Decree No. 494 / 2005 Coll.
Decree laying down analytical methods for the control of the composition of cosmetic products
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Effective from 01.01.2006
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01.01.2006
23.12.2005
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494
DECLARATION
of 7 December 2005
laying down analytical methods for checking the composition of cosmetic products
According to § 108 (1) of Act No. 258 / 2000 Coll., on the Protection of Public Health and on the amendment of certain related laws, as amended by Act No. 392 / 2005 Coll., ("the Act '), the Ministry of Health provides for the implementation of § 80 (2) of the Act:
(1) This decree (1) implements the relevant provisions of the European Community2) and regulates the following analytical methods for checking the composition of cosmetic products:
(a) sampling of cosmetic products;
(b) preparation of samples in the laboratory;
(c) the qualitative and quantitative determination of free sodium and potassium hydroxide;
(d) quantitative and qualitative determination of oxalic acid and its alkali salts in hair care products;
(e) quantitative determination of chloroform in toothpaste,
(f) quantitative determination of zinc,
(g) qualitative and quantitative determination of 4-hydroxybenzenesulfonic acid,
(h) qualitative determination of oxidising agents and quantitative determination of hydrogen peroxide in hair-care products;
(i) the qualitative and semi-quantitative determination of certain oxidative dyes in hair colours;
(j) the qualitative and quantitative determination of nitrites;
(k) quantitative determination of resorcinol in shampoos and hair lotions,
(l) quantitative determination of methanol with respect to ethanol or propan-2-ol,
(m) qualitative and quantitative determination of free formaldehyde,
(n) the quantitative determination of dichloromethane and 1,1,1-trichloroethane,
(o) the qualitative and quantitative determination of quinoline-8-ol and bis (quinoline-8-ol) sulphate,
(p) quantitative determination of ammonia,
(q) the qualitative and quantitative determination of nitromethane,
(r) qualitative and quantitative determination of thioglycollic acid (sulphanylacetic acid) in permanent ondulation, hair straightening and waxing products;
(s) the qualitative and quantitative determination of hexachlorophene (INN);
(t) the quantitative determination of sodium tosylchloramide (chloramine-T) (INN),
(u) quantitative determination of total fluorine in toothpaste;
(v) quantitative determination of organic mercury compounds;
(w) quantitative determination of alkali sulphides and alkali earth metals sulphides;
(x) qualitative and quantitative determination of 2,3-dihydroxypropyl-4-aminobenzoate,
(y) quantitative determination of chlorobutanol,
(z) qualitative and quantitative determination of quinine,
(aa) qualitative and quantitative determination of inorganic sulphites and hydrogen sulphites;
(bb) qualitative and quantitative determination of chlorates of alkali metals;
(cc) the qualitative and quantitative determination of sodium iodide,
(dd) the qualitative and quantitative determination of silver nitrate in cosmetic products;
(ee) qualitative and quantitative determination of the content of selenium sulphide in dandruff shampoos;
(ff) quantitative determination of soluble barium and strontium in pigments in the form of salts or complexes,
(gg) the qualitative and quantitative determination of benzyl alcohol,
(hh) qualitative determination of zirconium and quantitative determination of zirconium, aluminium and chlorine in non-aerosol antiperspirants;
(ii) the qualitative and quantitative determination of hexamidine, dibromohexamidine, dibromopropamidine and chlorhexidine,
(j) the qualitative and quantitative determination of benzoic acid, 4-hydroxybenzoic acid, sorbic acid, salicylic acid and propionic acid in cosmetic products;
(kk) the qualitative and quantitative determination of hydroquinone, hydroquinone monomethyl ether, hydroquinone monoethyl ether and hydroquinone monobenzylether in cosmetic products,
(ll) the qualitative and quantitative determination of 2-phenoxyethanol, 1-phenoxypropane-2-ol, methyl, ethyl, propyl, butyl and benzyl-4-hydroxybenzoate in cosmetic products.
(2) The content of the analytical methods for checking the composition of cosmetic products listed in paragraph 1 is set out in the Annex hereto.
This Decree shall take effect on 1 January 2006.
Minister:
MUDr. Rath v. r.
Annex to Decree No 494 / 2005 Coll.
