Important legal notice

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31984L0425

Tenth Commission Directive 84/425/EEC of 25 July 1984 establishing Community methods of analysis for the official control of feedingstuffs

Official Journal L 238 , 06/09/1984 P. 0034 - 0038 Finnish special edition: Chapter 3 Volume 18 P. 0038  Spanish special edition: Chapter 03 Volume 32 P. 0085  Swedish special edition: Chapter 3 Volume 18 P. 0038  Portuguese special edition Chapter 03 Volume 32 P. 0085  Special edition in Czech Chapter 03 Volume 06 P. 111  - 115 Special edition in Estonian Chapter 03 Volume 06 P. 111  - 115 Special edition in Hungarian Chapter 03 Volume 06 P. 111  - 115 Special edition in Lithuanian Chapter 03 Volume 06 P. 111  - 115 Special edition in Latvian Chapter 03 Volume 06 P. 111  - 115 Special edition in Maltese Chapter 03 Volume 06 P. 111  - 115 Special edition in Polish Chapter 03 Volume 06 P. 111  - 115 Special edition in Slovakian Chapter 03 Volume 06 P. 111  - 115 Special edition in Slovenian Chapter 03 Volume 06 P. 111  - 115

		Tenth Commission Directiveof 25 July 1984establishing Community methods of analysis for the official control of feeding-stuffs(84/425/EEC)THE COMMISSION OF THE EUROPEAN COMMUNITIES,Having regard to the Treaty establishing the European Economic Community,Having regard to Council Directive 70/373/EEC of 20 July 1970 on the introduction of Community methods of sampling and analysis for the official control of feedingstuffs [1], as last amended by the Act of Accession of Greece, and in particular Article 2 thereof,Whereas that Directive requires that official control of feedingstuffs for the purpose of checking compliance with requirements under the provisions laid down by law, regulation or administrative action concerning the quality and composition of feedingstuffs be carried out using Community methods of sampling and analysis ;Whereas Commission Directives 71/250/EEC [2], 73/46/EEC [3], 74/203/EEC [4], 75/84/EEC [5], 76/372/EEC [6], as last amended by Directive 81/680/EEC [7], Directives 71/393/EEC [8], 72/199/EEC [9], 78/633/EEC [10], as last amended by Directive 84/4/EEC [11], and Directive 81/715/EEC [12] have already established a number of Community methods of analysis; whereas the progress of work since then makes it advisable to adopt a new method ;Whereas the measures provided for in this Directive are in accordance with the opinion of the Standing Committee for Feedingstuffs,HAS ADOPTED THIS DIRECTIVE :Article 1Member States shall require that analyses for official controls of feedingstuffs, as regards their content of spiramycin be carried out in accordance with the method described in the Annex.Article 2Member States shall bring into force the laws, regulations or administrative provisions necessary to comply with this Directive by 30 June 1985 at the latest and shall forthwith inform the Community thereof.Article 3This Directive is addressed to the Member States.Done at Brussels, 25 July 1984.For the CommissionPoul DalsagerMember of the Commission[1] OJ No L 170, 3. 8. 1970, p. 2.[2] OJ No L 155, 12. 7. 1971, p. 13.[3] OJ No L 83, 30. 3. 1973, p. 21.[4] OJ No L 108, 22. 4. 1974, p. 7.[5] OJ No L 32, 5. 2. 1975, p. 26.[6] OJ No L 102, 15. 4. 1976, p. 8.[7] OJ No L 246, 29. 8. 1981, p. 32.[8] OJ No L 279, 20. 12. 1971, p. 7.[9] OJ No L 123, 29. 5. 1972, p. 6.[10] OJ No L 206, 29. 7. 1978, p. 43.[11] OJ No L 15, 18. 1. 1984, p. 28.[12] OJ No L 257, 10. 9. 1981, p. 38.--------------------------------------------------ANNEXDETERMINATION OF SPIRAMYCIN BY DIFFUSION IN AN AGAR MEDIUM1. Purpose and scopeThe method is for the determination of spiramycin in feedingstuffs and premixes. The lower limit of determination is 1 mg/kg (1 ppm) [1]2. PrincipleThe sample is extracted with a mixture of methanol/phosphate-bicarbonate buffer at pH 8. The extract is decanted or centrifuged and diluted. Its antibiotic activity is determined by measuring the diffusion of spiramycin in an agar medium inoculated with Micrococcus luteus. Diffusion is shown by the formation of zones of inhibition of the micro-organism. The diameter of these zones is taken to be in direct proportion to the logarithm of the antibiotic concentration over the range of antibiotic concentrations employed.3. Micro-organism : Micrococcus luteus ATCC 9341 (NCTC 8340, NCIB 8553)3.1. Maintenance of stack cultureInoculate tubes containing slopes of culture medium (4.1) with Micrococcus luteus and incubate for 24 hours at 30 o C. Store the culture in a refrigerator at about 4 o C. Reinoculate every two weeks.3.2. Preparation of the bacterial suspension [2]Harvest the growth from a recently prepared agar slope (3.1) with 2 to 3 ml of sodium chloride solution (4.3). Use this suspension to inoculate 250 ml of culture medium (4.1) contained in a Roux flask and incubate for 18 to 20 hours at 30 oC. Harvest the growth in 25 ml of sodium chloride solution (43) and mix. Dilute the suspension to 1/10 with sodium chloride solution (4.3). The light transmission of the suspension must be about 75 %, measured at 650 nm in a 1 cm cell against sodium chloride solution (4.3). This suspension may be kept for one week at about 4 oC.4. Culture media and reagents4.1. Culture medium [3]Meat peptone | 6,0 g |Tryptone | 4,0 g |Yeast extract | 3,0 g |Meat extract | 1,5 g |Glucose | 1,0 g |Agar | 10,0 to 20,0 g |Water | 1000 ml |pH 6,5 to 6,6 (after sterilization). | |4.2. Assay medium [3]Tryptone | 5,0 g |Yeast extract | 4,0 g |Meat extract | 3,0 g |Agar | 10,0 to 20,0 g |Water | 1000 ml |pH 8,0 (after sterilization). | |4.3. Sodium chloride solution 0,8 % (w/v)Dissolve 8 g of sodium chloride in water and dilute to 1000 ml; sterilize.4.4. Phosphate-bicarbonate buffer, pH 8,0Dipotassium hydrogen phosphate K2HPO4 | 16,7 g |Potassium dihydrogen phosphate KH2PO4 | 0,5 g |Sodium hydrogen carbonate NaHCO3 | 20,0 g |Water to | 1000 ml |4.5. Mixture of methanol phosphate-bicarbonate buffer (4.4)50/50 (v/v).4.6 Standard substanceSpiramycin of known activity (in IU).5. Standard solutionsDissolve an accurately weighed quantity of the standard substance (4.6) in the mixture (4.5) and dilute with the same mixture to give a stock solution containing 1000 IU spiramycin per millilitre. Stored in a stoppered flask at 4 o C this solution is stable for up to five days.From this stock solution prepare by successive dilution with the mixture (4.5) the following solutions :S8 | 1 | IU/ml |S4 | 0,5 | IU/ml |S2 | 0,25 | IU/ml |S1 | 0,125 | IU/ml |6. Preparation of the extract and assay solutions6.1. ExtractionWeigh out a quantity of sample of 20,0 g in the case of feedingstuffs, of 1,0 to 20,0 g for premixes. Add 100 ml of the mixture (4.5) and shake for 30 minutes. Centrifuge or decant and dilute the supernatant solution with the mixture (4.5) to obtain an expected spiramycin in content of 1 IU/ml (= Ug).For expected levels of spiramycin lower than 2,5 mg/kg of feedingstuff the extraction must be carried out as follows. Weigh out a quantity of sample of 20,0 g. Add 100 ml of the mixture (4.5) and shake for 30 minutes. Centrifuge for a few minutes, take 50 ml of the supernatant solution and evaporate to about 4 ml under reduced pressure in a rotary evaporator at a temperature not exceeding 40 oC. Dilute the residue with the mixture (4.5) to obtain an expected spiramycin content of 1 IU/ml (= U8).6.2. Assay solutionsFrom solution U8 prepare solutions U4 (expected content: 0,5 IU/ml), U2 (expected content: 0,25 IU/ml) and U1 (expected content: 0,125 IU/ml) by means of successive dilution (1 + 1) with the mixture (4.5).7. Assay procedure7.1. Inoculation of the assay mediumInoculate the assay medium (4.2) with the bacterial suspension (3.2) at about 50 oC . By preliminary trials on plates with assay medium (4.2) determine the quantity of bacterial suspension required to give the largest and clearest zones of inhibition with the various concentrations of spiramycin.7.2. Preparation of the platesDiffusion through agar is carried out in plates with the four concentrations of the standard solution (S8, S4, S2, S1) and the four concentrations of the assay solution (U8, U4, U2, U1). These four concentrations of extract and standard must necessarily be placed in each plate. To this effect, select plates big enough to allow at least eight holes with a diameter of 10 to 13 mm and not less than 30 mm between centres to be made in the agar medium. The test may be carried out on plates consisting of a sheet of glass with a faced aluminium or plastic ring placed on top, 200 mm in diameter and 20 mm high.Pour into the plates a quantity of the medium (4.2), inoculated as in 7.1, to give a layer about 2 mm thick (60 ml for a plate of 200 mm diameter). Allow to set in a level position, bore the holes and place in them exactly measured volumes of assay and standard solutions (between 0,10 and 0,15 ml per hole, according to the diameter). Apply each concentration at least four times so that each determination is subject to an evalution of 32 zones of inhibition.7.3. IncubationIncubate the plates for 16 to 18 hours at 30 ± 2 oC.8. EvaluationMeasure the diameter of the zones of inhibition to the nearest 0,1 mm. Record the mean measurements for each concentration on semi-logarithmic graph paper showing the logarithm of the concentrations in relation to the diameters of the zones of inhibition. Plot the best fit lines of both the standard solution and the extract, for example as below.Determine the "best fit" point for the standard highest level (SH) using the formula:(a) SL=7s1+4s2+s4-2s810Determine the "best fit" point for the standard lowest level (SL) using the formula:(b) SH=7s8+4s4+s2-2s110Similarly calculate the "best fit" points for the extract lowest level (UL) and the extract highest level (UH) by substituting u1, u2, u4 and u8 for s1, s2, s4 and s8 in the above formulae [4].Record the calculated SL and SH values on the same graph paper and join them to give the "best fit" line for the standard solution. Similarly record UL and UH and join them to give the "best fit" line for the extract.In the absence of any interference the lines should be parallel. For practical purposes the lines can be considered parallel if the values (SH — SL) and (UH — UL) do not differ by more than 10 % from their mean value.If the lines are found to be non-parallel either u1 and s1 or u8 and s8 may be discarded and SL, SH, UL and UH calculated, using the alternative formulae, to give alternative "best fit" lines :(a') SL=5s1+2s2-s46 ou 5s2+2s4-s86(b') SH=5s4+2s2-s16 ou 5s8+2s4-s26and similarly for UL and UH. The same criteria of parallelism should be satisfied. The fact that the result has been calculated from three levels should be noted on the final report.When the lines are considered as being parallel, calculate the logarithm of the relative activity (log A) by means of one of the following formulae, depending upon whether three or four levels have been used for the assessment of parallelism.For four levels(c) log. A =u1+u2+u4+u8-s1-s2-s4-s8× 0,602u4+u8+s4+s8-u1-u2-s1-s2For three levels(d) log. A =u1+u2+u4-s1-s2-s4× 0,401u4+s4-u1-s1ou(d') log. A =u2+u4+u8-s2-s4-s8× 0,401u8+s8-u2-s2Activity of sample extract = activity of relevant standard × A(U8 = S8 × A)If the relative activity is found to be outside the range of 0,5 to 2,0, then repeat the assay making appropriate adjustments to the extract concentrations or, if this is not possible, to the standard solutions. When the relative activity cannot be brought into the required range, any result obtained must be considered as approximate and this should be noted on the final report.When the lines are considered as not being parallel, repeat the determination. If, parallelism is still not achieved, the determination must be considered as unsatisfactory.Express the result in milligrams of spiramycin base per kilogram of feedingstuff.9. RepeatabilityThe difference between the results of two parallel determinations carried out on the same sample by the same analyst should not exceed:- 2 mg/kg, in absolute value, for contents of spiramycin base up to 10 mg/kg,- 20 % related to the highest value for contents of 10 to 25 mg/kg,- 5 mg/kg, in absolute value, for contents of 25 to 50 mg/kg,- 10 % related to the highest value for contents above 50 mg/kg.[1] 1 mg spiramycin base is equivalent to 3200 international units (IU).[2] Other methods may be used provided that it has been established that they give similar bacterial suspensions.[3] Any commercial culture medium of similar composition and giving the same results may be used.[4] The small letters "s" and "u" refer to the diameters of the zones of inhibition.--------------------------------------------------


