-W- Sugarcane Sirup
August - 1957

VI INSPECTION OF THE PRODUCT (Continued)

F Grade Factors Rated by Score Points. (Continued)

2 Flavor.

Both the flavor and odor of the sirup should be con-
sidered in evaluating the factor of flavor. The method of
manufacture or type of sugarcane sirup is taken into consid-
eration in scoring this factor. The open pan sirup will be
noticeably different in flavor from sulfured sirup. However,
each type should be evaluated on its own merits regardless of
individual preference. The sirup should be free from fermented
or off flavors of any kind.

To receive a score of 27 to 30 points in the Grade A
classification, the product should have a good characteristic
flavor for the type, free from objectionable flavors caused by
scorching, fermentation, or any foreign or disagreeable flavor
regardless of origin.

A score of 2) to 26 points may be given to ‘the product
having a reasonably good flavor. A limiting rule in this clas-
sification prevents sugarcane that is scored in this classifica-
tion from grading above U. S. Grade B regardless of the total
score. As previously indicated, the product should be free
from objectionable or off flavors of any kind. When the product
received a score of 21 to 23 points for flavor, a limiting rule
applies and the sirup cannot be graded above U. S. Grade C.
Sugarcane sirup having a fermented or scorched flavor or any off
flavor, regardless of the cause, should be scored in the Sub-
standard classification and cannot be graded above Substandard
due to the application of a limiting rule.

3 Defects.

This factor refers to the degree of cleanliness of the
product and to the degree of freedom from harmless extraneous
material such as particles of sugarcane fiber or any particle
of earthy material or other defects which may be in suspension
or deposited as sediment in the container,


7 29 - . Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
B Total Sugars. (Continued)
1 Reducing sugars. (Continued)

f Determination of reducing sugars. (Continued)

error resulting from this titration will not generally
exceed 1 percent. For greater precision repeat the
titration, adding almost the entire sugar solution re-
quired to reduce all copper. Then boil for about 15
seconds and add further quantities until only a faint
blue color remains. Add 2-5 drops of methylene blue
indicator and complete titration. The flask should
remain on wire gauze over Bunsen flame or on hot plate
throughout entire titration except when it may be
removed for a few seconds and held against a sheet of
white paper to ascertain if the end point has been
reached. The edge of the liquid will appear bluish if
the indicator is not completely decolorized. Find

- factor in Table No. 4 or Table No. 5 corresponring to

H titer (number cc used for titration) and apply correc-

° - tion previously determined. Estimate as follows:

Factor x 100 + titer = mg of sugar in 100 ml
of sugar solution.

Example: 40 ml of sugar solution required for

titration -
Factor from table -- 124.8
Correction from standardization -- 46.0
Corrected factor -- 130.8

130.8 x 100 + 0 = 327 mg reducing

- sugars per 100 ml of sample
100 ml of sample solution = 1 gram.sample
Reducing sugars = 32.7%


- 25 - Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS
A Brix Solids.

The double-dilution method for determining Brix solids by
means of a Brix spindle is preferred and should be used in the
event there may be some controversy in regard to results in the
Brix determination. If desired, the Brix determination may also
be made on the undiluted sample. In offices supplied with a
refractometer, the refractometric method may be used. This is
perhaps the most convenient method of determining Brix, however,
lower results are obtained by the refractometer than by the
double-dilution method. For this reason the double-dilution
method should be used if there isa possibility that a controversy
may arise regarding the results of the Brix determination, or in
any case where the degrees Brix are on the borderline of minimm
requirements for the grade.

Sirup containing sugar crystals should be liquified by
heating to approximately 54.4° Cc. (130° F.) and cooled to approxi-
mately 20° c. (68° F.) or to room temperature before making Brix
determinations.

1 Double-dilution method.

Pour approximtely 250 grams of sirup into one liter
beaker and pour an equal weight of distilled water into a
second liter beaker. Mix the two completely by pouring alter-
nately from one beaker into the other several times. Pour the
double-diluted sirup into a hydrometer cylinder and place a
clean, dry Brix hydrometer of the necessary range (31° - 41°)
in the sirup, being careful not to immerse the hydrometer too
deeply and making certain that the hydrometer does not touch
the cylinder wall. Allow to stand 15-30 minutes to permit air
bubbles to escape. Take temperature of sirup in cylinder at
the time the Brix reading is taken. Multiply reading by two
and apply temperature correction to obtain Brix degree of
sirup.

2 Direct spindle method.

Pour well mixed sirup sample in cylinder and take Brix
as described above except that 5-60 minutes should be allowed
before Brix reading is taken. It is desirable to have sirup
samples at or close to room temperature before making Brix
determinations by spindle. Apply temperature corrections to
spindle readings found in Table No. 3.


- -3u- Sugarcane Sirup
~ August - 1957 a

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
B Total Sugars. (Continued)
2 Sucrose. (Continued)

a Sucrose by polarization method (1). (Continued)

iv Determination. (Continued)

adding anhydrous sodium carbonate, a little at a time,
avoiding any excess; mix well; filter again, rejecting
at least the first 25 ml of the filtrate. (Instead of
weighing 52 grams into a 200 ml flask, two 26-gram
portions may be diluted to 100 ml each and treated
exactly as described. Depemiing upon the color of the
product, multiples or fractions of the normal weight
may be used, and the results reduced by calculation to
the basis of 26 grams in 100 ml.) Pipet one 50-ml por-
tion of the lead-free filtrate into a 100-ml flask,
dilute with water to the mark; mix well; and polarize
in a 200 mm tube. The result, mltiplied by 2, is the
direct reading (P of formula given below) or polariza-
tion before inversion. A 400 mm tube may be used, in
which case the direct reading as taken equals P.

v_ Invert reading.

First determine the quantity of acetic acid
necessary to render 50 ml of the lead-free filtrate
distinctly acid to methyl red indication; then to
another, 50 ml of the lead-free solution in a 100 ml
volumetric flask add the requisite quantity of acid and
5 ml of the invertase preparation. Fill the flask with
water nearly to the 100 ml mark and let stand overnight,
preferably at a temperature of got less than 20° c,

Cool and dilute to 100 ml at 20 c. Mix well and polar-
ize at 20° c. in a 200 m tube. If in doubt as to
completion of hydrolysis, allow a portion of the solution
to remain for several hours and again polarize. If there
is no change in the previous reading, the inversion is
complete. Carefully note the reading and temperature of
the solution. If it is necessary to work at a tempera-
ture other than 20° c., which is permissible within
narrow limits, the solutions must be made up to volume
and both direct and invert readings must be made at the

Ny


-8- Sugarcane Sirup
August - 1957

IV CANNING PROCEDURES (Continued)
A Preparation for Canning. (Continued)

3 Cooling.

After filling, the cans should pass through a spray of
water to wash off any adhering sirup. The cans may then be
air-cooled before labeling and casing. If the cans are cased
and sealed before cooling, considerable caramelization is
likely to occur which will adversely affect the color and flavor
of the sirup.

kh Containers.

Plain cans or glass containers are ordinarily used for
Sugarcane sirup. These should be types of containers which
can be hermetically sealed, such as the double-seamed metal
containers and glass containers provided with a suitable metal
closure. The use of friction top metal containers is not
recommended for sugarcane sirup due to the increased hazard of
spoilage. However, this type of container is frequently used,
particularly by producers with small production capacity.

Vv FOOD AND DRUG REQUIREMENTS
A General Requirements.

The overall provisions of the Food, Drug, and Cosmetic Act
apply in general to canned sugarcane sirup. The product must be
packed under sanitary conditions, mst not be adulterated or con-
timated with decay, insects, or filth, and must be truthfully
labeled.

B Standard of Identity.

No standard of identity or quality has been issued by the
Food and Drug Administration for sugarcane sirup. However, under
an advisory standard adopted as a guide for enforcement officials
the product was defined as follows: "Cane sirup. Sirup made by
the evaporation of the juice of the sugarcane or by the solution of
Sugarcane concrete. It contains not more than 30 percent of water
and not more than 2.5 percent of ash.”


- 60- Sugarcane Sirup

August - 1957
Table No. 7
Conversion of Ounces Avoirdupois
to Fluid Ounces of Sugarcane Sirup
Fluid ounces
Net Weight: m° + 75° 4 769 § 779 18 78° + 792 & go?
02. AV. t prix * prix ? prix ? Brix ? Brix * prix ? Brix
No. 2 Can : : : i 2 2 H

22-1/2 15.73 15.66 15.59 15.51 9 15.bh 15.37 15.30
22-3/k 15.91 15.83 15.76 915.69 15.661 5.5h 15.7
23 16.08 16.01 15.93 15.86 15.78 15.71 15.64
23-1/u 16.26 16.18 16.11 16.03 15.95 15.88 15,81
23-1/2 16.43 16.35 16.28 «= 16.20, 16.13 16.05 ~S «15.98
23-3/b 16.61 16.53 16.45 16.37 16.30 16.22 16,15
2h 16.78 16.70 16.62 16.55 16.47 16.39 16.32
2hel/h 16.96 16.88 16.80 16.72 16.6h 16.56 16.49
2h-1/2 17.13, 17.0 16.97 16.89 16.81 16.73 16.66
2h-3/k 17.31 617.220 17.14 17.06 16.98 ~=— 16.90) 16.83
25 17.48 = 17.40 -17.32) 17.24 = 17.16) 17.08 ~=—:17.00
25-1/4 17.66 17.57 17.U9 17.1 17.33 17.25 17.17
25-1/2 17.83 17.75, 17.66 = 17.58 = 17.50 176h2S17.3h
25-3/4 18.00 17.92 17.84 917.75 = «17.67 17.59) 17.51
26 18.18 18.09 18.01 17.93 17.81 17.76 17.68
26-1/h, 18.35 18.27 18.18 18.10 18.01 17.93 17.85
26-1/2 18.53 18.4h 18.36 18.27 18.19 18.10 18.02
26-3/4 18.70 18.62 18.53  18.4h 18.36 18.27 18.19
27 18.88 18.79 18.70 18.62 18.53 18.44 18.35
27-174 19.05 18.96 18.88 18.79 18.70 18.61 18,52
27-1/2 19.23, 19.1, 19.05 18.96 18.87 18.78 18.69
27-3/4 19.40 19.31 19.22 «19.13, 19.0, += 18.95 = 18.86
28 19.58 19.49 19.40 19.30 19.21 19.12 19.03
28-1/4 19.75 19.66 19.57 19.48 19.39 19.30 19.20
28-1/2 19.93 19.83 19.7h 19.65 19.56 19.47 19.37


- lb - Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)

E Sulfated Ash.

Weigh S grams of sample into a 50-100 ml platinum dish
(silica dish may be used in place of platinum), add 5 ml of 10
percent sulfuric acid (H2S0), ) and ignite until sample is well
carbonized, and then burn in a muffle furnace at about 550° c.,
cool, add 2-3 ml of 10 percent sulfuric acid and evaporate on

a steam bath then to dryness on a hot plate, and again ignite
at about 550° C. to constant weight. Express result as percent

sulfated ash.

1 Sulfated ash (alternate method).

The following alternate method may be used and is
recommended for making routine ash determinations:

Weigh approximately 10 grams of double diluted sample
into a platinum dish (silica dish may be used in place of
platinum), add 5 ml of 10 percent sulfuric acid (or several
drops of concentrated sulfuric acid) and char carefully
under an infra-red lamp (it requires approximately 30 minutes).
Heat in a muffle furnace at 550° ¢, Remove, cool, and add

2-3 ml of 10 percent sulfuric acid and evaporate to dryness
under infra-red lamp. Reheat to constant weight in a mffle
furnace at 550° c. (The commercially available 250-watt
infra-red lamps are suitable for evaporation and charring.)

F Ratio of Sulfated Ash to Brix Solids.

Multiply the percent of sulfated ash by 100 and divide
by the Brix.

Example: Sulfated ash 1.5%
Brix 15

1.5 x 100 = 2.0% ratio of sulfated ash to Brix
75 solids.


- 42 - Sugarcane Sirup
August = 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued )

B Total Sugars. (Continued)

2 Sucrose. (Continued)

d Sucrose by volumetric method, Lane-Eynon (alternate

i

ii

method). (Continued)
Inversion. (Continued)

to mark. Leave flask in bath at 20° C. at least 30
minutes longer and finally make to exact volume and
mix well. Exactly neutralize the acid and again
determine the reducing sugars, calculating to invert
sugar, using invert sugar column alone as given in
Table No. or Table No. 5. Deduct the percent of
invert sugar obtained from inversion from that ob-
tained after inversion and multiply the difference
by 0.95 to obtain the percent of sucrose. The solu-
tions used in both determinations should be diluted
so that not more than 230 milligrams of invert sugar
is present in the quantity required for reduction. It
is important that all lead be removed from the solu-
tion with dry sodium oxalate before reduction.

Calculation.

Use Table No. 4 if 10 ml of copper solution
has been used and Table No. 5 if 25 ml of copper
solution has been used. Under the proper column
heading for the amount of sucrose present in 100 ml
of the solution tested and opposite the milliliters
of solution required to precipitate the copper as
found by titration (titer) is the invert sugar fac-
tor. The amount of invert sugar in 100 ml of the
test solution is the factor times 100 titer which is
calculated in the column opposite the factor.

oTM


- 48 - Sugarcane Sirup (~
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
I Foreign Material.

1 Examination for foreign material.

The following methods may be used in examining sugar-
cane sirup for foreign material:

& Method No. l.

Mix the sample thoroughly and dissolve 200 grams
in 200 ml of hot water acidulated with 5 ml of nitric
acid (HNO3). Filter at once through a em rapid filter
in suction funnel. Wash with a minimum quantity of hot
water and examine microscopically.

b Method No. 2.
Dissolve 200 grams of sugarcane sirup in 500 ml of
hot water. Filter at once through a United States Standard
No. 120 woven wire sieve. Wash with a minimum quantity of
hot water and examine microscopically,
2 Microanalysis.
Microanalysis should be made for worm and insect frag-

ments in accordance with methods outlined in the AOAC, Eighth
Edition, 1955.

REFERENCES: "Official Methods of Analysis of the Association of Official
Agricultural Chemists," 8th Edition, 1955.

"Cane Sugar Handbook," 8th Edition, 19h, by Spencer-Meade,


= 52 -

Table No. 1 (Continued)

Sugarcane Sirup
August - 1957

Refractive Indices of Sucrose Solutions at 20° c.

