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S.I. No. 264/1957 - Fertilisers, Feeding Stuffs and Mineral Mixtures Regulations, 1957.

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  2. s)or rangeBliain nó blianta nó raon TypeCineál All Legislation Acts Statutory Instruments Advanced SearchCuardach Casta HomeBaile Statutory InstrumentsIonstraimí Reachtúla 1957 S.I. No. 264/1957 - Fertilisers, Feeding Stuffs and Mineral Mixtures Regulations, 1957. S.I. No. 264/1957 - Fertilisers, Feeding Stuffs and Mineral Mixtures Regulations, 1957. AmendmentsLeasuithe S.I. No. 264

  1. FERTILISERS, FEEDING STUFFS AND MINERAL MIXTURES REGULATIONS,
  2. I, PATRICK SMITH, Minister for Agriculture, in exercise

the powers conferred on me by section 11

the Fertilisers, Feeding Stuffs and Mineral Mixtures Act, 1955 (No. 8

1955), hereby make the following regulations (the sanction

the Minister for Finance having been given with respect to the fee specified in Article 6 and the Minister for Industry and Commerce having been consulted with respect to Article 13) : 1 Short title and commencement. 1.—

(1)These Regulations may be cited as the Fertilisers, Feeding Stuffs and Mineral Mixtures Regulations, 1957.
(2)These Regulations shall come into operation on the 1st day

January,

  1. 2 Definitions.
  2. In these Regulations— " the Act " means the Fertilisers, Feeding Stuffs and Mineral Mixtures Act, 1955 (No. 8

1955) ; " complex fertiliser " means any fertiliser which contains not less than two

the elements nitrogen, phosphorus and potassium and in which any such elements are associated either naturally or by chemical means only ; " liming material " means any fertiliser manufactured for use as a corrective

acidity in the soil ; " mixed fertiliser " means any fertiliser which has been manufactured by mixing together two or more substances and which contains not less than two

the elements nitrogen, phosphorus and potassium ; " single fertiliser " means any fertiliser which contains one only

the elements nitrogen, phosphorus and potassium ; " superphosphate " means any fertiliser which has been produced by the treatment

rock phosphate with phosphoric acid or with sulphuric acid or with both phosphoric acid and sulphuric acid. 3 Particulars to be contained in statement. 3.—

(1)A statement given for the purposes

subsection

(1)

section 2

the act in relation to any article other than a feeding stuff or a compound feeding stuff specified in the First Schedule to these Regulations shall contain the following particulars only : (a) the business name and address

the seller

the article to which the statement relates, (

  1. b)the date on which the article was sold to the purchaser, (
  2. c)the name under which the article was sold, (
  3. d)the identifying marks (if any) on the container or on a label affixed to the container

the article, and (e) such particulars

the article as are indicated in the next paragraph.

(2)The particulars referred to in subparagraph (e)

the foregoing paragraph are as follows, except that in the case

the articles mentioned in subparagraphs (b), (c) and (d)

this paragraph particulars as formerly prescribed under Article 9

the Emergency Powers (Manufacture and Sale

Fertilisers) Order, 1944 (No. 49

1944), shall continue to be given for the period ending 30th June, 1958 : (

  1. a)if the article is a liming material— (
  2. i)the minimum neutralising value

the article, and in the case

ground limestone— (ii) the amount

the article that will pass through a 1/8 inch sieve conforming to Irish Standard 24 : 1950, and (iii) the minimum amount

the article that will pass through a No. 100 sieve conforming to that Standard ; (

  1. b)if the article is basic slag— (
  2. i)the minimum amounts

— citric acid soluble phosphorus, and citric acid insoluble phosphorus, contained in the article, and (ii) the minimum amount

the article that will pass through a No. 100 sieve conforming to Irish Standard 24 : 1950 ; (c) if the article is superphosphate or a mixture

which superphosphate is the only source

phosphorus— (i) the minimum amounts (if any)

— nitrogen, water soluble phosphorus, and potassium, contained in the article, and (ii) the amount (if any)

boron contained in the article ; (

  1. d)if the article is any other fertiliser— (
  2. i)the minimum amounts (if any)

— nitrogen, water soluble phosphorus, citrate soluble phosphorus, citrate insoluble phosphorus, and potassium, contained in the article, (ii) the amount (if any)

boron contained in the article, and, in the case

ground rock phosphate, (iii) the minimum amount

the article that will pass through a No. 100 sieve conforming to Irish Standard 24 : 1950 ; (e) if the article is a feeding stuff or a compound feeding stuff and is described in the first column

the Second Schedule to these Regulations, the particulars mentioned in relation thereto in the second column

that Schedule ; (f) if the article is a feeding stuff or a compound feeding stuff and is not described in the first column

the Second Schedule to these Regulations— (i) the amount (if any)

oil, (ii) the minimum amount (if any)

crude protein, and (iii) the maximum amount (if any)

fibre, contained in the article ; (g) if the article is a mineral mixture, the minimum amounts (if any)

— calcium, phosphorus, salt (sodium chloride), magnesium, manganese (acid soluble), cobalt, copper, iodine and iron, contained in the article.

(3)For the purposes

the foregoing paragraph— (a) each amount shall be stated as a definite percentage

the weight

the article except that, in the case

betacarotene, the amount shall be stated in terms

parts per million as a definite proportion

the weight

the article ; (b) nitrogen, phosphorus and potassium shall be stated in terms

the elements N, P and K, respectively ; (c) the extent to which the article is capable

passing through the prescribed sieve or sieves shall be expressed as the fineness

the article ; (d) neutralising value shall be stated in terms

calcium carbonate ; (e) the amount

crude protein means the amount

nitrogen, other than ammoniacal or nitric nitrogen, if present, multiplied by 6·25 ; (f) the amount

true protein means the amount

nitrogen, other than ammoniacal or nitric nitrogen or non-protein organic nitrogen, if present, multiplied by 6·25. 4 Time

giving statement. 4. A statement for the purposes

subsection

(1)

section 2

the act shall be given on or before delivery

the article to the purchaser or as soon as reasonably practicable thereafter. 5 Limits

error in statement. 5. The limits

error for the purposes

section 2

the act shall be as follows : Article Limits

Error

(1)A liming material Neutralising value, one-thirtieth

the amount stated ; amount that will pass through a prescribed 1/8 inch sieve, one-fortieth

the amount stated ; amount that will pass through a prescribed No. 100 sieve, one-twentieth

the amount stated. Article Limits

Error

(2)A single fertiliser (other than a liming material), or a complex fertiliser. Nitrogen, one-fortieth

the amount stated ; phosphorus, one-twentieth

each amount stated ; potassium, one-twentieth

the amount stated ; amount that will pass through a prescribed No. 100 sieve, one-twentieth

the amount stated ; boron, one-fifth

the amount stated.

(3)A mixed fertiliser Nitrogen, 0·4 per cent. plus one-twentieth

the amount stated ; phosphorus, 0·4 per cent. plus one-twentieth

each amount stated ; potassium, 0·4 per cent. plus one-twentieth

the amount stated ; boron, one-fifth

the amount stated.

(4)A feeding stuff or compound feeding stuff or a mineral mixture. Oil, 0·75 per cent. or one-tenth

the amount stated whichever is the greater ; crude protein and true protein— (a) if the amount stated does not exceed 20 per cent.

the weight

the article, 1 per cent.

the weight

the article, (b) if the amount stated exceeds 20 per cent. but does not exceed 40 per cent.

the weight

the article, 2 per cent.

the weight

the article, and (c) if the amount stated exceeds 40 per cent.

the weight

the article, one-twentieth

the amount stated ; fibre, one-tenth

the amount stated ; calcium and phosphorus— (a) if the amount stated does not exceed 1 per cent.

the weight

the article, 0·2 per cent.

the weight

the article, (b) if the amount stated exceeds 1 per cent. but does not exceed 5 per cent.

the weight

the article, 0.3 per cent.

the weight

the article, and (c) if the amount stated exceeds 5 per cent.

the weight

the article, one-twentieth

the amount stated ; salt (sodium chloride), one-twentieth

the amount stated ; magnesium, one-tenth

the amount stated ; manganese, cobalt, copper, iodine and iron, one-half

the amount stated ; betacarotene, one-fifth

the amount stated. 6 Application to have sample taken for analysis. 6.—

(1)The period within which an application under section 3

the act may be made to the Minister shall be the period

twelve consecutive days commencing on the day on which the article sought to be sampled has been delivered to the purchaser or on which the relevant statement has been received by the purchaser, whichever is the later. For the purposes

this paragraph, an article consigned to a purchaser shall be deemed not to be delivered to him until it arrives at the place to which it is consigned, whether the consignment is by direction

the seller or the purchaser.

(2)An application under section 3

the act shall be in writing and shall be accompanied by a remittance, payable to the Minister for the amount

the fee, which shall be ten shillings for each article sought to be sampled. 7 Manner

taking sample. 7.—

(1)The manner in which a sample shall be taken and dealt with where under the Act a sample is required to be taken in the prescribed manner shall be as specified in the subsequent paragraphs

this Article.

(2)Where the quantity

the article to be sampled does not exceed or appear to exceed 2 cwt. in weight or is all contained in one container, the sample may consist

such a portion

the quantity as is fairly representative

the whole and the sample in duplicate shall be not less than 280 millilitres in volume. A sample shall be considered representative when taken in accordance with the method set out in subparagraph (b)

paragraph

(8)

this Article.

(3)In the case

articles in packages or other containers, unopened packages or containers shall be selected in preference to opened packages or containers for the purpose

the sample.

(4)A sample shall not be drawn from part

any quantity where that part bears the appearance

having received, in transit or after delivery, damage likely to have rendered it unrepresentative

the whole.

(5)It shall be assumed that the quantity to be sampled is composed

separate approximately equal parts and that the number

such parts is equivalent— (a) in the case

a mineral mixture which is in the state

separate blocks, bricks or other pieces

uniform shape and similar size, to the number

blocks, bricks or pieces composing the quantity to be sampled, (b) in the case

any other article which is in packages or other containers, to the number

packages or containers to be selected in accordance with subparagraph (a)

paragraph

(8)

this Article, and (c) in the case

an article in bulk, to the number

portions to be taken in accordance with paragraph

(9)

this Article. Packages, containers or portions for the purpose

the sample shall be selected one from each part and shall be drawn from different positions in each part.

(6)In every case the sampling shall be done as quickly as possible consistently with due care and the material shall not be exposed any longer than is necessary.
(7)If the article is a mineral mixture in the state

separate blocks, bricks or other uniform pieces, any one block, brick or uniform piece may be selected for the purpose

the sample. The selected block, brick or uniform piece shall be wrapped in a clean dry material and shall be finely broken on a clean dry smooth surface with a hammer or other suitable instrument. The fragments shall be thoroughly mixed together and the sample shall be taken in duplicate by transferring a quantity

the material approximately equal to 140 millilitres in volume into each

two clean dry bottles, each

which shall be provided with a close-fitting stopper or lid.