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31992L0072

Council Directive 92/72/EEC of 21 September 1992 on air pollution by ozone

Official Journal L 297 , 13/10/1992 P. 0001 - 0007 Finnish special edition: Chapter 15 Volume 11 P. 0204  Swedish special edition: Chapter 15 Volume 11 P. 0204

COUNCIL DIRECTIVE 92/72/EEC of 21 September 1992 on air pollution by ozoneTHE COUNCIL OF THE EUROPEAN COMMUNITIES,  Having regard to the Treaty establishing the European Economic Community, and in particular Article 130s thereof,  Having regard to the proposal from the Commission (1),  Having regard to the opinion of the European Parliament (2),  Having regard to the opinion of the Economic and Social Committee (3),  Whereas the 1987 fourth Community action programme on the environment (4) provides for the possibility of action on photochemical pollution, and in particular pollution by ozone, in view of its harmful effects and the state of knowledge concerning its  impact on human health and the environment;  Whereas, in order to protect human health, ozone concentrations in the air should be limited; whereas scientific and technical information needs to be utilized and promoted in order to obtain wider knowledge of this form of pollution and, in future,  take effective and appropriate measures to reduce it;  Whereas as complete a knowledge as possible of ozone pollution levels is required in all Member States;  Whereas to obtain this knowledge it is necessary to set up measurement stations to provide data on ozone concentrations in the air;  Whereas in order to obtain results which are comparable in the context of this Directive, the methods used by Member States to determine concentrations need to be equivalent;  Whereas, in view of the special nature of photochemical pollution, the reciprocal exchange of information between Member States and the Commission including, once it is effectively set up, the European Environment Agency (5), is essential for a better  understanding of the problem;  Whereas the setting of information or warning thresholds at which precautions should be taken by the public will make it possible to limit the impact of pollution episodes on health;  Whereas the numerical values of these levels should be based on the findings of work carried out in the framework of the World Health Organization (WHO), in particular as regards the dose-effect relationships established for the pollutant in question;  Whereas the information collected under this Directive should be regularly evaluated to make it possible to monitor the development of air pollution by ozone and the impact of national and Community provisions to reduce photochemical precursors and  establish in the future new provisions concerning ozone and air quality; whereas such evaluation and information should be the subject of a report to be submitted by the Commission as soon as possible and by the end of a period of four years from the  date of implementation of this Directive at the latest;  Whereas combating air pollution by ozone may also entail measures to reduce ozone precursors; whereas the Commission must therefore also submit, with the abovementioned report, proposals for controlling air pollution by ozone and, if necessary, reducing  emissions of ozone precursors;  Whereas action by the Community and Member States against photochemical pollution should be coordinated in order for maximum effect to be achieved,  HAS ADOPTED THIS DIRECTIVE:  Article 1  1. The purpose of this Directive is to establish a harmonized procedure:  - for monitoring,  - for exchanging information,  - for informing and warning the population,  with regard to air pollution by ozone in order to enable the competent authorities of the Member States and the Commission to obtain wider knowledge of this form of air pollution in the Community, optimize the action needed to reduce ozone formation and  guarantee a minimum amount of public information where concentration thresholds as referred to in points 3 and 4 of Annex I are exceeded.  2. For the purposes of this Directive:  - health protection threshold means the ozone concentration value given in Annex I, point 1, which should not be exceeded if human health is to be safeguarded in the event of prolonged pollution episodes,  - vegetation protection thresholds means the ozone concentration values given in Annex I, point 2, beyond which vegetation may be affected,  - population information threshold means the ozone concentration value given in Annex I, point 3, beyond which there are limited, temporary effects on human health in the event of short exposure of particularly sensitive sections of the population and  at which steps must be taken by the Member States as laid down in this Directive,  - population warning threshold means the ozone concentration value given in Annex I, point 4, beyond which there is a risk to human health in the event of short exposure and at which steps must be taken by the Member States as laid down in this  Directive.  Article 2  Each Member State shall designate a body to inform the Commission and to coordinate the implementation of the harmonized procedure set out in Article 1 (1), and shall forthwith inform the Commission thereof.  Article 3  Member States shall where appropriate designate or establish measuring stations to supply the data necessary for the implementation of this Directive. The number and the location of these stations shall be determined by Member States in compliance with  Annex II.  Article 4  1. For the measurement of ozone concentrations, Member States shall use:  - either the reference method specified in Annex V,  - or any other method of analysis shown to produce measurement results equivalent to those obtained using the reference method.  To this end, each Member State shall designate one or more laboratories responsible for evaluating the method used at national level in relation to the reference method in this Directive.  Furthermore, they shall organize at national level intercomparisons between laboratories taking part in the collection and analysis of the data.  2. Once the measuring stations have been established, Member States shall provide the Commission with the following information:  - the method used to determine ozone concentrations and, if it is different from the reference method in this Directive, proof of its equivalence with the latter,  - the geographical coordinates of the measuring stations, a description of the area covered by the stations, and the site-selection criteria,  - the results of any indicative measurement programmes carried out under the provisions of Annex II, point 2.  3. The Commission may organize, on a Community scale, intercomparison programmes between laboratories referred to in paragraph 1.  Article 5  In the event of the values given in Annex I, points 3 and 4, being exceeded, the Member States shall take the necessary steps for the public to be informed (e.g. by means of radio, television and the press), in accordance with Annex IV.  Article 6  1. As from 1 January 1995, Member States shall provide the Commission with the following information no later than six months following the annual reference period:  - the maximum, the median and the 98th percentile of the mean values over one hour and eight hours recorded during the year in each measuring station; the percentiles shall be calculated in accordance with the method given in Annex III,  - the number, date and duration of periods during which the thresholds laid down in Annex I, points 1 and 2, are exceeded.  A Member State may additionally submit information based on percentile 99,9.  2. Where the information threshold laid down in Annex I, point 3, is exceeded in the course of a calendar month, Member States shall inform the Commission by the end of the following month at the latest, of:  - the date(s) of occurrence(s),  - the duration thereof,  - the maximum hourly concentration recorded during each occurrence.  3. Where the warning threshold laid down in Annex I, point 4, is exceeded in the course of a week (from Monday to the following Sunday), Member States shall inform the Commission, by the end of the following month at the latest, of:  - the date(s) of the occurrence(s),  - the duration,  - the maximum hourly concentration during each occurrence.  This information shall be supplemented by relevant data which might explain the reasons for the occurrence.  4. Where the data referred to in paragraphs 1, 2 and 3 are available in the Member States for periods preceding the date referred to in Article 9, Member States shall send them to the Commission at the latest when they send the data relating to the  first reference period. The duration of the reference period shall not exceed five years.  5. All the data referred to in paragraphs 1 to 4 shall be forwarded by the Commission to the European Environment Agency as soon as it is operational.  Article 7  The Commission shall regularly, and in any event at least once a year, evaluate the data collected under this Directive. The findings of that evaluation shall be forwarded to the Member States.  In order to coordinate actions by the Community and the Member States against photochemical pollution, the Commission shall organize, together with Member States, which shall involve the responsible body referred to in Article 2, consultations on the  problem of photochemical air pollution, relating in particular to:  - the development of ozone concentrations throughout the Member States and whether any of the episodes recorded are of a transboundary nature,  - measures and programmes planned by the Member States to reduce air pollution by ozone,  - experience and knowledge concerning the problem of photochemical pollution.  Article 8  As soon as possible and no later than the end of a four-year period following the implementation of this Directive, the Commission shall submit to the Council a report on the information collected and on the evaluation of photochemical pollution in the  Community. This report shall be accompanied by any proposals the Commission deems appropriate on the control of air pollution by ozone and, if necessary, for reducing emissions of ozone precursors.  Article 9  Member States shall bring into force the laws, regulations and administrative provisions necessary to comply with this Directive no later than 18 months after its adoption. They shall forthwith inform the Commission thereof.  When Member States adopt such provisions, they shall contain a reference to this Directive or shall be accompanied by such a reference at the time of their official publication. The procedures for making such a reference shall be laid down by the Member  States.  Article 10  This Directive is addressed to the Member States.  Done at Brussels, 21 September 1992.  For the Council The President J. GUMMER (1) OJ No C 192, 23. 7. 1991, p. 17.(2) OJ No C 150, 15. 6. 1992, p. 228.(3) OJ No C 49, 24. 12. 1992, p. 1.(4) OJ No C 328, 7. 12. 1987, p. 1.(5) OJ No L 120, 11. 5. 1990, p. 1.   ANNEX I  THRESHOLDS FOR OZONE CONCENTRATIONS IN THE AIR (*)  (The values are expressed in ìg 03/m³. The volume must be standardized at the following conditions of temperature and pressure: 293 oK and 101,3 kPa) 1. Health protection threshold 110 ìg/m³ for the mean value over eight hours (**) 2. Vegetation protection thresholds 200 ìg/m³ for the mean value over one hour 65 ìg/m³ for the mean value over 24 hours 3. Population information threshold 180 ìg/m³ for the mean value over one hour 4. Population warning threshold 360 ìg/m³ for the mean value over one hour (*) Concentrations must be measured continuously.  (**) The mean over eight hours is a non-overlapping moving average; it is calculated four times a day from the eight hourly values between 0 and 9.00, 8.00 and 17.00, 16.00 and 1.00, 12.00 and 21.00. For the information to be provided pursuant to  Article 6 (1), first indent, the mean over eight hours is a simple moving average, calculated each hour h from the eight hourly values between h and h-9.   ANNEX II  MONITORING OF OZONE CONCENTRATIONS  1. The purpose of measuring ozone concentrations in ambient air is to assess:  (i) as closely as possible the individual risk of exposure of human beings to values in excess of the health protection thresholds;  (ii) the exposure of vegetation (e.g. forests, natural ecosystems, crops, horticulture) to the values given in Annex I.  2. The measurement points must be located at geographically and climatologically representative sites where:  (i) the risk of approaching or exceeding the thresholds laid down in Annex I is the highest;  (ii) it is likely that one of the targets referred to in paragraph 1 is exposed.  At places where the Member States do not have information concerning the sites referred to in (i) and (ii), they must carry out indicative measurement programmes in order to determine the siting of the measurement points to supply the data necessary for  the implementation of this Directive.  3. Member States must establish or designate additional measurement points in order to:  (i) contribute towards the identification and description of the formation and transport of ozone and its precursors;  (ii) monitor changes in ozone concentrations in areas affected by background pollution.  Mandatory measurement of oxides of nitrogen and that recommended for volatile organic compounds be carried out in order to provide information on ozone formation, to monitor transboundary flows of volatile organic compounds and to make it possible to  identify links between the different pollutants.  4. The final reading of the ozone measurement instruments must be carried out in such a way that the mean values over one hour and eight hours can be calculated, in accordance with Annexes I and III.   ANNEX III  CALCULATION OF THE MEASUREMENT RESULTS FOR THE ANNUAL REFERENCE PERIOD  1. Concentrations must be measured continuously.  2. The annual reference period will begin on 1 January and end on 31 December in any given calendar year.  3. For the validity of the calculation of the percentiles (¹) to be recognized, 75 % of the possible values must be available and, as far as possible, distributed uniformly throughout the period in question for the particular measurement site. If that  is not the case, this fact must be mentioned when the results are communicated.  The calculation of the 50th (98th) percentile on the basis of the values recorded throughout the year must be carried out as follows: the 50th (98th) percentile must be calculated from the values actually measured. The measured values must be rounded  off to the nearest ìg/m³. All the values are to be listed in increasing order for each site:  X1& {Ì9};X2& {Ì9};X3& {Ì9};. . . .& {Ì9};Xk& {Ì9};. . . . .& {Ì9};XN-1& {Ì9};XN.  The 50th (98th) percentile is the value of k, to be calculated from the following formula:  k = 0,50(0,98)·N N being the number of values actually measured. The value of 0,50(0,98)·N must be rounded off to the nearest whole number.   ANNEX IV The following information must be circulated on a sufficiently large scale as soon as possible to enable the population concerned to take all appropriate preventive protective action. The information in question must be  communicated to the media.  List of minimum details to be supplied to the public in the event of the occurrence of high ozone levels in the air 1. Date, hour and place of the occurrence of concentrations in excess of the thresholds defined in Annex I, points 3 and 4.  2. Reference to the type(s) of Community values exceeded (information or warning).  3. Forecasts: - change in concentrations (improvement, stabilization or deterioration),  - geographical area concerned,  - duration.  4. Population concerned.  5. Precautions to be taken by the population concerned.  (1) The median must be calculated as the 50th percentile.   ANNEX V  REFERENCE METHOD OF ANALYSIS TO BE USED FOR THE PURPOSES OF THIS DIRECTIVE  The reference method of analysis to be used in the context of this Directive to determine ozone is the UV absorption method. This method is being standardized by the ISO. Once  the latter has published the standard in question, the method described therein will constitute the reference method in this Directive.  The following points must be taken into consideration when the measurement methods and instruments are used by the Member States in the field:  1. the conformity of the operating characteristics of the measurement instrument with those indicated by the manufacturer, in particular background noise, response time and linearity, must be verified initially in the laboratory and in the field;  2. the instrument must be totally calibrated regularly, using a reference UV photometer as recommended by the ISO;  3. in the field, the instruments must be calibrated regularly, e.g. every 23 or 25 hours. In addition, the validity of the calibration must be verified by regularly operating in parallel an instrument calibrated in accordance with paragraph 1.  If the instrument inlet filter is changed before calibration, calibration must be carried out after an appropriate period of exposure (from 30 minutes to several hours) of the filter to ambient ozone concentrations;  4. the sampling head must be placed at least 1 m away from vertical screens in order to avoid any screening effect;  5. the sampling head opening must be protected against rain and insects.  No prefilter is to be used;  6. sampling must not be influenced by adjoining installations (air-conditioning or data-transmission equipment);  7. the sampling line must be of inert material (e.g. glass, PTFE, stainless steel) which is not affected by the presence of ozone. It must be exposed beforehand to appropriate ozone concentrations;  8. the sampling line between the sampling head and the analysis instrument must be as short as possible. In particular, the time taken for the gas volume sample to pass through the sampling line must be as short as possible (e.g. of the order of a few  seconds in the presence of other reagents such as NO);  9. condensation in the sampling line must be avoided;  10. the sampling line must be cleaned regularly, taking local conditions into account;  11. the sampling line must be tight and the flow rate must be inspected regularly;  12. sampling must not be influenced by gas discharges from the instrument or from the calibration system;  13. all necessary precautions must be taken to prevent temperature variations from producing measurement errors.