Sucrose Refrac- Sucrose Refrac- Sucrose Refrac- Sucrose Refrac-
percent tive percent tive percent tive percent tive
by index at by index at by index at by index at
weight 20° c. weight 20° c. weight 20° c. weight 20° c.
% a
36.0 1.3920 39.0 1.3978 wo 1.4036 45.0 1.096
al 1.3922 ol 1.3980 al 1.4038 el 1.4098
02 1.392h 22 1.3982 +2 1.40h0 4 1.4100
3 1.3926 +3 1.398) 3 1.042 3 1.4102
an 1.3928 an 1.3986 an 1.404 a 1.4104
5 1.3929 5 1.3987 5 1.4046 5 1.4107
6 1.3931 6 1.3989 6 1.4048 6 1.4109
-7 1.3933 7 1.3991 7 1.4050 7 1.4111
8 1.3935 8 1.3993 8 1.4052 8 1.4113
9 1.3937 oo 1.3995 9 1.405), 9 1.4n5
37.0 1.3939 40.0 1.3997 43.0 1.4056 46.0 1.4117
el 1.3941 el 1.3999 al 1.4058 el 1.49
22 1.3943 22 1.4001 22 1.4060 +2 1.4121
3 1.3945 3 1.4003 3 1.4062 3 1.4123
oh 1.3947 oh 1.4005 any 1.064 ary 1.4125
5 1.3949 5 1.4007 3 1.4066 5 1.4127
6 1.3950 6 1.4008 6 1.4068 6 1.4129
-7 1.3952 “7 1.4010 7 1.4070 7 1.4131
8 1.3954 8 1.4012 8 1.4072 8 1.4133
9 1.3956 9 1.4014 9 1.4074 9 1.4135
38.0 1.3958 41.0 1.4016 4.0 1.4076 47.0 1.4137
wl 1.3960 ol 1.4018 ol 1.4078 al 1.4139
22 1.3962 02 1.4020 2 1.4080 22 1.4141
3 1.3964 3 1.4022 3 1.4082 3 1.4143
ol 1.3966 oh 1.4024 oh 1.408), oh 1.4145
5 1.3968 5 1.4026 5 1.4086 5 1.4147
6 1.3970 6 1.4028 6 1.4088 6 1.4150
7 1.3972 7 1.4030 -7 1.4090 7 1.4152
8 1.3974 8 1.4032 8 1.4092 8 1.4154
9 1.3976 9 1.4034 &d 1.L094 o 1.4156


K

- ho - Sugarcane Sirup
August = 1957

DEFINITIONS AND METHODS OF ANALYSIS (Continued)

B Total Sugars. (Continued)

2 Sucrose. (Continued)

c

Sucrose by volunetric method, Lane-Eynon (for routine
inspections). (Continued)

ii Calculations.
Calculations using the above dilutions:

Titration (titer) (1st) 17.38 ml prepared sample
solution required
to reduce 10 ml
Fehlings solution

(2nd) 17.42 ml prepared sample
solution required
to reduce 10 ml
Fehlings solution

Average of two titrations 17.40 ml prepared sample
Solution required
to reduce 10 ml
Fehlings solution

Factor: 50.7

Obtain factor corresponding to titer from Table
No. l, first column, headed "Invert Sugar - No Sucrose."

From 1 f = 0,008 gram original sample in 1 ml double
diluted sample = 0.00) gram original sample,

50.7 x 100 = 50.7 x 25 = 72.8254 reducing sugar
and sucrose as reducing

17.40 x 0.00 x 1000 17.0
sugar.

25 is the factor to convert total Sugars to percent sample

basis this dilution.

72.825 - 18.490% reducing sugar at same. dilution =
54.335% sucrose as invert sugar.

oTM


- 18 - Sugarcane Sirup
August - 1957

VII CERTIFICATION (Continued)

E ‘tolerances.

When certifying samples that have been officially drawn
representing a specific lot, the grade will be determined in
accordance with provisions outlined in the regulations governing
inspection. In recording results of chemical analyses, consider-
ation should be made for variations in results which are within

the limits of experimental error.


a =~
- 30 - Sugarcane Sirup
August - 1957
TX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
B Total Sugars. (Continued)

1 Reducing sugars. (Continued)

g Determination of reducing sugars - optional method.

The following method may be used for routine
inspections. Reducing sugars are determined by the
Lane-Eynon method as follows:

Weigh 50 grams of double-diluted sirup from Brix
determination and transfer to a 250 ml volumetric flask.
Add 3.5 to 5.0 ml of a saturated solution of neutral
lead acetate (PbAco.3H20) solution and dilute to 250 ml.
Mix well and pour through a folded filter on which has
been placed about 1 teaspoon full of a filter aid
(Kieselguhr or diatomaceous earth, Super Cel, Filter
Cel). Reject the first 25 ml of filtrate. Add a small
quantity of deleading agent (made by mixing 70 grams of
disodium phosphate and 30 grams of potassium oxalate
dry) to the filtered solution and pour through a second
folded filter paper after mixing. Again reject the
first 25 ml of filtrate and reserve the remainder for
both reducing sugar and sucrose determination. Pipet
25 ml of the filtrate (second filtrate above) into a 250
ml volumetric flask and make up to 250 ml with distilled
water. This solution is usually of sufficient strength
to titrate 10 ml of the mixed Fehlings solution. The
titration varies with the amount of reducing sugar and
can be determined by trial. Titrate as directed under
1 f above.

h Calculations for reducing sugars.

Calculations for reducing sugars using above
dilutions;


Colum
No. 2

Apply

ert polarization

Sugarcane Sirup
August - 1957
t: Noo 1l ¢

(P - P!) = Clerget
2

value of P - P!.
which the inv
No.

6
:: No. 1

-59 -
Table No.
2

+ No.

Jackson-Gillis Clerget Method Iv*
1

23 No.

Corrected Clerget Divisor divided into 100
2

No.

t

Colum No. 1 is the algebraic sum of P - P! corrected to normality.

No. 2 is the Clerget Divisor correspmding to that

temperature correction for exact temperature at

was read.
Sucrose.
No. 1

PUP UVO OV SSRSSISARVEA BT
DAANNMNMNAANNOO HC

oe - oe ee ee ce oe oe oe wo NWO ~~

3 PRESRSSAIVALVERSH

THRAQUHQGINS ae

. oO

qgygysqggag ee we we 0s ce ce ae te oe we ot oF oe 80 oe oe oe

KONWKHVNDAYFROMOKNYN

we ee HRAQRSSHBSGASALARA

we en PQARAQYST rears

So Ss te oe ce on ee we ce we oe . SOAANMNNSANNOO EEO
SS SARhagSgn

ee ee we eee ve Ot ONOANNDe
PEEEE EERE ne RBRATHA ISAS ATH
nen uuuaune ta|en ae ee see oe we ene we te we we

nn ond mrONOAN
HBASRRSARHSHACASA
DOAANNMNMANNOO EO

O M0 Ww cor -O M0
ARASISHNAHSHILA
ODOAANANMNAANOOMEO

On DASH OMNOANNSO
°o DOAANNNMSANWNO EEO

con na caAasté al
a | AGFRAEVSHS SAIS HS
° ODOAANANMNAANMNO EEO

ORASHLILSIHSISS

d
: . ce eee oe ee
°o COAANANMNFIWWOO MO

Nn
3
2
rc)
ors
3
2
ro)
Ww
ro)
4
3}

Subtractive Temperature Corrections

131.98 33

The above table 18 based on sucrose concentration Instead of m solids con-

centration, which has been show to be the correct meth

*pur. Standards Scientific Papers 375

131.95

2| 8Q8QRenrdegenssy
i=) DOHANN MM =AAININO OE

5

7
10
R
1
17
20
22
25
30
35

fo) SANMAMO ET ORAANDAW
o AVCANKNVANAAN ANAM



August - 1957
Page

IX DEFINITIONS AND METHODS OF ANALYSIS ..seesesseccceccecvsccesse 25
A Brix Solids .eceeeeceeeeereneee sees 25
1 Double-dilution method . » 25
2 Direct spindle method .. - 25
3 Refractometric method ..... » 26
B Total Sugars ...csecseeeees - 26
1 Reducing Sugars .e.ceeesee 26
a Copper sulfate solution .. sees 26
b Alkaline tartrate solution .. 26
c Standard invert sugar solution 26
d Methylene blue indicator .... 27
e Standardization and titration ... 27
£ Determination of reducing sugars ....seeeeeeeeeceeces 28
g Determination of reducing sugars - optional method ... 30
h Calculations for reducing sugars ... 30
2 SUCrOSe cececcccsccccccccccrseccseccs 32
a Sucrose by polarization method (1) ...ceeseeee 32
b Sucrose by Jackson-Gillis Clerget modification ...... 35

¢ Sucrose by volumetric method, Lane-Eynon (for
routine inspectionS) sssceeee seeeceeeeveseee 39

d Sucrose by volumetric method, Lane-Eynon

(alternate method) .ccccccccccceccccscccsecccessees YL
C Total Sugars, Calculations .......... 43
D Ratio of Total Sugars to Brix Solids .. 43
L Calculations ..cccceccssccccccececeeees 43
E Sulfated ASH .scsseccesceccscnenes dy
1 Sulfated ash (alternate method) .. bb
F Ratio of Sulfated Ash to Brix Solids ... nn
G Total Sulfites; by Monier-Williams Method 4s
1 Calculations .......0.6- 6
H Total Sulfites; by Titration 4?
1 Calculations ...cccceeecessoees 7
I Foreign Material ...cccscececcerers 48
1 = Examination for foreign material . 48
2 Microanalysis ...scscecececececces 48

“ve Sugarcane Sirup

REFERENCE TABLES (See list, page vi)



- 62 -

Sugarcane Sirup

August - 1957
Table No. 7
Conversion of Ounces Avoirdupois
to Fluid Ounces of Sugarcane Sirup
Fluid Ounces

eet 7° : 75° : 76° ’ 77° 78° : 79° : 80°
No. 10 can; Brix Brix Brix, Brix Brix Brix, Brix
130 90.90 90.47 90.05 89.63 89.21 88.79 88.38
130-1/4 91.07 90.65 90.22 89.80 89.38 88.96 88.55
130-1/2 91.25 90.82 90.40 89.97 89.55 89.13 88.72
130-3/4 91.42 91.00 90.57 90.15 89.73 = 89.30 88.89.
131. 91.60 91.17 90.74 90,32 89.90 89.48 89.

131-1/h 91.77 91.34 = 90.92 90.49 90.07 89.65 89.23
131-1/2 91.95 91.52 91,09 90.66 += 90.2, —S 89.82 = 89. LO
131-3/4 92.12 91.69 91.26 = 90.8 = 90.41 89.99 89.57
132 92.30 91.87 = 91.4h 91.01 90.58 = 90.16 S897
132-1/h 92.47 92.0, 916191428 = 90.75 90.33 89.91
132-1/2 92.65 92.21 91.78 | 91.35 90,92 90.50 90.08
132-3/h 92.82 92.39 91.96 = 91.53. 91610 90.67 (90.25
133 93.00 92.56 92.13 91.70 91.27 90.84  90.h2
133-1/h 93-17 = 92.7h = 92430 91.87 91.4 = 9.019059
133-1/2 93.35 92.91 92.48 92.0h 91.61 91.18 90.76
133-3/k 93.52 93.08 92.65 92,22 91.78 91.35 90.93
13h 93.70 93.26 = 92.82 92.39 91.96 §= 9.52 9.10
134-1/u 93.87 93.43 93.00 92.56 += 92.13 91.69 = 9.27
134-1/2 94.05 93.61 93.17 92.73 92.30 91.687 9.43
134-3/4, 94.22 93.78 = 93.3K = 92.91 92.7 = :92.0 = :9..60
135 94.39 93.95 93.51 93.08 = 92.6, :92.21 91.477
135-1/h, 94.57 94013 93.69 93.25 92.82 92.38 = 91.9
135-1/2 9u.7h 94.30 93.86 = 93.42 92.98 )=— 92.55 92.
135-3/4 94.92 eB = HB 93.59 93416 © 92.72 92.28
136 95609 94.65 94.21 93.77 93.33 92.89 92.5
136-1/h 95.27 94.82 94.38 93.9, 93.50 93.06 92.62
136-1/2 95h 94.99 9455 1. 93.67 93.23 92.79

(

of


ie

-61-

Sugarcane Sirup

August = 1957
Table No. 7
Conversion of Ounces Avoirdupois
to Fluid Ounces of Sugarcane Sirup
Fluid ounces

Net Weight: 3 % t : 3
oz. Av. + 74° “: 75° 4 76° + 77° + 78° + 79° 4 80°

No. 2-1/2; Brix : Brix : Brix : Brix : Brix ; Brix +: Brix

Can 3 3 A 3 : 2 2

3h 23.77 23.66 23.55 23.L4 23.33 23.22 23.
3h-1/u 23.95 23.84 23.72 23.61 23.50 23.39 23.28
3u-1/2 24.12 = 2.0L = 23.90 23679 23.68 23.56 = 23.5
3-3/4 24.30 24.18 2.07 23.96 23.85 23.73 23.62
35 24.47 2h.36 2u.2h 24.13 24,02 23.91 23.79
35-1/4 24.65 24.53 2h 42 24.30 24.19 24.08 23.96
35-1/2 2h.82 ab.71 24.59 2h.48 2h.36 2h.25 24.13
35-3/k 25.00 24.88 24.76 24.65 24.53 2h.42 24.30
36 25.17 25.05 2h.9h 24.82 2.70 24.59 24.47
36-1/4 25.35 25.23 25.11 9 2h.99 24.88 = 2.76
36-1/2 25.52 25.40 25.28 25.17 25.05 24.93 24.81
36-3/4, 25.70 25.57 25.46 25.3h 25.22 25.10 24.98
37 25.87 25.75 25.63 25.51 25.39 25.27 25.15
37-1/4 26.05 25.92 25.80 25.68 25.56 25.ub 25.32
37-1/2 26.22 26,10 25.98 25.85 25.73 25.61 25.49
37-3/4 26.40 26.27 26.15 26.03 25.91 25.78 25.66
38 26.57 26.45 26.32 26.20 26.08 25.95 25.83
38-1/4 26.75 26.62 26.50 26.37 26.25 26.13 26.00
38-1/2 26.92 26.79 26.67 26.5 26.42 26.30 26.17
38-3/4 27.09 26.97 26.84 26.72 26.59 26.47 26.34
39 27.27 27.14 27.02 26.89 26.76 26.64 26.51
39-1/h 27.44 27.32 27.19 27.06 26.93 26.81 26.68
39-1/2 27.62 27.49 27.36 = 27.23 27.12 26.98 ~=— 26.85
39-3/4 27.79 27.66 27.53 27.41 27.28 27.15 27.02
Lo 27.97 27.84 27.71 = 27.58 27.45 27.32 27.19




- 23 - Sugarcane Sirup
August - 1957

VIII INSPECTION DURING PRODUCTION AND PACKING OPERATIONS (Continued)

A General. (Continued)

8

10

11

Filling. (Continued)

It should be pointed out that the maximum headspace indicated
is greater than will be found in well filled cans.

Cooling.

After filling, the cans should pass through a spray of
water to wash off any adhering sirup. Cans should be suffi-
ciently cooled before labeling, casing, and warehousing to
prevent caramelization which may adversely affect both the
color and the flavor of the sirup.

