‫م ق م ‪٢٠١٤ / ٢٣ -٧٧٨٩‬‬

‫‪EN 13130-23/2005‬‬

‫ﺍﳋﺎﻣﺎﺕ ﻭﺍﻷﺩﻭﺍﺕ ﺍﳌﻼﻣﺴﺔ ﻟﻠﻐﺬﺍء – ﻣﻮﺍﺩ ﺍﻟﺒﻼﺳﺘﻴﻚ ﺍﳌﻘﺪﺭﺓ‬

‫ﺍﳉﺰء ﺍﻟﺜﺎﻟﺚ ﻭﺍﻟﻌﺸﺮﻭﻥ ‪ :‬ﺗﻘﺪﻳﺮ ﺍﻟﻔﻮﺭﻣﺎﻟﺪﻫﻴﺪ ﻭﻫﻜﺴﺎ ﻣﻴﺜﻴﻞ‬

‫ﺗﱰﺍﻣﲔ ﻓﻰ ﻣﺸﺎﺑﻬﺎﺕ ﺍﻻﻏﺬﻳﺔ‬

‫جمھورية مصر العربية‬

‫الھيئة المصرية العامة للمواصفات والجودة‬

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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‫‪EN 13130-23:2005‬‬

‫تاريخ االعتماد ‪٢٠١٤ / ٩ / ٣٠ :‬‬

‫كل الحقوق محفوظة للھيئة‪ ،‬ما لم يحدد خالف ذلك‪ ،‬وال يجوز إعادة إصدار أى جزء من المواص فة أو االنتف اع ب ه‬

‫فى أى شكل وبأى وس يلة إليكتروني ة أو ميكانيكي ة أو خالفھ ا ويت ضمن ذل ك الت صوير الفوت وغرافى والميك روفيلم‬

‫بدون تصريح كتابى مسبق من الھيئة أو الناشر‪.‬‬

‫‪ -١‬الھيئة المصرية العامة للمواصفات والجودة‬

‫العنوان ‪ ١٦ :‬ش تدريب المتدربين – السواح – األميرية‪.‬‬

‫تليفون ‪٢٢٨٤٥٥٢٤ –٢ ٢٨٤٥٥٢٢ :‬‬

‫فاكس ‪٢٢٨٤٥٥٠٤ :‬‬

‫‪eos@idsc.net.eg‬‬ ‫بريد الكترونى ‪:‬‬

‫‪www.eos.org.eg‬‬ ‫موقع الكترونى ‪:‬‬

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫‪2/16‬اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ‬
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‫‪EN 13130-23:2005‬‬

‫م‪ .‬ق‪.‬م ‪٢٠١٤ /٢٣-٧٧٨٩ :‬‬

‫‪EN 13130-23/2005‬‬

‫ﻣﻘـﺪﻣـــﺔ‬

‫اﻟﺧﺎﺻﺔ ﺑـ "اﻟﺧﺎﻣﺎت واﻷدوات اﻟﻣﻼﻣﺳﺔ ﻟﻠﻐذاء – ﻣواد‬ ‫م‪.‬ق‪.‬م ‪٢٠١٤ / ٢٣-٧٧٨٩‬‬

‫اﻟﺑﻼﺳﺗﻳك اﻟﻣﻘدرة – اﻟﺟزء اﻟﺛﺎﻟث واﻟﻌﺷرون‪ :‬ﺗﻘدﻳر اﻟﻔورﻣﺎﻟدﻫﻳد وﻫﻛﺳﺎ ﻣﻳﺛﻳﻝ ﺗﺗراﻣﻳن ﻓﻰ‬
‫ﻣﺷﺎﺑﻬﺎت اﻻﻏذﻳﺔ " ﺗﺗﺑﻧﻲ اﻟﻣﺣﺗوي اﻟﻔﻧﻲ ﻟﻠﻣواﺻﻔﺔ اﻷوروﺑﻳﺔ رﻗم ‪٢٠٠٥/٢٣-١٣١٣٠‬‬

‫ﻗﺎم ﺑﺄﻋداد ﻫذﻩ اﻟﻣواﺻﻔﺔ ﻟﺟﻧﺔ اﻟﺗواﻓق رﻗم ‪ ١٧/٣‬اﻟﺧﺎﺻﺔ ﺑﺎﻟﻌﺑوات واﻟﺑﻳﺎﻧﺎت ‪.‬‬

‫‪ 3/16‬ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬
‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ‬
‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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EN 13130-23:2005

1 Scope
This document, part of EN 13130, specifies an analytical procedure for the chemical conversion of HMTA to
formaldehyde and the determination of formaldehyde in food simulants water, 3 % w/v aqueous acetic acid,
15 % v/v aqueous ethanol and rectified olive oil.

