JCAM No.

104-R1

Japan Customs Analysis Methods

No. 104

Analysis Method for Starch

1. Scope 4. Reagents

This analysis method is applied to goods which All chemicals must be JIS special reagent grade or
require quantitative determination of starch content equivalent, unless otherwise specified.
using the modified Ewers polarimetric method.
(a) 1.128% hydrochloric acid aqueous solution
2. Outline of Test Method This hydrochloric acid solution is prepared such
that 10 mL of the solution requires 30.94 mL of
This method determines starch content in flour
0.1 N sodium hydroxide for neutralization. The
and its preparations. The procedure is as follows.
indicator used for neutralization is methyl red (1%
(1) Sample preparation
solution in 95% ethyl alcohol).
(2) Measurement of total sugar content by
(b) 25% hydrochloric acid aqueous solution
saccharimeter.
Prepare this solution to obtain a specific gravity
(3) Measurement of sugar content of water soluble
of 1.126 (20 °C).
active substance by saccharimeter
(c) 4% sodium phosphotungstate aqueous solution
(4) Calculation of starch content.
(d) 40% zinc sulfate aqueous solution
3. Apparatus (e) 10% potassium ferrocyanide aqueous solution.
(f) Filter paper
(a) Saccharimeter Specified in JIS P 3801 Grade 2, 185 mm in
The apparatus should be equipped with a diameter, or equivalent product.
transmitted light source of a sodium vapor lamp
and a half-shadow angle of the Lippich polarizing 5. Sample Preparation
system. The scale should conform to the
Pulverize the sample to pass through a sieve with
International Sugar Scale adopted by the
1 mm openings.
International Commission for Uniform Methods of
Sugar Analysis (ICUMSA). 6. Measurement Procedure
(b) Observation tube
6.1. Measurement of Total Sugar Content
A tube of 200 mm (tolerance ± 0.03 mm) with a
swollen shape at one end, with an optically-inactive Mix the sample to obtain a homogenous mixture.
glass lid equipped with a gum washer, and a closing Weigh 2.500 g (± 0.001 g) of the sample in a 200-mL
metal fitting for the glass lid. Erlenmeyer flask. Add 25 mL of 1.128% hydrochloric
(c) Pulverizer acid aqueous solution. Mix until the hydrochloric acid
(d) Sieve with 1 mm openings. solution has thoroughly infiltrated the sample. Add
further 25 mL of 1.128% hydrochloric acid aqueous

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 JCAM No.104-R1
solution. Connect the flask to a straight tube and Use approximately 30 mL of the filtrate to rinse the
vigorously shake in a boiling water bath for 1 minute. observation tube. Then, use the 200-mm observation
After heating in the boiling water bath for 15 minutes, tube to measure the sugar content in the filtrate at
remove the Erlenmeyer flask and immediately cool to 20 °C(3). The sugar content is designated as S’.
20 °C. Transfer the content in the flask to a 100-mL
7. Calculation of Starch Content
volumetric flask. Wash the Erlenmeyer flask with water
at least three times and transfer all the washing liquid Calculate the starch content in the sample from the
into the volumetric flask. Add 10 mL of 4% sodium following formula and express as percentage of dry
phosphotungstate and mix (1). Dilute to the volume with weight.
water at 20 °C and filter (2). Discard the first 10 to 15 mL
of the filtrate. Use approximately 30 mL of the filtrate to 26.6 × 𝑁𝑁 × ( 𝑆𝑆 − 𝑆𝑆′) 100
𝐴𝐴, % = ×
[𝑎𝑎𝑎𝑎] 100 − М
rinse the observation tube. Then, use the 200-mm
observation tube to measure the sugar content in the Where –
filtrate at 20 °C (3). The sugar content is designated as S. A : starch content (%)
N : 26.0 (value using a Schmidt Haensch device)
Note 1) Instead of 4% sodium phosphotungstate,
[αD] :
5 mL of 40% zinc sulfate and 5 mL of 10%
Oat starch 181.3
potassium ferrocyanide may be added.
Barley starch 181.5
Note 2) If precipitation occurs after adding 4%
Wheat starch 182.7
sodium phosphotungstate into the filtrate,
Rye starch 184.0
repeat the procedure by increasing the initial
Corn starch 184.5
volume of the 4% sodium phosphate.
White potato starch 185.7
Note 3) Refer to Customs Analysis Method No. 101
Rice starch 185.9
“Determination of Sugar Content of Sugar” for
Other starch 184
the determination of sugar content.
S : sugar content determined in 6.1.
6.2. Measurement of Sugar Content of Water S’ : sugar content determined in 6.2.
Soluble Active Substance M : moisture content determined in Note 4.
Round down to the nearest first decimal place.
Measure 12.500 g (± 0.001 g) of the sample in a
beaker. Transfer this sample to a 250-mL volumetric Note 4) The moisture content of the sample is
flask with approximately 200 mL of water. Mix from time determined as follows.
to time to extract for 1 hour at room temperature. Dilute Accurately weigh 5 g (± 0.001 g) of the
the solution to volume with water and filter. Using a sample prepared in a weighing bottle. Dry in a
volumetric pipette, transfer 50 mL of the filtrate into a hot forced air oven at 105 °C (±1 °C) to constant
200-mL Erlenmeyer flask. Add 2.1 mL of a 25% weight. Transfer the weighing bottle to a
hydrochloric acid aqueous solution. Connect the flask to desiccator for 30 minutes to cool down before
an air condenser and vigorously shake in a boiling water weighing. The weight reduced is taken as
bath for 1 minute. After heating in the boiling water bath moisture content and is expressed as a
for 15 minutes, remove the Erlenmeyer flask and percentage. Sampling of the sample is
immediately cool to 20 °C. Transfer the content in the conducted simultaneously with the weighing of
flask to a 100-mL volumetric flask. Wash the the sample for 6.1. and 6.2.
Erlenmeyer flask with water at least three times and
8. Temperature Correction
transfer all the washing liquid into the volumetric flask.
Add 10 mL of 4% sodium phosphotungstate and mix (1).
When sugar content is determined at a
Dilute the solution to volume with water at 20 °C and temperature other than 20 °C, temperature correction of
filter (2). Discard the first 10 to 15 mL of the filtrate. the sugar content must be applied using the temperature

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 JCAM No.104-R1
at the weighing of the sample according to the following
formula.

𝑆𝑆𝑆𝑆20, % = 𝑆𝑆𝑆𝑆 − 0.02 × ( 20 − 𝑇𝑇𝑇𝑇 )

Where –
St20 : sugar content corrected at 20 °C
Sa : sugar content measured
Ta : temperature of sugar solution at the time
of measurement

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