Warehousing.

During the summer months cases may be open stacked to
permit quicker cooling of the product and lessen the possibil-
ity of "stack-burn," and loss of color. External corrosion of
the container may occur when canned foods are stored in damp
warehouse space, or if moisture condenses on the surface of
the container from the surrounding air. Canned foods stored
in warehouses should be protected from sudden changes in
temperature which may cause "sweating." Even a slight degree
of rusting causes the cans to become unsightly in appearance,
and loose and discolored labels may result in unmerchantable
containers,

Cases in storage should be examined frequently for
evidence of corrosion and spoilage.

Iabeling.

All labels mst show the name of the product, the net
contents of the container, and the name and address of the
processor, packer, or distributor. When the product is not
manufactured by the distributor the name of the distributor
must be qualified by the statement, "Manufactured for,"
"packed for," or "Distributed by," or sane similar expression.


-1b- Sugarcane Sirup
August - 1957

VI INSPECTION OF THE PRODUCT (Continued)
F Grade Factors Rated by Score Points. (Continued)

3 Defects. (Continued)

In determining sediment the contents of the container
should stand undisturbed for at least two hours at room
temperature. When time permits the sample should stand over-
night for the determination of defects in the product. The
amount of the defects deposited on sides and bottom of the
container can be observed and scored.

When the product is practically free from defects, a
score in the Grade A classification - 18 to 20 points - may
be given. To be practically free from defects the appearance
and eating quality of the sugarcane sirup are not affected by
the presence of harmless extraneous matter or other material
which may be in suspension or deposited as sediment in the
container.

When reasonably free from defects, the sirup may be
given a score of 16 or 17 points. Sugarcane sirup is consid-
ered to be reasonably free from defects when the presence of
harmless extraneous matter or other material does not materially
affect the appearance or edibility of the product. When scored
in the Grade B classification for flavor the product cannot be
graded above U. S. Grade B due to the application of a limiting
rule.

. A score of 14 or 15 points is given when the presence of
defects does not seriously affect the appearance and edibility
of the product. A limiting rule is applicable in this classifi-
cation.

When the product falls into the Substandard classifica-
tion for defects it cannot be graded above Substandard due to
the application of a limiting rule.

4 Clarity.

This factor has reference to the presence of fine
particles of mineral, colloidal, or amorphous material which
is in suspension or is dispersed throughout the sirup and its
effect on the clarity, appearance, or edibility of the product.


SPECIMEN NO. 2

Form Ys "7 UNITED STATES DEPARTMENT OF AGRICULTURE
PRODUCTION AND MARKETING ADMINISTRATION

CERTIFICATE OF QUALITY AND CONDITION
FOR

PROCESSED FRUITS AND VEGETABLES No. 100002

This certificate is admissible in all courts of the United States as prima facie evidence
afta truth, of the statements therein contained. This certificate does aol excuse No. A00002
failure to comply with any of the regul Tews enforced by the United Stat
Department of Agriculture or the Federal Food and Drug Administration.

Date. No:

ORIGINAL

TO.ceecene Dixie Sirup Company Address...

Address...

Shipper or Seller...

Receiver or Buyer

en gSteify tha tm compliance with the requ the Secretary of, Agricul tuapgction and certification of the product
lerignated herein, er get making appropriations for the United States Department of Aciculture, f inepected the vembel of tse
product as shown Below, and that the quality ‘and condition ae shown by the samples on the above dave were'ea follows; °

L:S+ Boudreau, in

Number, size, and
kind of containers....PeT.

yulati

ctor

Samples submitted by...

Product inspected... SUOARCANE. STRUP...

Code or other identification marks on containers.........0..1.

feb if'any).-...Deep South, Louisiana. Net Weight, 12 fluid ounces"
Net contents 12-1/2 to 13 fluid ounces
Vacuum 7 to 10 inches
Type Unsulfured OFFICIALLY SAMPLED
Brix Solids 74.8% Composite

Grade: U. S. GRADE A or U. S. FANCY
° Score 92 to 94 Points us. bur. oF sanrccTuer

Packed in glass jars with screw top closures, neatly labeled, clean,
and in good condition. Certificate of sampling attached indicates
samples drawn November 23, 1956, from a lot of 800 cases 2/12 fluid
ounce glass (applicant's count) packed in corrugated fiber cases,
located in Dixie Sirup Company Warehouse No. 2, Deep South,

Remarks:

P. 0. Box ipl

Address... Hammond, lout:
PLEASE REFER TO THIS CERTIFICATE BY NUMBER AND MARKET



VII

-17- Sugarcane Sirup
: August - 1957

CERTIFICATION (Continued )
B Product Inspected. (Continued)

Type: Applicant states product is sulfured
sugarcane sirup.

Type: Applicant states product is unsulfured
sugarcane sirup.

C Mandatory Requirements.

If the product is found to contain objectionable foreign
material or filth material such as insects or insect fragments,
the grade of the product should not be certified. A statement
should be inserted in the body of the certificate following the
word "grade" as follows:

Grade: Grade not certified account presence
of foreign material (insect fragments).

D Specimen Examples of Certificates.

Attached are specimen certificates which bllustrate
specific examples of certification of sugarcane sirup.

Specimen No. 1

Tllustrates certificate covering sulfured sugarcane sirup.
The applicant requested chemical analyses for total sulfates and
sulfated ash and a microscopic analysis for foreign material to
satisfy buyers' specifications. The cost of these analyses is
shown in the certificate. Analyses included ina normal inspection
fee for sugarcane sirup are the determination of color and Brix
solids. No extra charge is made for these determinations.

Specimen No. 2

Illustrates certificate covering 12 fluid ounces glass con-
tainers. The samples were officially drawn. In this illustration
the net contents of the container is stated on label in terms of
liquid measure.

Specimen No. 3.

ant Illustrates certificate covering sample submitted by appli-
cant.


- 2h - Sugarcane Sirup
August - 1957

VIII INSPECTION DURING PRODUCTION AND PACKING OPERATIONS (Continued )
A General. (Continued)
1l Labeling. (Continued)

The statement of net contents is expressed in terms
generally used to express the quantity of the product in the
container and to give the consumer accurate information on
the amount. In general, the statement of net contents should
be in terms of liquid measure for liquid products or in terms
of weight if the food is solid, semisolid, viscous, or a
mixture of solid and liquid. If desired, a statement of net
contents in terms of both liquid measure and weight may be
used. In either case, the statement of quantity should be in
terms of the largest unit of weight or measure. For example,
instead of 2) ounces the statement should be "1-1/2 pounds"
or "1 pound, 8 ounces." The statement of weight or measure
may be supplemented by a statement in terms of the metric
system of weight or measure.

The brand name, as well as information on the quality
of the product, may appear on the label together with other
appropriate material. Label statements should not be false
or misleading in any particular.

The labeling provisions of the Food, Drug, and Cosmetic
Act are under the jurisdiction of the Food and Drug Adminis-
tration, Department of Health, Education, and Welfare. When
questions arise concerning labeling of the product, the matter
should be referred to your supervisor.

12 Recommendations.

Daily reports should be prepared and promptly issued
to the company official designated to receive them. A
written report, in addition to the daily report, to cover
Special situations, may be necessary when an unsatisfactory
condition is not promptly corrected. The inspector should
endeavor to make recommendations to the management which will
be helpful in maintaining adequate control of quality. The
inspector should consult his supervisor for advice if any
unusual situation should develop. Suggestions should be made
to the management whenever the opportunity is presented for
improving quality and overcoming objectionable conditims.

fTM



-l- Sugarcane Sirup
August - 1957

VI INSPECTION OF THE PRODUCT (Continued)
D Recording Inspection Data on Score Sheet.

The information required for recording in the score sheet
includes size and kind of container, when packed in consumer
size containers, brand name, statement of net contents, name and
address of packer or distributor, code marks or other identifica-
tion, fill of container, and any other information which may be
essential in the evaluation of the quality and condition of the
product. .

E Fill of Container.
1 Net contents.

The net contents of the container when packed in con-
sumer size cans may be expressed in terms of weight or measure,
as sugarcane sirup falls into the category as a thick and
viscous fluid. Containers should be filled as full as practi-
cable. The sirup should occupy not less than 93 percent of the
total capacity of the container in containers of gallon capacity
and less. When inspecting bulk lots the quantity declared by
the packer should be recorded. If any question should arise as
to the quantity in bulk containers, the processor may be requested
to verify the amount by any suitable method such as weighing or
measuring that is satisfactory to the applicant or inspector.

The equivalent fill of container in terms of U. S. gallon and net
weight is given in Table No. 7 hereof.

The net contents of the container may be determined by
weight which can then be converted to liquid measure. The usual
procedure in making net weight determinations is to place a com-
plete clean, dry, empty container on the weight plate of the
scales or set the counterpoise on the tare beam to offset the
weight of the container. The weight can then be recorded
directly as the net weight of the product in the container. The
average net weight of all the containers in the sample should be
equal to or greater than the label statement of the net contents
of the container. The net weight of any container which falls
below the indicated label weight should be within the range of
variability of good commercial practice.


No

- 63 - Sugarcane Sirup
August - 1957

In constructing Table No. 7 the following specific gravities
were used for sugarcane sirup correspmding to the different densi-

ties of sirup:

Degrees
Brix

74
75
76
77
78
19
80

Specific gravity
@ 20/20° c. 1/
et

1.37496
1.38141
1.38790
1.394h2
1.40098
1.40758
1.41421

The following formula was used in the calculations:

Fl. Oz. =

Avoir. oz. x 0.9614
Pp. gre


- 50 - Sugarcane Sirup
August - 1957

Table No. 1 (Continued)
Refractive Indices of Sucrose Solutions at 20° c.

Sucrose Refrac- Sucrose Refrac- Sucrose Refrac- Sucrose Refrac-

percent tive percent tive percent tive percent tive
by index at by index at by index at ~~ by index at

weight 20° c. weight 20° c. weight 20° c. might 20° c.

12.0 1.35093 15.0 1.35567 18.0 1.36053 21.0 1.26551

a 1.35109 el 1.35583 ol 1.36069 al 1.36568
22 1.3512 +2 1.35599 22 1.36086 22 1.36585
3 1.35140 3 1.35615 3 1.36103 3 1.36601
an 1.35156 an 1.35631 oh 1.36119 oh 1.36618
5 1.35171 5 1.35647 5 1.36135 5 1.36635
6 1.35187 6 1.35664 6 1.36152 6 1.36652
7 1.35203 7 1.35680 7 1.36169 7 1.36669
8 1.35219 8 1.35696 8 1.36185 8 1.36685
9 1.3523 9 B.35712 9 1.36201 9 1.36702
13.0 1.35250 16.0 1.35728 19.0 1.36218 22.0 1.36719
ol 1.35266 wl 1.3574b 1 1.36235 el 1.36736
+2 1.35282 2 1.35760 +2 1.36251 2 1.36753
3 1.35297 3 1.35777 3 1.36268 3 1.36770
ar 1.35313 oh 1.35793 oh 1.3628) oh 1.36787
5 1.35329 5 1.35809 5 1.36301 5 1.36803
6 1.35345 6 1.35825 6 1.36318 6 1.36820
7 1.35361 7 1.35841 7 1.3633h 7 1.36837
8 1.35376 a) 1.35858 8 1.36351 a) 1.36854,
9 1.35392 9 1.35874 9 1.36367 9 1.36871
14.0 1.35408 17.0 1.35890 20.0 1.36384 23.0 1.36888
ol 1.3542h ol 1.35906 ol 1.36401 ol 1.36905
2 1.35440 +2 1.35923 2 1.36417 22 1.36922
3 1.35456 3 1.35939 3 1.36434 3 1.39639
oh 1.35472 an 1.35955 oh 1.36451 aly 1.36956
5 1.35487 5 1.35971 5 1.36467 5 1.36973
6 1.35503 6 1.35988 6 1.36484 6 1.3691
“7 1.35519 7 1.36004 7 1.36501 7 1.37008
8 1.35535 8 1.36020 8 1.36518 8 1.37025

9 1.35551 9 1.36037 9 1.3653h 9 1.37042


-he- Sugarcane Sirup
August - 1957

II PRODUCTION (Continued)

B Varieties of Sugarcane.

Sugarcane is a large grass belonging to the so-called
noble cane group which comprises all of the cultivated varieties
of the world. The development of varieties giving higher yields
of sugar has resulted in gradual replacement of the old with the
new varieties. The so-called native canes which have been culti-
vated in a given location for many years are principally used in
the production of sugarcane sirup. Some of the named varieties
are Canal Point and Coimbatore. These are varieties which are
also used for the commercial production of sugar (sucrose) ani
should not be confused with the sorghum canes which are used for

making sorghum sirup.

Sugarcane is grown from cuttings of the cane which are
planted end to end in a row, with a very shallow covering of
soil. The buds located at the nodes or joints produce a plant
which sends out several shoots or suckers. The suckers form a
group or clump of canes. Cuttings are usually planted but once
in several years under suitable climatic conditions. After har-
vesting, new plants spring up from the stubble. These are called
ratoons, which produce the second and later crops, being limited
in number by soil or climatic conditions. Frequently, this is
limited to one planting crop followed by two ratoon crops.

Sugarcane is harvested in the last quarter of the year,
usually as late as possible prior to freezing weather, to permit
the sugar content of the cane to approach its maximum. Produc-
tion usually begins in October and may continue through January.
November is the month of heaviest production. The type of soil
in which the cane is grown, the variety of cane grown, milling
equipment, and boiling house equipment, all have an effect on the
quality of the sirup.

1 Harvesting.

In harvesting sugarcane for sirup, the stalks may be
cut off close to the ground and should be topped just sbove
the highest colored joint. This may vary in different local-
ities, and in some instances the top joints, although having
a lower sucrose content, are not removed. The leaves are
removed at the same time the stalks are cut and topped, Hand
cutting is generally practiced but machine harvesting has been
used to some extent recently with the invention of two machines


-21- Sugarcane Sirup
August - 1957

VIII INSPECTION DURING PRODUCTION AND PACKING OPERATIONS (Continued)
A General. (Continued)
6 Methods of production. (Continued)

b Sulfured sirup. (Continued)

dioxide to an acidity of 3.5 to 4.00 cc after which the
acidity is reduced to 0.8 to 1.0 ce by the addition of
milk of lime. The juice is then brought to a boil and
the "mud" then allowed to settle out. The clear juice

is decanted or piped to open evaporators where the juice
is evaporated under vacuum to about 50° Brix and again
allowed to settle. The clear semi-sirup is further con-
centrated in open evaporators to the required consistency.
A large part of sulfited sirup is sold in bulk for blend-
ing with molasses or glucose for table use and cooking.