1. SAMPLING OF COSMETIC INSTALLATIONS
1. SCOPE AND SCOPE OF USE
The sampling procedure for cosmetic products shall be described taking into account their analysis in different laboratories.
2. DEFINITIONS
2.1. Basic sample:
unit quantity withdrawn from the lot offered for sale.
2.2. Total sample:
the sum of all basic samples taken from a lot of the same number.
2.3 Laboratory sample:
a representative part of the total sample to be analysed in each laboratory.
2.4. Test sample:
a representative part of the laboratory sample necessary for analysis.
2.5 Packaging:
an article containing a product which is in constant direct contact with the product.
3. SAMPLING PROCEDURE
3.1 Cosmetic products must be collected in the original packaging and delivered to the laboratory without being opened.
3.2 As regards cosmetic products which are marketed in bulk or which are sold in non-original packaging from the manufacturer, appropriate instructions should be issued for their collection at the point of use or sale.
3.3 The number of basic samples necessary for the preparation of the laboratory sample shall be determined by the analytical method and the number of analyses to be carried out by each laboratory.
4. IDENTIFICATION OF SAMPLING
4.1 Samples shall be secured at the sampling point against opening, confusion and contamination and marked in accordance with the rules in force in the Member State concerned.
4.2 Each basic sample taken shall be marked with the following information:
- name of cosmetic product and other available identification data (manufacturer / importer, event.distributor, batch)
- the date, time and place of sampling,
- the name of the person responsible for sampling,
- the name of the inspector.
4.3 The sampling protocol shall be drawn up in accordance with the rules applicable in the Member State concerned.
5. SAMPLING
5.1. The basic samples shall be kept in accordance with any manufacturer's instructions on the label.
5.2. If no other conditions are indicated, laboratory samples shall be kept in the dark at 10 to 25 ° C.
5.3 The primary samples shall not be opened until the beginning of the analysis.
2. SAMPLING IN LABORATORY
1. GENERAL
1.1 If possible, analysis should be performed with each laboratory sample. If the baseline sample is too small, a minimum number of baseline samples should be used. They should first be thoroughly mixed before sampling the test sample.
1.2 The packaging shall be opened in an inert atmosphere, if the analytical method so requires, and the required number of test samples shall be taken as quickly as possible. An analysis should then be carried out immediately. If the sample has to be maintained, the container should be closed again in an inert atmosphere.
1.3 Cosmetic agents may be in liquid or solid form or semi-solid form. If the phases of the original homogeneous product are separated, the product should be homogenised before the test sample is taken.
1.4 Where a cosmetic product is put up for sale in a special way which makes it impossible to follow these guidelines and appropriate test methods are not provided for, a procedure may be adopted provided that it is listed in writing as part of the analytical report.
2. CAPALINES
2.1 Products such as oil, alcohol and aqueous solutions, toilet waters, lotions or milk may be present in this form and may be packed in flasks, bottles, ampoules or tubes.
2.2. Sampling:
- shake the container vigorously before opening;
- the packaging opens;
- the appropriate amount of fluid shall be transferred to the test tube for visual examination of its properties for the purpose of sampling the test sample;
- the container is closed again, or
- the required test samples are taken;
- close the container carefully.
3. POTENTIAL SUBSTANCES
3.1. Products such as pastes, creams, emulsions and gels may be present in this form and may be packed in tubes, plastic bottles or cups.
3.2. Sampling:
3.2.1 Close throat packaging: At least the first centimeter of the device is removed. The test sample shall be pushed out and the container sealed immediately.
3.2.2. Packs with wide throat: The upper layer is scraped evenly. The test sample shall be taken and the container sealed immediately.
4. THE ACTIVE SUBSTANCE (S)
4.1 In this form, products such as free powder, compact powder, sticks and can be packed in a wide range of packaging.
4.2 Sampling:
4.2.1 Free powder: Shake the container vigorously before unlocking or opening. The packaging shall be opened and a test sample taken.
4.2.2 Compact powder or sticks: The upper layer is scraped evenly. A test sample shall be taken from the lower layer.
5. EQUIPMENT FOR AEROSOLS ("aerosol dispensers")
5.1 These products are defined in Article 2 of Council Directive 75 / 324 / EEC of 20 May 1975 (see OJ L 147, 9.6.1975, p. 40).