(8)If the article is not a mineral mixture in the state

separate blocks, bricks or other uniform pieces and is in packages or other containers— (a) when the article is in packages or other containers and the quantity to be sampled exceeds or appears to exceed 2 cwt. in weight, a number

packages or containers shall be selected as follows :— Quantity taken for sampling But not fewer packages or containers than Per cent. Where the quantity exceeds one package or container and does not exceed 20 packages or containers 10 2 Where the quantity exceeds 20 packages or containers and does not exceed 60 packages or containers 5 2 Where the quantity exceeds 60 packages or containers and does not exceed 200 packages or containers 4 3 Where the quantity exceeds 200 packages or containers and does not exceed 500 packages or containers 3 8 Where the quantity exceeds 500 packages or containers 2 15 When the number

packages or containers to be selected according to the above percentage scale contains a fraction, that fraction shall be counted as a whole number ; (

  1. b)if the article is not in a fluid or semi-fluid condition— (
  2. i)where the quantity does not exceed 60 packages or containers, each selected package shall beemptied on a clean dry surface and flattened as near as possible to a uniform depth ; 10 portions shall then be taken from different parts

, and as near as possible to the full depth

, the material ; (ii) where the quantity exceeds 60 packages or containers, one portion at least shall be taken from each selected package ; (iii) in either case (whether or not the quantity exceeds 60 packages), the several portions so obtained shall then be thoroughly mixed together with a suitable instrument ; the composite sample so obtained shall be reduced to a suitable quantity not less than 280 millilitres in volume by the use

a mechanical divider or riffle ; alternatively, except in the case

granular fertilisers, the reduction

the composite sample may be effected by placing the sample on a pliable surface and successively folding and unfolding that surface, the folding to be reversed occasionally so as to discard part

the material ; the process to be continued until the material remaining on the pliable surface is reduced to the required quantity ; a sample shall then be taken in duplicate by transferring a quantity

the material approximately equal to 140 millilitres in volume into each

two clean dry bottles, each

which shall be provided with a close-fitting stopper or lid ; (iv) where any appreciable portion

the material appears to be mouldy or to have undergone decomposition such as would render it unsuitable for the purpose for which it purports to be intended, separate samples shall be drawn

the apparently unsuitable portion and

the residue

the material, respectively ; (c) if the article is in a fluid or semi-fluid condition, the selected containers shall be well shaken or the contents agitated or otherwise treated to ensure uniformity ; an approximately equal proportion

the fluid shall then be taken immediately from each

the selected containers, emptied into a clean, dry non-metallic vessel and well mixed by stirring or shaking ; the sample shall be taken in duplicate by immediately pouring approximately 140 millilitres

the mixture into each

two clean dry bottles, each

which shall be provided with a close-fitting stopper or lid.

(9)If the article is not a mineral mixture in the state

separate blocks, bricks or other uniform pieces and is in bulk, a number

portions shall be taken in accordance with the following scale : Portions Where the quantity exceeds 2 cwt. and does not exceed 10 tons 10 Where the quantity exceeds 10 tons and does not exceed 20 tons 20 Where the quantity exceeds 20 tons and does not exceed 100 tons—for each additional 5 tons or part thereof in excess

20 tons 1 Where the quantity exceeds 100 tons—for each additional 10 tons or part thereof in excess

100 tons 1 The portions shall be treated and the sample drawn in the manner described in subparagraph (b)

paragraph

(8)

this Article.

(10)Each

the two bottles containing the sample in duplicate shall be so secured and sealed that it cannot be opened without breaking the seal. The authorised

ficer taking the sample shall affix to the outside

each bottle an adhesive label initialled by him and marked with the name

the article, the date and place

the sampling and a distinguishing mark or number. The label may also be initialled by the person on whose premises the sample is taken, or his representative.

(11)One

the sealed sample bottles shall be transmitted by the authorised

ficer to the seller

the article from which the sample was taken. 8 Period within which sample may be taken. 8. For the purposes

paragraph (a)

subsection

(4)

section 3

the act, the period after the expiration

which a sample may not be taken under section 3

the act shall be the period

twenty-one consecutive days commencing on the day on which the article has been delivered to the purchaser or on which the relevant statement has been received by the purchaser, whichever is the later. For the purposes

this paragraph an article consigned to a purchaser shall not be deemed to be delivered to him until it arrives at the place to which it is consigned, whether the consignment is by direction

the seller or the purchaser. 9 Manner

analysis

fertilisers. 9.—

(1)The manner in which a sample

a fertiliser shall be analysed for the purposes

the Act shall be as specified in the subsequent paragraphs

this Article.

(2)Determination

moisture (loss on drying) shall be effected as follows : A representative portion

the sample shall be weighed, with precautions against loss

moisture. It shall then be dried in a ventilated oven maintained at a temperature between 100°C. and 105°C., until 2 successive weighings after cooling in a desiccator, at intervals

not less than 3 hours in the oven, show an increment

loss

not more than 0·2 per cent.

the original weight. The loss in weight, calculated as a percentage

the original weight, shall be taken to be the moisture content. Determination

fineness. Ground limestone.

(3)(a) In the case

ground limestone, determination

fineness shall be effected as follows : a quantity

the dried material, approximately 100 grams in weight, weighed to an accuracy

0·1 gram, shall be sifted through a 1/8 inch test sieve conforming to Irish Standards 24 : 1950. Soft lumps shall be broken down with the fingers but shallnot be rubbed on the sieve. Any residue remaining on the sieve shall be weighed to an accuracy

0·1 gram, and the difference between its weight and the weight

the dried material taken for the test shall be expressed as a percentage

the latter weight and shall be reported as indicating the extent to which the material passed through the sieve. The material which has passed through the 1/8 in. test sieve shall be transferred to a No. 100 test sieve conforming to Irish Standard 24 : 1950 and shall be sifted continuously for 10 minutes, with occasional tapping

the sides

the sieve. The material which has then passed through the No. 100 test sieve shall be weighed to an accuracy

0·1 gram and the result shall be expressed as a percentage

the weight

the dried material taken for the test and shall be reported as indicating the percentage

the material which passed through the No. 100 test sieve. Basic slag and ground rock phosphate. (b) In the case

basic slag and ground rock phosphate, determination

fineness shall be effected as follows : the sample shall be mixed and an adequate quantity shall be dried at 100°C. and 20 grams thereof shall then be transferred to a No. 100 test sieve (fitted with a receiver) conforming to Irish Standard 24 : 1950. The sieve shall then be shaken for 10 minutes with occasional tapping

the sides

the sieve. At the end

10 minutes, the material which has passed through into the receiver shall be carefully brushed out into a suitable vessel and weighed. The receiver shall be replaced and the shaking repeated for another 10 minutes, when the sifted matter shall again be removed, mixed with the first portion and weighed. The process shall be repeated until not more than 0·2 per cent. is sifted during 10 minutes. Soft lumps which can be caused to crumble by application

the fibres

a bristle brush shall be broken down after each shaking period, but in such manner that the hard parts

the brush do not come into contact with the sieve. The brush shall not be used in any way to brush particles through the sieve. Preparation

the sample for analysis (other than determination

moisture, fineness or moisture and fineness).

(4)(a) Preparation

the sample for analysis (other than determination

moisture, fineness or moisture and fineness) shall be effected as specified in the subsequent subparagraphs

this paragraph. Powdered fertilisers in dry, or moderately dry, condition. (b) In the case

powdered fertilisers in a dry, or moderately dry, condition, the sample shall be passed through a sieve having apertures about one millimetre square. Adventitious materials which cannot be conveniently crushed, e.g., fragments

metal in basic slag, shall be removed and allowed for. Other substances dry enough to powder. (

  1. c)Other substances which are dry enough to powder, but which are not in a fine condition, shall be pulverised until the sample passes through a sieve having apertures about one millimetre square. Moist fertilisers. (
  2. d)Moist fertilisers which do not admit

being passed through a sieve shall be thoroughly mixed by the most suitable means. Substances gaining or losing water during pulverising or mixing. (e) In the case

substances which gain or lose water during the process

pulverising or mixing, the proportion

water shall be determined in the coarse and in the powdered condition respectively, and the results

the analysis

the powdered sample shall be calculated to the water content

the original coarse substance. Crystalline or saline materials. (f) Crystalline or saline materials, such as sulphate

ammonia, nitrate

soda or salts

potassium, may be prepared by being well mixed and rapidly ground in a stoneware mortar, the portion finally reserved for analysis being specially finely ground. Procedure after sieving and mixing or after mixing. (g) When the sample has been passed through the sieve and thoroughly mixed, or, if not passed through the sieve, has been thoroughly mixed, a part

it not being less than 100 grams shall be placed in a stoppered bottle and from this the portions for analysis shall be weighed. Determination

nitrogen.

(5)(a) Determination

nitrogen shall be effected as specified in the subsequent subparagraphs

this paragraph. Presence or absence

nitrates. (b) The presence or absence

nitrates shall first be ascertained. Nitrogen (organic and ammoniacal) in absence

nitrates. (c) Nitrogen (organic and ammoniacal) in absence

nitrates shall be determined as follows : a weighed portion

the sample shall be transferred to a Kjeldahl digestion flask, 25 millilitres

concentrated sulphuric acid (or more if necessary) shall be added and the flask gently heated until frothing ceases. 10 grams

potassium or sodium sulphate (anhydrous) shall then be added and the flask further heated until the colour

the clear liquid ceases to diminish. The digestion shall be continued for an hour thereafter to ensure complete oxidation

the organic matter. The operation may be accelerated by the addition

a suitable catalyst (e.g., copper sulphate or mercury or a mixture

mercuric oxide and selenium) to the liquid in the digestion flask. The quantity

ammonia present in the liquid shall be determined by distillation into standard acid after liberation with alkali and, where mercury or mercuric oxide has been used, with the addition also

sodium or potassium sulphide solution or sodium thiosulphate. Nitrogen (total, i.e., organic, ammoniacal and nitric) when nitrates are present. (

  1. d)(
  2. i)Nitrogen (total, i.e., organic, ammoniacal and nitric) when nitrates are present shall be determined as specified in the subsequent clauses

this subparagraph. (ii) The presence or absence

more than traces

chlorides shall first be ascertained. (iii) When chlorides are not present in more than traces, a weighed portion

the sample shall be transferred to a Kjeldahl digestion flask, 30 millilitres

concentrated sulphuric acid, containing 1 gram

salicylic acid or 1 gram

phenol, shall be added and the flask shall be shaken so as to mix its contents without delay. The shaking shall be continued at intervals during 10 minutes, the flask being kept cool, and then 10 grams

potassium or sodium sulphate (anhydrous) shall be added, together with either 5 grams

crystalline sodium thiosulphate or 2 grams

zinc dust. The flask shall be heated until the colour

the clear liquid ceases to diminish and for an hour thereafter. A further quantity

concentrated sulphuric acid may be added if necessary. Copper sulphate or mercury or a mixture

mercuric oxide and selenium may be used as indicated in subparagraph (c)

this paragraph. The quantity

ammonia shall be determined as described in subparagraph (c)

this paragraph. (iv) When chlorides are present in more than traces, about 2 grams

the sample, accurately weighed, and 3 grams

finely powdered Devarda metal shall be transferred to a 500 millilitre Kjeldahl digestion flask, and the sides

the flask shall be washed down with 50 millilitres

water. The flask shall be closed with a rubber stopper provided with (I) a tap funnel and (II) a delivery tube connected with a U-tube (with bulbs) containing 10 millilitres