7 Blending.

Sirup which is obtained from different producers may
vary considerably in color and flavor as well as in other
respects. Such sirups may be blended in order to maintain a
uniform quality product under a producer's or distributor's
label. A considerable amount of experience is required in
the blending of sirups. A careful grading and analysis of
each component is helpful in determining the quantities of
each of several different lots of sirup which should be used
in making a blend. Usually the final selection of sirups
for a blend is made by one individual who is thoroughly
familiar with the requirements of the product and has become
proficient in selecting suitable stock for blending through
many years of experience.

8 Filling.

The temperature of filling is usually sufficient for
sterilization without any additional heat treatment. The
rate of cooling must be taken into account in this connection.
When the product is air cooled, higher processing temperatures
may be necessary for sterilization during the winter months
than during the warm summer months. The following processing


-55 -

Table No. 2

Sugareane Sirup
August - 1957

correction Table for Determining the Percentage of Sucrose by
Means of the Refractometer when the Readings are Made at
Temperatures Other than 20° Cc.

(International Temperature Correction Table - 1936)

Percentage of Sucrose

Tem-
pra- O 5 10 15 20 25 30 35 4o us SO 55 60 65 70
ture
Subtract from the percentage of sucrose

0,

c.

10 0.50 0.5 0.58 0.61 0.64 0.66 0.68 0.70 0.72 0.73 0.7h 0.75 0.76 0.78 0.79
ls. e953 655 58 «660. . 65 .66 .67 . 69 470 .71
12 h2 .u5 UB 50. 52 25h 256 657 258 £59 660 661 .61l 63.83
13. +37) KO 42 ou 6 LB LG 650 51 652 53 SL SK 55 5D
1, 633. 635) 637-39 KO UD U2 3 UK eS US WG wT LB
1S 627) 629) 31 33 BLK «3D 036 37-37) 38039239 O««LO
16.22) 262526 027 28 28 629 230 30 0630 32 2312322
17. «.17,—«d18— 19 620 22 212 22 22 22 623 623 62323 ww
18.12.13: «613 ww ub. 5.15 615 15 16 1616.16
19.06 .06 .06 .07 .07 .07 .07 .08 .08 .08 .08 .08 .08 .08 .08

Add to the percentage of sucrose

21 0.06 0.07 0.07 0.07 0.07 0.08 0.08 0.08 0.08 0.08 0.08 0.08 0.08 0.08 0.08
22. 613: 613. . 15. 15. 15 616 616 416 616 «61616
23.19 620 621 622) «22 23 023 23 23 Kw
2h .26 627) «28 629) 630630 313132) 31 313232 32.12
25 33.35 36 637 638 638 «239 LO LO 6K ws wKOs«wLOOs“«wO.s «CO
26 «KO wW2 2U3 LUSK KT KBB OLB OLB WB UB OLB LLB
27) obB 50 652 53 SL 655 655 56 56 656 156 656 56 56 156
28 56.57 .60 .61 .62 .63 .63 .6h .6h 164) 16h 16h 16h 16h 1.6L
29 6h 665 668 669 71 672 67273-6730 73.-«73- 67373-67373
30 .72 .7h .77 .78 .79 .80 .80 .61 .81 .81 .81 .81 .81 .81 .81



-57- + Sugarcane Sirup
August - 1957

Table No. k

Factors for 10 Ml Soxhlet Solution to be Used in
Connection with Lane-Eynon General Volumetric Method

: +1 Gram Sucrose:5 Grams Sucrose:10 Grams Sucrose:
Titer;Invert Sugar: Per 100 Ml : Per 100Ml : Per 100 Ml :Dextrose
+: No Sucrose : Invert Sugar : Invert Sugar : Invert Sugar

15 50.5 49.9 47.6 46.1 49.2
16 50.6 50.0 47.6 L6.2 49.2
7 50.7 50.1 47.6 46.1 49.3
18 50.8 50.1 47.6 46.2 49.3
19 50.8 50.2 47.6 46.1 49.4
20 50.9 50.2 47.6 46.1 49.5
21 51.0 50.2 47.6 46.2 49.5
22 51.0 50.3 47.6 46.1 49.6
23 51.1 50.3 47.6 46.2 49.7
2h 51.2 50.3 47.6 46.1 49.8
25 51.2 50.4 47.6 46.0 49.8
26 51.3 50.4 47.6 46.0 49.9
27 51k 50.4 47.6 46.0 49.9
28 51.4 50.5 47.7 46.0 50.0
29 51.5 50.5 47.7 46.0 50.0
30 51.5 50.5 47.7 46.0 50.1
31 51.6 50.6 47.7 45.9 50.2
32 51.6 50.6 47.7 5.9 50.2
33 51.7 50.6 47.7 45.9 50.3
3h 51.7 50.6 7.7 45.8 50.3
35 51.8 50.7 47.7 45.8 50.4
36 51.8 50.7 47.7 45.8 50.4
3? 51.9 50.7 47.7 45.7 50.5
38 51.9 50.7 47.7 45.7 50.5
39 52.0 50.8 47.7 45.7 50.6
ho 52.0 50.8 47.7 U5 .6 50.6
41 52.1 50.8 47.7 45.6 50.7
2 52.1 50.8 47.7 45.6 50.7
43 52.2 50.8 47.7 45.5 50.8
Lh 52.2 50.9 47.7 45.5 50.8
LS 52.3 50.9 47.7 45.4 50.9
46 52.3 50.9 47.7 U5. 50.9
47 52.4 50.9 47.7 45.3 51.0
u8 52.4 50.9 47.7 45.3 51.0
ug 52.5 51.0 47.7 45.2 51.0
50 52.5 51.0 47.7 45.2 Sl.



- 58 - Sugarcane Sirup {~
August - 1957

Table No. 5

Factors for 25 Ml Soxhlet Solution to be Used in
Connection with Lane-Eynon General Volumetric Method

:1 Gram Sucrose:

Titer vert Sugar,” per 100 M1: Dextrose ; Levulose

1 No Sucrose . invert Sugar + t
15 123.6 122.6 120.2 127.4
16 123.6 122.7 120.2 27.4
17 123.6 122.7 120.2 127.5
18 123.7 122.7 120.2 127.5
19 123.7 122.8 120.3 127.6
20 123.8 122.8 120.3 127.6
21 123.8 122.8 120.3 127.7
22 123.9 122.9 120.4 127.7
23 123.9 122.9 120.4 127.8
2k 124.0 122.9 120.5 127.8
25 124.0 123.0 120.5 127.9
26 124.1 123.0 120.6 127.9
27 124.1 123.0 120.6 128.0
28 124.2 123.1 120.7 128.0
29 124.2 123.1 120.7 228.1
30 124.3 123.1 120.8 128.1
31 12h.3 123.2 120.8 128.1
32 124.4 123.2 120.8 128.2
33 124.4 123.2 120.9 128.2
3u 124.5 123.3 120.9 128.3
35 124.5 123.3 121.0 128.3
36 1224.6 123.3 121.0 128.4
37 12h.6 123.4 121.1 128.4
38 124.7 123.b 121.2 128.5
39 124.7 123.4 121.2 128.5
ho 124.8 123.4 121.2 128.6
41 124.8 123.5 121.3 128.6
h2 124.9 123.5 121.4 128.6
43 22.9 123.5 121.4 128.7
nny 125.0 123.6 121.5 128.7
us 125.0 123.6 121.5 128.8
6 125.1 123.6 121.6 128.8
47 125.1 123.7 121.6 128.9
48 125.2 123.7 121.7 128.9
ug 125.2 123.7 121.7 129.0
50 125.3 123.8 121.8 129.0




I

II

INSPECTORS! INSTRUCTIONS
FR
SUGARCANE SIRUP

August = 1957

GENERAL
A Purpose and Scope.

The instructions contained herein explain and furnish
technical information which will serve as a guide in the inspec-
tion of sugarcane sirup and will aid inspectors in attaining
uniformity in applying the United States Standards for grades
of this product and in the proper certification of the product.
These instructions will also serve to familiarize the inspectors
with the commercial product and the general packing procedure
used by industry.

B Caution.
Inspectors are reminded that these are administrative
instructions for their use only and are not for public distri-
bution.

C Keep Instructions Current.

These instructions may be revised, in whole or in part,
whenever the need for such revision is indicated. Therefore,
any comments or suggestions such as detection of errors or the
development of new and better inspection techniques should de
forwarded in detail to the Washington office.

PRODUCTION

The States in which sugarcane sirup is produced are Louisiana,
Mississippi, Georgia, Alabama, Florida, Texas, South Carolina, and
Arkansas. Sugarcane sirup is produced principally in Louisiana and
the Southeastern States. The mills in Louisiana generally are larger
than those in the Southeastern States and much of the sirup is "sul-
fured sirup" which is made by the sulfitation process. The sirup
produced in the Southeastern States is processed on small farm mills

“where the sulfitation process is not used. A considerable quantity

of it is canned at the mill for sale to wholesalers or retailers;
the remainder is barreled and sold to blendors or to accumlators for
resale or blending.


-vi- Sugarcane Sirup :
August - 1957

REFERENCE TABLES

Page
Table No. 1, Refractive Indices of Sucrose Solutions at 20° c.
(International Scale - 1936) 49
Table No. 2, Correction Table for Determining the Percentage
of Sucrose by Means of the Refractometer when ~
the Readings are Made at Temperatures Other :
than 20° Cc. 55
Table No. 3, Temperature Corrections to Readings of gaccharo-
meters (Brix Spindle) (Standard at 20° Cc.) 56
Table No. 4, Factors for 10 Ml Soxhlet Solution to be Used in
Connection with Lane-Eynon General Volumetric
Method 57
Table No. 5, Factors for 25 Ml Soxhlet Solution to be Used in
Connection with Lane-Eynon General Volumetric
Method 58
Table No. 6, Jackson-Gillis Clerget Method IV 59
Table No. 7, Conversion of Ounces Avoirdupois to Fluid Ounces
of Sugarcane Sirup 60


- 13 - Sugarcane Sugar
August - 1957

VI INSPECTION OF THE PRODUCT (Continued)
E Fill of Container. (Continued)
2 Headspace.

When the headspace appears to be excessive, careful
measurement of the headspace should be made with a depth gauge.
If the headspace is in excess of 7 percent of the total capac-
ity of the container, it should be classified as slack filled.

F Grade Factors Rated by Score Points.

1 Color.

The color of sugarcane sirup varies considerably with
the method used in production, the comlition of the cane,
and the canning procedure employed by the packer. Partially
crystallized sirup is liquefied by heating to approximately
54.49 c. (130° F.) and cooled to approximately 20° c. (60° F.)
before classifying the color of the product.

The sample is placed in a sample container which should
be clean and dry. Follow the procedure outlined in the stand-
ards. Compare the color of the sample with the U.S.D.A.
permanent glass color standards. Place the sample container
successively in compartments 2 and h of the comparator and make
the comparison visually by looking through the sample and the
color standard toward a diffuse source of natural or artificial
light.

To score in the Grade A classification - 27 to 30 points
the color must be equal to or lighter incolor than U.S.D.A. per-
manent glass color standard No. 1 for sugarcane sirup.

When the color is equal to or better than U.S.D.A. color
standard No. 2 a score in the Grade B classification - 2 to 26
points - may be given. As there is no limiting rule in the
Grade B color classification, the product may be graded U. S.
Grade A when the color falls into this classification, provided
that the total score for all factors is 90 points or over.

If the color is equal to or lighter than U.S.D.A. color
standard No. 3 it falls in the Grade C classification and may
be scored 21 to 23 points. When scored in this classification
the product cannot be graded above U. S. Grade C regardless of
the total score as this is a limiting rule.


Sugarcane Sirup

August - 1957
II PRODUCTION (Continued)
A Annual Production. (Continued)
PRODUCTION OF SUGARCANE SIRUP, BY STATES, 1910-54
(Thousand Gallons)
Year : La. : Ga. } Miss. ; Ala. ; Fla. } Texas : Ss. C.? ark. : Total
1940 1 $,720 + 2,530 + 1,380 ; 1,500 41,120; 750; 320; 125 ; 13,li5
191 + 6,240 + 3,564 + 3,235 + 2,760 11,600; 840; S00; 125 + 18,76
19h2 + $,760 + 3,900 + 3,300; 2,645 1,760; 665: LBS: 95 1 18,610
1943 + 7,975 1 4y250 + 2,992 + 2,875 1 2,0h0: 7001 64B: 95 + 21,575
Igy 1 6,670 + 4,356 + 3,630 + 2,760 1 2,2h01 7501 $70: 95 + 22,071
ISS 115,075 + hy56L + 3,520 1 2,860 + 2,090: 260; 3k2¢ — + 28,712
19h6 111,825 + 4,025 + 3,500 + 2,430: 1,980 2704 b20y = + 2h,US0
1947 : 8,460 : 4,070 : 2,600 : 2,160 ' 2,400 : 280 ' 300 : _- : 20,270
19bB + 2,200 + 3,600 + 2,890 + 2,2h0 + 1,980; 230; 3501 = 1 13,390
1949 : 2,600 ‘ 3,150 : 2,030 : 1,820 : 1,620 : 320 : 230 ' -- : 11,770
1950 : 3,960 : 2,100 : 1,00 : 1,150 : 980 t -- ' -- ‘ - : 9,230
1981 1 2,880 11,360; 3601 480: 9601 -=1 --1 -= ¢ 6,040
1952 13,2801 1,190; 360; 50: 725: <<: <4 <= 1 6,085
1953 : 2,225 : 1,260 : 560 : 450 : 1,080 : ~ : -- : -- : 5,575
19541 2,590 : 720 : 270 : 375 t BOr mt met et 4,795
t $ t 3 t t 3 t t
“preliminary.
Source: Agricultural Statistics.


SPECIMEN NO. 1

Form
a

FvV—209
-3-54)

UNITED STATES DEPARTMENT OF AGRICULTURE

AGRICULTURAL MARKETING SERVICE

ORIGINAL

Shipper or Seller

Receiver

CERTIFICATE OF QUALITY AND CONDITION

FOR
PROCESSED FRUITS

ts admissible in all courts of the United
of the statements therein contained.

This certificate
of the truth

.AOO000L
AND VEGETABLES No

ei es ag Drtma facle evidence NO. AQOOO]

failure to comply with any of the regulatory laws enforced by the United States
Department of Agriculture or the Federal Food and Drug Administration.

(Applicant)

or Buyer

Date - Dees 2051956 _. Hour_

Address. --- - - ~~

| certify that in compliance with the regulations of the Secretary of Agriculture governing the inspection and certification of the product
dc

designated’ herein,

samples on the above date were as stated below:

Lot ®

OWE No.__

title of “Creole Brand Sugarcane Sirup.

wurguant to the act caking appropnations tor the Usited States Deparutent of Agriculture I personallg dew at hontost
and inspected sazaplos believed by me to be representative of the lot descrived ‘below, and endition

that the quality and condition aa shown by the

Packed by Elwood Sirup Company,

label Lieey) Elwood, Louisiana, let Weight, 2 pounds, ounces."

