Decree of the Ministry of Industry and Trade No. 94 / 1999 Coll.
Decree of the Ministry of Industry and Trade laying down procedures for the quantitative analysis of three-component textile fibre mixtures
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94
DECLARATION
Ministry of Industry and Trade
of 29 April 1999
laying down procedures for the quantitative analysis of tricycle mixtures of textile fibres
The Ministry of Industry and Trade provides pursuant to Section 28a (a) of Act No. 634 / 1992 Coll., on Consumer Protection, as amended by Act No. 104 / 1995 Coll.:
Subject matter
(1) The Decree lays down procedures for the quantitative analysis of three-component textile fibre mixtures from which textile products placed on the market for sale to the consumer or intended for further processing.
(2) The procedures for the quantitative analysis of three-component fibre mixtures used to determine the composition of the material are set out in Annex 1 to this Decree.
(3) Examples of the calculation of the content of components in three-component fibre mixtures are given in Annex 2 to this Decree.
(4) An overview of the three-component fibre mixtures for which the methods for analysis may be used for the analysis of the two-component fibre mixtures contained in a separate legislation, 1) is set out in Annex 3 to this Decree.
Efficacy
This Decree shall take effect on 1 July 1999.
Minister:
Doc.
Příloha č. 1
Annex No 1 to Decree No 94 / 1999 Coll.
Procedures for quantitative analysis of three-component fibre mixtures
1. The Annex sets out the procedures for the quantitative analysis of triconstituent fibre mixtures carried out by:
(a) manually;
(b) chemically, or
(c) a combination of manual and chemical methods
and to obtain laboratory samples of suitable size for pre-treatment and for selection of test samples.
2. These procedures are used in particular to check the fibre content of textile products.
3. Basic terms
3.1 Lot: quantity of material evaluated based on a series of test results. It may include, for example, all material in a single supply of fabric or all fabric woven from a single warp cylinder, etc.
3.2 Sample of the lot: part of the lot which has been taken as a representative sample of the whole and which is available in the laboratory. The size and nature of this sample shall be sufficient, taking into account the ununiformity of the lot and at the same time allowing easy handling in the laboratory. 1)
3.3 Laboratory sample: part of a sample of a lot which is provisionally processed for removal of non-fibrous substances and from which test samples are taken. The size and nature of the sample shall be sufficient in view of the unevenness of the lot sample.
3.4 Test sample: part of the material needed to obtain individual test results and taken from a laboratory sample.
4. Sampling and preparation
4.1 The laboratory sample representing the batch shall be large enough to prepare the necessary number of test samples. The test sample shall be at least 1 g.
4.2 Sampling of loose fibres
4.2.1. Unoriented fibres
The laboratory sample shall be obtained by random selection of tubs from the sample lot. Mix the entire laboratory sample thoroughly with the laboratory washing machine. 2) The mixture containing free fibres and fibres attached to the equipment used for mixing shall be subjected to prior processing. Then a test sample of the appropriate mass shall be taken from the fleece or mixture, free fibres and fibres attached to the machinery. If the web of the washing machine remains intact after pre-treatment, the test samples shall be taken as described in 4.2.2. If the web of the carding machine is disturbed during preliminary processing, each test sample shall be prepared by random sampling of at least 16 small tubs of appropriate and approximately the same size, which shall be merged.
4.2.2 Oriented fibres (carded fibres, web, strands, rovings)
At least 10 samples shall be cut from randomly selected parts of the lot sample to cover the complete cross-section, each weighing approximately 1 g. The laboratory sample thus produced shall be subjected to prior processing. The individual cut-off parts shall be joined by being placed side by side and the test sample taken from the whole section so that the part of each of the ten cut-off parts is taken.
4.3. Sampling of yarns
4.3.1. Yarn on spools or hanks
4.3.1.1. Samples shall be taken from all coils of the lot sample. The appropriate equal lengths from each coil shall be removed either by winding into hanks with the same number of oats per winch (3) or by other means. The individual lengths shall be placed side by side either as a single hitch or as a cable and shall form a laboratory sample containing the same lengths from each coil in the hinge or cable. The laboratory sample shall be subjected to preliminary processing. The test samples shall be taken from the laboratory sample by cutting the bundle of yarns of equal length from the hanger or cable, making sure that the bundle contains all the yarn in the sample.