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31993L0001

Commission Directive 93/1/EEC of 21 January 1993 amending Directive 77/535/EEC on the approximation of the laws of the Member States relating to methods of sampling and analysis for fertilizers (Analysis methods for trace elements)

Official Journal L 113 , 07/05/1993 P. 0017 - 0036 Finnish special edition: Chapter 13 Volume 24 P. 0039  Swedish special edition: Chapter 13 Volume 24 P. 0039

COMMISSION DIRECTIVE 93/1/EEC of 21 January 1993 amending Directive 77/535/EEC on the approximation of the laws of the Member States relating to methods of sampling and analysis for fertilizers (Analysis methods for trace elements)THE  COMMISSION OF THE EUROPEAN COMMUNITIES,  Having regard to the Treaty establishing the European Economic Community,  Having regard to Council Directive 76/116/EEC of 18 December 1975 on the approximation of the laws of the Member States relating to fertilizers (1), as last amended by Directive 89/530/EEC (2), and in particular Article 9 (2) thereof,  Whereas Article 8a of the Treaty establishes an area without internal frontiers in which the free movement of goods, persons, services and capital is ensured;  Whereas Directive 89/530/EEC supplements and amends Directive 76/116/EEC in respect of the trace elements boron, cobalt, copper, iron, manganese, molybdenum and zinc in fertilizers;  Whereas Commission Directive 77/535/EEC (3), as last amended by Directive 89/519/EEC (4), provides for official controls for Community fertilizers for the purpose of checking compliance with the requirements imposed by Community provisions concerning  the quality and composition of fertilizers; whereas Directive 77/535/EEC should be supplemented so that fertilizers to which Directive 89/530/EEC applies can also be checked;  Whereas, in view of the scope and effects of the proposed action, the Community measures provided for by this Directive are not only necessary but also indispensable for the attainment of the stated objectives, whereas these objectives cannot be  achieved by Member States individually, and whereas their attainment at Community level is, in fact, already provided for by Directive 76/116/EEC;  Whereas the measures provided for in this Directive are in accordance with the opinion of the Committee on the Adaptation to Technical Progress of the Directives for the Removal of Technical Barriers to Trade in Fertilizers,  HAS ADOPTED THIS DIRECTIVE:  Article 1  The text set out in the Annex to this Directive is hereby added to Annex II to Directive 77/535/EEC.  The methods are applicable to Community fertilizers for the determination of each trace element the declared content of which is less than or equal to 10 %.  Article 2  1. Member States shall bring into force the provisions necessary to comply with this Directive by 31 December 1993. They shall immediately inform the Commission thereof.  When Member States adopt these provisions, these shall contain a reference to this Directive or shall be accompanied by such reference at the time of their official publication. The procedure for such reference shall be adopted by Member States.  2. Member States shall communicate to the Commission the texts of the provisions of national law which they adopt in the field covered by this Directive.  Article 3  This Directive is addressed to the Member States.  Done at Brussels, 21 January 1993.  For the Commission Martin BANGEMANN Member of the Commission (1) OJ No L 24, 30. 1. 1976, p. 21.  (2) OJ No L 281, 30. 9. 1989, p. 116.  (3) OJ No L 213, 22. 8. 1977, p. 1.  (4) OJ No L 265, 12. 9. 1989, p. 30.    ANNEX  'Methods 9 TRACE ELEMENTS Method 9.1 EXTRACTION OF TOTAL TRACE ELEMENTS 1. SCOPE This method defines the procedure for extracting the following trace elements: total boron, total cobalt, total copper, total iron, total manganese, total molybdenum and total zinc. The aim is to carry out the minimum number of extractions, making use  wherever possible of the same extract to determine the total level of each of the trace elements listed above.  2. FIELD OF APPLICATION This procedure concerns EEC fertilizers covered by Council Directive 89/530/EEC (1) containing one or more of the following trace elements: boron, cobalt, copper, iron, manganese, molybdenum and zinc. It is applicable to each trace element the declared  content of which is less than or equal to 10 %.  3. PRINCIPLE Dissolution in boiling dilute hydrochloric acid.  Note: The extraction is empirical and may not be quantitative depending on the product or the other constituents of the fertilizer. In particular, in the case of certain manganese oxides, the quantity extracted may be substantially smaller than the  total quantity of manganese which the product contains. It is the responsibility of the fertilizer manufacturers to ensure that the declared content actually corresponds to the quantity extracted under the conditions pertaining to the method.  4. REAGENTS 4.1. Dilute hydrochloric acid (HCI) solution, about 6 M:  Mix 1 volume of hydrochloric acid (r = 1,18 g/ml) with 1 volume of water.  4.2. Concentrated ammonia solution (NH4OH, r = 0,9 g/ml) 5. APPARATUS Electric hotplate with variable temperature control.  Note: Where the boron content of an extract is to be determined, do not use borosilicate glassware. As the method involves boiling, teflon or silica is preferable. Rinse the glassware thoroughly if it has been washed in detergents containing borates.  6. PREPARATION OF THE SAMPLE See Method 1 (Directive 77/535/EEC, OJ No L 213, 22. 8. 1977, p. 1).  7. PROCEDURE 7.1. Test sample Take a quantity of fertilizer weighing between 2 and 10 g depending on the declared content of element in the product. The following table shall be used to obtain a final solution which, after appropriate dilution, will be within the measuring range for  each method. Samples should be weighed to within 1 mg.   /* Tables: see OJ */      Place the sample in a 250 ml beaker.  7.2. Preparation of the solution If necessary moisten the sample with a little water, add 10 ml of dilute hydrochloric acid (4.1) per gram of fertilizer carefully, in small amounts, then add about 50 ml of water. Cover the beaker with a watchglass and mix. Bring to the boil on the  hotplate and boil for 30 minutes. Allow to cool, stirring occasionally. Transfer quantitatively to a 250 or 500 ml volumetric flask (see Table). Make up to volume with water and mix thoroughly. Filter through a dry filter into a dry container. Discard  the first portion. The extract must be perfectly clear.  It is recommended that the determinations be carried out without delay on aliquot portions of the clear filtrate, if not the containers should be stoppered.  Remark: Extracts in which the boron content has to be determined: Adjust the pH to between 4 and 6 with concentrated ammonia (4.2).  8. DETERMINATION The determination of each trace element is to be carried out on the aliquot portions indicated in the method for each individual trace element.  If necessary, remove organic chelating or complexing substances from an aliquot portion of the extract by using Method 9.3. In the case of determination by atomic absorption spectrometry, such removal may not be necessary.  Method 9.2 EXTRACTION OF WATER-SOLUBLE TRACE ELEMENTS 1. SCOPE This method defines the procedure for extracting water-soluble forms of the following trace elements: boron, cobalt, copper, iron, manganese, molybdenum and zinc. The aim is to carry out the minimum number of extractions,making use wherever possible of  the same extract to determine the level of each of the trace elements listed above.  2. FIELD OF APPLICATION This procedure concerns EEC fertilizers covered by Directive 89/530/EEC containing one or more of the following trace elements: boron, cobalt, copper, iron, manganese, molybdenum and zinc. It is applicable to each trace element the declared content of  which is less than or equal to 10 %.  3. PRINCIPLE The trace elements are extracted by shaking the fertilizer in water at 20 °C ± 2 °C.  Note: The extraction is empirical and may or may not be quantitative.  4. REAGENTS 4.1. Dilute hydrochloric acid (HCI) solution, about 6 M:  Mix 1 volume of hydrochloric acid (r = 1,18 g/ml) with 1 volume of water.  5. APPARATUS 5.1. Rotary shaker set at about 35 to 40 rpm.  5.2. pH-meter.  Note: Where the boron content of the extract is to be determined, do not use borosilicate glassware. Teflon or silica is preferable for this extraction. Rinse the glassware thoroughly if it has been washed in detergents containing borates.  6. PREPARATION OF THE SAMPLE See Method 1 (Directive 77/535/EEC, (OJ No L 213, 22. 8. 1977, P. 1)).  7. PROCEDURE 7.1. Test sample Take a quantity of fertilizer weighing between 2 and 10 g depending on the declared content of the element in the product. The following table shall be used to obtain a final solution which, after appropriate dilution, will be within the measuring range  for each method. The samples should be weighed to within 1 mg.   /* Tables: see OJ */      Place the sample in a 250 or 500 ml flask (according to the Table).  7.2. Preparation of the solution Add about 200 ml of water to the 250 ml flask or 400 ml of water to the 500 ml flask.  Stopper the flask well. Shake vigorously by hand to disperse the sample, then place the flask on the shaker and shake for 30 minutes.  Make up to volume with water and mix thoroughly.  7.3. Preparation of the test solution Filter immediately into a clean, dry flask. Stopper the flask. Carry out the determination immediately after filtering.  