Grade:

Remarks:

Net weights

vacuum

Type

Brix Solids

Sulfated Ash

Total Sulfates as SO,

U. S. GRADE A or U. S. FANCY
Score 92 to 96 Points

Packed in plain hermetically
and in good condition.

36-1/2 to 37-1/2 ounces
8 to 9 inches

Sulfured

74.6% Composite Sample
5.8% Composite Sample
92 ppm Composite Sample

sealed cans, neatly labeled, clean,

Samples drawn December 18, 1956, from a
lot of 1200 24/2-1/2 cans (applicant's count).

Packed in solid

fiber cases and located in Bay 5, Elwood Warehouse, Elwood,
Louisiana, under Lot No. 1217.

Chem Anal $10.00
Miero Anal 3.00

Fee----.- 13200__
Expenses. .---2200__
Total... . $35:00__

J. L. James
P. 0. Box 151

PLEASE REFER TO THIS CERTIFICATE BY NUMBER AND MARKET



UNITED STATES DEPARTMENT OF AGRICULTURE
AGRICULTURAL MARKETING SERVICE
FRUIT AND VEGETABLE DIVISION
PROCESSED PRODUCTS STANDARDIZATION AND INSPECTION BRANCH
WASHINGTON, 0, C.

——>——_—_—_—____
INSTRUCTIONS FOR INSPECTION

of

SUGARCANE SIRUP

SS

> FOR USE OF USDA PROCESSED FOODS INSPECTORS

AUGUST 1957


- 36 - Sugarcane Sirup
August - 1957

TX DEFINITIONS AND METHODS OF ANALYSIS (Continued)

B Total Sugars. (Continued)

2 Sucrose. (Continued)

b Sucrose by Jackson-Gillis Clerget modification. (Continued)

4a

iii

Polarization before inversion.

To one portion add 10 ml of a solution of sodium
chloride containing 231.5 grams per liter. Make up to
volume with distilled water at the temperature at which
the observations are to be made and polarize in a water
jacketed tube. The reading calculated to a normal weight
basis =P.

Polarization after inversion.

To the other 50 ml portion of the filtrate add 2
ml of hydrochloric acid (sp. gr. 1.1029 at 20°/k° ¢.) to
the cold solution. Insert a thermometer in the flask
and heat by immersing in a hot water bath until the
temperature is exactly 65° ¢, Remove the flask from the
bath, add 10 ml of hydrochloric acid, mix by rotating,
and set aside for thirty minutes. Longer standing does
not affect the results. Cool and make to volume at the
temperature at which the observations are to be made.
If the solution is too dark colored it may be treated
with successive small amounts of pure metallic zinc dust.
The coloring matter is destroyed by the nascent hydrogen.
No more zinc than is necessary should be used. Make the
polarization in a water jacketed tube with the temperature
carefully regulated to the same as that for direct
polarization. The reading calculated to normal weight
basis = - p', Polariscopic reading (both direct and
invert) should be the average of several concordant obser-
vations. Multiply these average readings by 6 to obtain
the values for P and P!,

The Walker method of inversion described above may
be insufficient to cause complete inversion in low purity
products (final molasses) in cool weather when cooling

may be rapid.


-6- Sugarcane Sirup
August - 1957

II PRODUCTION (Continued)

D Manufacture of Sugarcane Sirup. (Continued)

in the juices because of the heavy pressures applied, and it is
generally conceded that the best sugarcane sirup is produced when
extreme milling pressures are not in use.

1 Unsulfured sugarcane sirup.

Unsulfured sugarcane sirup is made by concentrating the
juice by boiling without any chemical treatment. This is the
type of sirup produced in plants of small capacity. The cane
is usually crushed in a single mill equipped with three rollers.
The juice is strained and run into clarifyers to remove sus-
pended material, and then to the evaporator. The evaporators
in the smaller plants are usually direct fired. The application
of heat clarifies the juice, the albuminoids are coagulated and
rise to the surface, entrapping small particles of extraneous
material from cane and forming a scum which is removed by skim-
ming or brushing. The skimming or brushing continues during
evaporation until the desired concentration is reached. Sirup
produced by this simple method will generally have an excellent
flavor.

2 Sulfured sugarcane sirup.

In the sulfitation process, the juice is treated with
sulfur dioxide and then with hydrated lime. The sulfured type
of sirup is generally produced by the larger processors. The
plant usually consists of a crusher with six or more rollers,
having a daily capacity of 200 tons of cane or more, depending
upon other plant facilities. The juice is strained and satu-
rated with sulfur dioxide. The juice should absorb sufficient
sulfur dioxide to give an acidity equivalent to 3.0 to h.O ml
of O.1N alkali per 10 ml of juice. This sulfitation is
followed by liming. The lime used is powered hydrated lime
(Ca(OH)5) or very finely pulverized quicklime. The acidity is
reduced by liming to 0.8 to 1.5 ml of 0.1N alkali per 10 ml of
juice. The juice is then boiled and allowed to settle. The
clear juice is then decanted or filtered. The clear juice may
then be partially evaporated and again allowed to settle, after
which the clear sirup is further evaporated in open evaporators
to the required Brix. The sirup is usually held for several
weeks in large tanks before canning. A large part of sulfured

sirup is sold in bulk for blending with molasses or glucose for
table use am for cooking.


-5- Sugarcane Sirup
August - 1957

II PRODUCTION (Continued )
B Varieties of Sugarcane. (Continued)
1 Harvesting. (Continued)

for this purpose. These are the M:nson-Thompson and the Wurtele
cane harvesters. AS sugarcane deteriorates rapidly, it should be
conveyed to the mill as soon as possible and ground immediately.
When freezes occur, the cane must all be cut immediately to pre-
vent fermentation and excessive deterioration which reduce yields
and lower the quality of the sirup. In some regions, it is
customary to cut, top, and strip cane in advance of freezing
weather. Such cane is piled and covered with leaves and tops to
protect it and keep it from freezing. If properly handled and

if weather is not too severe, this cane will keep satisfactorily
for a month or more.

C Types of Sugarcane Sirup.

Sugarcane sirup is of two types:
1 Unsulfured sugarcane sirup. ,
2 Sulfured sugarcane sirup.
D Manufacture of Sugarcane Sirup.

Sugarcane sirup is made directly from the juice of the cane
by concentrating to the required Brix degree without removing any
sugar. Essentially, the processing of sugarcane sirup is similar
in all mills with the exception of a single process, sulfitation,
which may or may not be used. Sugarcane is brought from the fields
after cutting, either directly to the mills by tractor and cart, or
first to a field derrick where the cane is loaded from the carts to
trucks or railroad cars for delivery to the mill. The sugarcane,
when unloaded, may go directly to the mill carrier or may be stored
for a short period of time before entering the milling process. It
is a perishable product and may deteriorate during the time that
elapses between cutting and milling. The cane passes through a
. battery of mills, the number and applied pressure of which vary con-
siderably as between the small farm type establishsents and the
large commercial mills. Generally, the greater the number of mills
and the higher the pressure applied, the greater will be the propor-
tion of the juice in the cane which is actually extracted. However,
the larger mills may also result in a higher proportion of impurities


- 49 - Sugarcane Sirup
August - 1957

Table No. 1
Refractive Indices of Sucrose Solutions at 20° Cc.

(International Scale - 1936)

Sucrose Refrac- Sucrose Refrac- Sucrose Refrac- Sucrose Refrac-
percent tive percent tive percent tive percent tive

by index at by index at by index at by index at
weight 20° c. weight 20° ¢. weight 20° c. weight 20°C.

% F é $

0.0 1.33299 3.0 1.33733 6.0 1.34176 9.0 1.34629

al 1.33313 a 1.33748 1 1.34191 1 1.30644

2 1.33328 +2 1.33762 2 1.33206 2 1.34660

3 1.333h2 3 1.33777 3 1.34221 3 1.3675

a an 1.33357 an 1.33792 any 1.34236 wh 1.3h691

i 5 1.33371 5 1.33807 5 1.34251 5 1.34706

6 1.33385 6 1.33821 6 1.34266 6 1.34721

7 1.33400 7 1.33836 7 1.34281 7 1.34737

8 1.33414 8 1.33851 8 1.34296 8 1.34752

9 1.33429 9 1.33865 ) 1.34311 9 1.34768

1.0 1.33443 4.0 1.33880 7.0 1.34326 10.0 1.34783

al 1.33457 wl 1.33895 wl 1.343h1 al 1.34798

2 1.33472 22 1.33909 4 1.34356 2 1.34814

3 1.33487 3 1.33924 3 1.34371 3 1.34829

an 1.33501 oh 1.33939 oh 1.34386 oh 1.3085

5 1.33515 5 1.33953 5 1.34401 5 1.34860

6 1.33530 6 1.33968 6 1.34417 6 1.34875

7 1.3355 +1 1.33983 7 1.34432 7 1.34891

8 1.33559 8 1.33998 8 1.34L47 8 1.34906

9 1.33573 9 1.34012 9 1.3462 9 1.34922

2.0 1.33588 5.0 1.34027 8.0 1.3bK77, 1.0 1.34937

1 1.33603 ol 1.34042 a1 1.34L92 ol 1.34953

- 2 1.33617 22 1.34057 2 1.34507 22 1.34968

3 1.33631 3 1.34072 3 1.34523 3 1.3498h

oh 1.33646 oh 1.34087 h 1.34538 ary 1.34999

5 1.33661 5 1.34101 5 1.34553 5 1.35015

6 1.33675 6 1.34116 6 1.30568 6 1.35031

7 1.33689 7 1.34131 7 1.3583 7 1.35046

8 1.33704 8 1.34146 8 1.34599 8 1.35062

9 1.33719 9 1.34161 9 1.34614 9 1.35077


- 32 - Sugarcane Sirup f
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
B Total Sugars. (Continued)
2 Sucrose.

Sucrose may be determined by one of the following
methods;

By polarization before and after inversion with
invertase (official).

By Jackson-Gillis Clerget Modification (Method h).

By titration before and after inversion using Fehlings
solution,

a Sucrose by polarization method (1).

i Invertase solution.

Use commercially prepared invertase solution.
The activity of the invertase solution is determined
as follows:

Dilute 1 ml of the invertase preparation to 200 ml.
Transfer 10 grams of sucrose (high grade large grain
granulated sugar) to a sugar flask graduated at 100

ml and 110 ml, and dissolve in about 76 ml of distilled
water. Add 2 drops of acetic acid and dilute to the
100 ml mark. To the 100 ml of sugar solution add 10
ml of the diluted invertase solution and mix thoroughly
and rapidly, noting the exact time at which the solu-
tions are mixed. At the termination of exactly 60
minutes make a portion of ‘the solution just distinctly
alkaline to litmus paper with sodium carbonate
(NagC030) and polarize in a 200 mm tube at 20° c. If
the invertase solution is sufficiently active the alka-
line solution will polarize about 31° § without correct-
ing for dilution to 110 ml and the optical activity of
the invertase solution.


{f~

- 20 - Sugarcane Sirup
August - 1957

VIII INSPECTION DURING PRODUCTION AND PACKING OPERATIONS (Continued)
A General. (Continued)
5 Reaction of cane juice.

The hydrogen ion concentration (pH) of the juice may
vary considerably but has been found to fall within narrow
limits in a given location. Louisiana crusher juice in some
years has averaged 5.38 pH with a range of 5.22 to 5.63 pH
for individual samples. The pH value has not been found to
be suitable for determining maturity of the cane, extent of
souring, or damage due to freezing. A wide difference from
the normal average pH should be investigated. The acid in
fermented juice is largely acetic which is volatile. The
normal acidity of juice is due to the presence of non-volatile
acid. If an excess acidity is indicated, 100 ml of the juice
is placed in a distillation flask and the first 25 ml of
distillate is titrated with 0.1N alkali solution. Excess
acidity of less than 1.0 ml can be detected by this method.

6 Methods of production.
a Unsulfured sirup.

In the production of unsulfured sirup the "boil and
skim" method of production is widely used. The cane may
be crushed in a single three-roller mill. The juice is
strained. and run into the clarifier and evaporator which
is usually direct fired. The juice isclarified simply by
heating. The albuminoids in the juice are coagulated by
heating and rise to the surface where the scum is removed
by sweeps or scoops made from metal screening or perforated
metal. The brushing and screening continue constantly
during evaporation to the required density.

b Sulfured sirup.

In the production of sulfured sirup the "sulfitation
process” is used. This process is used by the larger plants
with production capacity of several thousand gallons of
sirup per day. The cane is usually milled by first passing
through a crusher and then through six or more rollers on
which a little maceration water is used to aid extraction of
the juice. The juice is strained and saturated with sulfur


- 37 - Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)

B Total Sugars. (Continued)

2 Sucrose. (Continued)

b Sucrose by Jackson-Gillis Clerget modification. (Continued)

iii

iv

Polarization after inversion. (Continued)

If time permits, the inversion may be carried out
at room temperature. The AOAC recommends 2; hours if
the inversion is not below 20° c. and 10 hours if it is
above 25° c., but for low purity products such as
molasses and even for raw sugars a few hours longer at
these temperatures are needed to insure complete inver-
sion. As the 2h-hour period is usually the most conven-
dent, inversion may be assured in this period by placing
the flask in a warm place in the laboratory.

The U. S. Customs Regulations prescribe dnversion
as followss Immerse the flask in a water bati. at
exactly 60' « Agitate the solution continually for 3
minutes and allow it to remain in the bath for a total
time of 10 minutes. Cool quickly and make to volume at
the temperature at which the observations are to be made.
Shake and filter as rapidly as possible. polarize.

Calculations.
Calculate the sucrose as follows;

The Jackson-Gillis method () as adopted by the
U. S. Treasury Department and the International Commission
for uniform methods employs a table for the values of the
Clerget divisor, as given in Table No. 6, based on the
volume of P - P', i.e., the sucrose concentration. When
the Walker method in inversion is used, the sucrose may be
calculated by the following formula:

100 (P - P')
S = [52.63 ¢ 0.079L (M - 13) - 0.53 (T - 20)



-=19 - Sugarcane Sirup
August - 1957

VIII INSPECTION DURING PRODUCTION AND PACKING OPERATIONS
A General.

All applicable instructions in connection with continuous
inspection and plant inspection pack grading should be followed.
The requirements for plants operating under continuous inspection
as outlined in the regulations should be observed.

1 Raw stock.

The quality and condition of the sugarcane, whether
properly topped and stripped, should be noted, as well as
whether it has been frozen, fermented, or infested by borers
or insects.

2 Sanitation.

Tanks, pipe lines, and evaporating pans and other equip-
ment for handling juice and sirup should be washed at the end
of the day's run and should be maintained in a clean and sanitary
condition. .

3 Milling.

The milling operation should be carefully checked.
The crushing rolls should be properly adjusted for maximum
efficiency. The cane should be thoroughly disintegrated. A
little maceration water may be used on the rollers to aid
extraction. Mill sanitation should be observed to prevent the
accumulation of material which may become fermented and a
source of contamination of the juice. Proper attention should
be given to cleanliness and sanitation around the mills. A
small amount of sour bagasse can infect all of the juice with
which it comes in contact.

