DRAFT KENYA STANDARD     DKS 05-524: 2009 
                                                       ICS 67.060 
 
 
 
 
 
 
 
 
 
 
 
 
Pasta products -  Specification 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
© KEBS 2009        Fourth Edition 2009 
 
 
 
 KS 05-524: 2009                                                                                         ©KEBS  
2 TECHNICAL COMMITTEE REPRESENTATION 
 
The following organizations were represented on the  Technical Committee: 
 
National Cereals and Produce Board 
Ministry of Health — Department of Public Health 
— Division of Nutrition 
Egerton University 
Pembe Flour Mills Ltd. 
Nestle Foods 
Unga Ltd. 
Cap[well Industries Ltd 
Proctor and Allan (EA) Ltd. 
Ministry of Trade and Industry — Department of Indu stry 
Government Chemist’s Department 
Jambo Biscuits Ltd. 
Consumer Information Network (CIN) 
Kenyatta National Hospital 
Kenya Bureau of Standards ― Secretariat 
 
 
 
 
 
 
 
REVISION OF KENYA STANDARDS  
 
In order to keep abreast with the progress in the i ndustry, Kenya standards shall be regularly reviewe d. 
Suggestions for improvement of published standards are welcome and should be addressed to the 
Managing Director, Kenya Bureau of Standards. 
 
 
 
 
 
 
 
 
© Kenya Bureau of Standards, 2009 
 
Copyright. Users are reminded that by virtue of Sect ion 25 of the Copyright Act, Cap. 12 of 2001  of the  Laws of Kenya, 
copyright subsists in all Kenya Standards and except as provided under Section 26 of this Act, no Kenya Sta ndard 
produced by Kenya Bureau of Standards may be reproduce d, stored in a retrieval system in any form or tran smitted by 
any means without prior permission in writing from the Managing Director. 
 
 
 
 
 
 
 
 
 
 
 
 
 DRAFT KENYA STANDARD          DKS 05-524: 2009  
3  
        
 
 
 
 
 
 
 
 
 
 
 
Pasta products -  Specification 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
KENYA BUREAU OF STANDARDS (KEBS) 
 
Head Office:  P.O. Box 54974, Nairobi-00200, Tel.: (+254  020) 6054 90, 602350, Fax: (+254 020)  604031 
E-Mail: info@kebs.org,  Web:http://www.kebs.org  
 
Coast Region    Lake Region         Rift Valley Regi on  
P.O. Box 99376, Mombasa-80100  P.O. Box 2949, Kisumu-401 00       P.O. Box 2138, Nakuru-20100 
Tel.: (+254  041) 229563, 230939/40 Tel.: (+254 057 ) 23549, 22396       Tel.: (+254 051) 210553, 21055 5  
Fax: (+254  041) 229448   Fax: (+254 057) 21814 
 
 
 
 
 
 
 KS 05-524: 2009                                                                                         ©KEBS  
4  
 
 
Foreward 
 
This Draft Kenya Standard has been revised by the T echnical Committee on Processed Cereals and Pulses 
under the guidance of the Standards Project Committ ee, and it is in accordance with the procedures of the 
Kenya Bureau of Standards. 
 
Macaroni, Spaghetti, Vermicelli, etc. belong to a c lass of products generally known as pasta products.   
These products have gained fast popularity in cater ing and home use. 
 
The manufacturing process for macaroni or spaghetti  consists of dough preparation from durum wheat (ha rd 
wheat) and cold or lukewarm water, kneading process  and extrusion through the extrusion press fitted w ith a 
die for the desired shape.  The extruded products a re cut to a given length and then dried to a defini te 
moisture content under controlled temperature and h umidity. 
 
This revision aimed at updating various parameters in line with the best international practice.  
 
During the preparation of this standard reference w as made to the following documents: 
 
 IS 1485: Specification for macaroni, spaghetti and  vermicelli. 
 