NB: If the filtrate gradually becomes cloudy, make another extraction following 7.1 and 7.2 in a flask of volume Ve. Filter into a calibrated flask of volume W which has previously been dried and has received 5,00 ml of dilute hydrochloric acid (4.1).  Stop the filtration at the exact moment when the calibration mark is reached. Mix thoroughly.  Under these conditions the value of V in the expression of results is:  V = Ve × W / (W 5).  The dilutions in the expression of results depend on this value of V.  8. DETERMINATION The determination of each trace element is carried out on the aliquot portions indicated in the method for each individual trace element.  If necessary, remove organic chelating or complexing substances from an aliquot portion by using Method 9.3. In the case of determination by atomic absorption spectrometry, such removal may not be necessary.  Method 9.3 REMOVAL OF ORGANIC COMPOUNDS FROM FERTILIZER EXTRACTS 1. SCOPE This method defines a procedure for removing organic compounds from fertilizer extracts.  2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 9.1 and 9.2 for which a declaration of total and/or water-soluble element is required by Directive 89/530/EEC.  Note: The presence of small quantities of organic matter usually does not affect determinations by means of atomic absorption spectrometry.  3. PRINCIPLE The organic compounds in an aliquot portion of the extract are oxidized with hydrogen peroxide.  4. REAGENTS 4.1. Dilute hydrochloric acid (HCI) solution, about 0,5 M:  Mix 1 volume of hydrochloric acid (r = 1,18 g/ml) with 20 volumes of water.  4.2. Hydrogen peroxide solution (30 % H2O2, r = 1,11 g/ml), free from trace elements 5. APPARATUS Electric hotplate with variable temperature control.  6. PROCEDURE Take 25 ml of the extract solution obtained by Method 9.1 or Method 9.2 and place in a 100 ml beaker. In the case of Method 9.2, add 5 ml of the dilute hydrochloric acid solution (4.1). Then add 5 ml of the hydrogen peroxide solution (4.2). Cover with a  watchglass. Allow oxidation to occur at room temperature for about one hour, then bring gradually to boiling and boil for half an hour. If necessary, add a further 5 ml of the hydrogen peroxide to the solution once it has cooled. Then boil to remove the  excess hydrogen peroxide. Allow to cool and transfer quantitatively to a 50 ml volumetric flask and make up to volume. Filter where necessary.  Account should be taken of this dilution when taking aliquot portions and calculating the percentage of trace element in the product.  Method 9.4 DETERMINATION OF TRACE ELEMENTS IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY (GENERAL PROCEDURE) 1. SCOPE This document defines a general procedure for determining the levels of certain trace elements in fertilizer extracts by atomic absorption spectrometry.  2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 9.1 and 9.2 for which a declaration of total and/or water-soluble element is required by Directive 89/530/EEC.  Adaptations of this procedure for the various trace elements are detailed in the methods defined specifically for each element.  Note: In most cases the presence of small quantities of organic matter will not affect determinations by atomic absorption spectrometry.  3. PRINCIPLE After the extract has been treated where necessary to reduce or eliminate interfering chemical species, the extract is diluted so that its concentration is in the optimum range of the spectrometer at a wavelength suitable for the trace element to be  determined.  4. REAGENTS 4.1. Dilute hydrochloric acid solution (HCI), about 6 M:  Mix one volume of hydrochloric acid (r = 1,18 g/ml) with 1 volume of water.  4.2. Dilute hydrochloric acid solution (HCI), about 0,5 M:  Mix one volume of hydrochloric acid (r = 1,18 g/ml) with 20 volumes of water.  4.3. Lanthanum salt solutions (10 g of La per litre).  This reagent is used for determinations of cobalt, iron, manganese and zinc. It can be prepared either:  (a) with lanthanum oxide dissolved in hydrochloric acid (4.1). Place 11,73 g of lanthanum oxide (La2O3) in 150 ml of water in a 1 litre volumetric flask and add 120 ml of 6 M hydrochloric acid (4.1). Allow to dissolve and then make up to 1 litre with  water and mix thoroughly. This solution is approximately 0,5 M in hydrochloric acid; or (b) with solutions of lanthanum chloride, sulphate or nitrate. Dissolve 26,7 g of lanthanum chloride heptahydrate (LaCl3 7H2O) or 31,2 g of lanthanum nitrate hexahydrate [La(NO3)3 6H2O] or 26,2 g of lanthanum sulphate nonahydrate (La2(SO4)3 9H2O] in 150  ml of water, then add 85 ml of 6 M hydrochloric acid (4.1). Allow to dissolve and then make up to 1 litre with water. Mix thoroughly. This solution is approximately 0,5 M in hydrochloric acid.  4.4. Calibration solutions For the preparation of these, see the individual determination method for each trace element.  5. APPARATUS Atomic absorption spectrometer fitted with sources emitting radiation characteristic of the trace elements to be determined.  The analyst must follow the manufacturer's instructions and be familiar with the apparatus. The apparatus must allow background correction so that it can be used whenever necessary (Co and Zn). The gases to be used are air and acetylene.  6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Preparation of extract solutions of the trace elements to be determined See Method 9.1 and/or 9.2 and, if appropriate, 9.3.  6.2. Treatment of the test solution Dilute an aliquot portion of the extract obtained by Method 9.1, 9.2 or 9.3 with water and/or hydrochloric acid (4.1) or (4.2) so as to obtain, in the final solution for measurement, a concentration of the element to be determined that is appropriate to  the calibration range used (7.2) and a hydrochloric acid concentration of at least 0,5 M and not more than 2,5 M. This operation may require one or more successive dilutions.  Take an aliquot portion of the final solution obtained by dilution of the extract, let (a) be its volume in ml, and pour into a 100 ml volumetric flask. When determining the cobalt, iron, manganese or zinc content, add 10 ml of the lanthanum salt  solution (4.3). Make up to volume with the 0,5 M hydrochloric acid solution (4.2) and mix thoroughly. This is the final solution for measurement. Let D be the dilution factor.  7. PROCEDURE 7.1. Preparation of a blank solution Prepare a blank solution by repeating the whole procedure from the extraction stage, omitting only the test sample of fertilizer.  7.2. Preparation of calibration solutions From the working calibration solution prepared using the method given for each individual trace element, prepare in 100 ml volumetric flasks a series of at least five calibration solutions of increasing concentration within the optimum measuring range  of the spectrometer. If necessary, adjust the concentration of hydrochloric acid to bring it as close as possible to that of the diluted test solution (6.2). For determining cobalt, iron, manganese or zinc add 10 ml of the same lanthanum salt solution  (4.3) as used in 6.2. Make up to volume with the 0,5 M hydrochloric acid solution (4.2) and mix thoroughly.  7.3. Determination Prepare the spectrometer (5) for the determination and adjust to the wavelength given in the method for the individual trace element concerned.  Spray three times in succession the calibration solutions (7.2), the test solution (6.2) and the blank solution (7.1), noting each result and flushing the instrument with distilled water between individual sprayings.  Construct the calibration curve by plotting the average spectrometer reading for each calibration solution (7.2) along the ordinate and the corresponding concentration of the element, expressed in mg/ml, along the abscissa.  From this curve, determine the concentrations of the relevant trace element in the test solution xs (6.2) and in the blank solution xb (7.1), expressing these concentrations in mg per ml.  8. EXPRESSION OF RESULTS The percentage of trace element (E) in the fertilizer is equal to:  E (%) = [(xs   xb) × V × D] / (M × 104).  If method (9.3) has been used:  E (%) = [(xs   xb) × V ×2D] / (M × 104),  where:  E is the amount of the trace element determind, expressed as a percentage of the fertilizer;  xs is the concentration of the test solution (6.2), in mg/ml;  xb is the concentration of the blank solution (7.1), in mg/ml;  V is the volume of the extract obtained by Method 9.1 or 9.2, in ml;  D is the factor corresponding to the dilution carried out in (6.2);  M is the mass of the test sample taken in accordance with Method 9.1 or 9.2, in grams.  Calculation of dilution factor D:  If (a1), (a2), (a3), ., ., ., (ai) and (a) are the aliquot portions and (v1), (v2), (v3), ., ., ., (vi) and (100) are the volumes in ml corresponding to their respective dilutions, the dilution factor D will be equal to:  D = (v1/a1) × (v2/a2) × (v3/a3) × . × . × . × (vi/ai) × (100/a).  Method 9.5 DETERMINATION OF BORON IN FERTILIZER EXTRACTS BY MEANS OF SPECTROPHOTOMETRY WITH AZOMETHINE-H 1. SCOPE This method describes a procedure for determining boron in fertilizer extracts.  