4 stra .

The juice, as it comes from the mills, passes through
coarse and then fine strainers to remove particles of bagasse
fiber. All parts ofthe strainers should be frequently cleaned
and steamed to keep them in a thoroughly sanitary condition.




-2- Sugarcane Sirup
August = 1957

II PRODUCTION (Continued)
A Annual Production.

The annual production of sugarcane sirup increased during
the period of World Var II, during which time sugar was rationed.
Production declined sharply following this period due, in part, to
the competition of other sweeteners, unfavorable crop conditions,
and also to the unsatisfactory quality of the sirup offered. The
following table gives the annual production for the years indicated
in the principal producing areas;



-16- Sugarcane Sirup
August - 1957

VI INSPECTION OF THE PRODUCT (Contimed)
F Grade Factors Rated by Score Points. (Continued)

4 Clarity. (Continued)

When the sirup is practically clear it may contain not
more than a trace of finely divided particles which do not
affect the appearance or edibility of the product. A score in
the Grade A classification - 18 to 20 points - may be given.

When the sirup is reasonably clear the presence of finely
divided particles does not materially affect the appearance or
edibility of the product and a score of 16 or 17 points may be
given.

When fairly clear a score in the Grade C classification
is given and the product cannot be graded above Grade C due to
the application of a limiting rule. To score in this classifica-
tion the appearance or edibility of the sirup may be materially
but not seriously affected by the presence of defects.

VII CERTIFICATION
A General.

The certification of sugarcane sirup and preparation of
inspection reports shall be in accordance with applicable general
instructions as contained in Chapter IV of Instructions for Certi-
fication of Processed Products. The instructions in this section
relating to certification are those which may differ or supplement
such instructions as they apply to sugarcane sirup.

B Product Inspected.

The name of the product as indicated by the grade standards
is "Sugarcane sirup." This name should be show in the space for
indicating the product inspected. The type of sugarcane sirup,
whether "sulfured® or “unsulfured," should be shown in the body of
the certificate. Inspectors may not always be able to determine
whether the product is a “sulfured" or “unsulfured" sirup. This
is particularly true when the product is a blend of sirups. When
the processor or buyer desires to have the type of sirup shown in
the certificate and the inspector is unable to definitely identify
the type, a statement similar to the following may be used:


-h7 - Sugarcane Sirup
August 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued )

H Total Sulfites; by Titration.

The approximate percent of SO, in the sample can be +
determined by titration using standafdized iodine and’ thio-
sulfate solutions.

Add 50 grams of double diluted sirup from the Brix

determination to a 500 ml distillation flask. Add about 300

- ml of distilled water and 5 ml of 20 percent phosphoric acid
solution. Connect the distillation flask to a glass condenser
and allow the outlet of the condenser to dip below the surface
of 50 ml of N/20 iodine solution in a 500 ml Ehrlenmeyer flask.
Add about 1 gram of sodium bicarbonate of the distillation
flask and quickly insert the rubber stopper connecting flask
to condenser.

Distill over about 200 cc into the Ehrlenmeyer flask
containing the iodine solution, If all of the iodine in the
receiving flask is discharged before the distillation is com-
plete more N/20 iodine solution may be added. —

When distillation is completed add a few drops of starch
indicator to the distillate and titrate the excess iodine with
n/20 sodium thiosulfate solution until the blue color just dis-
appears, leaving a water white solution.

1 Calculations.

1 mi N/20 iodine solution = 0.0016 grams or
1.6 mg of SOp-
3.5 ml N/20 thiosulfate solution required for
titration = 5.6 mg SQ).
50 grams double diluted sirup = 25 grams original
sirup taken for analysis.
prix 7h° - 7h grams Brix solids in original sirup.
- 25 grams sirup x 7u° Brix 2 18.5 grams Brix solids
in sample.
5.6 mg SO, per 18.5 grams Brix solids.
0.302 mg fer 1 gram Brix solids.
302 mg per 1000 grams Brix solids.
302 parts per million SO, in sample.


- Sh -

Table No. 1 (Continued)

Sugarcane Sirup
August - 1957

Refractive Indices of Sucrose Solutions at 20° c.

Sucrose Refrac- Sucrose Refrac- Sucrose Refrac- Sucrose Refrac-
percent tive percent tive percent tive percent tive
by index at by index at by index at by index at
weight 20°C. weight 20°C. weight 20°c. weight 20°C.
— - % 54
60.0 1.4418 63.0 1.4486 66.0 1.4555 69.0 1.4627
al 1.4420 al 1.4488 al 1.4557 1 1.4629
22 1.423 +2 1.4491 2 1.4560 +2 1.4632
3 1.4h25 +3 1.4493 +3 1.4562 3 1.4634
any 1.4h27 oh 1.4h95 oh 1.4565 oh 1.4637
5 1.bh29 5 1.4497 5 1.4567 oy 1.4639
6 1.4432 6 1.4500 6 1.4569 6 1.46b1
7 1.4434 7 1.4502 7 1.4572 “7 1.46L4
8 1.4436 8 1.4504 8 1.4574 8 1.4646
9 1.4439 9 1.4507 oD 1.4577 9 1.4649
61.0 1.U4h2 64.0 1.4509 67.0 1.4579 70.0 1.4651
1 1.4443 ol 1.451. wl 1.4581 2 1.4653
2 1.4b46 22 1.4514 22 1.4584 +2 1.656
3 1.4h48 3 1.4516 3 1.4586 3 1.4658
oh 1.4450 an 1.4518 an 1.4589 an 1.4661
5 1.b453 5 1.4521 5 1.4591 5 1.4663
6 1.bh55 6 1.4523 6 1.4593 6 1.4666
7 1.4457 7 1.4525 7 1.4596 7 1.4668
8 1.4h59 8 1.4527 8 1.4598 08 1.4671
9 1.4h62 9 1.4530 9 1.4601 9 1.4673
62.0 1.4L64 65.0 1.4532 68.0 1.4603 71.0 1.4676
1 1.4L66 1 1.4534 el 1.4605 el 1.4678
2 1.4468 22 1.4537 +2 1.4608 22 1.4681
3 1.4u71 3 1.4539 3 1.4610 3 1.4683
an 1.4473 ay 1.45u1 an 1.4613 h 1.4685
5 1.4475 5 1.45by 5 1.4615 5 1.688
6 1.4477 6 1.4546 6 1.4617 6 1.4690
7 1.bh79 7 1.4548 +7 1.4620 7 1.4693
8 1.4482 8 1.4550 8 1.4622 8 1.4695
9 1.4484 9 1.4553 9 1.4625 9 1.4698

—_


- 27 - Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)

B Total Sugars. (Continued)

1 Reducing Sugars. (Continued)

c

Standard invert sugar solution. (Continued)

is neutralized with NaOH and diluted to the desired con-
centration immediately prior to use.

Standard invert sugar solution can also be made by
dissolving 1 gram of pure dextrose (NBS Standard or C. P.
quality) in about 100 ml of water. Transfer to 500 ml
flask and make up to volume with distilled water. 1 ml
of this solution =» 2 milligrams of dextrose.

Methylene blue indicator.

Dissolve 1 gram of methylene blue in distilled
water and make up 100 ml. This solution is quite stable
and will keep for months without change.

Standardization and titration.

Pipet accurately 25 ml of mixed Soxhlet solution
(equal parts of Soxhlet solutions a and b) into a 300-l,00
ml flask. Carefully neutralize 50 ml of the standard
invert sugar solution c in a 100 ml flask with NaOH and
make up to volume by the addition of distilled water.
Approximately 24.5 ml of this solution should reduce all
of the copper in 25 ml of the Soxhlet solution. Add
‘approximately 23.5 ml of the standard solution from bur-
ette to the Soxhlet solution. Heat the cold mixture to
boiling on a wire gauze over Bunsen flame or hot plate
and maintain in moderate ebullition for 2 minutes, lowering
temperature sufficiently to avoid bumping. Without removing
from hot plate add 2 to 5 drops of methylene blue inlicator
and complete titration within total boiling time of about 3
minutes by small additions of sugar solution from burette
to complete decoloration of indicator.

A small electric hot plate (provided with a wire
gauze) connected to a rheostat (powerstat) to control the
heat is convenient to use and permits close control of
ebullition. When the rheostat is set at 130 on the dial,
boiling occurs in 30-5 seconds. The temperature can
then be lowered by reducing the dial setting on the rheo-
stat to about 100 to maintain moderate ebullition. Add
methylene blue and bulk of sugar solution within 105
seconds after boiling begins. The temperature should be



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- 26 - Sugarcane Sirup cTM
August - 1957
IX DEFINITIONS AND METHODS OF ANALYSIS (Continued )
B Total Sugars. (Continued)
1 Reducing sugars. (Continued)

e@ Standardization and titration. (Continued)

increased as necessary to maintain boiling, increasing
rheostat setting to about 130 on dial. With a swirling
motion of flask complete titration within the final 60
seconds, adding a drop or two of methylene blue as
needed for sharp end point. Multiply the number of ml
of sugar solution (4.75 mg) to obtain the factor. Compare
with factor in Table No. 5 to determine correction, if
any, to be applied to table. Small deviations from
tabulated factors as given in the table may result from
variations in individual procedure or composition of
reagents. When only approximate results (within 1%) are
desired, the standardized procedure may be omitted, pro-
vided specifications of analysis are rigidly observed.

f Determination of reducing sugars.

For total sugars, ash, and sulfite determinations
prepare a composite sample by mixing together about 200
grams of the well mixed sample and make up to 500 ml in
volumetric flask. If approximate concentration of sugar
in sample is unknown, a preliminary titration by the
incremental method of titration is usually necessary, as
follows; Add to 10 or 25 ml of Soxhlet solution 15 ml
of the sugar solution from burette and heat to boiling
over wire gauze if gas flame is used, or on hot plate,
Boil about 15 seconds and add rapidly further quantities
of the sugar solution until only the faintest perceptible
blue color remains, Then add 2-5 drops of methylene blue
and complete titration by adding the sugar solution drop-
wise. In adding the sugar solution to the boiling
Soxhlet solution the burette should be held in the hand
and brought over the flask. The burette is fitted with a
small outlet tube bent twice at right angles so that the
body of the burette can be kept out of the steam while
the outlet tube is held over the flask. Burettes with
glass stopcocks are unsuitable for this purpose. The


- U3 - Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
B Total Sugars. (Continued)
2 Sucrose. (Continued)

. d Sucrose by volumetric method, Lane-Rynon (alternate
method). (Continued)

ii Calculation. (Continued)

Example: A solution containing 5 grams of sucrose per
100 ml required 28 ml to reduce 10 ml of
Soxhlet solution. The factor from Table No.

is 47.7.
100 _
L.7 x =H = 170.3

This is the number of milligrams of invert sugar in
100 ml of the test solution, which is the amount
shown corresponding to the factor. These are the
calculations which have been carried out in comput-
ing the table. Fractions of a milliliter may be
interpolated.

C Total Sugars, Calculations.

The total sugars present in the sugarcane sirup is the
sum of the percent of reducing sugars in the percent of sucrose
as determined in the methods herein prescribed.

D Ratio of Total Sugars to Brix Solids.

Multiply the percent of total sugars by 100 and divide
by the Brix. Express the results as percent.

- 1 Calculations.

70.0 x 100 = 93,3¢ ratio of total sugars to Brix
75 solids.




- 46 - Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)

G Total Sulfites; by Monier-Williams Method. (Continued)

This delivery tube (E) extends to bottom of receiver. One
Peligot tube has been found to be sufficient to catch traces

of sulfurous acid swept through flask (F). Use rubber stoppers
throughout. Receiver (F) contains 15 ml of pure neutral 3%
hydrogen peroxide (H202) while Peligot tube contains 5 ml of

3% hydrogen peroxide (H209) solution. Hydrogen peroxide usually
contains free sulfuric acid. Start with 30% Ho0., dilute some-
what, and neutralize with Ba(OH)9 solution, using bromphenol
blue as indicator. After reagent has settled in cold, filter
from the BaSo), and determine its concentration by titration with
potassium permanganate (KMnO4) and finally adjust to 3% concen-
tration. The bromphenol blue indicator in the H90) remains
unaffected for some time. After connecting the apparatus,
introduce into the flask 300 ml of Hj0 and 20 ml of HCl and boil
a short time in a current of CO). Add 50 grams of double-diluted
sirup from Brix determination directly to flask by means of the
dropping funnel. Wash dropping funnel into flask. after intro-
ducing sugarcane sirup, boil mixture-1 hour in slow eurrent of
CO, stopping flow of water in condenser just before end of 4
distillation. This causes condenser to become hot and drives
over residual traces of SO, retained in condenser. When delivery
tube above condenser becomes hot to touch remove stopper (J) imme-
diately. Wash delivery tube and Peligot tube contents into flask
(F) and titrate liquid at room temperature with 0.1N, NaOH, using
bromphenol blue as indicator. The NaOH must be standardized with
bromphenol blue. Bromphenol blue is unaffected by CO and also
gives distinct color change in cold HO).

1 Calculations.

1 ml of 0.1N NaOH = 3.2 milligrams of S09.
2.5 ml of O.1N NaOH required for titration =
8.0 milligrams SO.
50 grams double-diluted sirup = 25 grams original
sirup taken for analysis.
Brix 74° = 7h grams Brix solids in original sample.
8.0 mg SOp per 18.5 grams Brix solids.
0.432 mg per 1 gram Brix solids.
432 mg per 1,000 grams Brix solids.
432 parts per million in sample.


_— - Sha - Sugarcane Sirup
September - 1957

Table No. 1 (Continued)
Refractive Indices of Sucrose Solutions at 20° c.