 Sri Lanka Standard 420: Specification for pasta pr oducts (macaroni, spaghetti, vermicelli and noodles ). 
 
The assistance received from the above documents is  acknowledged with thanks. 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 DRAFT KENYA STANDARD          DKS 05-524: 2009  
5  
 
 
 
 
Pasta products - Specification 
 
1. Scope 
 
This Kenya Standard prescribes the requirements and  methods of test for pasta products. 
 
2. Types 
 
 Pasta products covered in this standard shall be o f the following types: 
  
(a) Macaroni 
(b) Spaghetti 
(c) Vermicelli 
(d) Noodles 
(e) Short-cut pasta 
(f) Lasagne 
 
3. Requirements 
 
3.1 Basic Ingredients — The dough for the manufacture of pasta products sha ll either be prepared 
from semolina derived from durum grains, hard wheat  varieties or any combination of two or more of 
the specific wheat flours. 
 
 
3.2 Description  
 
3.2.1 Macaroni — It shall be in the form of tubes of a minimum lengt h of 250 mm.  Outer diameter of the 
tube  shall  range  from 2.5 mm  to 7 mm  and  the  wall thickness shall be 1.0 mm with tolerance of 
± 0.1 mm. 
 
3.2.2 Spaghetti  — It shall be in the form of solid rods of a minimum length of 250 mm and minimum 
diameter of 1.6 mm with tolerance of ± 0.1 mm. 
 
3.2.3 Vermicelli  —  It shall be in the form of solid rods of minimum le ngth 250 mm and of diameter 
between 0.5 mm to 1.25 mm. 
 
3.2.4 Folded Vermicelli  — They shall be in the form of folded rods of diam eter between 0.5 mm to 1.25 
mm. 
 
3.2.5 Noodles  — They shall be in the form of solid rods of minim um length 250 mm and diameter between 
1.25 mm and 2.0 mm or ribbons of width from 1.5 mm to 15 mm and thickness ranging from 1.25 
mm to 2.0 mm. 
 
3.2.6 Folded Noodles  — These shall be in the form of folded ribbons of thickness ranging from 1.25 mm to 
2.0 mm. 
 
3.2.7 Short-cut Pasta  — These shall be products of various defined forms  such as shells, stars, squares, 
etc. 
 
3.2.8 Lasagne  — These shall be square or rectangular shaped past a products. 
 
3.2.9 Special Type Pasta  — These may contain eggs or vegetable products and  the final products shall 
have the appearance of the characteristic added mat erial such as yellow for egg pasta and green for 
spinach pasta. KS 05-524: 2009                                                                                         ©KEBS  
6  
3.2.10  Egg Pasta  — The egg macaroni, egg spaghetti, egg noodles or egg alimentary pasta shall contain 
not less than 4 per cent egg yolk solids when teste d according to the method in Appendix H. 
 
The egg yolk solids shall be derived from whole egg , frozen  egg yolk. 
 
3.3 Other Physical Characteristics  —  Pasta products shall be smooth, translucent, har d brittle and 
up to a point elastic, and when broken the fracture  shall appear glassy. 
 
3.3.1  The products shall not contain any added colouring  matter. 
 
3.3.2  Pasta products shall retain their shapes and show no sign of disintegration and shall swell 
appreciably when plunged into vigorously boiling wa ter and boiled in accordance with the time 
declared by the manufacturer for each variety of th e products. 
 
3.3.3  When cooked, pasta product shall retain its shape and a certain firmness and develop a clear 
characteristic odour of hard wheat and shall not be come pasty. 
 
3.4 Chemical Requirements  
 
3.4.1  Moisture Content  — Moisture content of macaroni, spaghetti, vermice lli, folded vermicelli noodles 
and folded noodles shall be not more than 13 per ce nt m/m when tested according to the method in 
Appendix A. 
 
3.4.2 The moisture content for short-cut pasta shall be n ot more than 13 per cent m/m when tested 
according to the method in Appendix A. 
 