The method is appropriate for the quantitative determination of formaldehyde in approximate analyte
concentration range of 3,0 mg to 30 mg formaldehyde per kilogram of food simulant, which corresponds to
2,3 mg to 23,3 mg hexamethylenetetramine per kilogram of food simulant.

NOTE The method should also be applicable to other aqueous food simulants as well as to other fatty food simulants
e.g. sunflower oil, corn oil or a mixture of synthetic triglycerides.

2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.

EN 13130-1:2004, Materials and articles in contact with foodstuffs – Plastics substances subject to limitation –
Part 1: Guide to test methods for the specific migration of substances from plastics to foods and food
simulants and the determination of substances in plastics and the selection of conditions of exposure to food
simulants.

3 Principle

HMTA is treated with acid and heated to release formaldehyde.

Formaldehyde in food simulant is determined by spectrophotometry. Formaldehyde reacts with chromotropic

acid in the presence of sulfuric acid. This solution is measured in a spectrophotometer at the wavelength of
574 nm, with cells of an optical path length of 10 mm. Quantification is achieved using an external standard.

Confirmation of formaldehyde is carried out by spectrophotometer. Formaldehyde reacts with

pentane-2,4-dione in the presence of ammonium acetate to form 3,5-diacetyl-1,4-dihydrolutidine. The
absorption of this extract is measured at 410 nm, with a spectrophotometer with cells of an optical path length
of 10 mm.

NOTE The confirmation procedure is also a quantitative method and can therefore be used as the method of
determination. In that case the method with chromotropic acid should be used as the confirmation procedure.

4 Reagents
NOTE All reagents should be of recognized analytical quality unless otherwise stated.

4.1 Analyte

Formaldehyde solution, CH2O, minimum 37 % (w/v), stabilized with approximately 10 % methanol.

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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4.2 Chemicals

4.2.1 Water, deionised.

4.2.2 Acetic acid, glacial 100 %.

4.2.3 Ethanol, absolute.

4.2.4 Olive oil, rectified (according to Directive 93/8/EEC)

4.2.5 Chromotropic acid disodium salt (dihydrate), 4,5-dihydroxy-2,7-naphthalene-disulfonic acid,

C10H6Na2O8S2.2H2O.

3
4.2.6 Sulfuric acid, density 1,84 g/cm .

4.2.7 Acetone

4.2.8 Starch, soluble

4.2.9 n-pentane

4.3 Solutions

4.3.1 90 % Acetone

Measure 900 ml of acetone (4.2.7) and make up with water (4.2.1) to 1 000 ml.

4.3.2 Stock solution of formaldehyde in water containing approximately 1,5 mg formaldehyde per
millilitre

Weigh to the nearest 1 mg approximately 0,8 g formaldehyde solution (4.1.1) into a 200 ml volumetric flask
and make up to the mark with water (4.2.1).

Determine the strength of this solution as follows.

Pipette 10,0 ml formaldehyde stock solution into a beaker, add 25,0 ml of a 0,05 mol standard iodine solution
(4.3.5) and 10,0 ml of 1 mol sodium hydroxide solution (4.3.6) to the beaker. Allow to stand for 5 min. Acidify
with 11,0 ml of 1 mol hydrochloric acid (4.3.7) and determine the excess iodine by titration with a 0,1 mol
standard sodium thiosulfate solution (4.3.8) using 0,1 ml of the starch solution (4.3.12) as indicator.

Make a blank test on the corresponding amount of standard iodine solution.

1 ml of 0,1 N iodine consumed is equivalent to 1,5 mg formaldehyde.

Calculate the concentration in mg formaldehyde per millilitre of solution.

Repeat the procedure to obtain a second stock solution.

Store the formaldehyde stock solution for up to 3 months in a refrigerator.

4.3.3 Stock solution of formaldehyde in 90 % acetone containing approximately 1 mg formaldehyde

per millilitre

Weigh to the nearest 1 mg approximately 0,3 g formaldehyde solution (4.1.1) into a 100 ml volumetric flask
and make up to the mark with 90 % acetone (4.3.1).