10 per cent. v/v sulphuric acid. 5 millilitres

sodium hydroxide solution (specific gravity 1·40) shall be added through the tap funnel. The flask shall be allowed to stand for half an hour and then heated to just short

boiling point for a further hour. At the end

this digestion the flask shall be cooled and 20 millilitres

sulphuric acid (specific gravity 1·50) shall be added through the tap funnel in such a manner that the sides

the Kjeldahl flask shall be washed down by the acid. The rubber stopper shall now be removed and the contents

the U-tube (with bulbs) shall be washed into the Kjeldahl flask. 25 millilitres

concentrated sulphuric acid shall be added to the flask and the flask shall be heated untilall the water has boiled

f. 10 grams

potassium or sodium sulphate (anhydrous) shall then be added and the flask further heated until the colour

the clear liquid ceases to diminish. The digestion shall be continued for 2 hours thereafter to ensure complete oxidation

the organic matter. Copper sulphate or mercury or a mixture

mercuric oxide and selenium may be used as indicated in subparagraph (c)

this paragraph. The quantity

ammonia shall be determined as described in subparagraph (c)

this paragraph. Nitrogen in form

ammonium salts. (

  1. e)(
  2. i)Nitrogen in form

ammonium salts shall be determined as specified in the subsequent clauses

this paragraph. (ii) In absence

organic matter, a weighed portion

the sample shall be dissolved in water and made up to a definite bulk. An aliquot part

the solution shall be transferred to a distillation flask and the quantity

ammonia shall be determined as described in subparagraph (c)

this paragraph. (iii) In presence

organic matter, a weighed portion

the sample shall be well shaken with water, filtered, the insoluble matter thoroughly washed, the filtrate transferred to a distillation flask, diluted with water to about 200 millilitres, 5 grams

magnesium oxide (free from carbonates) added, and the quantity

ammonia determined as described in subparagraph (c)

this paragraph. (iv) In the case

mixed or complex fertilisers containing calcium carbonate with small quantities

ammonium salts, the portion taken for analysis must be dissolved in or shaken with hydrochloric acid instead

water. Nitrogen in nitrates. (f) Nitrogen in nitrates shall be determined as follows : a weighed portion

the sample shall be dissolved in water and made up to a definite bulk. An aliquot part

the solution shall be transferred to a flask and a quantity

finely powdered Devarda metal (not less than six times the weight

the sample present in the aliquot part taken) added. An excess

concentrated alkali shall then be added and the flask at once connected with a distillation apparatus. After standing for 30 minutes to allow the reaction to proceed, heating gently if necessary, the ammonia shall be determined by distillation into standard acid. Distillation shall proceed for at least one hour. Control experiment in determination

nitrogen. (g) The materials used in any

the methods described in this paragraph shall be examined as to their freedom from nitrogen by means

a control experiment carried out under similar conditions with the same quantitiesof the reagents which have been employed in the actual analysis, in the case

subparagraph (c)

this paragraph one gram

pure sugar being used in place

the weighed portion

the sample. The quantity

standard acid found to have been neutralised in the control experiments shall be deducted from the total quantity

acid neutralised in the distillation

the sample. Determination

phosphorus.

(6)(a) Determination

phosphorus shall be effected as specified in the subsequent subparagraphs

this paragraph. Water soluble phosphorus. (

  1. b)(
  2. i)Water soluble phosphorus shall be determined as specified in the subsequent clauses

this subparagraph. (

  1. ii)Reagents shall be prepared as follows :— (
  2. a)Citric Molybdate reagent : 54 grams

molybdic anhydride shall be stirred with 200 millilitres

water and 11 grams

sodium hydroxide until the molybdic anhydride dissolves ; the mixture shall be heated to assist solution. 60 grams

citric acid shall be dissolved in a further 300 millilitres

water and 140 millilitres

concentrated hydrochloric acid added to it. The molybdate solution shall then be poured into the acid solution, which shall be stirred throughout the addition. The whole shall be cooled and if necessary filtered through a pad

filter paper pulp. The filtrate shall be diluted with water to a litre and the slight green or blue colour discharged by the dropwise addition

a 1 per cent. solution

potassium bromate. This reagent shall be stored in the dark. (b) Quinoline reagent : 60 millilitres

concentrated hydrochloric acid shall be diluted to 400 millilitres with water and heated to between 70° and 80°C., 50 millilitres

quinoline (laboratory reagent quality) shall be poured into the diluted acid in a thin stream with continuous stirring. After the quinoline has dissolved the solution shall be cooled, diluted to a litre with water, and filtered through a pad

filter paper pulp. The pulp shall not be washed. (c) Indicator : 0·10 gram

thymol blue shall be dissolved in 2·2 millilitres

0·1 N sodium hydroxide solution, 50 millilitres

methylated spirits shall be added and the whole diluted to 100 millilitres with water andmixed well. 3 volumes

this solution shall then be mixed with 1 volume

0·1 per cent. solution

phenolphthalein in 60 per cent. ethyl alcohol. (iii) The procedure shall be as follows : 20 grams

the sample shall be continuously agitated for 30 minutes in a litre flask with 800 millilitres

water at room temperature

about 20°C. The flask shall then be filled to the mark with water, shaken, and the contents filtered. The phosphorus shall be determined in the filtrate by the following method : An aliquot part (chosen so as to contain less than 30 milligrams

phosphorus and preferably about 20 milligrams

phosphorus)

the solution obtained as above described shall be transferred to a conical flask

about 500 millilitres capacity fitted with a stopper or a rubber bung and marked at 150 millilitres. The aliquot part shall be diluted to 150 millilitres and 50 millilitres

reagent (a) shall be added. The solution shall be heated to incipient ebullition and kept at this temperature for 3 minutes, then heated to the boiling point. 25 millilitres

reagent (b) shall be slowly run in from a burette, with constant swirling throughout, the first few millilitres being added dropwise, and the rest in a slow stream keeping the solution gently boiling throughout. The flask shall then be allowed to stand in a bath

boiling water for 5 minutes, after which it shall be cooled in running water to 15°C. The contents

the flask shall be filtered through a pad

filter paper pulp, and the flask, precipitate and filter shall be washed with successive small volumes

cold water until they are free from acid. The filter-pad and precipitate shall then be transferred to the original flask, using not more than 100 millilitres

water. A few drops

a dilute neutral solution

a surface active agent (e.g., a 0·5 per cent. solution

sodium dodecyl benzene sulphonate) may be added if desired to facilitate the dispersal

the precipitate. The flask shall then be stoppered and shaken vigorously until the pulp and precipitate are thoroughly dispersed. The stopper shall be removed and washed with distilled water, the washings being returned to the flask, then an accurately measured volume

0·5 N sodium hydroxide solution (free from carbon dioxide) shall be added, the volume added being such that it contains an excess

sodium hydroxide beyond that necessary to dissolve the precipitate. The stopper or bung shall be replaced, and the flask shaken until the precipitate is completely dissolved. The excessof sodium hydroxide shall be titrated with 0·5 N hydrochloric acid solution, about 0·5 to 1 millilitre

reagent (c) being added and the end point being taken as the sharp change from green-blue to yellow. The volume

0·5 N hydrochloric acid used shall be deducted from the volume

0·5 N sodium hydroxide, previously added, in order to ascertain the volume

0·5 N sodium hydroxide equivalent to the phosphorus. 1 millilitre 0·5 N sodium hydroxide solution is equivalent to 0·596 milligrams

phosphorus. A " blank " determination shall be carried out on all the reagents, omitting only the sample, and using 0·1 N solutions

acid and alkali for the titration. The " blank " shall be calculated in terms

0·5 N sodium hydroxide and the result first obtained corrected accordingly. Total phosphorus in all substances except basic slag. (

  1. c)(
  2. i)Total phosphorus in all substances except basic slag shall be determined as specified in the subsequent clauses

this subparagraph. (ii) In the absence

organic matter, 5 grams

the finely ground sample (if the phosphorus content does not exceed 6 per cent.) or 2·5 grams (if the phosphorus content exceeds 6 per cent.) shall be transferred to a 300 millilitre beaker and mixed with 10 millilitres

water. The beaker shall be covered by a watch glass and 10 millilitres

concentrated hydrochloric acid shall be added slowly and this shall be followed by 5 millilitres

concentrated nitric acid. The beaker and contents shall be heated to incipient ebullition on a hot plate and kept at this temperature for 10 minutes. The contents

the beaker shall be diluted with 100 millilitres

water and boiled for 10 minutes. The solution shall be cooled and transferred to a 500 millilitre volumetric flask and diluted to volume with water. The contents

the flask shall be thoroughly shaken and shall be filtered into a dry beaker through a dry paper. The first 20 millilitres

the filtrate shall be rejected. The phosphorus shall be determined in an aliquot part by the method described in, clause (iv)

this subparagraph. (iii) In the presence

organic matter, 5 grams

the finely ground sample (if the phosphorus content does not exceed 6 per cent.) or 2·5 grams (if the phosphorus content exceeds 6 per cent.) shall be transferred to a platinum dish, intimately mixed with 1 gram

calcium oxide, and thoroughly wetted with a little water. The mixture shall be dried and then heated to a temperature notexceeding 500°C. until the bulk

the organic matter is destroyed. The residue in the dish after cooling shall be transferred to a 300 millilitre beaker and shall be well mixed with 10 millilitres

water. The beaker shall be covered by a watch glass and 12 millilitres

concentrated hydrochloric acid shall be added slowly and this shall be followed by 5 millilitres

concentrated nitric acid. The beaker and contents shall be heated to incipient ebullition on a hot plate and kept at this temperature for 10 minutes. The contents

the beaker shall be diluted with 100 millilitres

water and shall be boiled for 10 minutes. The solution shall be filtered into a 500 millilitre flask, the insoluble matter washed with hot water, and the insoluble matter and filter paper then transferred to a dish and incinerated to a carbon-free ash. The ash shall be heated for 5 minutes with dilute hydrochloric acid (1 part

concentrated acid to 4 parts

water), then transferred to the filtrate in the 500 millilitre flask, well mixed, cooled, and the volume adjusted to the mark with water. The contents

the flask shall be thoroughly shaken and shall be filtered into a dry beaker through a dry paper. The first 20 millilitres

the filtrate shall be rejected. The phosphorus shall be determined in an aliquot part by the method described in clause (iv)

this subparagraph. (iv) 50 millilitres or 25 millilitres (chosen to contain less than 30 milligrams

phosphorus and preferably about 20 milligrams

phosphorus)

the solution obtained as above described shall be transferred to a conical flask

about 500 millilitres capacity filled with a stopper or a rubber bung and marked at 150 millilitres. The solution shall be diluted to about 100 millilitres and, if the sample does not contain calcium, 100 to 200 milligrams

pure calcium carbonate shall be added, then sodium hydroxide solution until a faint permanent precipitate or turbidity is formed. Dilute hydrochloric acid shall be added dropwise until the precipitate just dissolves. The solution shall then be diluted to 150 millilitres with water and the phosphorus determined as described in clause (iii)

subparagraph (b)

this paragraph beginning at the words " 50 millilitres

reagent (

  1. a)shall be added." Water insoluble phosphorus. (
  2. d)Water insoluble phosphorus shall be determined as follows : the quantity

phosphorus soluble in water as determined in accordance with subparagraph (b)

this paragraph shall be deducted from the quantityof phosphorus as determined in accordance with subparagraph (c)

this paragraph and the difference, if any, shall be taken as the quantity

insoluble phosphorus. Total phosphorus in basic slag. (

  1. e)(
  2. i)Total phosphorus in basic slag shall be determined as specified in the subsequent clauses

this subparagraph. (

  1. ii)Reagents shall be prepared as follows : (
  2. a)Citric molybdate reagent : 54 grams

molybdic anhydride shall be stirred with 200 millilitres

water and 11 grams

sodium hydroxide until the molybdic anhydride dissolves ; the mixture shall be heated to assist solution. 120 grams