4.3.1.2. For 10 g test samples, the length of yarn to be extracted from each coil shall be determined according to:
l = 106NT,
| kde | l | je délka příze v cm, |
| N | počet cívek ve vzorku partie, |
| t | délková hmotnost příze v tex. |
4.3.1.3. If the value of N. t is high, i.e. more than 2 000, the heavier hanger is rolled and cut across in two places to create a cable of suitable weight. The end of the samples in the form of a cable shall be reliably connected before preliminary processing and the test samples shall be taken from a point distant from that connection.
4.3.2.
The laboratory sample shall be taken by cutting off the part from the end of the warp of at least 20 cm in length, including all yarns in the warp, except for marginal yarns which are discarded. The volume shall be bound by yarn at one end. If the sample is too large for preliminary processing as a whole, it shall be divided into two or more parts which shall be processed individually. Each part shall be tied together at one end for pre-processing and after pre-processing the parts shall be reassembled. The test sample shall be taken by cutting the appropriate length from the laboratory sample from a free (unbound) end involving all yarns in the warp. In order to obtain a sample of 1 g, the length of the sample shall be determined by reference to:
l = 105NT,
| kde | l | je délka vzorku v cm, |
| N | počet nití v osnově, |
| t | délková hmotnost v tex. |
4.4 Sampling of surface fabrics
4.4.1 The stripe is cut from the sample of the lot represented by one cut of the surface fabric from one corner to the other, and the edges are removed. This strip is a laboratory sample. To obtain a laboratory sample of x, the area of the strip (laboratory sample) shall be determined according to the relation:
P = x 104G,
| kde | P | je plocha vzorku v cm2, |
| x | hmotnost vzorku v g, |
| G | plošná hmotnost vzorku v g/m2. |
The laboratory sample shall be subjected to pre-treatment and then cross-cut into four equal parts which shall be placed on each other. The test samples shall be taken from all parts of the supported material by cutting through all layers so that each sample contains the same length of each layer. If the fabric has a woven pattern, a laboratory sample shall be taken in the direction of the outline of a size equal to at least the warp of the pattern. If such a laboratory sample is too large to be processed as a whole, it shall be cut into the same parts. These shall be specifically preliminary and shall be placed on each other before the test sample is taken, making sure that the corresponding parts of the model are not on each other.
4.4.2 Each cut according to 4.4.1 shall be processed from a sample of the lot, which consists of several cuts, and each result shall be reported separately.
4.5 Sampling of ready-made products and finished piece products
The sample of the lot is usually a ready-made product or a finished piece product or a representative part thereof. When sampling, account should be taken of those parts of products which do not have the same fibre content. A laboratory sample shall be taken representing part of the prefabricated or finished article, the composition of which shall be indicated on the label. If the goods have several labels, representative laboratory samples shall be taken from each part corresponding to the label. Where the product is made from parts of different composition, laboratory samples shall be taken from each part of the product and the relative proportions of the individual parts shall be determined in relation to the whole product. The percentage shall then be calculated taking into account the shares of the parts from which they were collected.
Laboratory samples shall be subjected to pre-treatment and then tested.
5. Preparation of samples
5.1 Non-fibrous substances (fatty substances, binders, fillers, scouring and preparation agents, impregnating materials, dye and printing aids, substances to achieve special properties, etc.) shall be removed from the sample as they may be the cause of errors. Colour for colour fibres is considered as part of the filament and is not removed.
5.2 The extractable substances with petroleum and water are first removed by processing the sample in Soxhlet's petroleum device for 1 hour at a minimum speed of 6 cycles per hour. Allow the petroleum to evaporate from the sample and the sample is then directly extracted with water. Dip for 1 hour at room temperature, then soak at (65 ± 5) ° C for an additional hour after occasional mixing of the liquid. The spa ratio is 1: 100. The excess water is removed from the sample by squeezing, suction or centrifugation and then dried in the air.
5.3 Non-fibrous substances which cannot be removed by the procedure described in 5.2 shall be removed by another appropriate method which shall not affect the fibrous constituents.
5.4 For certain unbleached natural vegetable fibres (e.g. jute, coconut fibre) the procedure according to 5.2 does not remove all natural non-fibrous substances. However, further procedures for their removal are not used.