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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Calculate the concentration of formaldehyde in the 90 % acetone solution using the concentration of the 37 %
formaldehyde solution (4.1.1) derived from the result obtained in 4.3.2.

Repeat the procedure to obtain a second stock solution.

Store the solutions in well-closed containers in the dark for a maximum period of 3 months in a refrigerator.

4.3.4 Diluted standard solutions of formaldehyde in aqueous food simulants

Pipette into a series of five 100 ml volumetric flasks, 100 µl, 400 µl, 700 µl, 1 000 µl and 2 000 µl of the stock
solution (4.3.2). Make up to the mark with the appropriate food simulant. The standard solutions thus obtained
contain approximately 1,5 mg/l, 6,0 mg/l, 10,5 mg/l, 15 mg/l and 30 mg formaldehyde per litre.

Calculate the exact concentration in milligrams of formaldehyde per litre of solution corresponding to mg/kg
food simulant.

Repeat the procedure using the second standard stock solution to obtain a second set of diluted standard
solutions.

Store the solutions in well closed contained for a maximum period of 3 months in a refrigerator.

4.3.5 Iodine in aqueous solution, 0,05 M.

4.3.6 Sodium hydroxide in aqueous solution, NaOH, 1 M.

4.3.7 Hydrochloric acid in aqueous solution, HCl, 1 M.

4.3.8 Sodium thiosulfate in aqueous solution, Na2S5O3.5H2O, 0,1 M.

4.3.9 0,5 % chromotropic acid disodium salt (dihydrate)

Weigh 500 mg of chromotropic acid disodium salt (4.2.5) into a 100 ml volumetric flask and make to the mark
up with water (4.2.1). This solution shall be prepared freshly on the day of use.

4.3.10 Sulfuric acid solution

Measure 100 ml water (4.2.1) and make up with sulfuric acid (4.2.6) to 400 ml.

4.3.11 Sulfuric acid solution (4M)

Add carefully 222 ml sulfuric acid (4.2.6) to a flask containing approximately 700 ml of water. After cooling to
room temperature, make up to 1 000 ml with water (4.2.1).

4.3.12 Starch solution

Dissolve 1 g soluble starch (4.2.8) in 50 ml water (4.2.1). This solution shall be freshly prepared, in
accordance with the European Pharmacopoeia.

5 Apparatus
NOTE An instrument or item of apparatus is listed only where it is special or made to a particular specification, usual
laboratory glassware and equipment being assumed to be available.

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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5.1 Spectrophotometer, preferably with a double beam.

5.2 Water bath

5.3 Microsyringe, 0 ml to 1,0 ml.

5.4 Glass tubes, stoppered.

6 Samples

6.1 Preparation of test samples

6.1.1 General

Laboratory samples of the food simulant to be analyzed shall be obtained as described in EN 13130-1.
Analyte-free samples of the food simulants of the same type as those to be analyzed shall also be prepared
for use for calibration purposes.

6.1.2 Aqueous food simulants

6.1.2.1 For the determination of HMTA

Take 25 ml of the aqueous food simulant into a 50 ml volumetric flask and make up to the mark with the
diluted sulfuric acid (4.3.11). Immerse the flask in a water bath at 90 °C for 30 min. Shake while cooling.

Transfer 1,0 ml of this solution into a 12 ml glass stoppered tube (5.4). Treat the sample as described in 7.2.

6.1.2.2 For the determination of formaldehyde

Transfer 1,0 ml of food simulant obtained from the migration experiment into a 12 ml glass stoppered tube.
Treat the sample as described in 7.2.

6.1.3 Olive oil

6.1.3.1 For the determination of HMTA

Transfer 20,0 g ± 0,2 g of olive oil, obtained from the migration experiment, into a 250 ml separating funnel.
Add 40 ml of n-pentane and shake the mixture vigorously 4 times with 20 ml water (4.2.1), using fresh portions
of water on each occasion. Allow the phases to separate and run off the lower aqueous layer through a paper
filter into a 100 ml volumetric flask. Fill to the mark with water, and mix thoroughly. Pipette 25 ml of this
aqueous solution into a 50 ml volumetric flask and make up to the mark with the diluted sulfuric acid (4.3.11).
Immerse the flask in a water bath at 90 °C for 30 min. Shake while cooling.

