GENERAL55980

• Permit No: M1988112
• IBM Index Class Name: General Documents
• Doc Name: STANDARD TEST METHODS FOR CYANIDE IN WATER AUTOMATED METHODS FOR TOTAL CYANIDE & DISSOCIABLE CYANIDE
• Media Type: D
• Archive: No

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~~ D 4374
10.3 Cover the container tightly and store in a dark, cool
place. at about 5°C.
10.4 The use of dark containers and storage in a dark
place is to minimize sample exposure to UV irtadiation,
otherwise photodecomposition of cyanide complexes may
occur. The photodecomposition of iron complexes increases
the free cyanide significantly aid alters the relative cyanide
species distribution in the samtdes.
10.5 If the sample contains sulfides or oxidizing agents,
treat az prescribed in 6.3 and 6.4 respectively prior to
preservation with sodium hydn>xide (whenever possible).
10.6 Test for the presence of sulfides by placing a drop of
the sample on a strip of lead acetate paper moistened with
the phosphate buffer. Darkening of the test paper indicates
[he presence of sulfide. Presumably the presence of sulfide
indicates the absence of oxidizing agents.
10.7 Test for presence of o tidizing agents by placing a
drop of the sample on a strif of Potassium iodide-starch
paper moistened with the phosf~hate buffer. Appearance of a
dark bluish color indicates th< presence of oxidizing sub-
stances.
I1. Procedure for Total Cyanide
tion and
:II give a
tL of the
NaOH.to
ferricya-
= (fie • 3
~. .
(Prepared
-ricyanide
n distilled
',tnd dilute
dafk and
'..
With the
3.7.1) and
' the acid
tf (85 %)
hosphorus
. : '~.
iQ water,
,); -
~on-=Care-
and adjust
:he.dark.
20'mL of
-Place'l5 g
,6;°waier to
,.. coou[[
pp~ [a. 'raw ~~
'OIL'. 31_ "~
-nL ~~ SECTION 00
~~FIG. 3 Ultraviolet Irrediation Unit (l-amp, Coil end Nouaing)
wash the sides of the Flask and wet the barbituric acid. Add
75 mL of pyridine and mix. After dissolution add l5 mL of
HCI (sp gr 1.19), mix and let cool at room temperature, then
diltite to the mark. Keep in a brown glazs bottle and store in
fhe'dark. The reagent is stable for >3 months.
iti)Lr
9:~Safety Precautions
~tn~t.
C~9:I Because of the toxicity of cyanide, great care must be
exercised in its handling. Acidification of cyanide solutions
produces toxic hydrocyanic acid (HCN). All manipulations
should be done in the hood so that any HCN gas that might
escape is safely vented.
'k. 9.2 If a cyanide solution or acyanide-containing waste is
spilled on the skin, wazh i[ off with water. If it is splashed in
Il)e eyes, irrigate the eyes with running water for 15 min and
call a physician at once. If swallowed, call a physician and
gi ~e inhalations of amyl nitrite for 15 to 30 s every 15 min
for one 1 h. When the patient is conscious, give emetics
4warm sal[ water) unti his vomit Ouid is clear.
„, 9.3 Many of the reagents used in these test methods are
diRhly toxic. These reagents and their solutions must be
tsposed of properlyof properly.
;~-
~10. Sample Handling and Preservation
l Collect samples in accordance with Practices D 3370.
ties should be collected in dark polyethylene or glass
Liners, and analyzed az soon az possible.
2 If the sample cannot be analyzed immediately, and
not contain sulfides or oxidizing materials, add sodium
txide (pellets or concentrated solution) to raise the pH
2 for preservation. - ,
1 L I Sys[en: Preparation anc' Warm Up (?0 mint:
1 I.I.I Turn on the colorim~~tric and select the D-Mode
for direct color measurement.
11.1.2 Stan the pump using water instead of reagents.
11.1.3 Adjust the nitrogen flow rate to 3.9 to 4.0 mL/min
using the gas regulator and the flow controller. The [low
measurement could be made by a soap bubble flow meter or
a calibrated rotameter. Then connect the nitrogen gas to the
manifold properly.
11.2 Distillation Ratio, l7 to 20 %:
11.2.1 Measure the cold liquid volume Flowing through
the thin film distillation unit, Ity collecting the water from
the waste trap in a measuring cylinder, for 10 min. This
volume should be about 27 m]- according to the described
manifold.
11.2.2 Turn on the UV irtadiator and activate the tickler
if needed.
11.2.3 Turn on the variable transformer to heat the
aluminum bar. Wait about 12 min to reach a stable
temperature. The temperature ;hould be monitored by the
dial thermometer in the aluminum bar well (about 125°C).
11.2.4 Collect the hot water Gom the waste trap for 10
min. Wait till it cools to room temperature, then measure the
volume. This volume should be around 22 mL, otherwise
temperature adjustment by the Variac controls is necessary.
11.2.5 The distilled volume equals the difference between
the cold volume and the hot volume, and
Distillation Ratio, % = D stilled Volume X 100
-total Volume
This ratio must be 17 to 20 i,.
1 L3 E/ecrronic Calibration (Dai/yJ-Follow the manufac-
turer's instructions to adjust nxorder zero and full scale,
using the display rotary switch t.nd the operating controls of
the colorimeter (zero and full-scale adjusting screws).
11.4 Chemical Standard Calibration-The working cya-
nide concentration range could lte up to 500 µgJL, however a
0 to I00 µg/L is recommended. The following steps are given
to optimize the performance.
I09