Decree of the Ministry of Industry and Trade No. 93 / 1999 Coll.
Decree of the Ministry of Industry and Trade laying down procedures for the quantitative analysis of binary textile fibre mixtures
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93
DECLARATION
Ministry of Industry and Trade
of 29 April 1999
laying down procedures for the quantitative analysis of binary textile fibre mixtures
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) This decree (1) implements the relevant provisions of the European Communities (2) and establishes procedures for the quantitative analysis of binary textile fibre mixtures from which textile products marketed for sale to the consumer are manufactured or intended for further processing.
(2) The procedures for the quantitative analysis of binary fibre mixtures which may be used to determine the composition of the material are set out in Annex 1 to this Decree.
(3) The methods of quantitative chemical analysis of binary fibre mixtures are set out in Annex 2 to this Decree.
(4) An overview of the methods for chemical analysis and their area of use is contained 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 93 / 1999 Coll.
Procedures for quantitative analysis of binary fibre mixtures
1. The Annex lays down procedures for quantitative analysis of binary fibre mixtures carried out by:
(a) manually; or
(b) chemically,
and for obtaining laboratory samples of an appropriate size (i.e. weighing not more than 100 g), for pre-treatment and for the 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 shall be selected to represent the batch sample.
4.2 Test samples shall be taken from a laboratory sample so that each of them represents a laboratory sample.
4.3 Sampling of loose fibres
4.3.1. 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 from the washing machine remains intact after pre-treatment, the test samples shall be taken in accordance with 4.3.2. 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.
4.3.2 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.
4.4. Sampling of yarns
4.4.1. Yarn on spools or hanks
4.4.1.1. Samples shall be taken from all reels of the lot sample. The appropriate equal lengths shall be removed from each coil, 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.
4.4.1.2. For 10 g test samples, the length of yarn to be extracted from each coil shall be determined according to:
l = 106N t,
where l is the length of yarn in cm,
N number of coils in the sample lot,
d.
4.4.1.3 If the value of N. t is high, i.e. more than 2 000, the heavier hanger will roll 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.
4.4.2.
The laboratory sample shall be taken by cutting off the part from the end of the warp of at least 20 cm in length, comprising 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,
where l is the length of the sample in cm,
N number of yarns in the warp,
d.
4.5 Sampling of surface fabrics
4.5.1 From the sample of the lot represented by one cut of the surface fabric, cut the stripe along the diagonal from one corner to the other and remove the edges. 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 = x104G,
where P is the area of the sample in cm2,
x sample mass in g,
G sample weight in 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.
4.5.2 Each cut according to paragraph 4.5.1 shall be processed from a sample of a lot consisting of several cuts and each result shall be given separately.
4.6 Sampling of ready-made products and finished articles
The sample of the lot is usually a ready-made product, a finished piece product or a representative part of it. 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 In the case of elastolefin or fibre mixtures containing elastolefin and other fibres, which are wool, animal hair, silk, cotton, flax, hemp, jute, manila hemp, alpha, coconut fibre, broome, ramie, sisal, cupro fibres, modal fibres, protein, viscose, acryl, polyamide or nylon, polyester and elastomultiester, the procedure referred to in point 5.2 shall be slightly modified by replacing the petrolether with acetone.
5.4 In the case of dual-component mixtures containing elastolefin and acetate, the following procedure shall be used for the pre-treatment: the sample shall be extracted for 10 minutes at 80 ° C with a solution containing 25 g / l 50% orthophosphoric acid and 50 g / l urea. The spa ratio is 1: 100. Wash the sample with water, dry it, wash it with 0,1% sodium bicarbonate solution and lastly wash it with water.
5.5 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.
5.6 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
The cooling shall be carried out in a desiccator located next to the balance for at least 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 fibre, in the case of woven fabrics where the weft is of a different type of fibre than the warp, in the case of plaits 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 a temperature (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, boiling range 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 fibre types thus obtained shall be deposited 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 taking into account the weight loss during the preliminary preparation of the samples.