Transfer 1,0 ml of this solution into a 12 ml glass stoppered tube. Treat the sample as described in 7.2.

NOTE Separation of the aqueous and organic layer may influence the final extraction efficiency. Therefore it is
important that phases are well separated before drawing off.

6.1.3.2 For the determination of formaldehyde

Transfer 20,0 g ± 0,2 g of olive oil (4.2.9), obtained from the migration experiment, into a 250 ml separating
funnel. Add 40 ml of n-pentane and shake the mixture vigorously 4 times with 20 ml water. Using fresh
portions of water on each occasion. Allow the phases to separate and run off the lower aqueous layer through
a paper filter into a 100 ml flask. Fill to the mark with water, and mix thoroughly.

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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Transfer 1,0 ml of this aqueous solution into a 12 ml glass stoppered tube. Treat the sample as described in
7.2.

NOTE Separation of the aqueous and organic layer may influence the final extraction efficiency. Therefore it is
important that phases are well separated before drawing off.

6.2 Preparation of blank samples

Treat simulants which have not been in contact with packaging material in the same way as described in 6.1.

6.3 Preparation of calibration samples

6.3.1 Calibration curves in aqueous food simulants

Transfer 1,0 ml of each of the diluted standard solutions (4.3.4) into a 12 ml glass stoppered tube and treat the
calibration samples as described in 7.2.

6.3.2 Calibration curve in olive oil

Weigh 20 g ± 0,2 g olive oil into a series of six separating funnel. Add 0 µl, 30 µl, 100 µl, 200 µl, 300 µl and
600 µl of the formaldehyde stock solution in 90 % acetone (4.3.3) and mix. The solutions thus obtained
contain approximately 0 mg/kg, 1,5 mg/kg, 5,0 mg/kg, 10,0 mg/kg, 15,0 mg/kg and 30.0 mg formaldehyde per
kilogram of olive oil respectively. Add 40 ml of n-pentane. Shake the mixture vigorously 4 times with 20 ml
water. Using fresh portions of water on each occasion. Allow the phases to separate and run off the lower
aqueous layer through a filter into a 100 ml flask. Fill to the mark with water and mix thoroughly.

Transfer 1,0 ml of this aqueous solution into a 12 ml glass stoppered tube. Treat the sample as described in
7.2.

7 Procedure

7.1 Spectrophotometric analysis

The test samples, blanks and calibration samples prepared in 6.1 to 6.3 are submitted to a reaction procedure
with chromotropic acid. The absorption of reaction product is measured over the range of 650 nm to 450 nm.
The absorption at 574 nm is used for quantitative calculations.

Each solution shall be analyzed at least in duplicate.

7.2 Sample treatment

Add to each of the vials prepared under 6.1 to 6.3, 1 ml chromotropic acid solution (4.3.9) and 8 ml sulfuric
acid 75 % (4.3.10). Place the vials in a water bath at 60 °C for 20 min. Remove the vials from the water bath
and allow the vials to cool for one hour at room temperature.

Record the absorption curve of the solution obtained from 650 nm to 450 nm using cells with an optical path
length of 10 mm and a reagent blank solution or zero level of the calibration curve as a reference.

7.3 Calibration

Measure the absorption of the formaldehyde/chromotropic acid complex at 574 nm of the standard solutions.
Plot the absorption against the concentration of formaldehyde in the calibration samples in milligrams per
kilogram.

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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NOTE Commission Directive 2002/72/EC [1] states that the specific gravity of all simulants should conventionally be
assumed to be ‘1’. Milligrams of substance released per litre of simulant will thus correspond numerically to milligrams of
substance released per kilogram of simulant and, taking into account of the provisions laid down in Directive 82/711//EEC
[3], to milligrams of substance released per kilogram of foodstuff.

The calibration curves shall be rectilinear and the correlation coefficient shall be 0,996 or better.

The two sets of calibrant solutions made from independently prepared stock solutions shall be cross-checked
by generating two calibration curves which on the basis of absorption measurement should agree to ± 5 % of
one another.

7.4 Evaluation of data

NOTE The following calculations assume that for all measurements exactly the same mass or volume of food
simulant has been used.

7.4.1 Spectroscopic interferences

Possible interferences due to background colour in the sample are eliminated by the use of a reference
solution.