2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 9.1 and 9.2 for which a declaration of total and/or water-soluble boron is required by Directive 89/530/EEC.  3. PRINCIPLE In an azomethine-H solution, borate ions form a yellow complex the concentration of which is determined by molecular absorption spectrometry at 410 nm. Interfering ions are masked with EDTA.  4. REAGENTS 4.1. EDTA buffer solution Place in a 500 ml volumetric flask containing 300 ml of water:  - 75 g of ammonium acetate (NH4OOCCH3);  - 10 g of disodium salt of ethylene diamine tetraacetic acid (Na2EDTA);  - 40 ml of acetic acid (CH3COOH, r = 1,05 g/ml).  Make up to volume with water and mix thoroughly. The pH of the solution, checked by means of a glass electrode, must be 4,8 ± 0,1.  4.2. Azomethine-H solution Place in a 200 ml volumetric flask - 10 ml of the buffer solution (4.1);  - 400 mg of azomethine-H (C17H12NNaO8S2);  - 2 g of asorbic acid (C6H8O6).  Make up to volume and mix thoroughly. Do not prepare large quantities of this reagent as it is stable for only a few days.  4.3. Boron calibration solutions 4.3.1. Boron stock solution (100 mg/ml) Dissolve 0,5719 g of boric acid (H3B03) in water in a 1 000 ml volumetric flask. Make up to volume with water and mix thoroughly. Transfer to a plastic bottle for storage in a refrigerator.  4.3.2. Boron working solution (10 mg/ml) Place 50 ml of stock solution (4.3.1) in a 500 ml volumetric flask. Make up to volume with water and mix thoroughly.  5. APPARATUS Spectrometer fitted for molecular absorption with cells having a 10 mm optical path and set to a wavelength of 410 nm.  6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Preparation of the boron solution See Methods 9.1 and/or 9.2 and, if appropriate, 9.3.  6.2. Preparation of the test solution Dilute an aliquot portion of extract (6.1) to obtain a boron concentration as specified in 7.2. Two successive dilutions may be necessary. Let D be the dilution factor.  6.3. Preparation of the correction solution If the test solution (6.2) is coloured, prepare a corresponding correction solution by placing in a plastic flask 5 ml of test solution (6.2), 5 ml of EDTA buffer solution (4.1) and 5 ml of water and mix thoroughly.  7. PROCEDURE 7.1. Preparation of the blank solution Prepare a blank solution by repeating the whole procedure from the extraction stage, omitting only the test sample of fertilizer.  7.2. Preparation of the calibration solutions Transfer 0, 5, 10, 15, 20 and 25 ml of the working calibration solution (4.3.2) to a series of 100 ml volumetric flasks. Make up to 100 ml with water and mix thoroughly. These solutions contain between 0 and 2,5 mg/ml of boron.  7.3. Colour development Transfer 5 ml of the calibration solutions (7.2), test solutions (6.2) and blank (7.1) to a series of plastic flasks. Add 5 ml of the EDTA buffer solution (4.1). Add 5 ml of the azomethine-H solution (4.2).  Mix thoroughly and allow the colour to develop in the dark for 2 1/2 to three hours.  7.4. Determination Measure the absorbance of the solutions obtained at 7.3 and if appropriate the correction solution (6.3) against water at a wavelength of 410 nm. Rinse the cells with water before each new reading.  8. EXPRESSION OF RESULTS Plot a calibration curve of the concentration of the calibration solutions (7.2) along the abscissa and the absorbance given by the spectrophotometer (7.4) along the ordinate.  Read off the calibration curve the concentration of boron in the blank (7.1), the concentration of boron in the test solution (6.2) and, if the test solution is coloured, the corrected concentration of the test solution. To calculate the latter,  subtract the absorbance of the correction solution (6.3) from the absorbance of the test solution (6.2) and determine the corrected concentration of the test solution. Note the concentration of the test solution (6.2), with or without correction, X(xs)  and of the blank (xb).  The percentage of boron in the fertilizer is given by:  B % = [(xs   xb) × V × D] / (M ×104) If Method 9.3 is used:  B % = [(xs  xb) × V × 2D] / (M × 104) where:  B is the quantity of boron expressed as a percentage of the fertilizer;  xs is the concentration (mg/ml) in the test solution (6.2), with or without correction;  xb is the concentration (mg/ml) in the blank (7.1);  V is the volume in ml of extract obtained in accordance with Method 9.1 or 9.2;  D is the factor corresponding to the dilution carried out in 6.2;  M is the mass in grams of the test sample taken in accordance with Method 9.1 or 9.2.  Calculation of the dilution factor D: if (a1) and (a2) are succesive aliquot portions and (v1) and (v2) are the volumes corresponding to their respective dilutions, the dilution factor D is given by:  D = (v1/a1) × (v2/a2).  Method 9.6 DETERMINATION OF COBALT IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY 1. SCOPE This method describes a procedure for determining cobalt in fertilizer extracts.  2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 9.1 and 9.2 for which a declaration of total and/or water-soluble cobalt is required by Directive 89/530/EEC.  3. PRINCIPLE After suitable treatment and dilution of the extracts, the cobalt content is determined by atomic absorption spectrometry.  4. REAGENTS4.1. Hydrochloric acid solution, about 6 M.  See Method 9.4 (4.1).  4.2. Hydrochloric acid solution, about 0,5 M.  See Method 9.4 (4.2).  4.3. Lanthanum salt solutions (10 g of La per litre) See Method 9.4 (4.3).  4.4. Cobalt calibration solutions 4.4.1. Cobalt stock solution (1 000 mg/ml) In a 250 ml beaker, weigh to the nearest 0,1 mg, 1 g of cobalt, add 25 ml of 6 M hydrochloric acid (4.1) and heat on a hotplate until the cobalt is completely dissolved. When cool, transfer quantitatively to a 1 000 ml volumetric flask. Make up to  volume with water and mix thoroughly.  4.4.2. Cobalt working solution (100 mg/ml) Place 10 ml of the stock solution (4.4.1) in a 100 ml volumetric flask. Make up to volume with 0,5 M hydrochloric acid solution (4.2) and mix thoroughly.  5. APPARATUS Atomic absorption spectrometer: see Method 9.4, (5). The instrument must be equipped with a source of rays characteristic of cobalt (240,7 nm). The spectrometer must allow background correction to be made.  6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Cobalt extract solution See Methods 9.1 and/or 9.2 and, if appropriate, 9.3.  6.2. Preparation of the test solution See Method 9.4 (6.2). The test solution must contain 10 % (v/v) of a lanthanum salt solution (4.3).  7. PROCEDURE 7.1. Preparation of blank solution See Method 9.4 (7.1). The blank must contain 10 % (v/v) of the lanthanum salt solution used in 6.2.  7.2. Preparation of calibration solutions See Method 9.4 (7.2).  For an optimum determination range of 0 to 5 mg/ml of cobalt, place 0, 0,5, 1, 2, 3, 4 and 5 ml respectively of working solution (4.4.2) in a series of 100 ml volumetric flasks. If necessary adjust the hydrochloric acid concentration as closely as  possible to that of the test solution. Add to each flask 10 ml of the lanthanum salt solution used in 6.2. Make up to 100 ml with 0,5 M hydrochloric acid solution (4.2) and mix thoroughly. These solutions contain 0, 0,5, 1, 2, 3, 4 and 5 mg/ml  respectively of cobalt.  7.3. Determination See Method 9.4 (7.3). Prepare the spectrometer (5) for measurement at a wavelength of 240,7 nm.  8. EXPRESSION OF RESULTS See Method 9.4 (8).  The percentage of cobalt in the fertilizer is given by:  Co % = [(xs   xb) × V × D] / (M ×104) If Method 9.3 is used:  Co % = [(xs   xb) × V × 2D] / (M × 104) where:  Co is the quantity of cobalt expressed as a percentage of the fertilizer;  xs is the concentration in mg/ml of the test solution (6.2);  xb is the concentration in mg/ml of the blank solution (7.1);  V is the volume in ml of extract obtained in accordance with Method 9.1 or 9.2;  D is the factor corresponding to the dilution carried out in 6.2;  M is the mass in grams of the test sample taken in accordance with Method 9.1 or 9.2.  Calculation of the dilution factor D: if (a1), (a2), (a3), ., ., ., (ai) and (a) are aliquot portions and (v1), (v2), (v3), ., ., ., (vi) and (100) are the volumes in ml corresponding to their respective dilutions, the dilution factor D is given by:  D = (v1/a1) × (v2/a2) × (v3/a3) ×.×.×.×. × (vi/ai) × (100/a).  Method 9.7 DETERMINATION OF COPPER IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY 1. SCOPE This method describes a procedure for determining copper in fertilizer extracts.  2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 9.1 and 9.2 for which a declaration of total and/or water-soluble copper is required by Directive 89/530/EEC.  3. PRINCIPLE After suitable treatment and dilution of the extracts, the copper content is determined by atomic absorption spectrometry.  4. REAGENTS 4.1. Hydrochloric acid solution, about 6 M See Method 9.4, (4.1).  4.2. Hydrochloric acid solution, about 0,5 M See Method 9.4, (4.2).  4.3. Hydrogen peroxide solution (30 % H2O, r = 1,11 g/ml), free from trace elements.  4.4. Copper calibration solutions 4.4.1. Copper stock solution (1 000 mg/ml) In a 250 ml beaker weigh to the nearest 0,1 mg, 1g of copper, add 25 ml of 6M hydrochloric acid (4.1) add 5 ml hydrogen peroxide solution (4.3) and heat on a hotplate until the copper is completely dissolved. Transfer quantiatively to a 1 000 ml  volumetric flask. Make up to volume with water and mix thoroughly.  4.4.2. Copper working solution (100 mg/ml) Place 20 ml of the stock solution (4.4.1) in a 200 ml volumetric flask. Make up to volume with 0,5 M hydrochloric acid solution (4.2) and mix thoroughly.  5. APPARATUS Spectrometer equipped for atomic absorption: see Method 9.4 (5). The instrument must be fitted with a source of rays characteristics of copper (324,8 nm).  