citric acid shall be dissolved in a further 300 millilitres

water and 140 millilitres

concentrated hydrochloric acid added to it. The molybdate solution shall then be poured into the acid solution, which shall be stirred throughout the addition. The whole shall be cooled and if necessary filtered through a pad

filter paper pulp. The filtrate shall be diluted with water to a litre and the slight green or blue colour discharged by the dropwise addition

a 1 per cent. solution

potassium bromate. This reagent shall be stored in the dark. (b) Quinoline reagent : 60 millilitres

concentrated hydrochloric acid shall be diluted to 400 millilitres with water and heated to between 70° and 80°C. 50 millilitres

quinoline (laboratory reagent quality) shall be poured into the diluted acid in a thin stream with continuous stirring. After the quinoline has dissolved the solution shall be cooled, diluted to a litre with water, and filtered through a pad

filter paper pulp. The pulp shall not be washed. (c) Indicator : 0·10 gram

thymol blue shall be dissolved in 2·2 millilitres

0·1 N sodium hydroxide solution, 50 millilitres

methylated spirits shall be added and the whole diluted to 100 millilitres with water and mixed well. 3 volumes

this solution shall then be mixed with 1 volume

0·1 per cent. solution

phenolphthalein in 60 per cent. ethyl alcohol. (iii) The procedure shall be as follows : 2·5 grams

the finely powdered sample shall be transferred to a 300 millilitre beaker, thoroughly mixed with30 millilitres

water after which a further 70 millilitres

water shall be added with continuous stirring. The mixture shall be heated and, during stirring, 10 millilitres

concentrated hydrochloric acid shall be added dropwise followed by 5 millilitres

concentrated nitric acid. The whole shall be gently boiled for 10 minutes, cooled, transferred to a 250 millilitre volumetric flask, diluted to the mark with water and well mixed. This solution shall be filtered through a dry paper into a dry beaker, the first 20 or 30 millilitres

filtrate being rejected. According to the expected phosphorus content 50 millilitres or 25 millilitres shall be transferred to a conical flask

about 500 millilitres capacity fitted with a stopper or a rubber bung and marked at 150 millilitres. The solution shall be diluted to about 100 millilitres with water heated almost to boiling and a 20 per cent. solution

sodium hydroxide added drop by drop until there is a faint permanent precipitate. A few drops

dilute hydrochloric acid shall be added to the now boiling solution to redissolve the precipitate. The solution shall be diluted with water to 150 millilitres, 1 gram

citric acid added and then 50 millilitres

reagent (a). The solution shall be gently boiled for 3 minutes and then 25 millilitres

reagent (b) shall be slowly added from a burette, the flask being swirled continuously during the addition. The solution shall again be heated to boiling, and boiled gently for 2 minutes, after which it shall be kept hot but not boiling for a further 5 minutes, then cooled to 15°C. The contents

the flask shall be filtered through a pad

filter paper pulp, and the flask, precipitate and filter shall be washed with successive small volumes

cold water until they are free from acid. The filter pad and precipitate shall be transferred to the original flask, not more than 100 millilitres

water being used in effecting the transfer. A few drops

a dilute neutral solution

a surface active agent (e.g., a 0·5 per cent. solution

sodium dodecyl benzene sulphonate) may be added if desired to facilitate the dispersal

the precipitate. The flask shall be stoppered and well shaken until the pulp and precipitate are thoroughly dispersed. The stopper shall be removed and washed with distilled water, the washings being returned to the flask,then an accurately measured volume

0·5 N sodium hydroxide solution (free from carbon dioxide) shall be added, the volume added being such that it contains an excess

sodium hydroxide beyond that necessary to dissolve the precipitate. The flask shall be shaken until the precipitate is completely dissolved, and the excess

sodium hydroxide titrated with 0·5 N hydrochloric acid solution, about 0·5 to 1 millilitre

reagent (c) being added and the end point being taken as the sharp change from green-blue to yellow. The volume

0·5 N hydrochloric acid used shall be deducted from the volume

0·5 N sodium hydroxide previously added in order to ascertain the volume

0·5 N sodium hydroxide equivalent to the phosphorus. 1 millilitre 0·5 N sodium hydroxide solution is equivalent to 0·596 milligrams

phosphorus. A " blank " determination shall be carried out on all the reagents, omitting only the sample, and using 0·1 N solutions

acid and alkali for the titration. The " blank " shall be calculated in terms

0·5 N sodium hydroxide, and the result first obtained corrected accordingly. Citric acid soluble phosphorus (f) Citric acid soluble phosphorus shall be determined as follows : 5 grams

the sample shall be transferred to a stoppered bottle

about 1 litre capacity. 10 grams

citric acid shall be dissolved in water. The volume shall be made up to 500 millilitres at a temperature

about 20°C. and about 50 millilitres

this solution shall be added to the weighed portion

the sample in the bottle and the sample dispersed by vigorous stirring for a few minutes. The remainder

the citric acid solution shall be added and the bottle fitted into a mechanical shaking apparatus and continuously agitated during 30 minutes at a temperature

about 20°C. The solution shall then be filtered through a large rapid filter, the whole

the liquid being poured on the paper at once. If not clear the filtrate shall be again poured through the same paper. The determination shall be carried out on 50 millilitres or 25 millilitres (according to the amount

phosphorus present) as described in clause (iii)

subparagraph (e)

this paragraph beginning at the words " According to the expected phosphorus " except that no citric acid shall be added before 50 millilitres

the citric molybdate solution are added. Citric acid insoluble phosphorus. (g) Citric acid insoluble phosphorus shall be determined as follows : he quantity

phosphorus soluble in citric acid, as determined in accordance with subparagraph (f)

this paragraph, shall be deducted from the quantityof phosphorus determined in accordance with subparagraph (e)

this paragraph, and the difference (if any) shall be taken as the quantity

phosphorus insoluble in citric acid. Citrate soluble phosphorus. (

  1. h)(
  2. i)Citrate soluble phosphorus shall be determined as specified in the subsequent clauses

this subparagraph. (ii) Reagents shall be prepared as follows :—

(1)Ammonium citrate solution : 173 grams

citric acid shall be dissolved in 350 millilitres

distilled water in a 1-litre volumetric flask. 537 millilitres

ammonium hydroxide (specific gravity 0·960) shall be added slowly, the flask being cooled. When the flask and contents are cooled to 20°C. distilled water shall be added to the mark. The specific gravity

this solution shall be 1·082 to 1·083 and 1 millilitre

the solution shall contain 42 milligrams

nitrogen.

(2)Sulpho-molybdate solution : 100 grams

ammonium sulphate shall be transferred to a 2-litre volumetric flask and 900 millilitres

concentrated nitric acid shall be added. The mixture shall be shaken by hand. (A complete solution

the ammonium sulphate is not necessary). 300 grams

ammonium molybdate shall be dissolved in 800 millilitres

boiling water. The solution shall be cooled to room temperature and added cautiously to the ammonium sulphate-nitric acid mixture, shaking well after each addition. The mixture shall be again cooled to room temperature and made up to the mark with water. After 2 or 3 days the solution shall be filtered and stored in a cool and dark place.

(3)Acid mixture : 750 millilitres

concentrated nitric acid shall be mixed with 800 millilitres

water ; 60 millilitres

concentrated sulphuric acid shall then be added.

(4)Nitric acid (specific gravity 1·19 to 1·21) : 500 millilitres

concentrated nitric acid shall be added to 700 millilitres

water.

(5)Ammonium nitrate solution : 20 grams

ammonium nitrate shall be dissolved in a litre

water and nitric acid shall be added until the solution is distinctly acid to litmus. (iii) The procedure shall be as follows : 2 grams

the sample shall be transferred to a 500 millilitre Wagner shaking bottle. 100 millilitres

distilled water shall be added, followed by 100 millilitres

reagent

(1). The bottle shall then be placed in an end over end shaking apparatus and rotated for 1 hour at 40 revolutions per minute. The solution shall then be made up to the mark with reagent
(1). The solution shall then be filtered, the first 20 millilitres

the filtrate being discarded. 10 to 20 millilitres

the filtrate (containing not more than 10 milligrams

phosphorus) shall be transferred to a 250 to 300 millilitre beaker, water being added when necessary to give a final volume

20 millilitres. 50 millilitres

reagent

(3)or reagent
(4)if the sample contains sufficient sulphate) shall then be added. The beaker shall be heated until the solution begins to boil. It shall then be removed from the heat and the solution stirred. 50 millilitres

reagent

(2)shall immediately be added by means

a pipette taking care that the reagent does not touch the side

the beaker. Within 4 minutes after the addition

the reagent the solution shall be stirred for 30 seconds. The solution shall be allowed to stand overnight and filtered, with suction, through a weighed Gooch crucible. The beaker and crucible shall be washed with 4 x 10 millilitre portions

reagent

(5). The Gooch crucible shall then be placed on a second (dry) suction flask and washed first with 10 millilitres and then with 5 millilitres

acetone (analar quality). After the last washing, the suction shall be increased to remove the last traces

acetone from the precipitate and maintained for 1 minute more. The Gooch crucible shall then be removed and placed in a desiccator containing 40 per cent. sulphuric acid for 4 hours. The crucible shall be weighed and replaced in the desiccator until constant weight is obtained. The weight

the precipitate multiplied by 0·01426 shall be taken as the weight

phosphorus. From the result so obtained shall be deducted the quantity (if any)

water soluble phosphorus as determined as described in subparagraph (b)

this paragraph and the difference (if any) shall be taken as the quantity

citrate soluble phosphorus. Citrate insoluble phosphorus. (i) Citrate insoluble phosphorus shall be determined as follows : the quantity

phosphorus soluble in ammonium citrate solution, determined as described in subparagraph (h)

this paragraph ending with the words " The weight

the precipitate multiplied by 0·01426 shall be takenas the weight

phosphorus " shall be deducted from the quantity

phosphorus determined in accordance with subparagraph (c)

this paragraph and the difference (if any) shall be taken to be the quantity

phosphorus insoluble in ammonium citrate solution. Determination

potassium

(7)(a) Determination

potassium shall be effected as specified in the subsequent subparagraphs

this paragraph. Salts

potassium. (b) Salts

potassium shall be determined as follows : a quantity

the sample, about 2·5 grams in weight, accurately weighed, shall be heated nearly to boiling point with 10 millilitres

concentrated hydrochloric acid and 50 millilitres

water, breaking down with a stirring rod any crystals or lumps. It shall be diluted with water to about 100 millilitres and shall be boiled gently for a few minutes. It shall then be cooled, made up to 250 millilitres, or to such larger volume that 50 millilitres shall contain about 0·025 to 0·08 gram

potassium, and filtered. The potassium shall be determined in the filtrate as described in subparagraph (e)

this paragraph. Potassium in mixed fertilisers containing little or no organic matter. (c) Potassium in mixed fertilisers containing little or no organic matter shall be determined as follows : a quantity

the sample, about 2·5 grams in weight, accurately weighed, shall be boiled for 30 minutes with 125 millilitres

water and 50 millilitres

saturated ammonium oxalate solution. If necessary, a small quantity

a potassium-free anti-foaming agent may be added. It shall then be cooled, a slight excess

ammonium hydroxide added, made up to 250 millilitres, or to such larger volume that 50 millilitres shall contain about 0·025 to 0·08 gram

potassium, and filtered. The potassium shall be determined in the filtrate as described in subparagraph (e)

this paragraph. Potassium in mixed fertilisers containing organic matter. (d) Potassium in mixed fertilisers containing organic matter shall be determined as follows : 10 grams

the sample shall be gently incinerated at a temperature not exceeding 500°C. in order to destroy organic matter. The residue shall be boiled for 30 minutes with 125 millilitres

water and 50 millilitres

saturated ammonium oxalate solution. It shall then be cooled, a slight excess

ammonium hydroxide added, made up to 500 millilitres, or to such larger volume that 50 millilitres shall contain about 0·025 to 0·08 gram

potassium, and filtered. The potassium shall be determined in the filtrate as described in subparagraph (e)

this paragraph. Precipitation

potassium as potassium chloroplatinate. (e) Precipitation

potassium as potassium chloroplatinate shall be effected as follows : 50 millilitres

the filtrate, or such smaller quantity diluted to 50 millilitres as shall contain about 0·025 to 0·08 gram

potassium shall be transferred to a digestion flask

capacity about 300 to 500 millilitres, together with 10 millilitres

concentratednitric acid. If desired a small silica bead or granule weighing about 0·25 gram may be added to prevent bumping. This shall have been previously tared with a prepared Gooch crucible or sintered glass crucible having an average pore diameter