6. General instructions for conducting tests
6.1. Drying
All drying procedures shall be carried out in a drying room for a minimum of 4 hours and a maximum of 16 hours at (105 ± 3) ° C. If the drying time is less than 14 hours, it shall be determined whether a constant mass has been achieved, i.e. that the weight change after further drying for 60 minutes is less than 0,05%.
The sample and the filter cup are dried in a weighing bag with the lid next to it. After drying, the weighing device is closed before being removed from the oven and transferred quickly to the desiccator.
Handling of cups, scales and samples during drying, cooling and weighing shall not be carried out by hand.
6.2 Cooling
Cooling shall be carried out in a desiccator located next to the scales for a minimum of 2 hours.
6.3 Weights
After cooling, the weighing device shall be weighed so that the weighing is completed within 2 minutes after removal from the desiccator. Weigh to the nearest 0,0002 g.
6.4. Test air
Samples need not be conditioned or tested in air-conditioned air.
7. Manual separation method
7.1 Manual analysis is used preferably as it gives more accurate results. It can be used for all textiles where fibre components do not form an inseparable mixture. For example, in the case of yarns of different elements, each of which consists of one type of fibres, woven fabrics, where the weft is of a different type of filament than the warp, in the case of knitted fabrics which can be cut open and which are made of different yarns.
7.2. Essential of the test
After identification of textile components, non-fibrous material shall be removed by appropriate preliminary preparation. The fibres are separated manually, dried and weighed. The proportion of each fibre in the mixture shall then be calculated.
7.3. Instruments and appliances:
(a) weightings,
(b) a desiccant containing a silica gel with a moisture indicator;
(c) a drying room with an ventilation system for drying samples at 105 ± 3 ° C;
(d) analytical scales with an accuracy of 0,0002 g;
(e) Soxhlet extraction apparatus or other apparatus giving the same results;
(f) preparation needle,
(g) a curvature gauge or other device giving identical results.
7.4 Chemicals:
(a) redistilled petroleum ether, range of boiling points 40 ° C to 60 ° C;
(b) distilled or deionised water.
7.5 For test air see 6.4.
7.6 For sampling and preparation see 4.
7.7. Test procedure
7.7.1 Yarn analysis
A test sample of at least 1 g shall be taken from the laboratory sample after pre-preparation. For very fine yarns, the analysis shall be carried out on a minimum length of 30 m regardless of its weight. The yarn is cut into pieces of suitable length. Each fibre type shall be separated by means of a preparation needle and, if appropriate, by means of a curvature meter. The fibres thus obtained shall be stored in pre-weighed scales.
7.7.2. Analysis of surface fabrics
A test sample of at least 1 g in parallel with weft or warp threads shall be taken from the laboratory sample after pre-preparation. In the case of a netting, the sample shall be taken in the direction of columns or rows. The edges must be carefully trimmed to avoid shaking. The sample shall not contain edges. Individual types of fibres are separated and stored in pre-weighed scales.
7.7.3 Drying, cooling and weighing shall be carried out according to 6.1 to 6.3.
7.8 Calculation of results
7.8.1. The weight of each fibre component shall be expressed as a percentage of the total fibre weight of the mixture. The result shall be calculated on the basis of the net dry weight to be adjusted by means of the mark-up (4) and the correction factors (5) taking into account the weight loss during the preliminary preparation of the samples.
7.8.2. Calculation of the net dry fibre content as a percentage, regardless of weight loss during pre-processing:
P1 = 100 m1m1 + m2 + m3
P2 = 100 m2m1 + m2 + m3
P3 = 100-P1 + P2,
| kde | P1 | je obsah první čisté suché složky v %, |
| P2 | obsah druhé čisté suché složky v %, | |
| P3 | obsah třetí čisté suché složky v %, | |
| m1 | čistá suchá hmotnost první složky, | |
| m2 | čistá suchá hmotnost druhé složky, | |
| m3 | čistá suchá hmotnost třetí složky. |
7.8.3. Calculation of the contents of the components with correction by means of contractual increases and correction coefficients for weight loss during pre-preparation (if necessary) shall be carried out in accordance with 8.6.3.