3.4.3  Pasta products shall also comply with the composit ional requirements given in Table 1. 
 
 
 
TABLE 1.  COMPOSITIONAL REQUIREMENTS FOR PASTA PROD UCTS 
 
  
 
SL No. 
  
CHARACTERISTIC  
REQUIREMENT  
METHOD OF TEST 
 
(i) 
 
 
(ii) 
 
 
(iii) 
 
 
(iv) 
 
 
(v) 
 
 
 
(vi)  
Total ash (on dry basis) per cent 
by mass, max. 
 
Acid insoluble ash (on dry basis) 
per cent by mass, max. 
 
Total protein (N x 5.7) (on dry 
basis) per cent by mass, min. 
 
Cooking test: Total solids in gruel, 
per cent by mass, max. 
 
Free fatty acids as oleic acid of 
extracted oil, per cent by mass, 
max. 
 
Crude fibre content per cent by 
mass, max.  
 
1.0  
 
 
0.05 
 
 
10.5 
 
 
10 
 
 
 
0.8 
 
 
0.45  
 
B 
 
 
C 
 
 
D 
 
 
E 
 
 
 
F 
 
 
G 
 
 
 
 
 
 DRAFT KENYA STANDARD          DKS 05-524: 2009  
7 4. Hygiene 
 
4.1  Pasta products shall be manufactured in premises c omplying with the hygienic practices stipulated in 
the Public Health Act, Cap. 242, the Food, Drugs an d Chemical substances Act, Cap. 254 of the 
Laws of Kenya  and KS 05-1500, Code of practice for  food and drink manufacturing industry. 
 
4.2  The finished products shall be free from cracks, o ff-flavour, insect infestation, foreign matter and 
adulterants. 
 
4.3  The level of total aflatoxin in pasta products sha ll not exceed 10 ppb, wherein aflatoxin B 1 shall not 
be more than 5 ppb when tested according to KS ISO 16050 
 
4.4  When tested in accordance with the methods stipula ted in KS 05-220 *, pasta products shall be free 
from pathogenic organisms and shall comply with mic robiological limits stipulated in Table 2. 
 
TABLE 2. MICROBIOLOGICAL LIMITS FOR PASTA PRODUCTS 
 
SL No TYPE OF MICRO-ORGANISM MAXIMUM LIMIT OF COUNT S 
 
(i) 
 
(ii) 
 
(iii) 
 
(iv) 
 
(v)  
Total viable counts 
 
E. Coli 
 
Salmonella in 30 g 
 
Yeasts and moulds 
 
Staphylococcus aureus  
               10 4 per g 
 
Shall be absent 
 
Shall be absent 
 
                10 2 per g 
 
Shall be absent 
 
 
5.  Food additives  
 
Only the food additives permitted for use in pasta products by the Food, Drugs and Chemicals Substance s 
Act Cap 254 of the Laws of Kenya, CODEX STAN 195: C odex General Standard for food additives or KS 
660 Guide to the safe use of food additives may be used for the intended purpose within the specified limits.  
 
6. Packaging  
 
6.1 The product shall be packed in food grade material that shall ensure product safety and integrity. 
 
6.2  The fill of the package shall comply with the Weig hts and Measures Act, Cap. 513 of the Laws of 
Kenya. 
 
7 Labelling 
 
7.1   Labelling of dry milled maize meal products shall  be done in accordance with the provisions of KS 40  
In addition, the following shall be legibly and ind elibly marked: 
(i) Name of product. 
 
(ii) Name, physical location and address of manufac turer. 
 
(iii) List of ingredients. 
 
(iv) Net contents in g or kg. 
 
(v) Date of manufacture. 
 
                                                 
* Methods for the microbiological examination of foo ds. KS 05-524: 2009                                                                                         ©KEBS  
8 (vi) Batch number. 
 
(vii) Expiry date. 
 
