3ml of H2SO4 followed by 5ml of HNO3 to the

02 sample in the flask

Heat the sample on a hot plate at ca. 200◦C (boiling)

03 Brown-yellow fumes will be observed

Add 3-5 ml HNO3 and heat sample until the

04 solution is clear to straw yellow

37
 WET ASHING
Minerals remain in
solution

01 No volatilization
of minerals
Need constant 02
operator’s attention ADVEN-
01 DISAD TAGES Oxidation
VEN- 03 time is short
Corrosive
02 TAGES
reagents
03
Small numbers
of samples
38
 ASHING METHOD

Dry Ashing Wet Ashing

40
MICROWAVE ASHING
• Reduces sample analysis time to minutes
• Operate under pressure, higher boiling point
• Use less corrosive acid (nitric vs. perchoric)
• Multiple samples
01 can be processed

02 Ashing
Microwave Wet
03 Expensive
equipment
Microwave Dry Ashing
41
MICROWAVE ASHING- Instrumentation

Plants, dried egg yolks

t = 4h → 20 min
Lactose
t = 16h →35 min

42
 SUMMARY

✓ Dry ashing and wet oxidation (ashing), can be

done by conventional means or using microwave
systems.

✓ The procedure of choice depends upon the use of

ash following its determination, and limitations
based on cost, time, and sample numbers.

44
 SUMMARY WET ASHING

DRY ASHING Used as a preparation for

specific elemental analysis by
Incineration at high simultaneously dissolving
temperatures in a minerals and oxidizing all
muffle furnace. organic material.

Except for certain elements Wet ashing conserves volatile

(Cu, Fe, Pb, Hg…), the element, but requires more
residue may be used for operator time than dry ashing
further specific mineral and is limited to a smaller
analyses. number of samples.

45
 SUMMARY

Microwave ashing technology reduces the time for

analyses, and requires little additional equipment
(special fume hood) or space (heat room).

46
 THANKS!
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