6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Copper extract solution See Methods 9.1 and/or 9.2 and, if appropriate, 9.3.  6.2. Preparation of the test solution See Method 9.4, (6.2).  7. PROCEDURE 7.1. Preparation of blank solution See Method 9.4, (7.1).  7.2. Preparation of calibration solutions See Method 9.4, (7.2).  For an optimum determination range of 0 to 5 mg/ml of copper, place 0, 0,5, 1, 2, 3, 4 and 5 ml respectively of working solution (4.4.2) in a series of 100 ml volumetric flasks. If necessary adjust the hydrochloric acid concentration as closely as  possible to that of the test solution (6.2). Make up to 100 ml with 0,5 M hydrochloric acid solution (4.2) and mix thoroughly. These solutions contain 0, 0,5, 1, 2, 3, 4 and 5 mg/ml respectively of copper.  7.3. Determination See Method 9.4, (7.3). Prepare the spectrometer (5) for measurement at a wavelength of 324,8 nm.  8. EXPRESSION OF RESULTS See Method 9.4, (8).  The percentage of copper in the fertilizer is given by:  Cu % = [(xs   xb) × V × D] / (M ×104) If Method 9.3 is used:  Cu % = [(xs   xb) × V × 2D] / (M × 104) where:  Cu is the quantity of copper expressed as a percentage of the fertilizer;  xs is the concentration in mg/ml of the test solution (6.2);  Xb is the concentration in mg/ml of the blank solution (7.1);  V is the volume in ml of extract obtained in accordance with Method 9.1 or 9.2;  D is the factor of the dilution carried out in 6.2;  M is the mass in grams of the test sample taken in accordance with Method 9.1 or 9.2.  Calculation of the dilution factor D: if (a1), (a2), (a3) ., ., ., (ai) and (a) are aliquot portions and (v1), (v2), (v3), ., ., ., (vi) and (100) are the volumes in ml corresponding to their respective dilutions, the dilution factor D is given by:  D = (v1/a1) × (v2/a2) × (v3/a3) ×. ×. ×. × (vi/ai) × (100/a) Method 9.8 DETERMINATION OF IRON IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY 1. SCOPE This method describes a procedure for determining iron in fertilizer extracts.  2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 9.1 and 9.2 for which a declaration of total and/or water-soluble iron is required by Directive 89/530/EEC.  3. PRINCIPLE After suitable treatment and dilution of the extract, the iron content is determined by atomic absorption spectrometry.  4. REAGENTS 4.1. Hydrochloric acid solution, about 6 M See Method 9.4 (4.1).  4.2. Hydrochloric acid solution, about 0,5 M See Method 9.4 (4.2).  4.3. Hydrogen peroxide solution (30 % H2O2, r = 1,11 g/ml) free from trace elements.  4.4. Lanthanum salt solutions (10 g of La per litre) See Method 9.4, (4.3).  4.5. Iron calibration solutions 4.5.1. Iron stock solution (1 000 mg/ml) In a 500 ml beaker, weigh to the nearest 0,1 mg, 1 g of pure iron wire, add 200 ml of 6 M hydrochloric acid (4.1) and 15 ml of hydrogen peroxide solution (4.3). Heat on a hotplate until the iron is completely dissolved. When cool, transfer  quantitatively to a 1 000 ml volumetric flask. Make up to volume with water and mix thoroughly.  4.5.2. Iron working solution (100 mg/ml) Place 20 ml of the stock solution (4.5.1) in a 200 ml volumetric flask. Make up to volume with the 0,5 M hydrochloric acid solution (4.2) and mix thoroughly.  5. APPARATUS Atomic absorption spectrometer: see Method 9.4 (5). The instrument must be fitted with a source of rays characteristic of iron (248,3 nm).  6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Iron extract solution See Methods 9.1 and/or 9.2 and, if appropriate, 9.3.  6.2. Preparation of the test solution See Method 9.4 (6.2). The test solution must contain 10 % (v/v) of a lanthanum salt solution.  7. PROCEDURE 7.1. Preparation of blank solution See Method 9.4 (7.1). The test solution must contain 10 % (v/v) of the lanthanum salt solution used in 6.2.  7.2. Preparation of calibration solutions See Method 9.4 (7.2).  For an optimum determination range of 0 to 10 mg/ml of iron, place 0, 2, 4, 6, 8 and 10 ml respectively of working solution (4.5.2) in a series of 100 ml volumetric flasks. If necessary adjust the hydrochloric acid concentration as closely as possible  to that of the test solution. Add 10 ml of the lanthanum salt solution used in 6.2. Make up to volume with 0,5 M hydrochloric solution (4.2) and mix thoroughly. These solutions contain 0, 2, 4, 6, 8 and 10 mg/ml respectively of iron.  7.3. Determination See Method 9.4 (7.3). Prepare the spectrometer (5) for measurement at a wavelength of 248,3 nm.  8. EXPRESSION OF RESULTS See Method 9.4 (8).  The percentage of iron in the fertilizer is given by:  Fe % = [(xs  xb) × V × D)] / (M × 104) If Method 9.3 is used:  Fe % = [(xs  xb) × V × 2D)] / (M × 104) where:  Fe is the quantity of iron expressed as a percentage of the fertilizer;  xs is the concentration in mg/ml of the test solution (6.2);  xb is the concentration in mg/ml of the blank solution (7.1);  V is the volume in ml of extract obtained in accordance with Method 9.1 or 9.2;  D is the factor of the dilution carried out in 6.2;  M is the mass in grams of the test sample taken in accordance with Method 9.1 or 9.2.  Calculation of the dilution factor D: if (a1), (a2), (a3), ., ., ., (ai) and (a) are aliquot portions and (v1), (v2), (v3), ., ., ., (vi) and (100) are the volumes in ml corresponding to their respective dilutions, the dilution factor D is given by:  D = (v1/a1) × (v2/a2) × (v3/a3) ×. ×. ×. × (vi/ai) × (100/a).  Method 9.9 DETERMINATION OF MANGANESE IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY 1. SCOPE This method describes a procedure for determining manganese in fertilizer extracts.  2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 9.1 and 9.2 for which a declaration of total and/or water-soluble manganese is required by Directive 89/530/EEC.  3. PRINCIPLE After suitable treatment and dilution of the extracts, the manganese level is determined by atomic absorption spectrometry.  4. REAGENTS 4.1. Hydrochloric acid solution, about 6 M See Method 9.4, (4.1).  4.2. Hydrochloric acid solution, about 0,5 M See Method 9.4, (4.2).  4.3. Lanthanum salt solutions (10 g of La per litre) See Method 9.4, (4.3).  4.4. Manganese calibration solutions 4.4.1. Manganese stock solution (1 000 mg/ml) In a 250 ml beaker, weigh to the nearest 0,1 mg, 1 g of manganese, add 25 ml of 6 M hydrochloric acid solution (4.1). Heat on a hotplate until the manganese is completely dissolved. When cool, transfer quantitatively to a 1 000 ml volumetric flask. Make  up to volume with water and mix thoroughly.  4.4.2. Manganese working solution (100 mg/ml) Dilute 20 ml of the stock solution (4.4.1) in the 0,5 M hydrochloric acid solution (4.2) in a 200 ml volumetric flask. Make up to volume with the 0,5 M hydrochloric acid solution (4.2) and mix thoroughly.  5. APPARATUS Atomic absorption spectrometer: see Method 9.4 (5). The apparatus must be fitted with a source of lines characteristic of manganese (279,6 nm).  6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Manganese extract solution See Methods 9.1 and/or 9.2 and, if appropriate, 9.3.  6.2. Preparation of the test solution See Method 9.4, (6.2). The test solution must contain 10 % by volume of lanthanum salt solution (4.3).  7. PROCEDURE 7.1. Preparation of the blank solution See Method 9.4 (7.1). The blank solution must contain 10 % by volume of the lanthanum salt solution used in 6.2.  7.2. Preparation of the calibration solutions See Method 9.4 (7.2).  For an optimum interval of 0 to 5 mg/ml manganese, place 0, 0,5, 1, 2, 3, 4 and 5 ml, respectively, of the working solution (4.4.2) in a series of 100 ml volumetric flasks. Where necessary, adjust the hydrochloric acid concentration to bring it as close  as possible to that of the test solution. To each flask add 10 ml of the lanthanum salt solution used in 6.2. Make up to 100 ml with the 0,5 M hydrochloric acid solution (4.2) and mix thoroughly. These solutions contain 0, 0,5, 1, 2, 3, 4 and 5 mg/ml  manganese respectively.  7.3. Determination See Method 9.4 (7.3). Prepare the spectrometer (5) for measurements at a wavelength of 279,6 nm.  8. EXPRESSION OF RESULTS See Method 9.4 (8).  The percentage of manganese in the fertilizer is as follows:  Mn % = [(xs   xb) × V × D] / (M × 104) If Method 9.3 has been used:  Mn % = [(xs   xb) × V × 2D] / (M × 104) where:  Mn is the quantity of manganese expressed as a percentage of the fertilizer;  xs is the concentration in mg/ml of the test solution (6.2);  xb is the concentration in mg/ml of the blank solution (7.1);  V is the volume in ml of the extract obtained using Method 9.1 or 9.2;  D is the factor corresponding to the dilution performed in 6.2;  M is the mass in g of the test sample taken using Method 9.1 or 9.2.  Calculation of dilution factor D: where (a1), (a2), (a3), ., ., ., (ai) and (a) are aliquot portions and (v1), (v2), (v3), ., ., ., (vi) and (100) the volumes in ml corresponding to their respective dilutions, dilution factor D will be equal to:  D = (v1/a1) × (v2/a2) × (v3/a3) ×. ×. ×. × (vi/ai) × (100/a).  Method 9.10 DETERMINATION OF MOYLBDENUM IN FERTILIZER EXTRACTS BY SPECTOPHOTOMETRY OF A COMPLEX WITH AMMONIUM THIOCYANATE 1. SCOPE This method describes a procedure for determining molybdenum in fertilizer extracts.  2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 9.1 and 9.2 for which a declaration of total and/or water-soluble molybdenum is required by Directive 89/530/EEC.  3. PRINCIPLE Molybdenum (V) forms a complex [MoO(SCN)5]- - in an acid medium with SCN - ions.  