7.4.2 Calculation of analyte level

7.4.2.1 Graphical determination

Measure the absorbance at 574 nm and calculate the average of the absorption values obtained from the test
samples according to 7.2. Read the formaldehyde concentration of the test samples from the calibration graph
(7.3).

7.4.2.2 Calculation from the regression parameters

If the regression line equation is:

y = (a × x ) + b

where

y is the absorbance of formaldehyde/chromotropic acid complex;

a is the slope of the regression line;

x is the concentration of formaldehyde in the food simulant in milligrams per kilogram;

b is the intercept of the regression line,

then the concentration of formaldehyde of food stimulant is given by:

y −b
C For,fs =
a

where

CFor,fs is the concentration of formaldehyde of food simulant in milligrams per kilogram.

Both procedures yield directly the formaldehyde concentration in the food simulant in milligrams of
formaldehyde per kilogram of food simulant.

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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The method applying calculation from the regression parameters is the preferred method.

7.4.3 Calculation of the specific formaldehyde migration

Depending on the fill volume of the test material and on the surface area/food simulant, the formaldehyde
concentration in the test sample as determined according to 7.4.2 may need mathematical transformation to
calculate the specific migration value to be compared with the specific migration limit (SML). For guidance
see EN 13130-1:2004, Clause 13.

8 Precision

8.1 Validation

8.1.1 Determination of HMTA

This method was pre-evaluated by a collaborative trial with three laboratories. In each laboratory a
within-laboratory precision experiment using the four official EU food simulants for establishment of precision
data at the restriction criterion was carried out. Also within-laboratory migration tests were carried out with a
polymer sample, manufactured using hexamethylenetetramine as a monomer, being in contact for 10 d at
40 °C with 15 % v/v aqueous ethanol and olive oil, respectively.

8.1.2 Determination of formaldehyde

This method was pre-evaluated in 1993 by collaborative trial with two laboratories. In each laboratory a
within-laboratory precision experiment using the four official EU food simulants for establishment of precision
data at the restriction criterion was carried out as well as migration testing with formaldehyde containing
samples in contact for 10 d at 40 °C, with 15 % v/v aqueous ethanol and olive oil, respectively.

8.2 Repeatability

8.2.1 Determination of HMTA

Evaluation of the within-laboratory precision experiment results according to ISO 5725, at a concentration of
11,7 mg HMTA per kilogram of food simulant, (corresponding to 15 milligrams of formaldehyde per kilogram
for the 95 % probability level yielded the following performance characteristics (lab 1/lab 2/lab 3):

Repeatability: r = 0,2/0,8/1,0 mg formaldehyde per kilogram in water;

r = 0,8/0,7/1,9 mg formaldehyde per kilogram in 3% w/v aqueous acetic acid;

r = 0,6/0,6/2,6 mg formaldehyde per kilogram in 15% v/v aqueous ethanol;

r = 0,4/1,1/4,2 mg formaldehyde per kilogram in olive oil.

8.2.2 Determination of formaldehyde

Evaluation of the within-laboratory precision experiment results according to ISO 5725, at a concentration of
15 mg formaldehyde per kilogram of food simulant yielded the following performance characteristics at the
95 % probability level(lab 1/lab 2):

Repeatability: r = 0,5/0,2 mg formaldehyde per kilogram in water;

r = 0,3/0,2 mg formaldehyde per kilogram 3 % w/v aqueous acetic acid;

r = 0,4/0,1 mg formaldehyde per kilogram in 15 % v/v aqueous ethanol;

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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r = 0,5/0,5 mg formaldehyde per kilogram in olive oil.

8.3 Detection limit

8.3.1 Determination of HMTA

The within-laboratory detection limits (WDL), based on the calibration curve method according to DIN 32645,
were found to be in the range of 0,8 mg/kg to 3,0 mg/kg food simulant, depending on the type of food simulant.
Thus the method is capable of quantitative detection of HMTA, as formaldehyde at a minimum level of 3,0 mg
per kilogram food simulant.

8.3.2 Determination of formaldehyde

The within-laboratory detection limits (WDL), based on the calibration curve method according to DIN 32645,
were found to be in the range of 0,5 mg/kg to 3,0 mg/kg food simulant, depending on the type of food simulant.
Thus the method is capable of quantitative detection of formaldehyde at a minimum level of 3,0 mg/kg food
simulant.