Sucrose Refrac- Sucrose Refrac- Sucrose Refrac- Sucrose Refrac-

percent tive percent tive percent tive percent tive
by index at by index at by index at by index at

weight 20° c. weight 20° c. weight 20° Cc. weight 20° c.
% % % %

72.0 1.4700 75.3 1.4782 78.6 1.4865 81.9 1.4952
1 1.4703 an 1.478 7 1.4868

22 1.4705 5 1.4787 8 1.4871 82.0 1.4954

3 1.4708 6 1.4789 9 1.4873 al 1.4956

an 1.4710 7 1.4792 12 1.4959

5 1.4713 8 1.4794 79.0 1.4876 3 1.4962

6 1.4715 9 1.4797 a 1.4878 oh 1.4964,

7 1.4717 22 1.4881 5 1.4967

8 1.4720 76.0 1.4799 3 1.4883 6 1.4970

9 1.4722 ae 1.4802 an 1.4886 7 1.4972

2 1.4804 5 1.4888 8 1.4975

73.0 1.4725 3 1.4807 6 1.4891 9 1.4978
1 1.4727 ol 1.4810 7 1.4893

+2 1.4730 5 1.4812 8 1.4896 83.0 1.4980

: 3 1.4732 6 1.4815 9 1.4898 1 1.4983

> an 1.4735 7 1.4817 2 1.4985

5 1.4737 8 1.4820 80.0 1.4901 3 1.4988

6 1.470 9 1.4822 a 1.490), oh 1.4991

7 1.4742 2 1.4906 5 1.4993

8 1.U7bb 17.0 1.4825 3 1.4909 6 1.4996

9 1.4747 1 1.4827 an 1.4912 7 1.4999

12 1.4830 5 1.4914 8 1.5001

74.0 1.4749 3 1.4832 6 1.4917 9 1.5004
a 1.4752 ary 1.4835 7 1.4919

2 1.4754 5 1.4838 8 1.4922 84.0 1.5007

3 1.4757 6 1.4840 9 1.4925 1 1.5009

oh 1.4759 “7 1.4843 +2 1.5012

5 1.4762 8 1.4845 81.0 1.4927 3 1.5015

6 1.4764 9 1.48L8 a 1.4930 ob 1.5017

“7 1.4767 2 1.4933 5 1.5020

8 1.4769 78.0 1.4850 3 1.4935 6 1.5022

9 1.4772 a 1.4853 oh 1.4938 7 1.5025

22 1.4855 5 1.49b1 8 1.5028

75.0 1.477h 3 1.4858 6 1.4943 9 1.5030
1 1.4777 an 1.4860 7 1.496

22 1.4779 5 1.4863 8 1.49L9 85.0 1.5033


-iv-

Sugarcane Sirup
August - 1957

Page

VI INSPECTION OF THE PRODUCT sececeesseecsceeaseces teen eeeeee 9
A Sampling s.sceeseseeeeees sence trees eeeeseceee 10

B Inspection Equipment and Material .. wee 10

1 Equipment for inspection .e.cseeceeeeee . 10

2 Materials and supplies or information needed ....... 10

C General Inspection Procedure coseceecssscccecccesees 11
D Recording Inspection Data on Score Sheet ... 12 .

E Fill of Container ...sssececcsecsececcccacs 12

1 Net contents .. . . 12

2 Headspace ....cscceccecnccccccece 13

F Grade Factors Rated by Score Points .. 1.

1 Color ...... see eae 13

2 Flavor . . ners

3 Defects . lh

Lo Clarity cececececccece cece eececereceeseveeenes 15

VII CERTIFICATION cece cece cect cece recess eeeeceeecerssssesecseee 16

A General .oscscsessccccsccccccccesccceccescesecsceccecssces 16

B Product Inspected .... - 16

C Mandatory Requirements ...eeceeeses - 17

D Specimen Examples of Certificates . . 1

E Tolerances sesccsceseccecccneces » 18

VIII INSPECTION DURING PRODUCTION AND PACKING OPERATIONS ......... 19

A General .. see 19

1 Raw stock ... 19

2 Sanitation .. 19

3 Milling .... 19

uo Straining ..... see 19

S Reaction of cane juice . 20

6 Methods of production . 20

a Unsulfured sirup . 20

b Sulfured sirup .. 20

7 Blending ......... 21

8 Filling ..... 21

9 Cooling ..... 23

10 Warehousing ...... 23

1l Labeling ....... 23

12 Recommendations .... 2h


- 35 - Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
B Total Sugars. (Continued)
2 Sucrose. (Continued)
: a Sucrose by polarization method (1). (Continued)

v Invert reading. (Continued)

same temperature. Correct the invert reading for the
optical activity of the invertase solution and mltiply
by 2.

vi Calculations.

Calculate the percentage of sucrose by the follow-
ing formula:

100 (P - I)
S = [32 0.073 (M - 13) - 0.5 (7 - 20)

: in which

percentage of sucrose

direct reading, normal solution

invert reading, normal solution

temperature at which readings are made

grams of total solids in 100 ml of the
invert solution read in the polariscope.
Percent solids by refractometer multi-
plied by specific gravity of the solu-
tion gives grams of total solids,

s
P
I
T
M

b Sucrose by Jackson-Gillis Clerget modification.

i Preparation of normal solution.

Prepare a normal solution by weighing out 52
grams of sugarcane sirup, wash into a 300 ml volumetric
flask, make up to mark and mix thoroughly. Pour the
solution out into a cylinder (capacity 400 to 500 m1)
and add sufficient Horne's dry lead to clarify, avoiding
an excess ( to 6 grams are usually sufficient). Mix by
violent shaking and filter. Pipet two 50 ml portions of
the filtrate into 2 100 ml flasks and add 20 ml of water
to each flask.


-33- Sugarcane Sirup
August = 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued )

B Total Sugars. (Continued)

"2 sucrose. (Continued )

a Sucrose by polarization method (1). (Continued)

ii

Adi

iv

Basic lead acetate solution.

Heat to boiling for about half an hour 430 grams
of neutral lead acetate and 130 grams of litharge in
one liter of water. Cool, settle, and decant the clear
solution. Dilute the solution with cold, recently
boiled, distilled water to 1.25 sp. gr. (54.3 degrees
on Brix hydrometer). The solution may also be made by
dissolving the reagent know as Horne's dry lead in
recently boiled, distilled water to a density of about
1.25 sp. gr. (54.3 degrees on Brix hydrometer). Lead
subacetate solution stored in stock bottles for daily
use should be protected from the carbon dioxide in the
air by soda-lime tubes. The burettes used for dispens-
ing for routine analyses should be similariy protected.

Alumnia cream, aluminum hydroxide.

To a saturated solution of aluminum in water add
ammonium hydroxide (NH),0H) with constant stirring until
the solution is alkaline to litmus paper. Allow precip-
itate to settle and wash by decantation with water until
wash water gives only a slight test for sulfates with
barium chloride (BaClp) solution. Pour off excess water
and store residual cream in a stoppered bottle. Alumnia
cream is suitable for clarifying light colored sugar
products or as an adjunct to other agents when sugars
are determined by polariscopic or reducing sugar methods.

Determination.

Dissolve double the normal weight (52 grams) of
sugarcane sirup in water in a 200 ml flask; add basic
lead acetate solution carefully, avoiding any excess,
then 1 to 2 ml of alumnia cream; shake; dilute to mark
with water; mix well; and filter, rejecting at least
the first 25 ml of filtrate. When sufficient filtrate
has collected, remove the lead from the solution by


=

‘ 70

55 } 60

Sugarcane Sirup
August - 1957

50

- 56 -
No. 3
Subtract—

Table
Observed percentage of sugar

(Standard at 20° c.)

emperature Corrections to Readings of Saccharometers (Brix Spindle)

T

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-9- Sugarcane Sirup
August = 1957

V FOOD AND DRUG REQUIREMENTS (Continued)

B Standard of Identity. (Continued)

The recommended maximum ash content for the different
types of sugarcane sirup are in substantial agreement with the
Food and Drug advisory standard, the apparent difference being
due, in part, to different methods of analyses which may be
employed. The methods of analyses provided in the revised grade
standards are in general use in the industry, and data indicate
that the recommended maximum ash content reflects current produc-
tion practices.

C Required Label Statements.

In addition to the name of the product, "sugarcane sirup,"
the net contents and the name and address of the packer or dis-
tributor must be shown on the label. The brand name, vignette,
and other material such as recipes and descriptive material are
optional with the packer or distributor. However, the labeling
should not be false or misleading in any way.

VI INSPECTION OF THE PRODUCT

A Sampling.

The sampling rates prescribed in the Rules and Regulations
and applicable Inspectors! Instructions should be followed. The
condition of the containers in the lot, such as freedom from
swells, springers, leakers, and rusty containers should be ascer-
tained at time of sampling in accordance with applicable instruc-
tions. The number of cases in the lot and warehouse location
should be recorded as a means of identification in the event that
supervision of loading is requested. Whenever it appears that
there may be some question as to the grade of the lot or the
quality is likely to be irregular, or a wide variation in Brix
solids or some other deviation is anticipated, the appropriate
sampling plan should be selected in accordance with the plans pro-
vided in the regulations.


- 45 - Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
G Total Sulfites; by Monier-Williams Method.

MONIER- WILLIAMS APPARATUS FOR DETERMINATION OF SULFUROUS ACID

Connect a 750 ml round bottom Pyrex flask (B) to sloping reflux condenser (D)
the lower end of which is cut off at an angle. Pass CO from generator through a dilute
solution of sodium carbonate (Na2CO3). in (A) to remove chlorine. Also connect dropping
funnel (K) to (B) by 3-holed stopper (C). Use tube (E) to connect upper end of condenser
to 200 ml Erlenmeyer flask (F), which is followed by Peligot tube (G).


- 51 - Sugarcane Sirup
August - 1957

Table No. 1 (Continued)

Refractive Indices of Sucrose Solutions at 20° c.

Sucrose Refrac- Sucrose Refrac- Sucrose Refrac- Sucrose Refrac-
percent tive percent tive percent tive percent tive

by index at by index at by indgx at by indgx at
20° ¢ 20" ¢

weight 20°C. weight 20°C. weight weight
54 aa Fs %

24.0 1.37059 27.0 1.3758 30.0 1.3811 33.0 1.3865
ol 1.3708 2 1.3760 al 1.3813 el 1.3867
22 1.3709 2 1.3761 +2 1.3815 12 1.3869
3 1.3711 3 1.3763 3 1.3816 3 1.3870
an 1.3713 an 1.3765 an 1.3818 oh 1.3872
5 1.3715 5 1.3767 5 1.3820 5 1.387
6 1.3716 a) 1.3768 6 1.3822 6 1.3876
7 1.3718 7 1.3770 7 1.3824 7 1.3878
8 1.3720 8 1.3772 8 1.3825 8 1.3879
9 1.3721 9 1.3773 9 1.3827 9 1.3881

25.0 1.3723 28.0 1.3775 31.0 1.3829 34.0 1.3883
1 1.3725 al 1.3777 oe 1.3831 1 1.3885
22 1.3726 rd 1.3779 22 1.3833 2 1.3887
3 1.3728 3 1.3780 3 1.3834 3 1.3889
ar 1.3730 an 1.3782 an 1.3836 oh 1.3891
5 1.3731 5 1.378) 5 1.3838 5 1.3893
6 1.3733 6 1.3786 6 1.3840 6 1.3894,
7 1.3735 7 1.3788 7 1.3842 7 1.3896
8 1.3737 8 1.3789 8 1.3843 8 1.3898
9 1.3738 9 1.3791 9 1.3845 9 1.3900

26.0 1.3740 29.0 1.3793 32.0 1.3847 35.0 1.3902
1 1.3742 1 1.3795 2 1.38h9 ol 1.390h
22 1.3704 2 1.3797 22 1.3851 12 1.3906
3 1.3745 3 1.3798 3 1.3852 3 1.3907
an 1.3747 an 1.3800 an 1.3854, oh 1.3909
5 1.379 5 1.3802 5 1.3856 5 1.391.
6 1.3751 6 1.3804, 6 1.3858 6 1.3913
7 1.3753 7 1.3806 7 1.3860 7 1.3915
8 1.3754 8 1.3807 8 1.3861 8 1.3916

9 + 1.3756 9 1.3809 9 1.3863 9 1.3918


vI

-<hl- Sugarcane Sirup
Augpst - 1957

INSPECTION OF THE PRODUCT (Continued)
B Inspection Equipment and Material. (Continued) ©

2 Materials and supplies or information needed. (Continued)

d Sampling sheets.

e Score sheets.

f Contract instructions and specifications, location and size
of lot, name of applicant or contractor, am similar
applicable data.

Towels.

Marking crayons.

Sampling stamp.

Application for inspection.

re Fe Fr A

Regulations governing inspection and certification of proc-
essed fruits and vegetables and related products, July 1,
1957.

€ General Inspection Procedure.

The United States Standards for Grades of Sugarcane Sirup
define and describe the requirements for the different grades and
outline the procedure for inspecting the product. Certain of these
requirements are contained in the product description. These
include provision for the preparation of a clean, sound, liquid
sugarcane product. It is the policy of the Branch, in so far as
possible, to ascertain that the product complies with the basic
Food and Drug requirements in accordance with methods, procedures,
and administrative guides provided for the use of inspectors and
supervisors. Provision for the application of methods and proce-
dures and administrative guides not specifically outlined in the
standards is contained in Section 52.3105 of the grade standards
which states in part, "In addition to considering other require-
ments outlined in the stamiards ... ."


- iii - Sugarcane Sirup
August - 1957

INSPECTORS' INSTRUCTIONS
FOR
SUGARCANE SIRUP

August - 1957
Page
I GENERAL ceccsccccccccc cect crete neers ness s ces enenesersesenseses 1
A Purpose and SCOpe ceesseeeccceccssccecccceesssscccsescesees

1
B Caution cescecesescceceee cooe 1
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B Varieties of Sugarcane .. oe
Ll Harvesting .scccseeee
C Types of Sugarcane Sirup ... sqaeee
1 uUnsulfured sugarcane sirup
2 Sulfured sugarcane sirup ...-...
D Manufacture of Sugarcane Sirup ..
1 unsulfured sugarcane sirup

LIL DEFINITION ...ccccccccccscccscccccvcvcessessssssccncccscsessee

A Definitions ....scerevcvccceesees
1 Sugarcane Sirup ....seeeeee
2 Unsulfured sugarcane SUTUP .sceeseeceseereeeecsreeeseoee

IV CANNING PROCEDURES ....
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2 Filling

3 Cooling
kh Containers ....seeeeeves

DorIIy VY YvyA VY Bouwmunwleerw

V FOOD AND DRUG REQUIREMENTS occcseececccccccnsccccccccceesssces

A General Requirements .... esoee
B Standard of Identity ....++.
CG Required Label StatementS .esceeseesesecees

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- 26 - Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
A Brix Solids. (Continued)
3 Refractometric method.

o _ Determine refractometer reading of sirup at 20° c.
(68° F.) and obtain the corresponding percent of sucrose
from the direct reading if the refractometer is provided
with a sugar scale, or by referring to Table No. 1 if the
refractometer reading is in terms of refractive index. If
the reading is made at a temperature other than 20° c. ’
appropriate temperature correction should be applied as
given in Table No. 2.

B Total Sugars.
1 Reducing sugars.

Reducing sugars are determined by the Lane-Eynon
method as follows:

Soxhlet modification of Fehling solution. This solu-
tion is prepared by mixing immediately before using equal
volumes of the following solutions a and b;

a Copper sulfate solution. Dissolve 3.639 grams of copper
sulfate CuS0),.5 H20 in distilled water and dilute to
exactly 500 ml and filter through prepared asbestos.

b Alkaline tartrate solution. Dissolve 173 grams of Rochelle
salts (sodium potassium tartrate) and 50 grams of sodium
hydroxide in water, dilute to 500 ml, allow to stand for
two days, and filter through prepared asbestos. If pure
chemicals are used in the preparation of the above solutions
aandb, filtration may not be necessary.

ce Standard invert sugar solution.