5.2. Test sample:
After a thorough shake with a suitable clutch (see Figure 1: in specific cases, the use of another clutch may be required in the analytical method), transfer a representative amount of the aerosol dispenser content into a glass bottle coated with a plastic layer (Figure 4) and equipped with an aerosol valve but without a discharge tube. When you transfer to the bottle, the valve goes down. The content is visible when transferring. There are four options:
5.2.1 Aerosol in the form of a homogeneous solution which can be directly analysed.
5.2.2 The aerosol consists of two liquid phases. Each phase can be analysed after separation of the lower phase into the second bottle. In this case, the valve of the first bottle goes down. In this case, the lower phase is aqueous and does not contain propellant gas (e.g. butane / water).
5.2.3 Aerosol devices containing powder suspension. The liquid phase can be analysed after separation of powder.
5.2.4. Foam or cream products: 5 to 10 g of 2-methoxyethanol should be carefully weighed into the bottle first. This substance prevents foaming during degasification and thus it is possible to expel the propulsion gases without losing the liquid.
5.3. Help
The coupling (Figure 1) is made of dural or brass. It is designed to suit different valve systems by means of a polyethylene adapter. The figure gives an example; Other couplings may be used (see Figures 2 and 3).
The bottle (Figure 4) is made of white glass and is coated on the outside with a protective layer of transparent plastic. It has a volume of 50 to 100 ml. It is equipped with an aerosol valve without a discharge tube.
5.4. Procedure
In order to convert a sufficient quantity of the sample, air must be removed from the bottle. For this purpose, about 10 ml of dichlorodifluoromethane or butane (according to the aerosol medium to be examined) is introduced into the bottle and then degasified until the liquid phase has disappeared, with the valve pointing upwards. The clutch will come down. Weigh the bottle ("a 'grams). The aerosol dispenser to be sampled shall be shaken vigorously. The coupling shall be connected to the valve of the aerosol packaging to be taken (the container is facing the valve upwards) and the bottle (neck down) shall be attached to the clutch and pressed against it. The bottle is filled with about two thirds. If the transfer stops to compensate for pressures, it can be restored by cooling the bottle. Remove the coupling, weigh the filled bottle (" b' grams) and determine the weight of the transferred sample of aerosol m1 (m1 = b).
The sample thus obtained may be used:
1. to the usual chemical analysis,
2. for analysis of volatile components by gas chromatography.
5.4.1 Chemical analysis
With the bottle held upwards by the valve, proceed as follows:
- gas is expelled from the bottle; if foaming occurs, use a bottle in which a pre-weighed quantity of 2-methoxyethanol (5 to 10 g) has been placed in the syringe through the clutch;
- the volatile constituents are removed from the water bath at 40 ° C without losing the sample by shaking;
- reweigh the bottle ("c" grams) to determine the weight of the remaining m2 (m2 = c);
(Note: when calculating the weight of the residue, the weight of any 2-methoxyethanol used shall be deducted);
- the bottle opens by removing the valve;
- the remainder is quantitatively dissolved in a known quantity of suitable solvent;
- the required analysis shall be carried out with the aliquot.
Formula for calculation:
R = r × m2m1 and Q = R × P100,
where:
| m1 | = hmotnost aerosolu odebraného do lahve, |
| m2 | = hmotnost zbytku po zahřívání při 40 °C, |
| r | = obsah jednotlivé látky ve zbytku m2, vyjádřený v procentech (stanovený vhodnou metodou), |
| R | = obsah jednotlivé látky v odebraném aerosolu, vyjádřený v procentech, |
| Q | = celková hmotnost jednotlivé látky v aerosolovém rozprašovači, |
| P | = čistá hmotnost původního aerosolového rozprašovače (základní vzorek). |
5.4.2 Analysis of volatile components by gas chromatography
5.4.2.1. Principle
A sufficient quantity of the sample is taken from the bottle using a gas chromatography syringe. The contents of the syringe should be injected into the gas chromatograph.