5 to 15 microns. The mixture shall be boiled for 2 minutes and 10 millilitres

concentrated hydrochloric acid shall be added. It shall be boiled down to approximately 25 millilitres and 5 millilitres

concentrated hydrochloric acid and an excess

platinum chloride solution over that required by the total alkalies present shall be added. The platinum chloride solution shall contain 0·5 gram

platinum in 10 millilitres. The mixture shall be boiled down to 10 to 15 millilitres, rotating the flask occasionally and 5 millilitres

concentrated hydrochloric acid added. The heat shall be reduced and the mixture boiled down to 3 to 5 millilitres (depending on the amount

precipitate), rotating the flask frequently near the end

the evaporation. The flask shall be removed from the heat and swirled to dissolve any soluble residue on the walls. It shall be cooled and 25 millilitres

95 per cent. alcohol shall be immediately added so that it washes completely the neck

the flask. The flask shall be chilled under running water, swirled and allowed to stand for at least 5 minutes. The contents

the flask shall be decanted into the tared crucible, suction applied, and the precipitate, together with the silica bead or granule if used, shall be transferred to the tared crucible with a stream

95 per cent. alcohol and thoroughly washed. The suction shall be reduced and the precipitate carefully washed with 2 or 3 portions

10 millilitres each

a 20 per cent. aqueous solution

ammonium chloride saturated with potassium chloroplatinate at the temperature

washing and filtered immediately before use. Suction shall be increased and the precipitate washed 4 to 5 times with 10 millilitre portions

the wash solution. Finally the precipitate shall again be washed thoroughly with 95 per cent. alcohol. The crucible and contents shall be dried at 100°C. and weighed. The precipitate shall be calculated to its equivalent

potassium by multiplying its weight by 0·16084. Determination

boron.

(8)Determination

boron shall be effected as follows : a weighed quantity

the sample, from 2 to 5 grams depending on its probable boron content, shall be transferred to a 200 millilitre round-bottomed flask. 5 millilitres

orthophosphoric acid and 20 millilitres

methanol shall be added, and the flask shall be connected with a Liebig condenser by means

a short glass tube passing through the stopper

the flask. 100 millilitres

95 per cent. methanol shall be placed in a second 200 millilitre round-bottomed flask, which shall then be set in a water bath and connected to the first flask by means

a short bent glass tube passing through the stopper

the second flask and connected by rubber tubing to a long bent glass tube passing through the stopper

the first flask and reaching almost to the bottom. A receiving flask shall be placed in position, and sufficientheat applied to the water bath to keep a steady flow

bubbles

methanol passing through the first flask. In order to keep the volume in the first flask at about 25 millilitres, a little heat shall be applied. The distillation shall be continued until 100 millilitres

distillate is obtained (about 30 minutes). 2 or 3 drops

phenolphthalein and sufficient 0·1 N sodium hydroxide to produce a permanent pink colour shall then be added to the distillate. The receiving flask shall be stoppered, vigorously shaken and connected at once with the condenser by means

a splash head. The methanol shall be distilled

f, using a water bath, until the volume is reduced to about 10 millilitres. The residue shall be transferred to a platinum or porcelain dish, using as little water as possible, and shall be evaporated to dryness on the water bath. The contents

the dish shall be ignited below redness (450°C.) and shall then be cooled and acidified with a few drops

N hydrochloric acid. 20 to 25 millilitres

distilled water shall then be added. The solution shall be heated for 1 to 2 minutes on a steam bath and shall then be filtered into a 200 millilitre round-bottomed flask, the filter paper being thoroughly washed. The filtrate shall be diluted to 50 to 75 millilitres with distilled water. The flask shall be attached to an air condenser, and the contents shall be boiled gently for a few minutes to remove carbon dioxide. 3 or 4 drops

methyl red indicator shall then be added, followed by 0·1 N sodium hydroxide until the red colour just disappears. There shall then be added about 1 gram

mannitol, or a smaller quantity if only a little boron is thought to be present. 2 or 3 drops

phenolphthalein indicator shall be added, and the solution shall be titrated with 0·1 N sodium hydroxide. The reagents used for the analysis shall be tested by a " blank " determination. If the sodium hydroxide is free from carbon dioxide, the " blank " shall not be more than 0·2 millilitre. The result shall be calculated in accordance with the formula, 1 millilitre

0·1 N NaoH=0·00108 gram B., and shall be expressed in terms

percentage

boron. Determination

the neutralising value

a liming material

(9)Determination

the neutralising value

a liming material shall be effected as follows : a representative portion

the sample shall be dried in oven maintained at a temperature between 100°C. and 105°C. until two successive weighings after cooling in a desiccator, at intervals

not less than 3 hours in the oven, show an increment

loss

not more than 0·1 per cent.

the original weight. The material shall then be ground (if necessary) to a degree

fineness which permits the whole amount to pass through a No. 60 test sieve conforming to Irish Standard 24 : 1950 and shall be placed in an airtight container. A quantity

the material about 1 gram in weight, weighed to an accuracy

1 milligram, shall be transferred to an Erlenmeyer flask

about 250 millilitre capacity, and 50 millilitres

0·5 N hydrochloric acid shall be added. A small funnel shall be placed in the neck

the flask. The contents shall be heated, maintained at gentle boiling for 5 minutes, and then cooled. The residual acid shall be determined by titration against 0·25 N sodium hydroxide, using phenolphthalein as indicator. The weight

calcium carbonate equivalent to the weight

hydrochloric acid which has been neutralised by the material shall be calculated and shall be expressed as a percentage

the weight

the material. This result shall be reported as the neutralising value. 10 Manner

analysis

feeding stuffs, compound feeding stuffs and mineral mixtures. 10.—

(1)The manner in which a sample

a feeding stuff, compound feeding stuff or mineral mixture shall be analysed for the purposes

the Act shall be as specified in the subsequent paragraphs

this Article. Determination

moisture (loss on drying).

(2)Determination

moisture (loss on drying) shall be effected as follows : a representative portion

the sample shall be weighed, with precautions against loss

moisture. It shall then be dried in a ventilated oven maintained at a temperature between 100°C. and 105°C. until two successive weighings after cooling in a desiccator, at intervals

not less than 3 hours in the oven, show an increment

loss

not more than 0·2 per cent.

the original weight. The loss in weight, calculated as a percentage

the original weight, shall be taken to be the moisture content.

(3)Preparation

the sample for analysis (other than determination

moisture). (a) Preparation

the sample for analysis (other than determination

moisture) shall be effected as specified in the subsequent subparagraphs

this paragraph. Sample in fine condition. (

  1. b)If the sample is in a fine condition and passes through a sieve having apertures about one millimetre square, it shall be thoroughly mixed and a portion not less than 100 grams in weight shall be placed in a stoppered bottle. From this portion the quantities for analysis shall be taken. Sample passing through sieve having apertures from two to three millimetres square. (
  2. c)If the sample does not wholly pass through a sieve having apertures about one millimetre square and wholly passes through a sieve having apertures from two to three millimetres square, it shall be thoroughly mixed and a portion for the determination

the moisture shall be at once taken. Sample in coarse condition. (d) If the sample is in a coarse condition, it shall be carefully pulverised until the whole passes through a sieve having apertures from two to three millimetres square. It shall then be thoroughly mixed and a portion for the determination

the moisture shall be at once taken. Further powdering. (e) From the mixed sample as specified in subparagraph (c)

this paragraph, or from the coarsely crushed sample as specified in subparagraph (d)

this paragraph, a portion not less than 100 grams in weight shall be taken and further powdered and passed through a sieve having apertures about one millimetre square. The portion

the sample so prepared shall be placed in a stoppered bottle and from it the quantities for analysis shall be taken. Original sample appreciably moist. (f) If the original sample is appreciably moist, or if for any reason the operations

pulverisation and mixing are likely to result in loss or gain

moisture, the moisture in the bottled portion shall be determined as well as in the portion taken for that purpose under subparagraph (c) or (d)

this paragraph in order that the results

the analysis may be corrected to correspond with the sample in its original condition as regards moisture. Mixing in other cases. (g) Materials which cannot be conveniently pulverised or passed through a sieve shall be thoroughly mixed by the most suitable means. Determination

oil.

(4)Determination

oil shall be effected as follows : a weighed quantity

the sample shall be placed in an extraction thimble, which shall then be placed in an extraction apparatus and extracted with petroleum ether (b. pt. 40-60°C.). At the end

3 to 4 hours the thimble shall be removed from the apparatus, dried and its contents finely ground, preferably with sand, in a small mortar previously rinsed with petroleum ether. The substance shall then be returned to the thimble, the mortar being washed out with petroleum ether, and the extraction continued for another hour. The extract should be free from suspended matter. After evaporation

the solvent, the oil shall be dried at 100°C. and weighed. Determination

protein.