(viii) The declaration ‘Made in Kenya’ or country o f origin for imported products. 
 
(ix) The recommended cooking time for the pasta pro ducts. 
 
 
7.2 Any Health and/or Nutrition claim on maize flou r shall conform to the provisions of KS CAC/GL 23 
Guidelines for nutrition and health claims.  
 
 
 
 
 
 
 
 
 
 
 
A P P E N D I X   A 
 
DETERMINATION OF MOISTURE  
 
 
A1. PROCEDURE  
 
A1.1  Preparation of Sample   —  Grind in pestle and mortar about 30 g of the m aterial so that at least 90 
per cent passes through 425 micro sieve.  Transfer this prepared sample to a well-stoppered glass 
bottle for use as indicated in A1.2  and D3.1 . 
 
A1.2  Weigh accurately about 5 g of the prepared sample in a suitable moisture dish made of  porcelain, 
silica or platinum, previously dried in an air-oven  and weighed.  Place the dish in an air-oven 
maintained at 105 ± 2°C for five hours.  Cool the d ish in a desiccator and weigh the dish with the lid  
on.  Heat again at 105 ± 2°C in the air-oven for 30  minutes, cooling and weighing till the difference 
between two successive weighings is less than one m illigram.  Note the lowest mass. 
 
 NOTE : Preserve the dish containing the dried material f or the determination of ash ( see  B1 ). 
 
A2. CALCULATION  
 
Moisture, per cent by mass  = 
M1M)2M1(M  
−−100 
 
 
 where, 
 
  M1 = mass in g of the dish with the material before d rying, 
 
  M   = mass in g of the empty dish, and 
 
  M2 = mass in g of the dish with the material after dr ying. 
 
 
 
 
 
 
 
 DRAFT KENYA STANDARD          DKS 05-524: 2009  
9  
 
 
 
 
 
 
A P P E N D I X   B 
 
DETERMINATION OF TOTAL ASH  
 
B1. PROCEDURE  
 
 Ignite the dried material ( see  A1.2)  in the dish with a flame of suitable burner for ab out one hour till 
the material is completely charred.  Complete the a shing by keeping in a muffle furnace at 600 ± 
20°C until  grey ash results.  Cool in a desiccator and weigh.  Repeat the process of heating for 30 
minutes, cooling and weighing till the difference i n mass between two successive weighings is less 
than one milligram.  Note the lowest mass. 
 
 NOTE:  Preserve the dish containing this ash for  the det ermination of acid insoluble ash ( see  C2 ). 
 
B2. CALCULATION 
 
B2.1  Total ash (on dry basis), per cent by mass = 
M1MM) 2(M  
−−100 
   
           
 where, 
  
  M2  =  mass in g of the dish with the ash, 
 
  M   =   mass in g of the empty dish, and 
 
  M1  =  mass in g of the dish with the dried material ( see  M2 in A2 ). 
 
 
 
 
 
 
 
 
A P P E N D I X   C 
 
DETERMINATION OF ACID INSOLUBLE ASH  
 
C1. REAGENTS 
 
 Dilute Hydrochloric Acid  — Approximately 5 N prepared by diluting concentrated  hydrochloric acid 
with distilled water. 
 
C2. PROCEDURE 
 
 To the ash contained in the dish ( see  B1 ) add 25 mL of dilute hydrochloric acid, cover with  watch-
glass and heat on water-bath for 10 minutes.  Allow  to cool, filter the contents from the dish through  
Whatman filter paper No 42 or its equivalent.  Wash  the filter paper until the washings are free from 
the acid and return it to the dish.  Keep it in an air-oven maintained at 105 ± 2°C for about three 
hours.  With the flame  of a suitable burner, compl ete the ashing in a muffle furnace at 600 ± 20°C 
for one hour. Cool the dish in a desiccator and wei gh.  Heat again at 600 ± 20°C  in the muffle 
furnace for 30 minutes.  Cool the dish in the desic cator and weigh.  Repeat the process of heating KS 05-524: 2009                                                                                         ©KEBS  
10 for 30  minutes, cooling and  weighing till the difference in mass between succes sive weighings is less 
than 1 milligram.  Note the lowest mass. 
 