9 Confirmation

9.1 Requirement for confirmation

If the specific migration of HMTA, expressed as formaldehyde, or formaldehyde, calculated in accordance with
7.4.3 exceeds the restriction, e.g. a specific migration of 15 mg/kg, the result of the determination shall be
confirmed. The confirmation procedure is quantitative. In collaborative trials with three laboratories
comparable results using the chromotropic acid method and the acetyl acetone method were found for the
detection limits, repeatability, recovery and migration of formaldehyde. Therefore the method of determination
and the confirmation procedure are interchangeable.

9.2 Principle

Formaldehyde is reacted with pentane-2,4-dione in the presence of ammonium acetate to form

3,5-diacetyl-1,4-dihydrolutidine. The absorbance of this complex is measured at 410 nm with a
spectrophotometer.

9.3 Reagents

NOTE Only additional chemicals required for the confirmation procedure are listed.

9.3.1 Chemicals

9.3.1.1 Ammonium acetate, anhydrous.

9.3.1.2 Pentane-2,4-dione (acetyl acetone), C5H8O2, distilled.

9.3.2 Solutions

9.3.2.1 Pentane-2,4-dione reagent

This reagent shall be freshly prepared on the day of use, as follows.

Dissolve 15 g ammonium acetate (9.3.1.1) in a 100 ml volumetric flask containing approximately 75 ml of

water. Add 0,2 ml pentane-2,4-dione (9.3.1.2) and 0,3 ml acetic acid (4.2.2).

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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Make up to 100 ml with water (4.2.1) (pH of solution approximately 6,4).

9.3.2.2 Reagent without pentane-2,4-dione

Prepare the reagent solution as described in 9.3.2.1 while omitting the addition of pentane-2,4-dione.

9.4 Preparation of test samples

9.4.1 Sample preparation

9.4.1.1 Determination of HMTA

Transfer into a 50 ml flask 10,0 ml of aqueous solution, obtained according to 6.1.1.1 and 6.1.2.1, 5 ml of
sodium hydroxide solution (4.3.6) and 15 ml of water. Check the pH of the solution, and if necessary adjust to
pH 4 to pH 6 using a few drops of sodium hydroxide solution (4.3.6) or sulfuric acid solution (4.3.11), as
appropriate. Add 5 ml of pentane-2,4-dione reagent (9.3.2.1) and continue as described in 9.5.

9.4.1.2 Determination of formaldehyde

Transfer into a 50 ml flask 5,0 ml of aqueous food simulant, obtained according to 6.1.1.2, add 20,0 ml water
or, in the case of fatty food simulants, 25,0 ml of extract obtained according to 6.1.2.2. Add 5,0 ml of
pentane-2,4-dione reagent (9.3.2.1).

9.4.2 Preparation of blank samples

Treat simulants that have not been in contact with packaging material, obtained according to 6.2, in the same
way as described in 9.4.1.

9.4.3 Preparation of calibration samples

Transfer into a 50 ml flask 5,0 ml of diluted standard solutions (4.3.4) and 20 ml water or 25 ml of the extracts
obtained in 6.3.2 and add 5,0 ml of pentane-2,4-dione reagent.

9.4.4 Reference solution

Transfer into a 50 ml flask 5,0 ml aqueous food simulant (6.2), 20 ml water and 5,0 ml of the reagent without
pentane-2,4-dione (9.3.2.2). In the case of olive oil, transfer into a 50 ml flask 25,0 ml of oil extract (6.2) and
5,0 ml of the reagent without pentane-2,4-dione (9.3.2.2).

NOTE Possible interferences due to background colour in the test sample are eliminated by the use of this reference
solution.

9.5 Sample treatment

Shake the mixtures prepared in 9.4. Immerse the flasks in a water bath at 60 °C for exactly 10 min. Allow to
cool for 2 min in a bath of iced water. Within 25 min from the moment when the flasks are placed in the water-
bath measure the absorbance at 410 nm of the sample solution with the reference solution in the reference
cell.

9.6 Evaluation of data

Evaluate the data following the procedure described in 7.3 and 7.4.

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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10 Test report
The test report shall include at least the following, where applicable:

a) identification of the sample;

b) name of the laboratory;

c) name of responsible analyst;

d) date of report;

e) date of analysis;

f) analyte;

g) a reference to this method;

h) performance characteristics of the method;

i) sample details, such as:

1) type of food/food simulant/material/article;

2) origin and denotation of the sample;

3) date and method of obtaining the laboratory sample;

4) storage conditions;

j) results expressed in milligrams of formaldehyde or hexamethylenetetramine per kilogram of food simulant.