(5)(a) Determination

protein shall be effected as specified in the subsequent subparagraphs

this paragraph. Crude protein. (b) (i) The percentage

crude protein shall be ascertained by multiplying the percentage

nitrogen, other than nitrogen present as ammoniacal or nitric nitrogen, by 6·25. The presence

nitrogen in these latter forms shall be tested for (according to the methods for determination

ammoniacal nitrogen and nitric nitrogen specified in subparagraph

(5)

Article 9

these Regulations) and the quantity so present, if any, shall be determined and deducted from the total nitrogen. (ii) The determination

total nitrogen in the absence

nitrates shall be effected as follows :— A weighed portion

the sample shall be transferred to a Kjeldahl digestion flask, 25 millilitres

concentrated sulphuric acid (or more if necessary) shall be added and the flask gently heated until frothing ceases. 10 grams

potassium or sodium sulphate (anhydrous) shall then be added and the flask further heated until the colour

the clear liquid ceases to diminish. The heating shall be continued for an hour thereafter to ensure complete oxidation

the organic matter. The operation may be accelerated by the addition

a suitable catalyst (e.g. copper sulphate or mercury or a mixture

mercuric oxide and selenium) to the liquid in the digestion flask. The quantity

ammonia present in the liquid shall be determined by distillation into standard acid after liberation with alkali and, where mercury or mercuric oxide has been used, with the addition also

sodium or potassium sulphide solution or sodium thiosulphate. The materials used shall be examined as to their freedom from nitrogen by means

a control experiment carried out under similar conditions with the same quantities

the reagents which have been employed in the actual analysis, 1 gram

pure sugar being used in place

the weighed portion

the sample. The quantity

standard acid found to have been neutralised in this control experiment shall be deducted from the total quantity

acid neutralised in the distillation

the sample. If nitrates are present, the digestion and subsequent distillation shall be carried out as specified in clause (i)

subparagraph (d)

paragraph

(5)

Article 9

these Regulations. True protein (

  1. c)(
  2. i)True protein shall be determined as follows : 0·7 gram

the sample shall be placed in a beaker and 100 millilitres

water shall be added. If the sample is

a substance rich in starch, the mixture shall be heated on a steam bath for 10 minutes ; in any other case, the mixture shall be heated to boiling. There shall be added such a quantity

the cupric hydroxide reagent prepared as described in clause (ii)

this subparagraph, as shall contain about 0·5 gram cupric hydroxide. The mixture shall be stirred thoroughly, filtered when cold, and washed with cold water without removing the precipitate from the filter. The percentage

nitrogen in the precipitate shall be determined as described in subparagraph (c)

paragraph

(5)

Article 9

these Regulations. That percentage multiplied by 6·25, shall be taken to be the percentage

true protein contained in the sample. If the sample is

a substance rich in alkaline phosphates, 1 or 2 millilitres

10 per cent. solution

ammonia-free sodium aluminium sulphate shall, before the addition

the cupric hydroxide, be added to the mixture in order to prevent the formation

cupric phosphate and free alkali and the consequent partial solution

the copper-protein precipitate in the alkaline liquid. (ii) Cupric hydroxide shall be prepared as follows : 100 grams

crystalline copper sulphate shall be dissolved in 5 litres

water. There shall beadded 2·5 millilitres

glycerol and then 10 per cent. sodium hydroxide solution until the liquid is slightly alkaline. The mixture shall be filtered and the precipitate rubbed in a mortar with water containing 5 millilitres

glycerol per litre. The precipitate shall be washed by decantation or filtration until the washings are no longer alkaline. The precipitate shall be again rubbed in a mortar with water containing 10 per cent.

glycerol until a uniform gelatinous mass measurable by pipette is produced. The quantity

cupric hydroxide in 5 millilitres shall be determined by diluting to 50 millilitres with water, filtering, washing, igniting, and weighing as cupric oxide. Determination

fibre.

(6)(a) Determination

fibre shall be effected as specified in the subsequent subparagraphs

this paragraph. Preparation

Buchner funnel. (b) The Buchner funnel shall be prepared as follows : The holes shall be covered with a disc

cotton cloth cut from bleached cotton drill conforming to the following specification : Threads per half inch : Warp, 50 : Weft, 34 : Weight per linear yard, 28 inches wide : 6½ oz. Boiling water shall be poured into the funnel and allowed to remain until the funnel is hot, whereupon suction shall be applied. Procedure (c) 2 or 3 grams, accurately weighed, shall be extracted with petroleum ether (b. pt. 40-60°C.) in an extraction apparatus, the residue dried and transferred to a litre conical flask. The material must not be further ground during extraction. A volume

200 millilitres

a solution containing 1·25 grams

sulphuric acid per 100 millilitres measured at ordinary temperature and brought to boiling point, shall be added to the flask and heated. The contents

the flask must come to boiling within 1 minute and the boiling throughout must be gentle and continuous for exactly 30 minutes, the original volume being maintained. The flask shall be rotated every few minutes in order to mix the contents and remove particles from the sides. At the end

30 minutes the flask shall be removed and the contents shall be poured at once into a Buchner funnel prepared as described in the previous subparagraph. After filtration

the bulk

the 200 millilitres through the Buchner funnel the residue shall be washed with hot water until the washings are free from acid. The residue shall then be washed from the disc

cotton cloth back into the flask with 200 millilitres

a solution

sodium hydroxide, containing 1·25 grams

sodium hydroxide per 100 millilitres free or nearly free from sodium carbonate, measured at ordinary temperature and brought to boiling point. The contents

the flask shall be boiled for exactly 30 minutes, the precautions given for thetreatment with acid being observed. At the end

30 minutes the flask shall be removed and its contents immediately filtered through a disc

cotton cloth, as before. The residue collected on the disc shall be washed with hot water until free from acid and then transferred to a beaker with hot water from a wash bottle. The contents

the beaker shall then be filtered through a prepared Gooch crucible, the beaker and crucible being washed several times with hot water. The residue in the Gooch crucible shall be washed twice with 95 per cent. alcohol, and 3 times with ether and dried at about 100°C. in an oven until the weight

the crucible and its contents is found to be constant. The contents

the crucible shall then be incinerated at a dull read heat. The weight

the crucible and its contents after incineration shall be subtracted from the weight

the crucible and its contents immediately before incineration and the difference (if any) shall be reported as fibre. Determination

phosphorus.

(7)Determination

phosphorus shall be effected as follows : a weighed portion

the sample shall be treated as described in clause (iii)

subparagraph (c)

paragraph

(6)

Article 9

these Regulations and the phosphorus in an aliquot part

the solution obtained thereby shall be determined by the method described in clause (iv)

that subparagraph. Determination

betacarotene.

(8)Determination

betacarotene shall be effected as follows : 1 or 2 grams

the sample, depending on its probable betacarotene content, shall be boiled with 50 millilitres

petroleum ether (b. pt. 80-100°C.) in a large Kjeldahl flask on a steam bath for an hour. The flask and its contents shall then be cooled and the liquid decanted onto a column

bone meal previously wetted with petroleum ether (b. pt. 40-60°C.). Light suction shall be applied to the bone-meal column so that the eluate drops slowly through. The flask and the residue therein shall be repeatedly rinsed with small quantities

petroleum ether (b. pt. 40-60°C.), each rinsing being passed through the column, until a colourless eluate appears. The total eluate obtained shall then be made up to 200 millilitres and the betacarotene content shall be determined colorimetrically by means

an absorptiometer or a spectrophotometer. Determination

ash.

(9)Determination

ash shall be effected as follows : a weighed quantity

the sample, from 2 to 5 grams, shall be transferred to a suitable dish and incinerated at a temperature not exceeding 500°C. The dish and contents shall be cooled, weighed, and the percentage

ash calculated. Determination

sand and silicious matter.

(10)Determination

sand and silicious matter shall be effected as follows : the ash obtained by the method described in paragraph

(9)

this Article shall be moistened with hydrochloric acid and evaporated to dryness and shall then be repeatedly extracted with hot dilute hydrochloric acid (1 part

concentrated hydrochloric acid to 4 parts

water). The solution shall be filtered and the insoluble matter washed, incinerated and weighed. The quantity obtained shall be taken as sand and silicious matter. Determination

calcium.

(11)Determination

calcium shall be effected as follows : 0·4 gram

ash obtained by the method described in paragraph

(9)

this Article shall be transferred to a 250 millilitre beaker and about 6 millilitres

water and 10 millilitres

concentrated hydrochloric acid shall be added. The beaker and contents shall be heated on a steam bath for a few minutes until decomposition is complete. The solution shall then be diluted to about 50 millilitres and heated almost to boiling. About 100 millilitres

a hot (90°C.) 5 per cent. ammonium oxalate solution, together with a few drops

0·1 per cent. methyl orange, shall then be added. The calcium oxalate shall be precipitated (at an initial temperature

about 80°C.) by adding successive drops

a solution

ammonia obtained by mixing 1 volume

water with 1 volume

ammonia solution (specific gravity 0·880) until a pH

approximately 4 is seen to be obtained by comparison

the colour

the solution with the colour

an equal volume

0·1 molar potassium hydrogen phthallate containing the same quantity

indicator. The solution shall be allowed to stand for 20 minutes and then filtered through a prepared Gooch crucible. The beaker and precipitate shall be well washed with 8 or 10 portions (amounting in all to not more than 100 millilitres)

very cold water. The crucible and its contents shall be transferred to the original beaker, and about 100 millilitres

water and 5 to 6 millilitres

concentrated sulphuric acid shall be added. The solution shall be titrated at about 90°C. with 0·1 N potassium permanganate which shall have been standardised under the same conditions against standard sodium oxalate dried at 110°C. The result shall be calculated in accordance with the formula : No.

millilitres

0·1 N K Mn 04 x 1·25==the percentage

CaCO3 present when 0·4 gram sample is used. Determination

magnesium.

(12)Determination

magnesium shall be effected as follows : an accurately weighed quantity

the sample, equivalent to not more than 2 grams

magnesium, shall be transferred to a large conical flask, to which 30 millilitres

concentrated hydrochloric acid shall be added. The flask shall be rotated so as to facilitate the elimination

carbon dioxide. 70 millilitres

water shall then be added. The solution shall be heated to boiling-point and allowed to stand on the steam-bath for 1 hour. The contents

the flask shall then be filtered, with suction, through a small Buchner funnel and washed with small quantities

hot water. The filtrate shall be cooled and then transferred to a 200 millilitre graduated flask and diluted to volume with water. An aliquot portion (X millilitres)

the filtrate, containing the equivalent

approximately 0·1 gram

magnesium, shall be transferred to a beaker, to which 10 per cent. ammonium carbonate solution shall be added dropwise until a white precipitate is produced. The precipitate shall be just dissolved by the careful addition

0·5 N hydrochloric acid solution. 15 per cent. ferric chloride solution shall then be added dropwise until a yellow colour is produced, at which point 2 grams

sodium acetate trihydrate shall be added. The mixture shall be stirred and more ferric chloride added until a brown colour is produced in the solution. The solution shall then be diluted to about 400 millilitres with water, and boiled for 1 minute. The contents

the flask shall then be filtered, with suction, through a Buchner funnel and washed with hot water. The filtrate shall be transferred to a litre beaker and, if necessary, made slightly acid with 0·5 N hydrochloricacid solution. 1 gram

oxalic acid and 2 grams

ammonium chloride shall then be added. The whole shall be heated to boiling-point and made slightly alkaline—to litmus—by the dropwise addition

dilute ammonia solution. The precipitate shall be allowed to settle for no more than 15 minutes, then filtered, with suction, through a Buchner funnel and washed with hot water. The filtrate shall be transferred to a large beaker and 10 millilitres

20 per cent. diammonium hydrogen phosphate solution added, following which the whole shall be boiled. (If a precipitate is produced at this stage it shall be dissolved by the addition

the minimum quantity

concentrated hydrochloric acid). 30 millilitres

strong solution

ammonia shall then be added. The beaker shall be allowed to stand on the steam-bath for at least 4 hours. Its contents shall then be filtered through a filter paper and washed with 2 per cent. ammonia solution until free from chloride. The filter paper shall be transferred to a tared platinum crucible, moistened with a few drops

ammonium nitrate solution, dried, and finally ignited in a muffle furnace to constant weight. The content

magnesium present in the sample shall be calculated in the following manner :— Determination

salt (sodium chloride).

(13)Determination

salt (sodium chloride) shall be effected as follows : 5 grams

the sample shall be mixed with 1 gram

pure sodium carbonate and thoroughly wetted with a little water. The mixture shall be dried and heated to a temperature not exceeding 500°C. in order to destroy organic matter. The residue shall be extracted with water, the volume made up to 250 millilitres and the solution filtered. The chlorine shall be determined, by titration with silver nitrate, in an aliquot portion

the filtrate and the percentage

sodium chloride calculated. Determination

manganese (acid soluble).