C3. CALCULATION 
 
 Acid insoluble ash (on dry basis), per cent by mas s  
M1MM) 2(M  
−−100 
 
     
 where, 
   
M2  = mass in g of the dish with acid insoluble ash, 
   
  M   = mass in g of the empty dish, and 
 
  M1  = mass in g of the dish with the dried material ( see  M2 in A2 ). 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
A P P E N D I X   D 
 
DETERMINATION OF TOTAL PROTEIN  
 
 
 
D1. APPARATUS  
 
 A recommended apparatus as assembled in Figure 1. DRAFT KENYA STANDARD          DKS 05-524: 2009  
11  
 
FIG. 1 – APPARATUS FOR DETERMINATION OF PROTEIN 
 
 
D1.1  Description  — The assembly consists of a round bottomed flask A o f 100 mL capacity fitted with a 
rubber stopper through which passes one  end of the  connecting bulb tube B.  The other end of the 
bulb is connected to the condenser C which is attac hed by means of a rubber tube to a dip tube D 
which dips into a known quantity of standard sulphu ric acid contained in beaker E of 250 mL 
capacity. 
 
D1.2  Kjeldahl Flask   — Of capacity 500 mL. 
 
D2. REAGENTS 
 
D2.1  Anhydrous sodium sulphate. 
 
D2.2 Copper sulphate. 
 
D2.3 Concentrated sulphuric acid.  
 
D2.4  Sodium Hydroxide Solution  — Dissolve about 225 g of sodium hydroxide in 500 mL of water. 
 
D2.5  Standard Sulphuric Acid  — 0.1 N. 
 
D2.6  Methyl Red Indicator Solution  — Dissolve one gram of methyl in 200 mL of rectified spirit (95 per 
cent by volume). 
 
D2.7  Standard Sodium Hydroxide Solution  — 0.1 N.  
 
D3. PROCEDURE 
KS 05-524: 2009                                                                                         ©KEBS  
12  
D3.1  Transfer carefully about one gram of the prepared sample ( see  A1.1 ), accurately weighed, to a 
Kjeldahl flask, taking precaution to see that parti cles of the material do not stick onto the neck of the 
flask.  Add about 10 g of anhydrous sodium sulphate , about 0.2 g to 0.3 g of copper sulphate and 20 
mL of concentrated sulphuric acid. 
 
 Add a few pieces of pumice stone to prevent bumpin g.  Place the flask in an inclined position.  Heat 
below the boiling point of the acid until frothing ceases.  Increase heat until acid boils vigorously  and 
digest for 30 minutes after the mixture becomes cle ar and pale green or  colourless.  Cool the 
content of the flask.  Transfer quantitatively to a  round bottomed flask, with distilled water, the to tal 
quantity of  distilled water used being about  200 mL.  Add about 50 mL of the sodium hydroxide 
solution (which is sufficient to make solution alka line) carefully through the side of the flask so th at it 
does not mix at once with the acid solution but for ms 3 layers below the acid solution. 
 
 Assemble the apparatus taking care that the dip tu be extends below the surface of the  standard 
sulphuric acid contained in the beaker.  Mix the co ntents of the flask by shaking and distill until al l 
ammonia has passed over into the standard sulphuric  acid.  Shut off the burner and immediately 
detach the flask from the condenser.  Rinse the con denser thoroughly with water into the beaker.  
Wash the dip tube carefully so that all traces of t he condensate are transferred to the beaker.  When 
all the washings have drained into the solution, ti trate with the standard sodium hydroxide solution. 
 
D3.2  Carry out a blank determination using all reagents  in the same quantities but without the material to  
be tested. 
 