8. Chemical Methods
8.1 Background
The chemical method is based on the gradual dissolution of the individual components of the mixture. Four options are possible:
8.1.1 Two samples shall be used. Component A is removed from the first sample and component B from the second sample
8.1.2 Two samples shall be used. From the first sample remove component A and from the second sample component A and B
8.1.3 Two samples shall be used. From the first sample remove components A and B and from the second sample remove components B and C
8.1.4. One sample shall be used. Folder A and Component B are gradually removed.
The determined net dry weight of the samples and the insoluble residues shall be determined by the content of each component. It is appropriate to use two of the above options for checking.
8.2 Instruments and appliances
(a) filter cups;
(b) weightings,
(c) pump,
(d) a silica gel desiccant with a moisture indicator;
(e) a drying room with ventilation for drying of samples at a temperature (105 ± 3 ° C);
(f) analytical scales with an accuracy of 0,0002 g;
(g) Soxhlet extraction apparatus or other apparatus giving the same results;
(h) suction flask.
8.3 Chemicals:
(a) redistilled petroleum ether, range of boiling points 40 ° C to 60 ° C;
(b) distilled or deionised water;
(c) other chemicals. 5)
The chemicals must be clean, p. a.
8.4. Conditions for use of chemical methods
(a) before analysis, all fibres in the mixture must be identified;
(b) the correction coefficients apply to the non-degraded fibres. Other correction factors shall be used for degraded fibres,
(c) if it is not technically difficult, the component with higher representation in the mixture shall be dissolved as a priority.
8.5. Test procedure:
(a) A test sample of at least 1 g shall be taken from the laboratory sample. The sample shall be cut into pieces of about 10 mm long and shall be broken as much as possible. Each sample shall be dried in a weighing vessel, cooled in a desiccator and weighed according to 6.3.
b) The sample shall be transferred to the glass container and the weighing device shall be immediately transported. The dry weight of the sample shall be calculated from the difference in weight. The test shall then be performed as specified at the relevant point of the method used. 5) The rest of the sample shall be examined under a microscope to determine whether the soluble fibres have actually been removed by the procedure.
(c) Testing according to the above procedure shall be carried out at least twice.
8.6 Calculation of results
8.6.1. The weight of each component in the mixture shall be expressed as a percentage of the total weight of the fibres in the mixture. The result shall be calculated on the basis of dry weight, corrected by the contractual increases and correction factors taking into account weight loss during sample preparation and analysis.
8.6.2. Calculation of the net dry weight of fibres in percentage regardless of loss of fibre weight during the preliminary preparation of the sample:
8.6.2.1 variant 1
Two test samples shall be used. A is removed by solvent from the first sample and B from the second sample. The insoluble residues of each sample shall be weighed and the content of each constituent of the relationships calculated:
P1 = 100d2d1-d2r1m1 + r2m21-d2d1
P2 = 100d4d3-d4r2m2 + r1m11-d4d3
P3 = 100-P1 + P2,
| kde | P1 | je obsah první čisté suché složky rozpuštěné v prvním vzorku prvním činidlem v %, |
| P2 | obsah druhé suché čisté složky rozpuštěné ve druhém vzorku druhým činidlem v %, | |
| P3 | obsah třetí suché čisté složky, která nebyla rozpuštěna v obou vzorcích v %, | |
| m1 | suchá hmotnost prvního vzorku po předběžné přípravě, | |
| m2 | suchá hmotnost druhého vzorku po předběžné přípravě, | |
| r1 | suchá hmotnost zbytku po odstranění první složky z prvního vzorku prvním činidlem, | |
| r2 | suchá hmotnost zbytku po odstranění druhé komponenty ze druhého vzorku druhým činidlem, | |
| d1 | opravný koeficient pro ztrátu hmotnosti druhé složky nerozpustné v prvním činidle – v prvním vzorku, | |
| d2 | opravný koeficient pro ztrátu hmotnosti třetí složky nerozpustné v prvním činidle – v prvním vzorku, | |