(14)(a) Determination

manganese (acid soluble) shall be effected as specified in the subsequent subparagraphs

this paragraph. (b) A reagent shall be prepared as follows : 1·4383 grams

potassium permanganate shall be dissolved by boiling with water, then diluted to 1 litre and allowed to stand for several days. The solution shall then be filtered through an asbestos pad on a Gooch crucible and standardised with sodium oxalate. The solution so obtained shall contain at least 500 parts per million

manganese. An aliquot part

the solution containing 20 milligrams

manganese shall be transferred to a beaker. 100 millilitres

water, 15 millilitres

orthophosphoric acid and 0·3 gram

potassium periodate shall then be added. The solution shall be brought to boiling point, cooled and then diluted to 1 litre. The solution shall be protected from light. The solution (containing 20 parts per million

manganese) shall be diluted with water which has been boiled with 0·3 gram

potassium periodate per litre, to make convenient working standards

known concentrations approximately the same as those to be compared. Procedure (c) The procedure shall be as follows : a weighed quantity

the sample containing from 5 to 15 grams shall be incinerated at dull red heat in a porcelain dish and subsequently cooled. The ash so obtained shall be transferred to a beaker with 20 to 30 millilitres

water ; 5 millilitres

concentrated sulphuric acid and 5 millilitres

concentrated nitric acid shall then be added and the mixture evaporated to white fumes. Further quantities

concentrated nitric acid may be added until the carbon is destroyed. The mixture shall then be cooled slightly and transferred to a 100 millilitre volumetric flask. 50 millilitres

dilute orthophosphoric acid (8 + 92) shall then be added. The mixture shall be cooled and diluted to volume with water, mixed and either filtered or allowed to stand until clear. 50 millilitres

clear solution shall then be pipetted into a 100 millilitre flask, followed by 30 millilitres

water. The solution so obtained shall be heated nearly to boiling point with stirring. 0·3 gram

potassium periodate shall be added for each 15 milligrams

manganese present. The solution shall be maintained at 90-100°C. for 30 to 60 minutes or until colour development is complete. The solution shall next be cooled and diluted to 100 millilitres ; and shall then be compared with standard potassium permanganate solution (prepared as described in subparagraph (b)

this paragraph) using a colorimeter or spectrophotometer at 530 mµ. The content

manganese present in the sample shall then be calculated. Determination

cobalt.

(15)(a) Determination

cobalt shall be effected as specified in the subsequent subparagraphs

this paragraph. Reagents. (

  1. b)Reagents shall be prepared as follows : (
  2. i)Cobalt sulphate solution : 0·2385 gram

cobalt sulphate shall be dissolved in water and diluted to 1 litre. (1 millilitre

this solution is equal to 0·05 milligram

cobalt). The solution shall be diluted to a suitable concentration to prepare standard curve. (ii) Nitroso—R salt solution : 1 gram

Nitroso—R salt shall be dissolved in water and diluted to 500 millilitres. (iii) Spekker acid : 150 millilitres

85 per cent. orthophosphoric acid shall be mixed with 150 millilitres

concentrated sulphuric acid and the mixture diluted with water to 1 litre. (iv) Sodium acetate solution : 500 grams

crystalline sodium acetate shall be dissolved in water and the solution made up to 1 litre. Standard curve (c) A standard curve shall be prepared as follows : to 1, 2, 3 etc. millilitres

reagent (i) in 100 millilitre volumetric flasks shall be added 2 millilitres

reagent (iii),10 millilitres

reagent (ii) and 10 millilitres

reagent (iv), A " blank " shall be prepared by using 2 millilitres

reagent (iii) and 10 millilitres

reagent (iv), omitting reagent (ii). The standards and " blank " shall be brought to the boil on a hot plate. 5 millilitres

concentrated nitric acid shall be added and the solutions boiled for a period between 1 and 2 minutes. The solutions (standards and blank) shall be cooled and diluted with water to 100 millilitres. A standard curve shall then be plotted from these solutions using a colorimeter or spectrophotometer. Procedure. (d) The procedure shall be as follows : 2 grams

the sample shall be weighed and incinerated for 2 hours at 600°C. The ash shall be transferred to a 200 millilitre volumetric flask with 20 millilitres

hydrochloric acid and 50 millilitres

water. The mixture shall be boiled for 5 minutes, cooled and diluted to volume with water. The precipitate shall be allowed to settle and a suitable aliquot

the clear liquid shall be pipetted into a small flask. (In the case

samples containing 0·01 to 0·2 per cent. cobalt, an aliquot corresponding to 0·25 gram

the sample shall be used. In the case

other samples the aliquot shall be so chosen that it contains not more than 0·5 milligram

cobalt). A brisk current

hydrogen sulphide shall then be passed through the solution for 10 minutes. The solution shall next be filtered into a 100 millilitre volumetric flask through Whatman No. 40 filter paper and then washed with about 50 millilitres

1 per cent. sulphuric acid, which has been saturated with hydrogen sulphide. 2 small glass beads shall be added and the hydrogen sulphide shall then be boiled

f. Each flask shall be given individual attention and shaken

ten. 5 millilitres

concentrated citric acid shall then be added and the solution boiled until nitrous fumes no longer appear. The solution shall be removed from the hot plate at first indication

bumping and cooled. 2 drops

phenolphthalein shall be added and the solution brought to the first faint pink with about a 30 per cent. sodium hydroxide solution. 2 millilitres

reagent (iii) shall immediately be added, followed by 10 millilitres

reagent (ii) and 10 millilitres

reagent (iv). The mixture shall then be brought to boil vigorously. 5 millilitres

concentrated nitric acid shall then be carefully added, and the mixture boiled for not less than 1 but not more than 2 minutes. The solution shall be cooled and diluted to volume with water. Its colour shall be compared with that

standard cobalt solution, in a colorimeter (using green or No. 54 filter) or in spectrophotometer at 540 mµ. The colour shall be read within 2 hours and the content

cobaltpresent in the sample shall then be calculated from the standard curve. Determination

Copper.

(16)(a) Determination

copper shall be effected as specified in the subsequent subparagraphs

this paragraph. Preparation

standard curve. (b) A standard curve shall be prepared as follows : 1·9645 grams

crystalline copper sulphate shall be dissolved in water and diluted to 500 millilitres. (1 millilitre

this solution is equal to 1 milligram

copper). From 1 to 10 millilitres

this solution shall be used to prepare a set

standards in 100 millilitre Pyrex glass-stoppered volumetric flasks. 4 millilitres

concentrated hydrochloric acid shall be added and the solution diluted to 50 millilitres. 5 millilitres

tetraethylenepentamine shall then be added ; the solution so obtained shall be diluted to mark with water, stoppered and subsequently mixed. A " blank " shall be prepared by using all reagents except copper. The standards and " blank " shall be filtered before reading colour, as indicated in the determination referred to in the next subparagraph. A standard curve shall then be plotted from these solutions, using a colorimeter or spectrophotometer. Procedure. (c) The procedure shall be as follows : 8 grams

the sample shall be weighed and incinerated for 2 hours at 600°C. The ash shall be transferred to a 200 millilitre volumetric flask with 20 millilitres

hydrochloric acid and 50 millilitres

water. The mixture shall be boiled for 5 minutes, cooled and diluted to volume with water. The precipitate shall be allowed to settle. A 50 millilitre aliquot

the clear liquid shall be pipetted into a 100 millilitre Pyrex glass-stoppered volumetric flask. 5 millilitres

tetraethylenepentamine shall be added, the solution diluted to volume with water, stoppered and mixed thoroughly. The solution shall then be filtered and the colour compared with the standards within 30 minutes in a colorimeter (red or No. 66 filter) or shall be read in a spectrophotometer at 620 mµ. The content

copper present in the sample shall then be calculated from the standard curve. Determination

Iodine.

(17)Determination

iodine shall be effected as follows : a weighed portion

the sample containing 3 to 4 milligrams

iodine shall be placed in a 200-300 millilitre nickel dish. There shall be added about 5 grams

anhydrous sodium carbonate, 5 millilitres

sodium hydroxide solution (1 + 1) and 10 millilitres alcohol, care being taken to ensure that the entire sample is moist. The dish and its contents shall be dried at 100°C. for about 30 minutes and then heated in a muffle furnace to 500°C. the temperature being maintained at 500°C. for 15 minutes. The dish and contents shall then be cooled. 25 millilitres

water shall be added and the dish then covered with a watch glass,the contents being boiled gently for 10 minutes. The contents

the dish shall then be transferred on to filter paper 18 centimetres in diameter. The dish and paper shall be washed with boiling water into a 600 millilitre beaker until the filtrate is approximately 300 millilitres. The filtrate shall be neutralised to methyl orange with 85 per cent. orthophosphoric acid adding 1 millilitre

acid in excess. Excess bromine water shall be added and the solution boiled until colourless and for a further five minutes thereafter. A few crystals

salicylic acid shall then be added and the solution cooled to about 20°C. 1 millilitre

85 per cent. orthophosphoric acid and about 0·5 gram

potassium iodide shall be added and the solution titrated with 0·005 N sodium thiosulphate. The content

iodine present in the sample shall then be calculated. Determination

Iron.

(18)(a) Determination

iron shall be effected as specified in the subsequent subparagraphs

this paragraph. Preparation

standard curve. (b) A standard curve shall be prepared as follows : a solution containing 50 parts per million solution

iron shall be prepared and the following quantities transferred to colorimeter tubes marked at 10 millilitres—0·4, 0·8, 1·2, 1·6 and 2·0 millilitres, giving 20, 40, 60, 80 and 100 milligrams

iron respectively. To each tube shall then be added 1 millilitre

20 per cent. citric acid solution and sufficient distilled water to bring the volume to approximately 5 millilitres. A " blank " shall be prepared by adding to another tube 1 millilitre

20 per cent. citric acid solution and 4 millilitres

distilled water. To each tube shall be added 3 drops

thioglycollic acid followed, after the contents have been thoroughly mixed, by such quantity (about 4 millilitres)

10 per cent. ammonia solution as will suffice to produce a stable reddish colour. The contents

each tube shall then be diluted to volume with water and mixed thoroughly. A standard curve shall then be plotted from these solutions using a colorimeter or spectrophotometer. Procedure. (c) The procedure shall be as follows : a sample containing about 1 milligram

iron shall be transferred to a 100 millilitre conical flask. 4 grams

citric acid and 80 millilitres

water shall then be added. The contents shall be well mixed and then allowed to stand for about 1 hour. The mixture shall then be diluted to volume and filtered. A 5 millilitre aliquot

the solution so obtained shall be transferred to a marked colorimeter tube, to which 3 drops

thioglycollic acid shall be added, followed by 10 per cent. ammonia solution dropwise until a stable reddish colour develops (care being taken to avoid adding excess ammonia). This solution shall be diluted to 10 millilitres with water and the colour compared with the standards in a colorimeter or spectrophotometer. The content

iron present in the sample shall then be calculated from the standard curve. 11 Form

certificate

result

analysis. 11. For the purposes

sections 3 and 8

the Act, the prescribed form

the result

the analysis shall be such one

the forms set out in the Third Schedule to these Regulations as may be applicable to the case. 12 Prohibition

sale and manufacture for sale

certain compound feeding stuffs 12. A person shall not sell or manufacture for sale any compound feeding stuff the ingredients

which include any one or more

the following articles : (

  1. a)cocoa shells whether alone or mixed with any other article and whether whole or ground, (
  2. b)corozo nut meal, (
  3. c)grass seed cleanings, (
  4. d)hoof meal or horn meal or any other substance produced by the grinding

hoofs or horns, (e) husks derived from the milling or dehulling

oats, hulls so derived, or shudes so derived, whether such husks, hulls or shudes are alone or are mixed with any other article and whether they are whole or ground, (f) a by-product

oat-milling which contains, if it is unground, more than 20 per cent.

fibre or, if it is ground, more than 16 per cent.

fibre. 13 Restriction

manufacture for sale

fertilisers, compound feeding stuffs and mineral mixtures. 13.—

(1)A person shall not manufacture for sale— (
  1. a)any fertiliser, (
  2. b)any compound feeding stuff other than any mixture which consists solely

— (i) any two or more

the following articles : ground barley, flaked barley, crushed barley, ground wheat, flaked wheat, crushed wheat, ground maize, flaked maize, crushed maize, ground milo maize, flaked milo maize and crushed milo maize, (ii) two or more by-products

oat-milling none

which is husks derived from the milling or dehulling

oats, hulls so derived, or shudes so derived, or (iii) molasses and sugar beet pulp, or (c) any mineral mixture, save under and in accordance with a licence granted to him by the Minister under these Regulations.