D4. CALCULATION 
 
 Total protein (on dry basis, per cent by mass)   =  
M) (1MA)N (B 
−−
100  789  
 
where, 
 
  B   = volume in mL of the standard sodium hydroxide s olution used to neutralize the acid 
in the blank determination, 
 
A   = volume in mL of the standard sodium hyroxide s olution used to neutralize the 
excess of acid in the test with the material, 
 
N   = normality of  the standard sodium hydroxide so lution, 
 
M1  = mass in g of the prepared material taken for th e test, and  
 
M   = moisture, per cent by mass of the material ( see  A2 ). 
 
 
 
 
 
 
 
 
 
 
A P P E N D I X    E 
 
DETERMINATION OF TOTAL SOLIDS IN GRUEL  
 
 
E1. APPARATUS 
 
E1.1  Lipless Beaker — Tall-form, of capacity 500 mL. 
 DRAFT KENYA STANDARD          DKS 05-524: 2009  
13 E1.2  Oil Bath. 
 
E1.3 Electric Heater. 
 
E2. PROCEDURE  
 
Take 250 mL water in the lipless beaker and heat ov er an oil bath kept at about 102°C by electric 
heating.  Introduce exactly 25 g of the pasta produ ct (previously) broken into 10 mm lengths in case 
of long pasta products and cook at a constant tempe rature of about 98°C at sea level with 
occasional stirring. 
 
NOTE:  The cooking time required by this appparatus is on  an average two minutes more than 
that recommended on the package (i.e. more than tha t required with free boiling water).  
Allow the cooked pasta to drain for five minutes.  Measure the volume of gruel collected.  
Pipette out 20 mL of the gruel, after stirring well  to give an even distribution of the solid 
content, into a tared petri dish and evaporate to d ryness on a water-bath.  Transfer the 
petri dish and evaporate to dryness on a water-bath .  Transfer the petri-dish to a hot air-
oven maintained at 105 ± 2°C and dry to constant ma ss. 
 
E3. CALCULATION 
 Total solids in gruel, per cent by mass   
5)12( VMM−
=        
   
      
where, 
 
 M2  = mass in g of petri dish with total solids per cen t in 20 mL of gruel, 
 
 M1  =  mass in g of empty petri dish, and 
 
 V   =  volume of gruel in mL. 
 
 
 
 
 
 
 
 
 
 
 
 
 
 
 KS 05-524: 2009                                                                                         ©KEBS  
14  
A P P E N D I X   F 
 
DEGREE OF  ACIDITY OF RAW  PASTA  
 
F1. PROCEDURE 
 
Weigh 4 g of milled raw pasta into an Erlenmeyer fl ask and carefully suspend 100 mL of neutralized 
50 vol. per cent ethanol.  Stopper the flask to avo id solvent loss and leave for one hour at room 
temperature.  The contents should be whirled by han d four times during this period.  At the end, 
agitate the suspensions vigorously, clear by centri fuging (3 minutes at 300 rpm) or filtration (funnel  
sitting directly on the neck of another Erlenmeyer flask and flute paper filter (15 cm) covered with 
petri dish, both measures to avoid solvent losses).     The suspension shall be filtered in total and 
also 100 mL 50 vol. per cent neutralized ethanol sh all be filtered in the same way to be used as a 
blank (to compensate for any absorption on the filt er paper).   To 50 mL of the cleared-extract and 50  
mL of the filtered blank (in case of centrifuging n o blank is necessary), three drops of 1 per cent 
phenolphthalein in ethanol are added.  These aliquo ts are titrated with 0.1 N NaOH from a burette 
with  0.02 mL graduation  until the first reddish t int appears and remains visible for at least 10 s 
(change in colour from greenish yellow to reddish y ellow in sample extracts). 
 