Dissolve 9.5 grams of pure sucrose (high grade large
grain granulated sugar) in a small amount of water, add 5
ml of hydrochloric acid (sp. gr. 1.19), and dilute with
water to about 100 ml and let stand at room temperature for
3 days at 20° to 25° c., then dilute to 1L. This acidified
1 percent invert sugar solution is stable over a period of
several months. Immediately before using, the amount required

—_








- 38 - Sugarcane Sirup
August - 1957

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
B Total Sugars. (Continued)
2 Sucrose. (Continued)

b Suerose by Jackson-Gillis Clerget modification. (Continued)

iv Calculations. (Continued)

For 60° inversion the basic value is 132.56
instead of 132.63, and for room temperature inversion
the basic value is 132.66. Polariscopic readings (both
direct and invert) should be the average of several
concordant observations. Multiply these average read-
ings by 6 to obtain the values for P and P!.

In the above formula P = P! are the direct and
invert readings ‘(average of several readings) multiplied
by 6, M is the grams of solids in 100 ml of the solution
and }. 53 (T - 20°) is the temperature correction. For
| sugarcane sirup of usual density the calculation 132.63
+ 0.079) (M - 13) may be dispensed with and the figure

131.88 may be used without appreciable error. The
temperature correction 0.53 (T = 20) can be calculated
or may be obtained from Table No. 6.

Example:
Direct reading + 5.6x6 = 33.6 (P)
Reading after inversion - 2.3x6 = - 13.8 (P!) .
7.4 (P = Pt)

Temperature = 2l.3° C.
Factor 131.88
Temperature correction (from table) 2.28

129-60

Sucrose = wes x 100 = 36.57


fTM~

- 22 - Sugarcane Sirup
August - 1957

VIII INSPECTION DURING PRODUCTION AND PACKING OPERATIONS (Continued)
A General. (Continued)
8 Filling. (Continued)

and filling temperatures are suggested for sugarcane sirup in
the can sizes indicated when the cans are labeled from the line,
cased in fiber cases, and air cooled;

Can size Processing temperature Filling temperature

Degrees F. Degrees F.
No. 2 187 117
No. 2-1/2 187 177
No. 10 170 160

The above temperatures are suggested only and may serve as a
guide in establishing filling temperatures which will be ade-
quate under the particular conditions encountered. All con-
tainers should be adequately code marked for identification at
time of filling. .

The container should be filled with sirup as full as
practicable in accordance with good commercial practice. This
means that the headspace should not be excessive. Cans having
excessive headspace will be considered to be slack filled
regardless of whether the quantity in the container agrees with
the label statement of net contents. AS a guide in avoiding
slack fill, the container should be filled to not less than 93
percent of its total capacity. Frequent inspection should be
made in order to make sure that the headspace is not excessive.
If there is any question as to whether the headspace may be
excessive, it should be measured by means of a headspace gauge.
The maximum allowable headspace for the various sizes of sani-
tary type cans in general use is given in the following list:

Sanitary Type Cans
(Measured from top of double seam)

Maximum headspace

Can name Dimensions Sixteenths of an inch
No. 1 Picnic 211 x 400 7.0
No. 300 300 x 407 7.5
No. 303 303 x 406 7.5
No. 2 307 x 09 7.7
No. 2-1/2 hol x 111 7.8
No. 10 603 x 700 10.4


-31- Sugarcane Sirup

August - 1957
I DEFINITIONS AND METHODS OF ANALYSIS (Continued)
B Total Sugars. (Continued)
1 Reducing sugars. (Continued)
h Calculations for reducing sugars. (Continued)
Titration (titer) (1st) 27.56 ml prepared sugar

solution required
to reduce 10 m1
Fehlings solution.

(2nd) 27.60 ml prepared sugar
solution required
to reduce 10 ml
Fehlings solution.

Average of two titrations 27.58 ml prepared sugar
solution required
to reduce 10 ml
Fehlings solution.

Factor: 51.0

Obtain factor corresponding to titer of 28 from Table
No. h corrected for approximately 50 percent sucrose. At
this particular dilution this corresponds to 0.5 grams of
sucrose per 100 ml of solution. Interpolate between column
under heading "1 Gm SucroSe per 100 M1 Invert Sugar't and
column under heading "Invert Sugar - No Sucrose."

51.4 = 50.5 = 0.93 0.9 x 0.5 = 0.45 correction to be applied
to 51.4, gives corrected factor # 51.0

50 grams of double diluted sirup diluted to 250 ml
25 ml of this solution is diluted to 250 ml
1 ml of final dilution = 0.01 gram in original sample

51.0 x 100 = 51.0 x 10 = 18.49 percent reducing
27.58 x 0.01 x 1000 mgs 27.55 sugar.

10 is the factor to convert to percent sample basis for this
particular dilution. Other dilutions will require a differ-
ent factor depending upon the weight of the sample taken.


_— SPECIMEN NO. 3

Form FY.147

(51-52) UNITED STATES DEPARTMENT OF AGRICULTURE
PRODUCTION ANS MARKETING ADMRLETHATTON
ORIGINAL CERTIFICATE OF QUALITY AND CONDITION
FOR
PROCESSED FRUITS AND VEGETABLES No. 400003
Tot epuent ate tat souts of the United Sate az ima facie wrdenes No 4.00003
failure to comply with any of the regulatory laws enforced by the United States
Department of "Agriculture or the Federal Food and Drug "Adminiatration
Date.
To..........boisel Sirup Company Address.

(Applicant)

Address.............

Shipper or Seller.
Address...

I certify that in compliance with the regulations of the Secretary of Agriculture governing the inspection and certification of the product
designated herein, pursuant to the act making appropriations for the United States Department of Agriculture, | inspected the samples of the
product as shown below, and that the quality and condition ae thown by the samples on the above date were ae follows!

Receiver or Buyer...

Applicant

Product inspected........... SUGARCANE STRUP

Samples submitted by.

Code or other identification marks on containers...

WOld Southern Brand

Principal title of

y
label (if any)... Weight, 2 pounds, ow
Net weight range 36 to 37 ounces
Vacuum range 5 to 9 inches
Type Unsulfured
Brix Solids 74.2% Composite Sample
Grade: U. S. GRADE B or U. S. CHOICE

Score 82 to 85 points

THE ABOVE STATEMENT IS THE GRADE OF UNOFFICIALLY DRAWN
SAMPLE SUBMITTED BY THE APPLICANT.

Remarks: Packed in plain friction top cans, neatly labeled, clean, and
in good condition. Samples not officially drawn.

J. L. James Official Inspector.
Expenses. P.O. Box 151
Total... Address.... Ha?

PLEASE REFER TO THIS CERTIFICATE BY NUMBER AND MARKET



-7- Sugarcane Sirup
August - 1957

III DEFINITION
A Definitions.

1 "Sugarcane sirup" means the liquid product obtained by
evaporating the juice of sugarcane or by dissolving sugar-
cane concrete in water without removing any of the sugar
therefrom.

2 “Unsulfured sugarcane sirup" is sugarcane sirup made with-
out the use of the sulfitation process.

3 "Sulfured sugarcane sirup" is sugarcane sirup made by the
sulfitation process.

IV CANNING PROCEDURES

A Preparation for Canning.

1 Blending.

In the preparation of blends of sirup for earning,
considerable skill is required to maintain uniform color
and flavor in the finished camed product. Sirup from
different sources or different batches by the same producer
may vary considerably due to the method of manufacture, con-
dition and variety of the cane, or skill in handling plant
operations. Careful blending is necessary to maintain uni-
form quality in the canned product.

2 Filling.

After blending, the sirup is heated to a filling
temperature of 180° to 185° F. In larger plants the sirup
is heated in copper or stairiless steel processing pans
equipped with steam coils. These pans have a capacity of
six to eight barrels (300 to 00 gallons). In smaller
plants the cans may be filled direct from the evaporator
or from holding tanks which are supplied direct from the
evaporator. When filling direct from the evaporator, pro-
visions should be made for cooling the sirup to prevent
overheating and caramelization in the can.


- 53 - Sugarcane Sirup
August - 1957

Table No. 1 (Continued)

°
Refractive Indices of Sucrose Solutions at 20 C.

Sucrose Refrac- Sucrose Refrac- Sucrose Refrac- Sucrose  Refrac-

percent tive percent tive percent tive percent tive
by index at by index at by index at by index at

weight 20°C. weight 20°C. weight 20°c. weight 20°C.
% z g &

48.0 1.4158 51.0 1.4221 54.0 1.4285 57.0 1.4351
2 1.4260 al 1.4223 1 1.4287 el 1.4353
22 1.42162 12 1.4225 22 1.4289 +2 1.4355
3 1.4164, 3 1.4227 3 1.4292 3 1.4358
an 1.4166 an 1.4229 oh 1.b294 oh 1.4360
5 1.4169 5 1.4231 5 1.4296 - 5 1.4362
6 1.4171 6 1.4234 6 1.4298 6 1.4364,
7 1.4173 7 1.4236 7 1.4300 7 1.4366
8 1.4175 8 1.238 8 1.4303 8 1.4369
9 1.4177 9 1.4240 29 1.4305 9 1.4371

49.0 1.4179 52.0 1.L2h2 55.0 1.4307 58.0 1.4373
1 1.4181 al 1.42bh wl 1.4309 1 1.4375
22 1.4183 22 1.4246 +2 1.4311 22 1.4378
33 1.4185 3 1.42h9 3 1.4313 3 1.4380
ol 1.4187 ol 1.4251 oh 1.4316 an 1.4382
5 1.4189 5 1.4253 5 1.4318 5 1.4385
6 1.4192 6 1.4255 6 1.4320 6 1.4387
7 1.4194 “7 1.4257 7 1.4322 7 1.4389
8 1.4196 8 1.4260 8 1.4325 8 1.4391
od 1.4198 9 1.4262 9 1.4327 9 1.439b

50.0 1.4200 53.0 1.4264 56.0 1.4329 59.0 1.4396
al 1.4202 ol 1.4266 al 1.4331 ol 1.4398
2 1.4204 +2 1.4268 +2 1.4333 22 1.4400
3 1.4206 3 1.4270 3 1.4336 3 1.4403
ar 1.4208 4 1.4272 oh 1.4338 an 1.405
5 1.4211 5 1.4275 5 1.43h0 5 1.4407
6 1.4213 6 1.4277 6 1.43h2 6 1.4409
7 1.4215 7 1.4279 7 1.43bh 7 1.4411
38 1.4217 .8 1.4281 8 1.43L7 8 1.4b1y
9 1.4219 9 1.4283 9 1.4349 9 1.4416


- 39 - Sugarcane Sirup
August - 1957

TX DEFINITIONS AND METHODS OF ANALYSIS (Continued)

B Total Sugars. (Continued)

2 Sucrose. (Continued)

c© Sucrose by volumetric method, Lane-Zynon (for routine

inspections).

The following method may be used for routine inspec-

tions. Sucrose is calculated after inversion with invertase
by the Lane-fynon method as follows;

i

Preparation of invert solution.

Pipet 10 ml of the prepared solution of sugarcane
sirup, as used in determining reducing sugar in 1 g above,
into a 250 ml volumetric flask and add 5 ml of invertase
solution. The invertase solution is made by dissolving 1
gram of Wallerstein Blue Label dry invertase in distilled
water and make up to 100 ml. (Other invertase prepara-
tions are available and may be used.) After adding the
invertase solution to the prepared sugarcane sirup solu-
tion, add 5-6 drops of glacial, acetic acid, mix well and
place in a hot water bath or on a hot plate, so adjusted
that the temperature is kept at 55° to 60° c. for one hour,
or leave at room temperature (not below 20° c.) for 2h
hours. After one hour of heating (hot water bath or hot
plate) at 55° to 60° C., cool flask to about 20° c, and
make up to 250 ml. Carefully neutralize to litmus paper
with anhydrous sodium carbonate, and then titrate using 10
ml of mixed Fehlings solution. Titrate as directed under
1 f above.


-ul- Sugarcane Sirup
August - 1557

IX DEFINITIONS AND METHODS OF ANALYSIS (Continued)
B Total Sugars. (Continued)
2 Sucrose. (Continued)

e¢ Sucrose by volumetric method, Lane-Eynon (for routine
Inspections). (Continued)

ii Calculations. (Continued)

54.335 x 0.95 = 51.62% sucrose.

0.95 is the factor to convert invert sugar to sucrose.

d Sucrose by volumetric method, Lane-Eynon (alternate method).

Determine reducing sugars before and after inversion
with HCl. Dry sodium oxalate should be added to the prepared
soluticn at the rate of C.5 gram per 500ml and clarified with
neutral lead acetate. The solution is then filtered. A
small amount of Kieselguhr may be added as an aid to filtering.
After filtration, proceed as outlined under 1 f Calculate as
J invert sugar.

i Inversion.

Invert the solution as follows: Pipet a 50 ml
portion of lead free filtrate into a 100 ml flask and
add 25 ml of water. Add a little at a time while
rotating flask 10 ml of hydrochloric acid (sp. gr.
1.1029 at 20/4° or 24.95° on Brix hydrometer at 20° c.).
Place the flask with thermometer inserted in a water bath
at 70° Cc. and regulate temperature at about that point.
Agitate the flask continuously until contents reach a
temperature of 67° c. This preliminary heating should
require about 2-1/2 to 2-3/l minutes. When the thermom-
eter in the flask indicates 67° C., leave flask in bath
for exactly 5 minutes longer, during which time the
temperature should gradually rise to about 69.5° Cc. At
the end of the 5 minute period place the flask immediately
in water at about 20° c. when the contents have cooled
to about 35° C., remove the thermometer, rinsing the solu-
tion from the thermometer into the flask, and fill almost


-10- Sugarcane Sirup
August - 1957

VI INSPECTION OF THE PRODUCT (Continued)

B Inspection Equipment and Material.

: The following lists comprise the minimum equipment and
supplies needed by the inspector on a field trip. These items of
equipment would be needed when laboratory facilities are not avail-
able at the plant or warehouse where the inspection is to be made.
A telephone call to the applicant or processor before proceeding
on a field trip is often desirable to obtain information which will
facilitate the handling of the inspection.

1 Equipment for inspection.

a Grading scales.

b Vacuum gauge.

¢ Can opener.

d Trays, white enamel, shallow, about 10" x 1".

e Depth gauge.

f Ruler.

g U.S.D.A. permanent glass color standards for sugarcane sirup.

h Two U.S.D.A. cane sirup sample containers.

»

200 ml beakers.

j  Refractometer.

k Cylinders.

1 Brix hydrometers.

2 Materials and supplies or information needed.

a U. S. Standards for Grades of Sugarcane Sirup.
b Federal Specifications.

c Inspectors' Instructions for sugarcane sirup and any supple-
mental instructions.