7.8.2. Calculation of the net dry fibre content in%, regardless of weight loss during pre-processing:
P1 = 100m1m1 + m2
P2 = 100-P1,
where P1 is the content of the first clean dry component in%,
P2 content of the second clean dry component in%,
m1 net dry mass of the first component,
m2 net dry weight of the second component.
7.8.3. Calculation of the contents of the components with correction using the contractual increases and correction factors for weight loss during pre-preparation (if necessary) shall be carried out in accordance with 8.8.
8. Chemical Methods
8.1 Nature of chemical methods
8.1.1 The chemical method is based on the selective dissolution of one of the components of the mixture. The net dry weight of the sample and the insoluble residue shall be determined by the contents of each component.
8.1.2. The additional procedure for individual methods is set out in Annex 2 to this Decree.
8.1.3. If the analysis is based on a principle other than selective dissolution, all details are given in Annex 2 to this Decree.
8.1.4 It is appropriate to use an alternative procedure for checking the dissolution of the component which in the standard procedure formed the remainder.
8.2. Conditions for use of chemical methods:
(a) before analysis, all fibres in the mixture must be identified;
(b) the weightings 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.
8.3. Aids and devices:
(a) filter cups;
(b) weightings,
(c) pump,
(d) a silica gel desiccant with a moisture indicator;
(e) a drying room with an ventilation system for drying 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.
8.4 Chemicals:
(a) redistilled petroleum ether, boiling range 40 ° C to 60 ° C;
(b) distilled or deionised water;
(c) acetone,
(d) orthophosphoric acid,
(e) urea,
(f) sodium bicarbonate; and
(g) other chemicals specified for each method in Annex 2 to this Decree.
The chemicals must be clean, p. a.
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 is dried in the weighing vessel according to 6.1, cooled in the desiccator according to 6.2 and weighed in accordance with 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 carried out as specified in the relevant part of the method used (see Annex 2 to this Decree). The rest of the sample shall be examined under a microscope to determine whether the soluble fibre has actually been completely removed by the procedure.
(c) Testing according to the procedure referred to in 8.5 (a) and (b) shall be performed twice.
8.6 Calculation of results
8.6.1. The insoluble component shall be expressed as a percentage of the total fibre mass of the mixture.
8.6.2. The proportion of the soluble component shall be obtained from the difference between the total weight of the fibres in the mixture and that of the insoluble component.
8.6.3. The result shall be calculated on the basis of a net dry weight corrected by:
8.6.3.1 of the contractual maturity5), and
8.6.3.2 correction coefficients to take into account the effect of weight loss during sample preparation and analysis.
8.6.4. The calculations shall be performed according to the formula in 8.8.
8.7. Calculation of the insoluble component content by percentage on the basis of net dry weight, regardless of loss of fibre weight during pre-preparation of the sample:
P1 = 100rdm,
where P1 is the net dry insoluble component content in%,
m dry weight of the sample after pre-preparation,
r dry weight of the residue,
d correction factor for loss of the mass of the component in the reagent during analysis.
Note: Suitable values for d are given for each method - Annex 2 to this Decree. These values are applicable to chemically undegraded fibres.
8.8 Calculation of the insoluble component content using the contractual increases and correction factors taking into account weight loss during the preliminary preparation of the sample:
P1A = 100 P11 + a1 + b1100P11 + a1 + b1100 + 100-P11 + a2 + b2100,
where P1A is the insoluble component content, including moisture content and weight loss, expressed in% during pre-preparation;
P1 content of the net dry insoluble component in%, calculated according to the formula in 8.7,
a1 contractual premium for insoluble component in%,
a2 contractual premium for the soluble component in%;
b1 loss of insoluble component mass during pre-preparation in%,
b2 weight loss of soluble component during pre-preparation in%.