F2. CALCULATION  
 
 Acidity degree (pasta dry matter)    = 
mnn
−−
 100 100  x 5 x )o (
  
 
 where, 
 
 n   =   mL 0.1 N NaOH for 50 mL extract, 
   
no   =  mL 0.1 N for 50 mL blank, and 
 
m   =     moisture content of raw pasta. 
 
 
 
 
 
 
 
 
A P P E N D I X   G 
 
DETERMINATION OF CRUDE FIBRE CONTENT 
 
 
G1. PREPARATION OF SAMPLE 
 
Break  the  pasta product into small fragments with  hands or in mill, and mix well.  Grind 300 g to 
500 g in mill until all material passes through No 20 sieve.  Keep ground sample in sealed container 
to prevent moisture changes. 
 
G2. REAGENTS 
 
G2.1  Sulphuric Acid Solution —  0.255 ± 0.005 N 1.25 g H 2SO 4/100 mL.  The concentration must be 
checked by titration. 
 
G2.2 Sodium Hydroxide Solution  — 0.313 ± 0.005 N 1.25 g  NaOH/100 mL, free or nea rly so from 
Na 2CO 3.  Concentration must be checked by titration. 
 DRAFT KENYA STANDARD          DKS 05-524: 2009  
15 G2.3 Prepared Asbestos  — Spread a thin layer of acid washed, medium or lo ng fibre asbestos in an 
evaporation dish and heat  for 16 h at 600 oC in furnace.  Boil for 30 minutes with 1.25 H 2SO 4, filter, 
wash thoroughly with water, and boil for 30 minutes  with 1.25 per cent NaOH.  Filter, wash once with 
1.25 g per cent, H 2SO 4, wash thoroughly with water, dry and ignite for 2 h at 600 oC. 
 
Determine blank by treating 1.0 g prepared asbestos  with acid and alkali.  Correct crude fibre results  
of any blank, which should be negligible (about 1 g ).  Asbestos  recovered from the determination 
may be used in subsequent  determinations. 
 
G2.4 Alcohol   — 95 per cent or reagent MeOH or isopropanol. 
 
G2.5  Antifoam Compound A  — Dilute (1 + 4) with mineral spirits or pot ether , or water, dilute antifoam B 
emulsion (1 + 4).  Do not use antifoam spray. 
 
G2.6 Bumping Chips or Granules  — Broken Alumdum crucibles or equivalent granules are satisfactory. 
 
G3. APPARATUS 
 
G3.1 Digestion Apparatus  — With condenser to fit 600 mL beaker, and  hot pl ate adjustable to 
temperature so that it will bring 200 mL water at 2 5 oC to rolling boil in 15 ± 2 minutes.  
 
G3.2  Ashing Dishes  — Silica, vireosil 70 mm x 15 mm;  or porcelain, c oors, No 450, size 1 or equivalent. 
 
G3.3 Desiccator  — With efficient desiccator such as 4 to 5 mesh dr ierite (CaCl 2 is not satisfactory). 
 
G3.4 Filtering Device  — With No 200 type 304 or 316 stainless steel scre en easily washed free of 
digested residue, use any suitable filter funnel e. g. Buchner filter funnel. 
 
G3.5 Suction Filter  — To accommodate filtering devices.  Attach suctio n flask to trap in line with aspirator 
or other source of vacuum with valve to break vacuu m. 
 
G3.6 Liquid Preheater — For preheating water, 1.25 per cent H 2SO 4 and 1.25 per cent NaOH solution to 
boiling point of H 2O. 
 
G4. PROCEDURE  
 
G4.1  Extract 2 g of ground  material with ether or pet ether.  Transfer to a 600 mL beaker avoiding fibre 
contamination from paper or brush.  Add about 1 g o f prepared asbestos, 200 mL boiling 1.25 per 
cent  H 2SO 4 and 1 drop diluted antifoam.  (Excess antifoam may  give results, use only if necessary 
to control foaming.)  Bumping chips of granules may  also be added.  Place the beaker on digestion 
apparatus with pre-adjusted hot plate and boil for exactly 30 min rotating the beaker periodically to 
keep solids from adhering to sides.  Remove the bea ker and any suitable filter funnel. 
 