| d3 | opravný koeficient pro ztrátu hmotnosti první složky nerozpustné ve druhém činidle – ve druhém vzorku, | |
| d4 | opravný koeficient pro ztrátu hmotnosti třetí složky nerozpuštěné ve druhém činidle – ve druhém vzorku. |
8.6.2.2 variant 2
Two test samples shall be used. Component A is removed by dissolution from the first sample and two components A and B from the second sample. The insoluble residues of each sample shall be weighed and the content of each constituent of the relationships calculated:
P1 = 100-P2 + P3
P2 = 100 d1r1m1-P3d1d2
P3 = 100 d4r2m2,
| kde | P1 | je obsah první čisté suché složky rozpuštěné v prvním vzorku prvním činidlem v %, |
| P2 | obsah druhé čisté suché složky rozpuštěné současně s první složkou ve druhém vzorku druhým činidlem v %, | |
| P3 | obsah třetí čisté suché složky, která nebyla rozpuštěna v obou vzorcích, v %, | |
| m1 | suchá hmotnost prvního vzorku po předběžné přípravě, | |
| m2 | suchá hmotnost druhého vzorku po předběžné přípravě, | |
| r1 | suchá hmotnost zbytku po odstranění první složky z prvního vzorku prvním činidlem, | |
| r2 | suchá hmotnost vzorku po odstranění první a druhé složky ze druhého vzorku druhým činidlem, | |
| d1 | opravný koeficient pro ztrátu hmotnosti druhé složky nerozpuštěné v prvním činidle – v prvním vzorku, | |
| d2 | opravný koeficient pro ztrátu hmotnosti třetí složky nerozpuštěné v prvním činidle – v prvním vzorku, | |
| d4 | opravný koeficient pro ztrátu hmotnosti třetí složky nerozpuštěné ve druhém činidle - ve druhém vzorku. |
8.6.2.3 variant 3
Two test samples shall be used. Two components A and B are removed by dissolution from the first sample and two components B and C are removed from the second sample. The insoluble residues of each sample shall be weighed and the content of each constituent of the relationships calculated:
P1 = 100 d3r2m2
P2 = 100-P1 + P3
P3 = 100 d2r1m1,
| kde | P1 | je obsah první čisté suché složky rozpuštěné v prvním vzorku prvním činidlem v %, |
| P2 | obsah druhé čisté suché složky rozpuštěné v prvním vzorku prvním činidlem a ve druhém vzorku druhým činidlem v %, | |
| P3 | obsah třetí čisté suché složky, rozpuštěné ve druhém vzorku druhým činidlem v %, | |
| m1 | suchá hmotnost prvního vzorku po předběžné přípravě, | |
| m2 | suchá hmotnost druhého vzorku po předběžné přípravě, | |
| r1 | suchá hmotnost zbytku po odstranění první a druhé složky z prvního vzorku prvním činidlem, | |
| r2 | suchá hmotnost zbytku vzorku po odstranění druhé a třetí složky ze druhého vzorku druhým činidlem, | |
| d2 | opravný koeficient pro ztrátu hmotnosti třetí složky nerozpuštěné v prvním činidle – v prvním vzorku, | |
| d3 | opravný koeficient pro ztrátu hmotnosti třetí složky nerozpuštěné ve druhém činidle – ve druhém vzorku. |
8.6.2.4 variant 4
Only one test sample shall be used. One of the components is removed by dissolution and the remainder of the two other components is weighed. One of the two types of fibres in the rest shall be removed by dissolution and the undissolved component weighed and the content of each component of the relationships shall be calculated:
P1 = 100-P2 + P3
P2 = 100 d1r1m-P3d1d2
P3 = 100 d3r2m,
| kde | P1 | je obsah první čisté suché složky (první rozpuštěné složky) v %, |
| P2 | obsah druhé čisté suché složky (druhé rozpuštěné složky) v %, | |
| P3 | obsah třetí čisté suché složky (nerozpuštěné složky) v %, m suchá hmotnost zkušebního vzorku po předběžné přípravě, | |
| m | suchá hmotnost zkušebního vzorku po předběžné přípravě, | |
| r1 | suchá hmotnost zbytku po odstranění první složky prvním činidlem, | |
| r2 | suchá hmotnost zbytku po odstranění první a druhé složky prvním a druhým činidlem, | |
| d1 | opravný koeficient pro ztrátu hmotnosti druhé složky v prvním činidle, | |
| d2 | opravný koeficient pro ztrátu hmotnosti třetí složky v prvním činidle, | |
| d3 | opravný koeficient pro ztrátu hmotnosti třetí složky v prvním a druhém činidle. |
8.6.3. Calculation of the content of the ingredient using the contractual increases and correction factors taking into account weight loss during the preliminary preparation of the sample:
A = 1 + a1 + b1100 B = 1 + a2 + b2100 C = 1 + a3 + b3100