The complex is extracted with n-butyl acetate. Interfering ions such as those of iron remain in the aqueous phase. The yellow-orange colour is determined by molecular absorption spectrometry at 470 nm.  4. REAGENTS 4.1. Dilute hydrochloric acid solution (HCl), about 6 M See method 9.4 (4.1).  4.2. Copper solution (70 mg/l) in 1,5 M hydrochloric acid Dissolve 275 mg of copper sulphate (CuSO4 5H2O) weighed to within 0,1 mg in 250 ml of the 6 M hydrochloric acid solution (4.1) in a 1 000 ml volumetric flask. Make up to volume with water and mix thoroughly.  4.3. Ascorbic acid solution (50 g/l) Dissolve 50 g of ascorbic acid (C6H8O6) in water in a 1 000 ml volumetric flask. Make up to volume with water, mix thoroughly and keep in a refrigerator.  4.4. n-butyl acetate 4.5. Ammonium thiocyanate solution, 0,2 M Dissolve 15,224 g of NH4SCN in water in a 1 000 ml volumetric flask. Make up to volume with water; mix thoroughly and store in a dark-coloured bottle.  4.6. Stannous chloride solution (50 g/l) in 2 M hydrochloric acid This solution must be perfectly clear and prepared immediately before use. Very pure stannous chloride must be used otherwise the solution will not be clear.  To prepare 100 ml of solution, dissolve 5 g of (SnCl22H2O) in 35 ml of 6 M HCl solution (4.1). Add 10 ml of the copper solution (4.2). Make up to volume with water and mix thoroughly.  4.7. Molybdenum calibration solutions 4.7.1. Molybdenum stock solution (500 mg/ml) Dissolve 0,920 g of ammonium molybdate [(NH4)6Mo7O24 4H2O] weighed to within 0,1 mg in the 6 M hydrochloric acid (4.1) in a 1 000 ml volumetric flask. Make up to volume with that solution and mix thoroughly.  4.7.2. Molybdenum intermediate solution (25 mg/ml) Place 25 ml of the stock solution (4.7.1) in a 500 ml volumetric flask. Make up to volume with 6 M hydrochloric acid (4.1) and mix thoroughly.  4.7.3. Molybdenum working solution (2,5 mg/ml) Place 10 ml of the intermediate solution (4.7.2) in a 100 ml volumetric flask. Make up to volume with 6 M hydrochloric acid (4.1) and mix thoroughly.  5. APPARATUS 5.1. Spectrometer fitted for molecular absorption with cuvettes having a 20 mm optical path and set to a wavelength of 470 nm.  5.2. 200 or 250 ml separating funnels.  6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Molybdenum extract solution See Methods 9.1 and/or 9.2 and, if appropriate, 9.3.  6.2. Preparation of the test solution Dilute an aliquot portion of the extract (6.1) with 6 M hydrochloric acid solution (4.1) so as to obtain an appropriate molybdenum concentration. Let D be the dilution factor.  Take an aliquot portion (a) from the extract solution containing 1 to 12 mg molybdenum and place it in the separating funnel (5.2). Make up to 50 ml with the 6 M hydrochloric acid solution (4.1).  7. PROCEDURE 7.1. Preparation of the blank solution Prepare a blank solution by repeating the whole procedure from the extraction stage, omitting only the test sample of fertilizer.  7.2. Preparation of the series of calibration solutions Prepare a series of at least six calibration solutions of increasing concentration corresponding to the optimum response range of the spectrometer.  For the interval 0-12,5 mg molybdenum, place 0, 1, 2, 3, 4 and 5 ml, respectively, of the working solution (4.7.3) in the separating funnels (5.2). Make up to 50 ml with 6 M hydrochloric acid (4.1). The funnels contain, respectively, 0, 2,5, 5, 7,5, 10  and 12,5 mg molybdenum.  7.3. Development and separation of the complex To each separating funnel (6.2, 7.1 and 7.2), add in the following order:  - 10 ml of the copper solution (4.2) - 20 ml of the ascorbic acid solution (4.3);  mix thoroughly and wait for two or three minutes. Then add:  - 10 ml of n-butyl acetate (4.4), using a precision pipette;  - 20 ml of the thiocyanate solution (4.5).  Shake for one minute to extract the complex in the organic phase; allow to precipitate; after the separation of the two phases, draw off the entire aqueous phase and discard it; then wash the organic phase with:  -10 ml of the stannous chloride solution (4.6).  Shake for one minute. Allow to precipitate and draw off the entire aqueous phase. Collect the organic phase in a test tube; this will make it possible to collect the drops of water in suspension.  7.4. Determination Measure the absorbencies of the solutions obtained at 7.3 at a wavelength of 470 nm using the 0 mg/ml molybdenum calibration solution (7.2) as a reference.  8. EXPRESSION OF RESULTS Construct the calibration curve by plotting the corresponding masses of molybdenum in the calibration solutions (7.2) expressed in mg along the abscissa and the corresponding values of the absorbancies (7.4) given by the spectrometer reading along the  ordinate.  From this curve determine the mass of molybdenum in the test solution (6.2) and the blank solution (7.1). These masses are designated (x5) and (xb) respectively.  The percentage of molybdenum in the fertilizer is: Mo % = [(xs   xb) × V/a × D] / (M × 104) If Method 9.3 has been used:  Mo % = [(xs   xb) × V/a × 2D] / (M × 104) where:  Mo is the quantity of molybdenum expressed as a percentage of the fertilizer;  a is the volume in ml of the aliquot taken from the last dilute solution (6.2);  xs is the Mo mass in mg in the test solution (6.2);  xb is the Mo mass in mg in the blank solution (7.1) the volume of which corresponds to the volume (a) of the aliquot of the test solution (6.2);  V is the volume in ml of the extract solution obtained in accordance with Method 9.1 or 9.2;  D is the factor corresponding to the dilution performed in 6.2;  M is the mass in g of the test sample taken in accordance with Method 9.1 or 9.2.  Calculation of the dilution factor D: where (a1), (a2) are successive aliquot portions and (v1), (v2) are the volumes corresponding to their respective dilutions, the dilution factor D will be:  D = (v1/a1) × (v2/a2).  Method 9.11 DETERMINATION OF ZINC IN FERTILIZER EXTRACTS BY ATOMIC ABSORPTION SPECTROMETRY 1. SCOPE This method describes a procedure for determining zinc in fertilizer extracts.  2. FIELD OF APPLICATION This procedure is applicable to analysing samples of fertilizers extracted by Methods 9.1 and 9.2 for which a declaration of total and/or water-soluble zinc is required by Directive 89/530/EEC.  3. PRINCIPLE After suitable treatment and dilution of the extracts, the zinc level is determined by atomic absorption spectrometry.  4. REAGENTS 4.1. Hydrochloric acid solution, about 6 M See Method 9.4 (4.1).  4.2. Hydrochloric acid solution, about 0,5 M See Method 9.4 (4.2).  4.3. Lanthanum salt solutions (10 g of La per litre) See Method 9.4 (4.3).  4.4. Zinc calibration solutions 4.4.1. Zinc stock solution (1 000 mg/ml) In a 1 000 ml volumetric flask dissolve 1 g of zinc powder or flakes weighed to within 0,1 mg in 25 ml of 6 M hydrochloric acid (4.1). When completely dissolved, make up to volume with water and mix thoroughly.  4.4.2. Zinc working solution (100 mg/ml) In a 200 ml volumetric flask, dilute 20 ml of the stock solution (4.4.1) in 0,5 M hydrochloric acid solution (4.2). Make up to volume with the 0,5 M hydrochloric acid solution and mix thoroughly.  5. APPARATUS Atomic absorption spectrometer: See Method 9.4, (5). The apparatus must be fitted with a source of lines characteristic of zinc (213,8 nm). the spectrometer must allow background correction to be made.  6. PREPARATION OF THE SOLUTION TO BE ANALYSED 6.1. Zinc extract solution See Methods 9.1 and/or 9.2 and, if appropriate, 9.3.  6.2. Preparation of the test solution See Method 9.4, (6.2). The test solution must contain 10 % by volume of lanthanum salt solution.  7. PROCEDURE 7.1. Preparation of the blank solution See Method 9.4, (7.1). The blank solution must contain 10 % by volume of the lanthanum salt solution used in 6.2.  7.2. Preparation of the calibration solutions See Method 9.4, (7.2).  For an optimum interval of 0 to 5 mg/ml of zinc, place 0, 0,5, 1, 2, 3, 4 and 5 ml, respectively, of the working solution (4.4.2) in a series of 100 ml volumetric flasks. Where necessary, adjust the concentration of hydrochloric acid to bring it as  close as possible to that of the test solution. Add 10 ml of the lanthanum salt solution used in (6.2) to each volumetric flask. Make up to 100 ml with the 0,5 M hydrochloric acid solution (4.2) and mix thoroughly. These solutions contain, respectively:  0, 0,5, 1, 2, 3, 4, and 5 mg/ml of zinc.  7.3. Determination See Method 9.4 (7.3). Prepare the spectrometer (5) for measurements at a wavelength of 213,8 nm.  8. EXPRESSION OF RESULTS See Method 9.4 (8).  The percentage of zinc in the fertilizer is equal to:  Zn % = [(xs   xb) × V × D] / (M × 104) If method 9.3 has been used:  Zn % = [(xs   xb) × V × 2D] / (M × 104) where:  Zn is the quantity of zinc expressed as a percentage of the fertilizer;  xs is the concentration in mg/ml of the test solution (6.2);  xb is the concentration in mg/ml of the blank solution (7.1);  V is the volume in ml of the extract solution obtained in accordance with Method 9.1 or 9.2;  D is the factor corresponding to the dilution performed in (6.2);  M is the mass in g of the test sample taken in accordance with Method 9.1 or 9.2.  Calculation of the dilution factor D: where (a1), (a2), (a3), ., ., ., (ai) and (a) are successive aliquot portions and (v1), (v2), (v3), ., ., ., (vi) and (100) are the volumes corresponding to their respective dilutions, the dilution factor D will be:   D = (v1/a1) × (v2/a2) × (v3/a3) ×. ×. ×. × (vi/ai) × (100/a).' (1) OJ No L 281, 30. 9. 1989, p. 116.