G4.1.1  Treatment of Residue  — Dry mat and residue for 2 h at 130 ±  2 oC, cool in desiccator and weigh.   
Ignite for 30 min at 600 ± 15 oC.  Cool in a desiccator and reweigh. 
 
G5. CALCULATION 
 
Per cent  crude fibre in ground sample  
 
 C 
sample  of  Weight100)  x blank  asbestos  of   weightin  loss      ignition  on   weight in  (loss −=   
 
 Report results to 0.1 per cent. 
 
 
 
 
 
 
 
 KS 05-524: 2009                                                                                         ©KEBS  
16  
A P P E N D I X   H 
 
DETERMINATION OF EGG YOLK SOLIDS 
 
H1. PREPARATION OF SAMPLE 
 
 Grind in pestle and mortar about 30 g of the mater ial so that at least 90 per cent passes through 425  
micro sieve.  Transfer this prepared sample to a we ll-stoppered glass bottle for use. 
 
H2. PROCEDURE 
 
H2.1  Reflux 100 g sample in a Soxhlet apparatus using 1 00 cm 3 pure methanol for two hours.  Decant 
and add a further 100 cm 3 pure methanol fractions.  Evaporate to dryness.  C arry out a phosphorus 
determination as detailed below. 
 
H2.2 Phosphorus Determination 
 
 Weigh 0.05 g of sample into a platinum dish.  Add 5 cm 3 of analytical grade chloroform.  Add 8 cm 3 
of 4 per cent alcoholic potash and evaporate to dry ness in an oven held at 105 oC.  Char using an 
Argand burner and then ash at dull red heat in a mu ffle furnace.  When  the  dish  has  cooled,  add 
5 cm 3 concentrated hydrochloric acid and evaporate to dr yness.  Extract the residue with 10 cm 3 mL 
hydrochloric acid.  Filter through a Whatman No 54 grade filter paper into a 100 cm 3 graduated flask.  
Wash any residue well with hot distilled water.  Ne utralize with normal sodium hydroxide using 
phenolphthalein as indicator.  Make to the mark wit h distilled water. 
 
Take a sufficient volume, by pipette, of the prepar ed solution containing 5 to 5 mg phosphorus and 
transfer to a stout boiling tube. 
 
 The total volume should be 5 cm 3, if lower than this add distilled water.  Add, by  fast running pipette, 
1 cm 3 10 M sulphuric acid 1 cm 3 2.5 per cent ammonium molybdate and 1 cm 3 20 per cent 
potassium iodide solution (containing 0.5 per cent sodium carbonate).  Swirl stopper with a glass ball  
and hold in a boiling water bath for fifteen minute s.  Remove and cool in an ice bath. 
 
 Add sufficient freshly prepared 0.5 per cent sodiu m sulphate to remove the iodine colour and to give 
a light excess.  Transfer the solution and make up to 50 cm 3 in a graduated flask (or smaller volume 
if found necessary).  Measure the colour strength o f the solution when held in a 1 cm glass cell using  
14 and 608 filters on the Spekker absorptiometer.  Carry out a check on the absorptionmeter using 
distilled water in the cell.   Calculate the phosph orus content by reference to the reference curve fo r 
a standard phosphorus solution. 
 
 This solution can be prepared by dissolving 4.388 g analytical grade potassium dihydrogen 
phosphate in distilled water, adding 2 cm 3 in graduated flask.  The solution contains 1 000 µ g 
phosphorus/cm 3, lower concentrations can be obtained by dilution.   For comparison purposes, in a 
series of tests 1 µg phosphorus/cm 3 gave a Spekker absorptiometer of 0.285. 
 
H3. CALCULATION  
 
 Egg yolk solids  = P 2O5 x 56