Results shall be reported as the average value from two or more determinations satisfying the
repeatability criterion of 8.2;

k) details of confirmation procedure, if any;

l) reasons for modifications introduced into the test method, if any.

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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Bibliography

[1] Commission of the European Communities, Commission Directive 2002/72/EC of 6 August 2002 relating to
plastics materials and articles intended to come into contact with foodstuffs, Official Journal of the European
Communities, 15 August 2002, no. L220, p18.

[2] Commission of the European Communities, Council Directive of 21 December 1988 on the approximation
of the laws of the Member States relating to materials and articles intended to come into contact with foodstuff
(89/109/EEC), Official Journal of the European Communities, 11 February 1989, no. L 40, p 38.

[3] Commission of the European Communities, Council Directive of 18 October 1982 laying down the basic
rules necessary for testing migration of the constituents of plastics materials and articles intended to come into
contact with foodstuffs (82/711/EEC), Official Journal of the European Communities, 23 October 1982, no. L
297, p 26.

[4] Commission of the European Communities, Commission Directive of 15 March 1993 amending Council
Directive 82/711/EEC laying down the basic rules necessary for testing migration of the constituents of
plastics materials and articles intended to come into contact with foodstuffs (93/8/EEC), Official Journal of the
European Communities, 14 April 1993, no. L 90, p 22.

[5] Commission of the European Communities, Commission Directive of 97/48/EC of 29 July 1997 amending
Council Directive 82/711/EEC laying down the basic rules necessary for testing migration of the constituents
of plastics materials and articles intended to come into contact with foodstuffs, Official Journal of the European
Communities, 12 August 1997, no. L 222, p 10.

[6] Commission of the European Communities, Council Directive of 19 December 1985 laying down the list of
simulants to be used for testing migration of constituents of plastics materials and articles intended to come
into contact with foodstuffs (85/572/EEC), Official Journal of the European Communities, 31 December 1985,
no. L372, p14.

[7] ISO 5725, Accuracy (trueness and precision) of measurement methods and result.

[8] DIN 32645, Chemical analysis; decision limit; detection limit and determination limit; estimation in case of
repeatability; terms, methods, evaluation.
th
[9] European Pharmacopia. 4 edition, published 2001, Strasbourg, Council of Europe.

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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‫‪ ‬الھيئة المصرية العامة للمواصفات والجودة‪‬‬