P1A = 100P1AP1A + P2B + P3C
P2A = 100P2B1A + P2B + P3C
P3A = 100P3CP1A + P2B + P3C,
| kde | P1A | je obsah první čisté suché složky včetně obsahu vlhkosti a ztráty hmotnosti vzniklé během předběžné přípravy v %, |
| P2A | obsah druhé čisté suché složky včetně obsahu vlhkosti a ztráty hmotnosti vzniklé během předběžné přípravy v %, | |
| P3A | obsah třetí čisté suché složky včetně obsahu vlhkosti a ztráty hmotnosti vzniklé během předběžné přípravy v %, | |
| P1 | obsah první čisté suché složky v % vypočtený podle jednoho ze vzorců uvedených v 7. 8. 2, | |
| P2 | obsah druhé čisté suché složky v % vypočtený podle jednoho ze vzorců uvedených v 7. 8. 2, | |
| P3 | obsah třetí čisté suché složky v % vypočtený podle jednoho ze vzorců uvedených v 7. 8. 2, | |
| a1 | smluvní přirážka pro první složku v %, | |
| a2 | smluvní přirážka pro druhou složku v %, | |
| a3 | smluvní přirážka pro třetí složku v %, | |
| b1 | ztráta hmotnosti první složky během předběžné přípravy v %, | |
| b2 | ztráta hmotnosti druhé složky během předběžné přípravy v %, | |
| b3 | ztráta hmotnosti třetí složky během předběžné přípravy v %. |
If a special method of pre-preparation according to 5.3 is used, values b1, b2, b3 are determined by pre-preparation with each fibre component. This shall be done with fibres removed from all non-fibrous materials except those which normally contain and are in the state in which they are found in the material analysed.
If clean separated fibres, which are components of the mixture, are not available, the mean values b1, b2, b3 shall be used when testing clean fibres similar to those in the test mixture.
If a normal method of pre-preparation is used, i.e. extraction by kerosene and water, correction coefficients b1, b2, b3 are not taken into account. The exception is for unbleached cotton, unbleached flax and unbleached hemp, where weight losses during the preliminary preparation represent 4% and 1% for polypropylene.
Note: Examples for calculation are given in Annex 2 to this Decree.
9. Manual and chemical separation method
9.1. Essential of the test
Priority shall be given to manual separation (where technically possible). The rest is analysed by chemical method.
9.2 The procedures for manual method and chemical methods are set out in points 7 and 8.
10. Conformity of methods
10.1 In order to determine the conformity of the analysis of the individual three-component mixture methods, the values given in the two-component mixture analysis methods used for the analysis of the three-component mixtures shall normally be used.
10.2 For four variants of chemical methods of analysis of three-component mixtures, a double dilution correction shall be made. Provided that E1 and E2 indicate the conformity of the two methods for analysis of the two-component mixtures, the conformity of the results for each component is shown in Table 1.
Table 1: Determination of conformity of results
| Vlákenná složka | Varianta 1 | Varianta 2 a 3 | Varianta 4 |
|---|---|---|---|
| A | E1 | E1 | E1 |
| B | E2 | E1 + E2 | E1 + E2 |
| C | E1 + E2 | E2 | E1 + E2 |
Note: When using variant 4 it may be found that the conformity is lower than that determined in Table 1. This is due to the interference of the first reagent on the remainder consisting of components B and C. This effect is difficult to evaluate.
11. Test report
The test report shall contain the following information:
(a) the variant (s) used for analysis, methods, reagents and correction factors;
(b) a detailed description of any special preparation;
(c) the individual results and the arithmetic mean of the results given in one decimal place;
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Regulation Information
| Citation | Decree of the Ministry of Industry and Trade No. 94 / 1999 Coll., laying down procedures for quantitative analysis of three-component textile fibre mixtures |
|---|---|
| Regulation Type | Order |
| Author | - |
| Collection | Code of Laws |
| Date of Promulgation | 28.05.1999 |
|---|---|
| Effective from | 01.07.1999 |
| Effective until | - |
| Status | Valid |
The regulation text is for informational purposes only.
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