5.4.2.2. Help
Precision gas chromatography syringe A2 to 25 μl to 50 μl (Figure 5) or equivalent syringe. This syringe is equipped with a sliding valve at the end of the needle. The syringe is connected to the bottle with the coupling on the bottle and the polyethylene tube on the syringe (length 8 mm, inside diameter 2,5 mm).
5.4.2.3. Procedure
After transferring a sufficient quantity of aerosol product into the bottle as described in paragraph 5.4.2.2, the conical end of the syringe shall be attached to the bottle. The valve shall be opened and sufficient liquid drawn. The air bubbles are removed by moving the plunger several times (the syringe is cooled as necessary). When there is sufficient liquid in the syringe without bubbles, the valve is closed and the syringe is disconnected from the bottle. Attach the needle, insert the syringe into the gas chromatograph injection device, open the valve and inject.
5.4.2.4 Internal standard
If an internal standard is required, it will be introduced into the bottle (a simple glass syringe using the clutch).
Figure 1
Coupling P1
Figure 2
M2 clutch
for conversion between the intake valve and the hug valve
Figure 3
Connector M1
for transmission between two intake valves
Figure 4
50 to 100 ml bottle
Figure 5
Gas chromatography syringe
3. QUALITATIVE AND QUANTITATIVE COMPOSITION OF THE FREE HYDROXIDE OF SODIUM AND PRESENT
1. SCOPE AND SCOPE OF USE
The method provides a procedure for identifying cosmetic products containing significant amounts of free sodium and / or potassium hydroxide and a procedure for quantitative determination of free sodium and / or potassium hydroxide in hair straightening devices and nail skin removers.
2. DEFINITIONS
The quantity of free sodium and potassium hydroxide is given by the quantity of the volumetric solution of the acid needed to neutralise the device under the prescribed conditions, the resulting quantity being expressed as free sodium hydroxide in% (m / m).
3. PRINCIP
Dissolve or disperse the sample in water and titrate with a graduated acid solution. The pH value shall be recorded in parallel with the addition of the acid; for simple solutions of sodium or potassium hydroxide, the equivalence point shall be given at the maximum rate of change of the recorded pH value.
A simple titration curve can be distorted in the presence of
(a) ammonia and other weak organic principles which themselves show a relatively flat titration curve. The ammonia is removed by evaporation at reduced pressure at room temperature in this method;
(b) salt of weak acids which may cause the titration curve to exhibit several inflex points. In such cases, neutralisation of hydroxyl ions originating from free sodium or potassium hydroxide corresponds only to the first part of the curve up to the first inflex point.
The method provides an alternative method of titration in alcohol for cases where intense interference with salts of weak inorganic acids occurs.
Although there is a theoretical possibility that high pH could be caused by other soluble strong principles such as lithium hydroxide or quaternary ammonium hydroxides, their presence in these types of cosmetic products is highly unlikely.
4. QUALITATIVE
4.1 Reaction agents
Standard alkaline buffer, pH 9,18 at 25 ° C: 0,05M solution of sodium tetraborate decahydrate.
4.2 Instruments and appliances
4.2.1. Usual laboratory glass
4.2.2 pH-meter with recorder
4.2.3 Glass membrane electrode
4.2.4 Standard calomel reference electrode
4.3. Procedure
The pH-meter with electrodes is calibrated using a standard alkaline buffer solution. Prepare 10% aqueous solution or aqueous dispersion of the product to be analysed and filter. The pH shall be measured. If the pH is 12 or more, a quantitative determination must be made.
5. QUALITATIVE
5.1 Titration in an aqueous medium
5.1.1. Reaction reagent
5.1.1.1. Propelling solution of hydrochloric acid, 0,1 mol / l
5.1.2. Instruments and appliances
5.1.2.1. Usual laboratory glass
5.1.2.2 pH-meter with recorder
5.1.2.3 Glass membrane electrode
5.1.2.4 Standard calomel reference electrode
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Regulation Information
| Citation | Decree No. 494 / 2005 Coll., laying down analytical methods for checking the composition of cosmetic products |
|---|---|
| Regulation Type | Order |
| Author | - |
| Collection | Code of Laws |
| Date of Promulgation | 23.12.2005 |
|---|---|
| Effective from | 01.01.2006 |
| Effective until | - |
| Status | Valid |
The regulation text is for informational purposes only.
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