‫‪ -١‬أنشئت الھيئة المصرية العامة للتوحيد القياسى عام ‪ ١٩٥٧‬بالقرار الجمھورى رقم ‪ ٢٩‬لسنة ‪١٩٥٧‬‬
‫الذى نص على اعتبارھا المرجع القومى المعتمد للشئون التوحيد القياسى ونص القانون رقم ‪ ٢‬لسنة‬
‫‪ ١٩٥٧‬على أن المواصفة ال تعتبر قياسية إال بعد اعتمادھا من الھيئة‪.‬‬
‫‪ -٢‬فى عام ‪ ١٩٧٩‬صدر القرار الجمھورى رقم ‪ ٣٩٢‬لسنة ‪ ١٩٧٩‬الذى قرر ضم مركز ضبط الجودة‬
‫إلى الھيئة‪.‬‬
‫‪ -٣‬فى عام ‪ ٢٠٠٥‬صدر القرار الجمھورى رقم ‪ ٨٣‬لسنة ‪ ٢٠٠٥‬بإعادة تسمية الھيئة لتصبح الھيئة‬
‫المصرية العامة للمواصفات والجودة ‪ ،‬وبناء عليه فإن الھيئة تختص بما يلى ‪:‬‬
‫‪ -‬إعداد وإصدار المواصفات القياسية للخامات والمنتجات والخامات واألجھزة ونظم اإلدارة والتوثيق‬
‫والمعلومات ومتطلبات األمن والسالمة وفترات الصالحية وأجھزة القياس‪.‬‬
‫‪ -‬التفتيش الفنى واالختبار والرقابة وسحب العينات وإصدار شھادات المطابقة للمواصفات المعتمدة‬
‫وشھادات المعايرة ألجھزة القياس‪.‬‬
‫‪ -‬الترخيص بمنح عالمة الجودة للمنتجات الصناعية وعالمات وشھادات الجودة والمطابقة المنتجات‬
‫للمواصفات القياسية‪.‬‬
‫‪ -‬تقديم المشورة الفنية وخدمات التدريب فى مجاالت المواصفات والجودة القياس والمعايرة‬
‫واالختبار والمعلومات لجميع األطراف المعنية‪.‬‬
‫‪ -‬تمثيل مصر فى أنشطة المنظمات الدولية واإلقليمية العامة فى مجاالت المواصفات والجودة واالختبار‬
‫والمعايرة‪.‬‬
‫‪ -‬تقوم الھيئة بتنفيذ متطلبات واشتراطات اتفاقية العوائق الفنية على التجارة لمنظمة التجارة العالمية حيث أن‬
‫الھيئة ھى نقطة االستعالم المصرية لإلمداد بالمعلومات والوثائق فى مجال المواصفات وتقييم المطابقة‪.‬‬
‫‪ -٤‬يدير الھيئة مجلس إدارة برئاسة وكيل أول الوزارة رئيس الھيئة‪ ،‬ويضم المجلس فى عضوية‬
‫ممثلين عن مختلف الجھات المعنية للتوحيد القياسى وجودة اإلنتاج واالختبار والمعايرة فى مصر‬
‫باإلضافة إلى عدد من األكاديميين والعلميين والخبراء والقانونيين ورجال اإلعالم‪.‬‬
‫‪ -٥‬يتم إعداد المواصفات القياسية من خالل لجان فنية يربو عددھا على مائة لجنة يشارك فيھا خبراء‬
‫طبقا ً للمعايير الدولية ومتخصصون من جميع الجھات المعنية ويقوم باألمانة الفنية لھا أعضاء من‬
‫العاملين بالھيئة‪.‬‬
‫‪ -٦‬يتم توزيع مشاريع المواصفات على قاعدة عريضة من الجھات المعنية والبالد العربية إلبداء‬
‫المالحظات خالل فترة ستين يوما ً كما تعرض ھذه المشاريع على لجنة الصياغة ولجان عامة للمراجعة‬
‫قبل العرض على مجلس اإلدارة‪.‬‬
‫‪ -٧‬تتبع الھيئة نظام الترخيص للمصانع باستخدام عالمات الجودة على السلع والمنتجات المطابقة‬
‫للمواصفات المصرية وذلك حماية المستھلكين وخدمة للصانعين لرفع جودة منتجاتھم‪ .‬ويوجد بالھيئة‬
‫مجموعة كبيرة من المعامل الحديثة الختبار المنتجات الكيمائية ومواد البناء والتشييد والمنتجات‬
‫الھندسية والغذائية ومنتجات الغزل والنسيج باإلضافة إلى معامل للقياس والمعايرة الميكانيكية‬
‫والكھربائية والفيزيائية‪.‬‬
‫‪ -٨‬يتوفر بالھيئة وحدة لحماية المستھلك لتتلقى شكواھم وتعمل على حلھا وقد القت أعمال الوحدة نجاحا ً‬
‫كبيراً‪.‬‬
‫‪ -٩‬يتوفر بالھيئة المكتبة الوحيدة فى مصر المتخصصة فى المواصفات القياسية تحتوى على‬
‫أكثر من ‪ ١٣٠‬ألف مواصفة دولية وأجنبية وإقليمية وعربية ومصرية‪.‬‬

‫‪ 15/16‬ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬
‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ‬
‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
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 ES:7789-23/2014
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MATERIALS AND ARTICLES IN CONTACT WITH

FOODSTUFFS – PLASTICS SUBSTANCES SUBJECT
TO LIMITATION – PART 23: DETERMINATION OF
FORMALYELEHYDE AND
HEXAMETHYLENETETRAMINE IN FOOD
SIMULANTS

ICS : 67.250

Arab Republic of Egypt

Egyptian Organization for Standardization and Quality

‫اھداء ﻣن اﻟﮭﯾﺋﺔ اﻟﻣﺻرﯾﺔ اﻟﻌﺎﻣﺔ ﻟﻠﻣواﺻﻔﺎت واﻟﺟودة‬

‫اﻟﻰ اﻟﻣﻧظﻣﺔ اﻟﻌرﺑﯾﺔ ﻟﻠﺗﻧﻣﯾﺔ اﻟﺻﻧﺎﻋﯾﺔ واﻟﺗﻌدﯾن‬
13-5-2015