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31986L0102

Council Directive 86/102/EEC of 24 March 1986 amending for the fourth time Directive 74/329/EEC on the approximation of the laws of the Member States relating to emulsifiers, stabilizers, thickeners and gelling agents for use in foodstuffs

Official Journal L 088 , 03/04/1986 P. 0040 - 0041 Finnish special edition: Chapter 13 Volume 15 P. 0062  Swedish special edition: Chapter 13 Volume 15 P. 0062

*****COUNCIL  DIRECTIVE  of 24 March 1986  amending for the fourth time Directive 74/329/EEC on the approximation of the laws of the Member States relating to emulsifiers, stabilizers, thickeners and gelling agents for use in foodstuffs  (86/102/EEC)  THE COUNCIL OF THE EUROPEAN COMMUNITIES,  Having regard to the Treaty establishing the European Economic Community, and in particular Article 100 thereof,  Having regard to the proposal from the Commission (1),  Having regard to the opinion of the European Parliament (2),  Having regard to the opinion of the Economic and Social Committee (3),  Whereas Directive 74/329/EEC (4), as last amended by Directive 85/6/EEC (5), lays down a list of emulsifiers, stabilizers, thickeners and gelling agents which may be authorized for use in foodstuffs;  Whereas Annex II to Directive 74/329/EEC indicates the designations of the substances which may be temporarily authorized by Member States for use in foodstuffs, and whereas the validity of each authorization is limited to 30 September 1985;  Whereas the period of temporary authorization for the polysorbates must be prolonged so that these substances may be re-evaluated in the light of any new information not previously assessed;  Whereas the use of Tragacanth gum (E 413) should be re-evaluated after an enquiry by the Commission;  Whereas, for Karaya gum and thermally oxidized soya bean oil interacted with mono- and di-glycerides of fatty acids, a further period of temporary authorization must be provided to permit the completion of certain toxicological and technological investigations so that a decision can be taken on the possibility of inclusion of these substances in Annex I to Directive 74/329/EEC or their deletion from the said Directive;  Whereas in the light of the recent toxicological investigations, pectin and amidated pectin can be considered as equivalent;  Whereas polyoxyethylene (8) stearate, polyoxyethylene (40) stearate, lactylated fatty acid esters of glycerol and propylene glycol, and dioctyl sodium sulphosuccinate must no longer be used in foodstuffs after a temporary period to allow the sale of foodstuffs containing these substances which are already on the market,  HAS ADOPTED THIS DIRECTIVE:  Article 1  Directive 74/329/EEC is hereby amended as follows:  1. Paragraph 2 of Article 2 shall be replaced by the following:  '2. However, as regards Tragacanth gum referred to in Annex I under E 413, the Commission shall make an enquiry and, on the basis of the results of this enquiry, propose where appropriate to the Council, that a decision be taken by not later than 31 December 1988, in accordance with the procedure provided for in Article 100 of the Treaty, to delete it form the Annex or otherwise change its status as appropriate.';  2. Article 3 shall be replaced by the following:  'Article 3  1. By way of derogation from Article 2 (1), Member States may authorize until 31 December 1988 the use in foodstuffs of the substances listed in Annex II. However, as regards Karaya gum and thermally oxidized soya bean oil interacted with mono- and di-glycerides of fatty acids, the Council, acting in accordance with the procedure provided for in Article 100 of the Treaty, may decide, by 31 December 1988 and on the basis of a study by the Commission, to delete them from that Annex or otherwise change their status.  Member States may authorize up to 31 March 1987 the marketing of foodstuffs containing the following substances:  - Polyoxyethylene (8) stearate,  - Polyoxyethylene (40) stearate,  - Lactylated fatty acid esters of glycerol and propylene glycol,  - Dioctyl sodium sulphosuccinate.  2. Where a Member State exercises the option under paragraph 1 other than by merely retaining the legislation in force at the time of notification of this Directive, it shall forthwith inform the other Member States and the Commission of the measures taken and shall furnish evidence which in its view justifies such measures.  3. Without prejudice to the first subparagraph of paragraph 1 and before the end of the period provided therein, the Council may, in accordance with the procedure laid down in Article 100 of the Treaty, include in Annex I the substances referred to in Annex II.  In the case referred to in paragraph 2, the Council may, in accordance with the procedure laid down in Article 100 of the Treaty decide on any other appropriate measure.';  3. In Annex I the designations E 440 a (pectin) and E 440 b (amidated pectin) shall be amended as follows:  'E 440 (i) pectin  (ii) amidated pectin'  4. Annex II shall be replaced by the following:  'ANNEX II  DENOMINATIONS  Karaya gum (synonym: sterculia gum),  Polyoxyethylene (20) sorbitan monolaurate (synonym: polysorbate 20),  Polyoxyethylene (20) sorbitan monopalmitate (synonym: polysorbate 40),  Polyoxyethylene (20) sorbitan monostearate (synonym: polysorbate 60),  Polyoxyethylene (20) sorbitan tristearate (synonym: polysorbate 65),  Polyoxyethylene (20) sorbitan monooleate (synonym: polysorbate 80),  Thermally oxidized soya bean oil interacted with mono- and di-glycerides of fatty acids'.  Article 2  Article 1 shall take effect as from 1 October 1985.  Article 3  Member States shall, within one year of the notification of this Directive, amend their laws in accordance with the preceding provisions, and shall forthwith inform the Commission thereof. The laws thus amended shall be implemented two years after notification of this Directive.  Article 4  This Directive is addressed to the Member States.  Done at Brussels, 24 March 1986.  For the Council  The President  G. BRAKS  (1) OJ No C 247, 15. 9. 1984, p. 3.  (2) OJ No C 12, 14. 1. 1985, p. 109.  (3) OJ No C 44, 15. 2. 1985, p. 2.  (4) OJ No L 189, 12. 7. 1974, p. 1.  (5) OJ No L 155, 3. 1. 1985, p. 21.


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31983L0585

Council Directive 83/585/EEC of 25 November 1983 amending for the 17th time Directive 64/54/EEC on the approximation of the laws of the Member States concerning the preservatives authorized for use in foodstuffs intended for human consumption

Official Journal L 335 , 30/11/1983 P. 0038 - 0038 Spanish special edition: Chapter 13 Volume 14 P. 0242  Portuguese special edition Chapter 13 Volume 14 P. 0242

*****COUNCIL  DIRECTIVE  of 25 November 1983  amending for the 17th time Directive 64/54/EEC on the approximation of the laws of the Member States concerning the preservatives authorized for use in foodstuffs intended for human consumption  (83/585/EEC)  THE COUNCIL OF THE EUROPEAN  COMMUNITIES,  Having regard to the Treaty establishing the European Economic Community, and in particular Article 100 thereof,  Having regard to the proposal from the Commission (1),  Having regard to the opinion of the European Parliament (2),  Having regard to the opinion of the Economic and Social Committee (3),  Whereas Directive 64/54/EEC (4), as last amended by Directive 81/214/EEC (5), sets out a list of preservatives the use of which for the protection of foodstuffs intended for human consumption against deterioration caused by micro-organisms is authorized;  Whereas the Commission proposal currently under review aims, on the one hand, to add to the list of authorized preservatives potassium bisulphite and natamycin and, on the other hand, to authorize thiabendazol for surface treatment of citrus fruit and bananas without any time limit;  Whereas pending a Council Decision on the whole of this proposal and without prejudice to current discussions on this subject the authorization for thiabendazol should, as a precautionary measure, be extended on a transitional basis with effect from 1 July 1982 to 15 December 1983 in order to avoid any interruption in the traditional trade flows concerning citrus fruit and bananas,  HAS ADOPTED THIS DIRECTIVE:  Article 1  In No E 233 c) of Section I of the Annex to Directive 64/54/EEC, '1 July 1982' is hereby replaced by '16 December 1983'.  Article 2  Member States shall bring into force the laws, regulations and administrative provisions necessary to comply with this Directive with effect from 1 July 1982 and shall forthwith inform the Commission thereof.  Article 3  This Directive is addressed to the Member States.  Done at Brussels, 25 November 1983.  For the Council  The President  G. MORAITIS  (1) OJ No C 330, 17. 12. 1981, p. 7.  (2) OJ No C 125, 17. 5. 1982, p. 147.  (3) OJ No C 178, 15. 7. 1982, p. 4.  (4) OJ No 12, 27. 1. 1964, p. 161/64.  (5) OJ No L 101, 11. 4. 1981, p. 10.


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31996L0028

Commission Directive 96/28/EC of 10 May 1996 adapting to technical progress Council Directive 76/116/EEC on the approximation of the laws of the Member States relating to fertilizers (Text with EEA relevance)

Official Journal L 140 , 13/06/1996 P. 0030 - 0031

COMMISSION DIRECTIVE 96/28/EC of 10 May 1996 adapting to technical progress Council Directive 76/116/EEC on the approximation of the laws of the Member States relating to fertilizers (Text with EEA relevance)THE COMMISSION OF THE EUROPEAN COMMUNITIES,Having regard to the Treaty establishing the European Community, and in particular Article 100a thereof,Having regard to Council Directive 76/116/EEC of 18 December 1975 on the approximation of the laws of the Member States relating to fertilizers (1), as last amended by Directive 89/530/EEC (2), and in particular Article 9 (1) thereof,Whereas Article 7a of the Treaty envisages an area without internal frontiers in which the free circulation of goods, persons, services and capital is assured;Whereas Directive 76/116/EEC laid down rules for the marketing of fertilizers within the internal market;Whereas new fertilizers need to be added to Annex I to Directive 76/116/EEC to enable them to benefit from the Community marking provided for in Annex II to that Directive;Whereas notice 94/C 138/04 (3) establishes a procedure that should be observed by any person (manufacturer or his representative) wanting to apply to a fertilizer the Community marking provided for in Annex II to Directive 76/116/EEC, by way of submitting a technical file to the Member State authorities which will act as rapporteur for the file to the Working Party on Fertilizers of the European Commission;Whereas the measures provided for in this Directive are in accordance with the opinion of the Committee on the Adaptation to Technical Progress of the Directives for Removing Technical Barriers to trade in Fertilizers,HAS ADOPTED THIS DIRECTIVE:Article 1 Annex I to Directive 76/116/EEC shall be amended as follows:1. The fertilizer included in Annex I to this Directive shall be added to Part A, point 1 entitled 'Nitrogenous fertilizers`2. The fertilizers included in Annex II to this Directive shall be added to Part D entitled 'Secondary nutrient fertilizers`.Article 2 The following product and tolerance is added under A.1 in Annex III to Directive 76/116/EEC:>TABLE>Article 31. Member States shall bring into force the laws, regulations and administrative provisions necessary to comply with this Directive by 31 May 1997. They shall forthwith inform the Commission thereof.2. Member States shall communicate to the Commission the provisions of national law which they adopt in the field covered by this Directive.Article 4 This Directive is addressed to the Member States.Done at Brussels, 10 May 1996.For the CommissionMartin BANGEMANNMember of the Commission(1) OJ No L 24, 30. 1. 1976, p. 21.(2) OJ No L 281, 30. 9. 1989, p. 116.(3) OJ No C 138, 20. 5. 1994, p. 4.ANNEX I ANNEX I A. STRAIGHT FERTILIZERS 1. Nitrogenous fertilizers >TABLE>ANNEX II ANNEX I D. SECONDARY NUTRIENT FERTILIZERS >TABLE>