The content of the second component (P2A) is calculated from difference 100 - P1A.
If a special method of pre-preparation is used, b1 and b2 values are determined by pre-preparation with each fibre component from the mixture.
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, average b1 and b2 values shall be used when testing clean fibres similar to those in the test mixture.
If the normal method of pre-preparation, i.e. extraction by kerosene and water, is used, the correction coefficients b1 and b2 need not be taken into account. The exception is for unbleached cotton, unbleached flax and unbleached hemp, where weight loss during the preliminary preparation is 4% and for polypropylene 1%.
8.9 Methods of quantitative chemical analysis
8.9.1 Individual chemical methods for the analysis of textile fibre mixtures are set out in Annex 2 to this Decree.
8.9.2 An informative overview of the methods for chemical analysis and their area of use is given in Annex 3 to this decree.
Note: The names of each fibre type are the same as those of Decree No. 92 / 1999 Coll., which specifies the method of labelling textile products with the material composition. The figures below follow Annex 3.
8.9.3. In the implementation of chemical methods, the principles of occupational safety in chemical laboratories must be respected.
9. Conformity of methods
The conformity of analysis of individual methods is characterised by a critical difference at 95% probability.
10. Test report
The test report shall contain the following information:
(a) a statement that the analysis has been carried out in accordance with the relevant method;
(b) a detailed description of any special preparation;
(c) the individual results and the arithmetic mean of the results given in one decimal place;
(d) the date of the test and the signature of the worker responsible.
Methods - summary table
| Metoda číslo | Oblast použití | Činidlo | |
|---|---|---|---|
| Rozpustná složka | Nerozpustná složka | ||
| 1 | acetát | další stanovená vlákna | aceton |
| 2 | stanovená proteinová vlákna | další stanovená vlákna | chlornan |
| 3 | viskóza, měďnatá vlákna nebo stanovené typy modalových vláken | bavlna, elastolefin nebo melamin | kyselina mravenčí a chlorid zinečnatý |
| 4 | polyamid nebo nylon | další stanovená vlákna | kyselina mravenčí 80 % (hmot.) |
| 5 | acetát | triacetát, elastolefin nebo melamin | benzylalkohol |
| 6 | triacetát nebo polylaktid | další stanovená vlákna | dichlormetan |
| 7 | stanovená celulózová vlákna | polyester, elastomultiester nebo elastolefin | kyselina sírová 75 % (hmot.) |
| 8 | akryl, stanovená modakrylová nebo stanovená chlorovlákna | další stanovená vlákna | dimetylformamid |
| 9 | stanovená chlorovlákna | další stanovená vlákna | sirouhlík/aceton, 55,5/44,5 % (obj.) |
| 10 | acetát | stanovená chlorovlákna, elastolefin nebo melamin | bezvodá (ledová) kyselina octová |
| 11 | hedvábí | vlna, zvířecí chlupy, elastolefin nebo melamin | kyselina sírová 75 % (hmot.) |
| 12 | juta | stanovená živočišná vlákna | metoda určující obsah dusíku |
| 13 | polypropylen | další stanovená vlákna | xylen |
| 14 | další stanovená vlákna | chlorovlákna (homopolymery vinylchloridu), elastolefin nebo melamin | metoda s koncentrovanou kyselinou sírovou |
| 15 | chlorovlákna, stanovená modakrylová, stanovená elastanová, acetátová, triacetátová vlákna | další stanovená vlákna | cyklohexanon |
| 16 | melamin | bavlna nebo aramid | horká kyselina mravenčí 90 % (hmot.) |
Příloha č. 2
Annex No 2 to Decree No 93 / 1999 Coll.
Methods of quantitative chemical analysis of binary fibre mixtures
1. Method 1 Acetate and other specified fibres (acetone method)
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Regulation Information
| Citation | Decree of the Ministry of Industry and Trade No. 93 / 1999 Coll., laying down procedures for quantitative analysis of binary 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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