(2)A licence granted by the Minister under (a) the emergency Powers (Manufacture and Sale

Fertilisers) Order, 1944 (S. R. & O. No. 49

1944), or (b) Article 3

the Emergency Powers (Feeding Stuffs) Order, 1944 (S. R. & O. No. 196

1944), or (c) the Emergency Powers (Manufacture and Sale

Mineral Mixtures) Order, 1944 (S. R. & O. No. 50

1944), in force immediately before the commencement

these Regulations shall, on and after such commencement, be deemed to be a licence under these Regulations. 14 Prohibition

sale

certain articles as feeding stuffs. 14. A person shall not sell as a feeding stuff— (

  1. a)any cocoa shells, whether whole or ground, (
  2. b)any husks derived from the milling or dehulling

oats, hulls so derived, or shudes so derived, whether such husks, hulls, or shudes are alone or are mixed with any other article and whether they are whole or ground, (c) any article which— (i) has been produced by grinding any by-product

oat-milling other than husks, hulls, or shudes, or (ii) is a mixture, whether whole or ground,

two or more such by-products and contains more than 16 per cent.

fibre, or (d) any article which purports to consist wholly or mainly

oatmeal and which contains more than 5 per cent.

fibre. 15 Restriction

sale

grass meal. 15.—

(1)A person shall not sell grass meal under the description

High Grade or Grade I unless it contains at least 16 per cent. protein and 220 parts per million

carotene.

(2)A person shall not sell grass meal under the description

Standard Grade or Grade II unless it contains at least 14 per cent. protein and 150 parts per million

carotene.

(3)A person shall not sell as a feeding stuff any grass meal unless it contains at least 14 per cent. protein. 16 Restriction

sale

meat and bone meal. 16. A person shall not sell any feeding meat and bone meal containing less than 40 per cent.

protein. 17 Exception for sales for export. 17. Sales for export shall be excepted from the application

Articles 14, 15 and 16

these Regulations. 18 Prohibition

bringing

certain articles into certain premises. 18. A person shall not bring into any premises where any feeding stuff, compound feeding stuff or mineral mixture intended for sale is manufactured, packed, stored or sold, any husks derived from the milling or dehulling

oats, hulls so derived, or shudes so derived, whether such husks, hulls, or shudes are alone or are mixed with any other article and whether they are whole or ground. Article 3

(1). FIRST SCHEDULE. A mixture consisting solely

any two or more

the following articles : ground barley, flaked barley, crushed barley, ground wheat, flaked wheat, crushed wheat, ground maize, flaked maize, crushed maize, ground milo maize, flaked milo maize and crushed milo maize. Antibiotic feed supplements. Barley meal. Bean meal. Beet pulp (whether wet, dried or pressed). Brewery grains, distillery grains or grains part

which consists

brewery grains and the remainder

which consists

distillery grains. Dried molassed beet pulp. Flaked barley. Flaked maize. Flaked milo maize. Flaked oatmeal. Flaked wheat. Ground oats, crushed oats or rolled oats. Ground wheat. Maize meal (Indian meal). Milo maize meal. Molasses or treacle. Oatmeal. Pea meal. Vitamin supplements containing synthetic vitamins. Wheat

fals. Article 3

(2)(e). SECOND SCHEDULE. Article Particulars to be contained in Statement Blood meal Amount

oil ; minimum amount

crude protein. Bone flour or bone meal Minimum amounts

phosphorus and calcium, respectively. Coconut or copra cake or meal Amount

oil ; minimum amount

crude protein. Cotton cake or meal or cotton seed meal Amount

oil ; minimum amount

crude protein; whether decorticated or undecorticated. Dried yeast Minimum amount

crude protein. Earth nut or ground nut cake or meal Amount

oil ; minimum amount

crude protein ; whether decorticated or undecorticated. Feeding meat and bone meal, or any other product

meat (including whale meat) and bone for feeding purposes Amount

oil ; minimum amounts

crude protein, phosphorus and calcium, respectively. Feeding meat meal, or any other product

meat (including whale meat) for feeding purposes Amount

oil ; minimum amounts

crude protein, phosphorus and calcium respectively. Fish meal—including any product (other than shark meal) obtained by drying and grinding or otherwise treating fish or fish waste Amount

oil ; minimum amounts

crude protein, phosphorus and calcium, respectively. Article Particulars to be contained in Statement Grass meal, lucerne meal, or clover meal—in any form Minimum amounts

crude protein and betacarotene, respectively. Linseed cake or meal Amount

oil ; minimum amount

crude protein. Locust bean meal Amount

oil ; minimum amount

crude protein. Malt culms Minimum amount

crude protein ; maximum amount

fibre. Oat dust or other by-product

oat milling Minimum amount

crude protein ; maximum amount

fibre. Palm kernel cake or meal Amount

oil ; minimum amount

crude protein. Rape cake or meal Amount

oil ; minimum amount

crude protein. Sesame cake or meal Amount

oil ; minimum amount

crude protein. Shark meal Amount

oil ; minimum amount

true protein. Soya bean cake or meal Amount

oil ; minimum amount

crude protein. Sunflower cake or meal Amount

oil ; minimum amount

crude protein; whether decorticated or undecorticated. Article 11. THIRD SCHEDULE. FORM F.F.1 (a). Ref. No................ CERTIFICATE

RESULT

ANALYSIS

A LIMING MATERIAL. Sample

............................................................ ...marked............................................................ .................... received by the State Chemist on............................................................ ....................................................... from............................................................ ............................................................ ........................................ (taken at the premises

............................................................ ............................................................ .....). This is to certify that the above-mentioned sample, which was duly fastened and sealed, has been analysed by...................................... under the direction

the State Chemist or the Assistant State Chemist and that the result

the analysis is as follows :— per cent. Neutralising value, expressed in terms

calcium carbonate ..................... Fineness:

(1)Amount found to pass through a prescribed 1/8 inch sieve .....................
(2)Amount found to pass through a prescribed No. 100 sieve ..................... *On comparison

the result

the analysis with the particulars accompanying the sample it appears that the particulars furnished— *are correct, subject to the prescribed limits

error. *are not correct, subject to the prescribed limits

error, in the following respects :— This certificate is given under section *3/8*

the Fertilisers, Feeding Stuffs and Mineral Mixtures Act, 1955. Date.................... Signed................... State Chemist. *Delete if inapplicable. Form F. F. 1 (b). Ref. No............... CERTIFICATE

RESULT

ANALYSIS

A FERTILISER OTHER THAN A LIMING MATERIAL. Sample

............................................................ .. marked............................................................ ............. received by the State Chemist on............................................................ ................................................ from............................................................ ............................................................ ....................................... (taken at the premises

............................................................ ............................................................ ..). This is to certify that the above-mentioned sample, which was duly fastened and sealed, has been analysed by...........................under the direction

the State Chemist or the Assistant State Chemist and that the result

the analysis is as follows : Per cent. Nitrogen ....................................... Phosphorus Water Soluble ...................................... Citric Acid Soluble ....................................... Citrate Soluble ....................................... *Water/*Citric Acid/*Citrate insoluble. ....................................... Potassium ...................................... *Amount found to pass through a prescribed No. 100 sieve ....................................... *On comparison

the results

the analysis with the particulars accompanying the sample it appears that the particulars furnished— *are correct, subject to the prescribed limits

error. *are not correct, subject to the prescribed limits

error, in the following respects :— This certificate is given under section *3/*8

the Fertilisers, Feeding Stuffs and Mineral Mixtures Act,

  1. Date....................................................... Signed.................................... State Chemist. Form F.F.
  2. Ref. No................ CERTIFICATE

RESULT

ANALYSIS

A FEEDING STUFF OR A COMPOUND FEEDING STUFF (OTHER THAN A MINERAL MIXTURE). Sample

............................................................ ............. marked............................................................ ...... received by the State Chemist on............................................................ ....................................................... from............................................................ ............................................................ ......................................... (taken at the premises

............................................................ ............................................................ .......).. This is to certify that the above-mentioned sample, which was duly fastened and sealed, has been analysed by............................ under the direction

the State Chemist or the Assistant State Chemist and that the result

the analysis is as follows :— Per cent. Oil ................................... Protein (*crude/*true) ................................... Fibre ................................... *On comparison

the result

the analysis with the particulars accompanying the sample it appears that the particulars furnished— *are correct, subject to the prescribed limits

error. *are not correct, subject to the prescribed limits

error, in the following respects :— *Delete if inapplicable. This certificate is given under section *3/*8

the Fertilisers, Feeding Stuffs and Mineral Mixtures Act,

  1. Date............................................................ .......... Signed.............................................. State Chemist. Form F.F.
  2. Ref. No................... CERTIFICATE

RESULT

ANALYSIS

A MINERAL MIXTURE. Sample

............................................................ ....... marked............................................................ ............... received by the State Chemist on............................................................ ....................................................... from............................................................ ............................................................ .......................................... (taken at the premises

............................................................ ............................................................ ....).. This is to certify that the above-mentioned sample, which was duly fastened and sealed, has been analysed by.................... under the direction

the State Chemist or the Assistant State Chemist and that the result

the analysis is as follows :— Per cent. Calcium .................................... Phosphorus .................................... Salt (sodium chloride) .................................... Magnesium .................................... Manganese (acid soluble) .................................... Cobalt .................................... Copper .................................... Iodine .................................... Iron .................................... *On comparison

the result

the analysis with the particulars accompanying the sample it appears that the particulars furnished— *are correct, subject to the prescribed limits

error. *are not correct, subject to the prescribed limits

error, in the following respects :— This certificate is given under section *3/8*

the Fertilisers, Feeding Stuffs and Mineral Mixtures Act, 1955. Date............................................................ ........ Signed.............................................. State Chemist. GIVEN under my

ficial Seal, this 20th day

December, 1957. (Signed) PATRICK SMITH Minister for Agriculture. EXPLANATORY NOTE. The Regulations control the sale and manufacture for sale

fertilisers, feeding stuffs and mineral mixtures and provide for the sampling and analysis

such articles. *Delete if inapplicable. *Delete if inapplicable. Privacy Statement Accessibility European Legislation Identifier (PDF) Open Data License Ráiteas Príobháideachais Inrochtaineacht Aitheantóir Eorpach Reachtaíochta (ELI) Ceadúnas Sonraí Oscailte Liosta Fianán © Government

Ireland. Oireachtas Copyright Material is reproduced with the permission

the Houses

the Oireachtas © Rialtas na hÉireann. Atáirgtear ábhar faoi Chóipcheart le cead ó Thithe an Oireachtais

🔗 To official source

AI explanation based on the official legal text. Indicative, not a substitute for legal advice.